#------------------------------------------------------------------------------
#$Date: 2019-09-08 06:42:15 +0300 (Sun, 08 Sep 2019) $
#$Revision: 218078 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021766.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2021766
loop_
_publ_author_name
'Guillet, Gary L.'
'Pitts, Skyler L.'
'Sheriff, Kirkland W.'
'Rucker, Donna N.'
'Rogers, Aaryn L.'
_publ_section_title
;
Synthesis, characterization, and crystal structures of organonickel(II)
complexes coordinated to novel
1-bromo-2,6-bis{[(\l^5^-phosphanylidene)imino]methyl}benzene NCN-pincer
ligands
;
_journal_coeditor_code JX3045
_journal_issue 10
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229619012038
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac '[Ni Br (C44 H49 N2 P2)], 0.5C4 H10 O1'
_chemical_formula_moiety 'C44 H49 Br N2 Ni P2, C2 H5 O0.5'
_chemical_formula_sum 'C46 H54 Br N2 Ni O0.5 P2'
_chemical_formula_weight 843.47
_chemical_name_systematic
;(2,6-Bis{[(cyclohexyldiphenyl-\l^5^-phosphanylidene)imino]methyl}phenyl-\k^3^N,C^1^,N')bromidonickel(II)
butanol hemisolvate
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 74.892(6)
_cell_angle_beta 85.365(6)
_cell_angle_gamma 89.151(6)
_cell_formula_units_Z 2
_cell_length_a 10.1057(7)
_cell_length_b 13.8342(10)
_cell_length_c 15.3868(11)
_cell_measurement_reflns_used 2165
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 22.9720
_cell_measurement_theta_min 2.5200
_cell_volume 2070.0(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'Rigaku XtaLAB area detector'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'Graphite Monochromator'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0417
_diffrn_reflns_av_unetI/netI 0.1027
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 12542
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.483
_diffrn_reflns_theta_min 1.768
_diffrn_source 'Sealed Tube'
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 1.547
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.98698
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2018)
;
_exptl_crystal_colour 'clear dark red'
_exptl_crystal_density_diffrn 1.353
_exptl_crystal_density_method "'not measured"
_exptl_crystal_description block
_exptl_crystal_F_000 882
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.3
_refine_diff_density_max 0.755
_refine_diff_density_min -0.617
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 500
_refine_ls_number_reflns 9359
_refine_ls_number_restraints 78
_refine_ls_restrained_S_all 1.044
_refine_ls_R_factor_all 0.0989
_refine_ls_R_factor_gt 0.0540
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1043
_refine_ls_wR_factor_ref 0.1310
_reflns_number_gt 6137
_reflns_number_total 9359
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jx3045sup1.cif
_cod_data_source_block x95777res
_cod_original_formula_sum 'C46 H54 Br N2 Ni O0.50 P2'
_cod_database_code 2021766
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 2 8.60 2.32
0 0 -3 2060.99 37.65
0 0 3 2026.52 48.85
0 0 3 2081.71 38.05
0 0 -4 2368.99 44.27
0 0 4 2252.24 58.31
0 0 5 242.54 19.01
0 0 -5 258.65 12.11
0 0 -6 889.88 26.46
0 0 6 947.46 41.19
0 0 7 190.92 11.26
0 0 7 201.45 19.81
0 0 8 1262.35 55.51
0 0 8 1251.40 34.34
0 0 9 267.22 15.09
0 0 9 271.85 26.86
0 0 10 517.68 22.17
0 0 10 553.23 40.17
0 0 11 711.78 49.67
0 0 11 668.23 26.27
0 0 12 47.70 15.96
0 0 13 519.51 46.80
0 0 14 136.67 24.91
0 0 15 134.20 23.32
0 0 16 -6.11 11.14
0 0 17 23.17 12.32
0 0 18 -11.40 13.35
0 0 19 13.29 12.07
0 -1 18 9.26 8.60
0 -1 17 19.87 16.09
0 -1 16 -1.16 11.18
0 -1 15 74.81 20.82
0 -1 14 476.49 47.24
0 -1 13 5.86 8.98
0 -1 12 622.43 48.79
0 -1 11 226.43 15.46
0 -1 11 242.92 28.96
0 1 -10 195.16 14.92
0 -1 10 208.85 24.68
0 -1 9 1450.62 65.42
0 1 -9 1324.17 41.04
0 1 -8 417.28 20.97
0 -1 8 452.44 33.33
0 1 -7 13.20 2.83
0 -1 7 10.19 6.76
0 -1 6 4.28 5.21
0 1 -6 9.02 3.03
0 1 -5 692.14 24.35
0 -1 5 718.69 34.60
0 -1 4 92.90 11.37
0 1 -4 113.75 8.80
0 1 -3 771.51 22.56
0 -1 2 208.61 10.00
0 1 -2 202.30 9.84
0 -1 -1 2549.49 43.08
0 1 2 242.41 9.24
0 1 2 272.75 11.89
0 -1 -2 242.78 9.31
0 1 3 289.10 10.82
0 1 3 300.25 15.30
0 -1 -3 291.18 10.84
0 1 4 3.57 1.48
0 1 4 14.75 5.17
0 1 5 739.55 21.50
0 1 5 736.30 31.84
0 1 6 900.16 25.58
0 1 6 868.69 38.69
0 1 7 126.76 9.25
0 1 7 136.11 15.82
0 1 8 128.15 16.79
0 1 8 105.72 8.94
0 1 9 392.56 31.82
0 1 9 370.66 17.83
0 1 10 544.31 40.19
0 1 10 538.45 22.41
0 1 11 1.88 5.02
0 1 11 2.95 2.97
0 1 12 276.95 30.54
0 1 13 30.67 13.64
0 1 14 189.38 28.00
0 1 15 624.82 53.96
0 1 16 -0.90 9.38
0 1 17 18.43 8.76
0 1 18 30.39 19.02
0 1 19 39.18 14.60
0 -2 18 74.49 21.62
0 -2 17 101.04 24.47
0 -2 16 3.87 8.41
0 -2 15 258.86 37.63
0 -2 14 7.75 12.72
0 -2 13 153.16 25.33
0 -2 12 -5.46 13.31
0 2 -11 83.10 11.01
0 -2 11 61.81 13.68
0 -2 10 1490.83 72.26
0 2 -10 1375.96 46.73
0 2 -9 182.98 15.30
0 -2 9 180.33 23.80
0 -2 8 1068.42 54.38
0 2 -8 1090.26 39.35
0 2 -7 83.89 10.03
0 -2 7 118.12 16.87
0 2 -6 718.29 29.54
0 -2 6 753.88 40.38
0 -2 5 484.81 30.17
0 2 -5 454.19 21.89
0 2 -4 52.98 7.24
0 2 -3 1467.01 39.27
0 2 -2 256.34 14.30
0 2 -1 17.86 3.68
0 2 0 1901.57 42.98
0 -2 -1 2076.34 40.63
0 2 1 1968.78 43.62
0 2 2 76.53 6.72
0 2 2 58.99 6.02
0 2 3 1224.74 33.75
0 2 3 1120.45 30.27
0 2 4 171.30 12.91
0 2 4 169.65 10.58
0 2 5 154.05 14.02
0 2 5 167.53 10.70
0 2 6 2980.88 60.43
0 2 6 2975.86 77.58
0 2 7 84.54 8.04
0 2 7 84.85 12.23
0 2 8 0.52 4.01
0 2 8 4.18 2.74
0 2 9 171.37 12.26
0 2 9 159.91 19.12
0 2 10 42.37 6.65
0 2 10 34.36 9.68
0 2 11 2.93 3.15
0 2 11 5.13 5.67
0 2 12 0.24 7.30
0 2 13 470.77 41.33
0 2 14 276.08 33.48
0 2 15 -11.08 11.85
0 2 16 189.91 30.82
0 2 17 48.41 18.35
0 2 18 91.92 24.75
0 2 19 152.66 29.71
0 -3 18 25.57 15.78
0 -3 17 68.71 21.76
0 -3 16 9.61 11.79
0 -3 15 -0.20 12.07
0 -3 14 37.87 13.41
0 -3 13 -4.50 11.60
0 -3 12 98.02 19.64
0 -3 11 111.65 19.96
0 3 -11 85.73 12.54
0 3 -10 26.76 7.29
0 -3 10 48.83 14.58
0 3 -9 1143.16 45.13
0 -3 9 1210.62 63.52
0 3 -8 833.88 36.89
0 -3 8 1014.78 54.56
0 -3 7 778.20 45.34
0 3 -7 696.63 32.93
0 3 -6 29.01 6.55
0 3 -5 8.75 3.72
0 3 -4 749.99 31.49
0 3 -3 1687.08 48.83
0 3 -2 683.85 28.59
0 3 -1 39.73 6.30
0 3 0 5611.74 104.60
0 3 1 639.15 26.05
0 -3 -1 674.95 23.51
0 3 2 205.09 12.86
0 3 2 168.18 12.75
0 3 3 518.38 22.61
0 3 3 524.50 22.28
0 3 4 1038.83 35.16
0 3 4 999.16 32.96
0 3 5 2334.41 61.17
0 3 5 2206.31 54.04
0 3 6 44.45 6.58
0 3 6 45.80 8.99
0 3 7 1523.26 54.64
0 3 7 1417.66 42.28
0 3 8 184.82 14.21
0 3 8 202.61 20.60
0 3 9 -0.33 4.19
0 3 9 2.86 2.89
0 3 10 -3.57 4.28
0 3 10 5.56 3.52
0 3 11 -8.23 7.63
0 3 11 3.39 3.19
0 3 12 6.49 3.36
0 3 12 5.99 4.76
0 3 13 21.21 11.56
0 3 14 123.77 23.41
0 3 15 418.31 43.92
0 3 16 70.42 19.04
0 3 17 40.33 12.41
0 3 18 185.90 30.85
0 3 19 -3.92 15.41
0 -4 17 321.89 48.78
0 -4 16 39.53 18.93
0 -4 15 -23.68 17.70
0 -4 14 17.04 13.32
0 -4 13 34.36 14.02
0 -4 12 9.45 10.35
0 4 -11 31.15 7.65
0 -4 11 22.44 11.60
0 4 -10 406.08 28.55
0 -4 10 332.80 35.70
0 -4 9 415.47 38.07
0 4 -9 414.66 28.53
0 -4 8 867.16 53.86
0 4 -8 806.26 39.83
0 4 -7 1265.43 49.95
0 4 -6 4.88 3.48
0 4 -5 999.51 42.00
0 4 -4 1457.43 50.67
0 4 -3 373.96 24.03
0 4 -2 21.81 5.78
0 4 -1 342.88 22.05
0 4 0 2119.68 59.51
0 -4 -1 133.75 11.69
0 4 1 154.19 14.03
0 4 2 709.47 31.11
0 -4 -2 705.82 27.42
0 4 3 1087.00 36.48
0 4 3 1039.13 38.31
0 4 4 996.67 36.28
0 4 4 958.27 36.51
0 4 5 1586.49 50.70
0 4 5 1657.86 49.77
0 4 6 4265.50 97.32
0 4 6 4129.59 90.58
0 4 7 84.66 12.36
0 4 7 82.78 10.44
0 4 8 232.58 17.54
0 4 8 236.50 21.63
0 4 9 415.91 31.37
0 4 9 470.74 25.67
0 4 10 45.10 7.84
0 4 10 63.12 12.06
0 4 11 430.98 36.43
0 4 11 423.87 25.05
0 4 12 49.74 12.34
0 4 12 53.75 9.18
0 4 13 267.48 31.31
0 4 14 475.89 44.71
0 4 15 53.28 13.71
0 4 16 20.81 11.52
0 4 17 311.41 40.92
0 4 18 4.13 12.57
0 4 19 106.77 28.22
0 -5 17 -5.04 12.57
0 -5 16 144.23 32.32
0 -5 15 15.01 14.35
0 -5 14 55.28 18.50
0 -5 13 30.10 13.53
0 -5 12 76.69 21.66
0 5 -11 -3.97 3.73
0 -5 11 2.06 7.31
0 5 -10 178.61 19.77
0 -5 10 154.18 25.60
0 5 -9 150.29 18.72
0 -5 9 140.49 24.89
0 5 -8 1714.59 64.89
0 -5 8 1766.78 82.18
0 5 -7 2.23 4.37
0 5 -6 54.21 10.66
0 5 -5 473.56 30.84
0 5 -4 37.95 8.85
0 5 -3 2620.37 76.93
0 5 -2 119.48 15.25
0 5 -1 57.72 10.39
0 5 0 757.80 36.71
0 5 1 13.13 5.04
0 -5 -2 51.86 7.62
0 5 2 44.25 9.05
0 -5 -3 44.61 7.27
0 5 3 38.32 8.09
0 5 4 200.18 17.93
0 5 4 174.08 15.25
0 5 5 1555.78 51.62
0 5 5 1475.57 52.24
0 5 6 97.39 13.41
0 5 6 96.95 13.02
0 5 7 620.78 32.30
0 5 7 643.93 35.32
0 5 8 901.29 39.75
0 5 8 927.31 45.46
0 5 9 -1.72 5.90
0 5 9 10.72 4.57
0 5 10 819.96 37.79
0 5 10 762.43 45.61
0 5 11 3.26 3.40
0 5 11 5.60 7.01
0 5 12 26.79 9.13
0 5 12 20.89 6.95
0 5 13 -0.62 7.75
0 5 13 5.59 4.73
0 5 14 87.85 18.79
0 5 15 67.37 17.42
0 5 16 34.87 13.87
0 5 17 1.60 10.65
0 5 18 203.91 36.36
0 5 19 16.06 13.45
0 -6 16 -45.80 21.14
0 -6 15 7.85 11.23
0 -6 14 64.22 20.24
0 -6 13 -16.14 14.13
0 -6 12 48.50 14.21
0 -6 11 28.20 14.92
0 6 -11 22.55 8.54
0 6 -10 0.66 4.82
0 -6 10 7.24 10.40
0 6 -9 471.92 35.03
0 -6 9 429.91 43.60
0 6 -8 317.57 28.56
0 6 -7 61.47 11.71
0 6 -6 17.48 6.77
0 6 -5 572.28 36.63
0 6 -4 3304.28 95.86
0 6 -3 55.61 11.32
0 6 -2 1108.54 50.86
0 6 -1 104.65 13.85
0 6 0 13.25 4.98
0 6 1 607.76 35.74
0 -6 -2 298.21 21.05
0 6 2 304.15 24.75
0 6 3 17.98 6.86
0 -6 -3 6.08 4.24
0 -6 -4 363.35 23.59
0 6 4 361.70 26.36
0 6 5 108.47 15.44
0 6 5 123.64 14.15
0 6 6 1757.84 60.57
0 6 6 1779.69 62.92
0 6 7 1130.20 49.04
0 6 7 1190.19 50.22
0 6 8 41.24 9.54
0 6 8 39.76 9.08
0 6 9 710.66 42.22
0 6 9 727.66 38.91
0 6 10 36.26 10.14
0 6 10 34.72 8.08
0 6 11 332.10 31.31
0 6 11 360.44 27.39
0 6 12 100.58 17.85
0 6 12 119.11 16.24
0 6 13 65.80 14.43
0 6 13 63.60 12.47
0 6 14 -1.09 7.78
0 6 15 18.33 9.51
0 6 16 -6.32 9.62
0 6 17 163.64 29.63
0 6 18 19.84 9.80
0 6 19 200.29 35.48
0 -7 15 22.25 8.65
0 -7 14 10.05 9.84
0 -7 13 319.99 44.69
0 -7 12 36.36 15.17
0 7 -11 21.72 9.18
0 -7 11 44.76 17.07
0 -7 10 52.44 19.28
0 7 -10 46.88 12.94
0 -7 9 61.13 19.31
0 7 -9 23.37 8.03
0 7 -8 24.97 6.76
0 7 -7 62.88 13.66
0 7 -6 40.99 11.36
0 7 -5 728.53 44.83
0 7 -4 31.55 9.28
0 7 -3 1152.52 55.88
0 7 -2 795.61 45.34
0 7 -1 -7.54 7.78
0 7 0 2.31 7.60
0 7 1 155.37 19.36
0 7 2 1627.05 64.42
0 -7 -3 412.68 26.63
0 7 3 383.20 30.06
0 7 4 124.10 17.08
0 -7 -4 119.09 14.52
0 7 5 470.16 33.38
0 -7 -5 458.43 28.96
0 7 6 430.74 31.55
0 7 6 468.32 31.10
0 7 7 120.96 15.75
0 7 7 164.06 19.40
0 7 8 323.09 27.35
0 7 8 323.34 27.74
0 7 9 28.29 9.84
0 7 9 22.48 6.80
0 7 10 570.79 37.20
0 7 10 517.08 37.82
0 7 11 1433.99 68.14
0 7 11 1401.40 60.40
0 7 12 22.18 9.39
0 7 12 22.86 9.65
0 7 13 179.12 26.21
0 7 13 178.20 21.52
0 7 14 20.95 8.46
0 7 14 23.95 8.28
0 7 15 2.83 10.77
0 7 16 -7.90 11.00
0 7 17 71.06 21.04
0 7 18 46.23 14.45
0 7 19 54.73 19.62
0 -8 14 47.17 18.04
0 -8 13 34.94 17.42
0 -8 12 375.30 48.51
0 8 -11 92.63 19.10
0 -8 11 151.47 27.46
0 8 -10 -3.58 5.03
0 -8 10 26.71 16.93
0 8 -9 0.48 5.53
0 8 -8 117.88 20.43
0 8 -7 5.03 6.95
0 8 -6 77.33 17.37
0 8 -5 205.73 25.51
0 8 -4 1239.70 62.88
0 8 -3 1042.78 56.89
0 8 -2 52.63 13.22
0 8 -1 2091.61 82.25
0 8 0 440.01 35.42
0 8 1 705.53 44.21
0 8 2 1186.35 57.71
0 -8 -3 27.41 7.97
0 8 3 21.13 7.32
0 -8 -4 42.62 9.83
0 8 4 47.24 11.70
0 8 5 8.76 5.21
0 -8 -5 0.42 3.58
0 -8 -6 331.77 26.73
0 8 6 337.16 29.85
0 8 7 124.29 17.96
0 8 7 146.85 18.50
0 8 8 170.03 19.90
0 8 8 187.40 22.39
0 8 9 866.22 49.69
0 8 9 760.92 46.18
0 8 10 965.31 52.80
0 8 10 962.16 53.54
0 8 11 51.17 12.48
0 8 11 61.44 15.23
0 8 12 98.57 18.77
0 8 12 124.81 18.76
0 8 13 189.67 23.33
0 8 13 160.94 24.00
0 8 14 104.75 18.35
0 8 14 111.92 21.22
0 8 15 41.69 15.38
0 8 16 56.95 15.44
0 8 17 16.74 8.51
0 8 18 11.40 10.08
0 8 19 83.84 23.19
0 -9 14 -0.26 12.62
0 -9 13 124.66 31.12
0 -9 12 173.52 34.10
0 -9 11 59.61 23.14
0 9 -11 59.47 16.06
0 9 -10 132.50 24.19
0 -9 10 193.98 33.97
0 9 -9 26.93 11.85
0 9 -8 12.92 6.35
0 9 -7 62.07 14.95
0 9 -6 35.47 12.51
0 9 -5 121.56 20.99
0 9 -4 196.49 25.72
0 9 -3 80.86 17.67
0 9 -2 395.82 35.93
0 9 -1 44.88 13.62
0 9 0 156.50 21.08
0 9 1 1005.85 58.04
0 9 2 269.35 28.61
0 9 3 843.79 51.14
0 9 4 -6.82 7.52
0 -9 -4 8.06 5.60
0 9 5 109.72 17.60
0 -9 -5 125.68 17.25
0 9 6 52.07 12.79
0 -9 -6 45.35 9.91
0 -9 -7 19.68 7.47
0 9 7 9.72 7.45
0 9 8 25.26 7.62
0 9 8 34.02 10.63
0 9 9 49.61 11.86
0 9 9 56.01 15.47
0 9 10 216.54 25.99
0 9 10 187.85 23.81
0 9 11 287.24 29.79
0 9 11 307.64 31.88
0 9 12 48.26 12.12
0 9 12 47.39 13.82
0 9 13 54.04 13.34
0 9 13 23.39 10.56
0 9 14 620.40 44.83
0 9 14 607.61 51.13
0 9 15 13.33 10.11
0 9 16 214.78 31.19
0 9 17 -14.73 12.62
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4 1 2 5.19 5.44
4 1 3 386.52 26.00
4 1 4 60.76 10.72
4 1 5 51.76 8.96
4 1 6 268.70 23.67
4 1 7 157.41 18.15
4 1 7 192.69 17.04
4 1 8 43.45 9.10
4 1 8 30.58 9.09
4 1 9 1355.45 55.56
4 1 9 1392.13 59.90
4 1 10 202.02 23.30
4 1 10 188.59 21.07
4 1 11 139.08 18.73
4 1 11 147.86 20.54
4 1 12 477.93 37.04
4 1 12 510.22 39.67
4 1 13 51.47 12.77
4 1 13 41.76 9.78
4 1 14 70.63 14.99
4 1 14 73.24 17.63
4 1 15 65.26 14.81
4 1 15 91.15 20.84
4 1 16 1.91 5.31
4 1 16 12.65 8.55
4 1 17 112.69 23.76
4 1 18 6.95 13.16
4 1 19 -12.80 16.30
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-4 -2 12 14.00 7.87
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-4 -2 9 -9.40 7.28
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4 2 -7 19.68 4.56
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4 2 -4 104.65 11.27
4 2 -3 1394.27 46.28
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4 2 -2 636.32 30.20
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4 2 -1 46.57 8.50
4 2 0 1291.88 47.29
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4 2 1 275.31 21.54
4 2 2 92.20 12.76
4 2 2 97.52 5.98
4 2 3 174.11 18.37
4 2 4 169.22 18.06
4 2 5 932.41 28.38
4 2 5 945.26 44.89
4 2 6 6.11 4.78
4 2 6 11.81 3.74
4 2 7 21.20 7.72
4 2 7 26.04 5.50
4 2 8 449.91 26.74
4 2 8 447.36 32.35
4 2 9 844.87 40.93
4 2 9 994.98 50.50
4 2 10 599.76 39.85
4 2 10 545.99 34.55
4 2 11 149.79 20.08
4 2 11 155.53 18.93
4 2 12 33.70 10.17
4 2 12 39.09 11.43
4 2 13 312.79 30.38
4 2 13 346.05 33.14
4 2 14 319.58 33.68
4 2 14 379.50 34.67
4 2 15 43.18 13.46
4 2 15 31.42 11.03
4 2 16 37.97 14.66
4 2 16 10.29 6.68
4 2 17 32.79 11.68
4 2 18 -1.79 8.68
4 2 19 71.43 22.74
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4 3 -5 21.62 5.87
4 3 -4 2.89 3.07
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4 3 1 644.49 34.78
4 3 2 656.56 35.92
4 3 3 -0.61 3.16
4 3 4 524.87 34.10
4 3 5 1745.17 34.50
4 3 5 1845.67 65.25
4 3 6 10.18 2.62
4 3 6 9.42 5.41
4 3 7 0.32 2.44
4 3 7 8.49 5.55
4 3 8 447.88 24.77
4 3 8 446.97 33.37
4 3 9 81.51 14.55
4 3 9 64.75 10.18
4 3 10 227.99 24.78
4 3 10 242.80 21.73
4 3 11 108.08 17.21
4 3 11 117.10 16.84
4 3 12 1200.17 60.44
4 3 12 1102.52 54.97
4 3 13 90.04 17.53
4 3 13 78.89 15.24
4 3 14 -12.29 10.66
4 3 14 15.26 6.37
4 3 15 525.19 40.89
4 3 15 401.47 38.67
4 3 16 4.43 7.29
4 3 16 2.80 8.31
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4 3 18 19.74 14.12
4 3 19 12.28 13.32
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4 4 -5 39.09 9.14
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4 4 2 118.05 16.48
4 4 3 420.23 30.91
4 4 4 590.74 36.39
4 4 5 11.23 4.93
4 4 6 1374.27 31.34
4 4 6 1469.45 60.63
4 4 7 90.54 8.88
4 4 7 113.55 16.71
4 4 8 -2.43 4.64
4 4 8 6.45 3.67
4 4 9 73.60 10.52
4 4 9 64.75 12.33
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4 4 11 37.43 9.97
4 4 11 25.43 9.81
4 4 12 172.54 22.83
4 4 12 234.09 23.75
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4 4 13 121.45 19.84
4 4 14 1597.27 74.43
4 4 14 1491.57 70.58
4 4 15 44.70 11.12
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4 5 -7 0.89 4.18
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4 5 4 124.01 17.58
4 5 5 3114.03 95.79
4 5 6 257.69 25.28
4 5 7 570.25 39.25
4 5 7 526.94 20.44
4 5 8 5.78 6.35
4 5 8 5.83 3.51
4 5 9 4.00 5.29
4 5 9 0.23 2.92
4 5 10 17.76 10.22
4 5 10 4.13 3.26
4 5 11 241.93 27.48
4 5 11 226.26 21.31
4 5 12 0.45 5.17
4 5 12 7.92 4.05
4 5 13 402.78 36.87
4 5 13 395.98 32.03
4 5 14 68.98 16.28
4 5 14 70.96 13.48
4 5 15 558.32 44.03
4 5 15 501.71 40.57
4 5 16 36.03 12.48
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4 6 8 365.62 32.42
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4 6 11 17.26 7.49
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4 7 4 88.25 16.42
4 7 5 1259.10 62.56
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4 7 8 269.90 27.94
4 7 9 -0.79 4.63
4 7 9 3.60 3.00
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4 7 10 29.82 6.84
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4 8 8 56.55 15.29
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4 8 11 26.54 7.01
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4 13 5 31.50 14.48
4 13 6 92.77 25.00
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9 1 0 2.62 4.82
9 1 0 12.17 6.74
9 1 1 4.31 3.54
9 1 1 -4.95 7.65
9 1 2 128.88 15.28
9 1 2 124.37 21.52
9 1 3 23.94 9.25
9 1 4 130.34 24.37
9 1 5 32.84 12.52
9 1 6 71.21 16.58
9 1 7 164.24 27.23
9 1 8 40.01 13.88
9 1 9 83.21 18.81
9 1 10 183.49 31.01
9 1 11 -2.75 12.94
9 1 12 323.94 41.43
9 1 13 36.01 17.99
9 1 14 24.62 13.22
9 1 15 12.55 16.81
-9 -2 12 82.98 25.24
-9 -2 11 0.40 9.69
-9 -2 10 1.87 7.85
-9 -2 9 12.22 10.83
-9 -2 8 -14.93 11.44
-9 -2 7 10.99 6.09
9 2 -6 53.96 12.35
-9 -2 6 60.30 15.49
9 2 -5 67.42 13.95
-9 -2 5 87.30 18.23
-9 -2 4 290.35 30.70
9 2 -4 373.41 34.41
-9 -2 3 22.61 9.12
9 2 -3 25.44 5.90
-9 -2 2 395.37 32.20
9 2 -2 515.33 42.34
9 2 -1 9.20 8.17
-9 -2 1 -0.97 4.45
9 2 0 455.54 40.68
9 2 1 182.42 27.62
9 2 2 -5.61 7.98
9 2 3 9.44 8.80
9 2 4 15.71 9.22
9 2 5 23.84 11.38
9 2 6 65.23 16.26
9 2 7 14.74 6.87
9 2 8 23.53 11.87
9 2 9 258.39 36.25
9 2 10 43.03 14.66
9 2 11 724.94 61.86
9 2 12 65.98 20.06
9 2 13 5.15 10.38
9 2 14 5.12 8.92
9 2 15 31.31 16.94
-9 -3 11 194.21 32.53
-9 -3 10 -5.12 15.66
-9 -3 9 33.25 14.52
-9 -3 8 -14.77 10.27
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9 3 -6 -2.73 5.95
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9 3 -2 -4.35 5.47
9 3 -1 371.19 35.88
-9 -3 1 295.06 25.59
9 3 0 249.81 32.93
9 3 1 -18.66 12.21
9 3 2 1109.53 67.70
9 3 3 22.50 12.88
9 3 4 12.98 10.13
9 3 5 -4.26 6.31
9 3 6 -3.14 6.90
9 3 7 82.04 21.68
9 3 8 11.06 9.64
9 3 9 20.23 14.02
9 3 10 658.44 58.54
9 3 11 67.88 19.37
9 3 12 107.64 25.54
9 3 13 14.08 14.27
9 3 14 -8.83 7.97
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-9 -4 11 8.53 10.85
-9 -4 10 243.90 35.54
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9 4 -3 4.64 6.66
-9 -4 3 -0.20 5.93
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9 4 -2 269.06 30.17
9 4 -1 98.84 18.97
9 4 0 33.17 13.67
9 4 1 810.98 56.93
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9 4 3 280.93 32.65
9 4 4 33.17 14.28
9 4 5 20.70 8.05
9 4 6 -6.89 9.49
9 4 7 67.70 16.35
9 4 8 6.81 8.76
9 4 9 210.98 32.79
9 4 10 -4.72 11.97
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9 5 -2 20.75 11.97
9 5 -1 377.23 38.75
9 5 0 219.25 28.58
9 5 1 107.04 21.22
9 5 2 371.86 39.24
9 5 3 394.02 40.83
9 5 4 2.51 9.68
9 5 5 198.03 30.99
9 5 6 230.25 31.87
9 5 7 44.66 16.16
9 5 8 111.40 24.26
9 5 9 -6.66 10.46
9 5 10 475.61 49.82
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9 5 12 0.20 8.31
9 5 13 27.39 14.01
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9 6 -1 139.25 24.27
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9 6 3 20.44 7.43
9 6 4 117.50 22.92
9 6 5 19.23 8.15
9 6 6 182.27 29.73
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9 6 8 6.14 9.71
9 6 9 5.76 12.70
9 6 10 58.34 19.12
9 6 11 4.93 9.43
9 6 12 12.01 13.59
9 6 13 6.50 9.84
9 6 14 84.33 24.56
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9 7 -4 14.35 7.90
9 7 -3 12.07 8.34
9 7 -2 26.63 11.59
9 7 -1 59.11 17.11
9 7 0 37.19 14.25
9 7 1 40.64 13.97
9 7 2 197.18 30.87
9 7 3 151.36 26.48
9 7 4 53.98 16.13
9 7 5 59.82 17.88
9 7 6 156.69 27.50
9 7 7 23.06 9.11
9 7 8 247.92 37.46
9 7 9 23.49 14.64
9 7 10 51.45 17.17
9 7 11 3.46 12.04
9 7 12 -13.00 14.79
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9 7 14 23.99 15.16
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9 8 -3 149.19 27.03
9 8 -2 22.52 12.49
9 8 -1 72.20 19.72
9 8 0 12.28 12.04
9 8 1 -2.21 7.64
9 8 2 149.93 27.82
9 8 3 23.24 13.95
9 8 4 216.87 32.61
9 8 5 82.31 20.91
9 8 6 78.15 19.84
9 8 7 612.98 57.11
9 8 8 62.45 19.63
9 8 9 -1.39 12.74
9 8 10 37.90 17.47
9 8 11 -11.77 10.98
9 8 12 83.79 22.57
9 8 13 1.55 9.49
9 8 14 -15.25 17.93
9 9 -4 25.46 10.66
9 9 -3 3.49 11.38
9 9 -2 307.09 40.02
9 9 -1 39.41 17.92
9 9 0 45.60 18.31
9 9 1 -14.05 12.08
9 9 2 23.38 15.74
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9 9 4 14.36 13.23
9 9 5 96.06 23.48
9 9 6 361.79 45.35
9 9 7 27.05 11.21
9 9 8 261.43 39.10
9 9 9 105.81 25.39
9 9 10 6.79 11.96
9 9 11 192.05 37.02
9 9 12 96.55 23.66
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9 10 -3 225.67 34.98
9 10 -2 88.00 23.01
9 10 -1 75.60 22.43
9 10 0 11.40 9.46
9 10 1 19.16 12.65
9 10 2 5.55 11.39
9 10 3 85.42 22.59
9 10 4 5.65 10.10
9 10 5 48.27 20.49
9 10 6 3.53 12.95
9 10 7 271.16 42.27
9 10 8 250.59 40.76
9 10 9 2.85 12.74
9 10 10 7.58 10.21
9 10 11 54.03 18.78
9 10 12 98.92 27.41
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9 11 -2 162.79 31.63
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9 11 0 4.58 10.20
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9 11 5 -1.09 8.06
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9 11 8 14.14 11.79
9 11 9 31.74 17.25
9 11 10 12.29 12.86
9 11 11 83.95 25.17
9 11 12 288.60 44.10
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9 12 1 -10.55 12.74
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9 12 3 236.88 40.85
9 12 4 -24.59 15.16
9 12 5 5.59 11.25
9 12 6 34.67 17.42
9 12 7 40.97 19.25
9 12 8 28.18 16.05
9 12 9 20.47 15.68
9 12 10 26.87 16.31
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9 13 4 278.89 46.23
9 13 5 61.75 23.72
9 13 6 18.55 12.89
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10 -11 -5 244.80 39.51
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10 -11 -4 2.44 16.65
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10 -10 -7 18.38 11.31
10 -10 -6 95.82 26.52
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10 -10 -5 -24.02 17.30
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10 -10 -3 11.96 12.89
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10 -9 -9 18.29 10.40
10 -9 -8 4.12 10.37
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10 -9 -6 -20.68 16.04
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10 -9 -5 53.18 19.40
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10 -9 -4 10.61 9.18
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10 -9 -3 46.06 18.85
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10 -9 -2 74.23 19.59
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10 -8 -8 -8.45 15.76
10 -8 -7 -5.77 11.83
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10 -8 -6 21.35 8.53
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10 -8 -5 8.50 9.83
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10 -8 -3 25.45 13.89
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10 -8 -2 -11.80 14.22
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10 -8 -1 176.84 32.26
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10 -7 -7 -7.79 7.74
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10 -7 -4 -17.53 9.55
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10 -6 -6 -11.16 13.38
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10 -5 -5 -10.05 9.14
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10 -3 -2 -16.21 12.81
10 -3 -2 -3.24 7.55
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10 -3 1 6.14 7.45
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-10 2 9 41.75 16.71
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-10 2 7 15.53 8.33
10 -2 -6 94.54 18.39
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10 -2 -5 246.43 29.21
-10 2 5 198.95 29.78
10 -2 -4 261.74 31.27
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10 -2 -3 15.18 7.05
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10 -2 -2 198.78 26.49
10 -2 -2 157.17 24.12
10 -2 -1 6.45 7.38
10 -2 -1 8.33 6.92
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10 -2 3 13.35 8.60
10 -2 4 -23.44 13.88
10 -2 5 127.24 25.71
10 -2 6 251.20 36.47
10 -2 7 39.18 14.88
10 -2 8 51.66 15.56
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10 -2 10 3.23 12.06
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10 -2 12 -12.78 12.44
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10 -1 -6 80.69 16.72
10 -1 -5 50.69 14.45
-10 1 5 25.09 10.46
10 -1 -4 76.85 15.88
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10 -1 -2 -5.62 8.06
10 -1 -2 7.57 5.57
10 -1 -1 144.34 21.07
10 -1 -1 122.17 21.09
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10 -1 1 21.33 6.40
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10 -1 3 48.70 16.13
10 -1 4 69.05 19.12
10 -1 5 332.84 39.34
10 -1 6 -17.68 11.58
10 -1 7 97.92 21.19
10 -1 8 9.46 9.56
10 -1 9 32.65 11.70
10 -1 10 487.49 51.98
10 -1 11 101.67 24.88
10 -1 12 6.62 13.04
10 -1 13 11.07 10.67
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10 0 -1 4.32 5.45
10 0 -1 16.22 6.72
10 0 0 82.54 15.01
10 0 0 69.24 15.95
10 0 1 270.45 33.27
10 0 1 292.23 27.08
10 0 2 56.83 16.21
10 0 3 -6.27 8.00
10 0 4 5.17 6.76
10 0 5 -9.84 7.75
10 0 6 75.93 19.76
10 0 7 3.20 10.24
10 0 8 88.75 22.94
10 0 9 245.20 35.90
10 0 10 -17.76 10.20
10 0 11 108.38 25.98
10 0 12 46.53 16.77
10 0 13 12.12 9.62
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-10 -1 8 40.61 15.67
-10 -1 7 70.74 20.59
-10 -1 6 19.22 8.92
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10 1 -3 363.66 37.16
-10 -1 3 347.72 33.69
10 1 -2 -10.76 8.79
-10 -1 2 8.81 8.47
10 1 -1 249.03 25.90
10 1 -1 268.21 33.17
10 1 0 116.34 16.67
10 1 0 147.32 25.10
10 1 1 41.69 10.71
10 1 2 282.78 35.82
10 1 3 89.92 19.83
10 1 4 5.54 12.20
10 1 5 9.55 10.83
10 1 6 22.13 7.32
10 1 7 87.47 21.64
10 1 8 2.77 7.38
10 1 9 47.99 14.48
10 1 10 219.35 36.61
10 1 11 113.84 24.59
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-10 -2 3 21.43 9.94
10 2 -3 22.91 10.16
10 2 -2 138.26 24.64
-10 -2 2 95.10 17.34
10 2 -1 5.98 6.00
10 2 0 85.61 19.01
10 2 1 650.93 52.88
10 2 2 554.06 50.70
10 2 3 29.31 12.45
10 2 4 216.15 31.84
10 2 5 0.85 11.59
10 2 6 3.15 11.27
10 2 7 -5.04 12.41
10 2 8 84.11 23.05
10 2 9 160.36 31.04
10 2 10 37.43 16.11
10 2 11 21.18 11.28
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10 2 13 20.63 11.78
10 2 14 91.21 29.23
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10 3 -1 92.29 19.22
10 3 0 243.83 32.15
10 3 1 1078.70 69.12
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10 3 3 339.27 40.94
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10 3 5 76.41 22.80
10 3 6 -3.53 14.37
10 3 7 -15.80 14.43
10 3 8 -17.79 14.91
10 3 9 3.87 8.33
10 3 10 195.56 33.31
10 3 11 16.07 8.99
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10 4 -3 7.82 8.72
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10 4 -1 6.17 6.33
10 4 0 23.16 12.58
10 4 1 8.22 9.58
10 4 2 605.14 52.63
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10 4 4 300.86 37.95
10 4 5 67.76 20.52
10 4 6 56.63 16.74
10 4 7 261.05 37.25
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10 4 9 78.81 22.12
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10 5 -1 16.87 11.92
10 5 0 112.81 24.49
10 5 1 147.10 26.95
10 5 2 4.19 8.59
10 5 3 5.31 10.02
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10 5 5 134.79 26.09
10 5 6 346.89 42.62
10 5 7 3.41 11.92
10 5 8 96.43 24.74
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10 7 8 84.70 23.35
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10 10 1 27.01 13.74
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12 5 8 0.96 12.06
12 6 -1 -31.49 13.92
12 6 0 125.57 28.59
12 6 1 80.93 20.36
12 6 2 14.79 10.23
12 6 3 1.32 8.61
12 6 4 12.78 13.73
12 6 5 29.07 20.31
12 6 6 52.41 18.33
12 6 7 18.66 12.71
12 7 1 -15.08 15.16
12 7 2 64.16 23.65
12 7 3 74.86 24.63
12 7 4 9.43 12.21
12 7 5 -8.94 14.38
12 7 6 -8.17 11.94
13 -2 0 136.54 29.12
13 -2 1 -7.95 8.96
13 -1 -1 28.10 16.30
13 -1 0 24.03 16.50
13 -1 1 127.00 28.50
13 -1 2 0.44 12.97
13 -1 3 115.50 28.69
13 0 -1 8.68 9.68
13 0 0 2.28 10.50
13 0 1 14.09 9.37
13 0 2 84.70 24.77
13 0 3 90.97 27.92
13 0 4 4.15 10.82
13 1 0 -14.73 15.66
13 1 1 29.17 14.76
13 1 2 -3.50 11.15
13 1 3 35.15 16.64
13 1 4 62.36 23.37
13 2 1 64.33 21.58
13 2 2 169.82 34.05
13 2 3 47.72 17.09
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 76833
_shelx_res_file
;
x95777res.res created by SHELXL-2014/7
TITL x95777res_a.res in P-1
CELL 0.71073 10.1057 13.8342 15.3868 74.892 85.365 89.151
ZERR 2 0.0007 0.001 0.0011 0.006 0.006 0.006
LATT 1
SFAC C H Br N Ni O P
UNIT 92 108 2 4 2 1 4
DFIX 1.54 O1 C90 O1 C90A C90 C91 C90A C91A
DFIX 2.6 O1 C91 O1 C91A
DELU O1 C90 C91 C90A C91A
SIMU O1 C90 C91 C90A C91A
RIGU O1 C90 C91
RIGU O1 C90A C91A
L.S. 4
PLAN 6
fmap 2 53
acta
BOND $H
OMIT -1 1 2
OMIT 0 1 2
OMIT -1 2 1
OMIT -2 1 2
REM
REM
REM
WGHT 0.035600
FVAR 0.49405 0.57488
BR1 3 0.524729 0.232793 0.850847 11.00000 0.02860 0.03775 =
0.02729 -0.00807 -0.00101 -0.00738
NI1 5 0.705805 0.343000 0.770948 11.00000 0.02512 0.02429 =
0.02218 -0.00629 -0.00166 -0.00261
P1 7 0.799178 0.307883 0.979463 11.00000 0.02423 0.02533 =
0.02159 -0.00672 -0.00143 -0.00077
P2 7 0.559277 0.265618 0.624360 11.00000 0.02637 0.02810 =
0.02339 -0.00690 -0.00374 -0.00084
O1 6 1.000000 0.000000 0.500000 10.50000 0.16241 0.18582 =
0.16391 -0.06885 -0.03267 -0.05930
N1 4 0.800238 0.364003 0.873236 11.00000 0.03259 0.02057 =
0.02344 -0.00378 -0.00254 -0.00589
N2 4 0.666657 0.336214 0.649701 11.00000 0.03309 0.03003 =
0.02232 -0.00225 -0.00455 -0.00645
C1 1 0.802045 0.453930 0.707796 11.00000 0.02596 0.02251 =
0.02762 -0.00642 -0.00306 -0.00187
C2 1 0.873377 0.507453 0.753270 11.00000 0.02851 0.02223 =
0.02344 -0.00739 -0.00076 -0.00066
C3 1 0.946881 0.590937 0.705617 11.00000 0.04080 0.03004 =
0.03298 -0.00934 -0.00202 -0.00820
AFIX 43
H3 2 0.995709 0.626247 0.736040 11.00000 -1.20000
AFIX 0
C4 1 0.947253 0.621637 0.612086 11.00000 0.04175 0.03847 =
0.03521 0.00162 0.00101 -0.01597
AFIX 43
H4 2 0.995651 0.678137 0.580022 11.00000 -1.20000
AFIX 0
C5 1 0.875747 0.568431 0.566159 11.00000 0.04354 0.04354 =
0.02597 -0.00179 -0.00446 -0.01411
AFIX 43
H5 2 0.876764 0.588976 0.503543 11.00000 -1.20000
AFIX 0
C6 1 0.802545 0.484185 0.614350 11.00000 0.03126 0.03442 =
0.02469 -0.00472 -0.00309 -0.00647
C7 1 0.863079 0.465304 0.853715 11.00000 0.03737 0.02363 =
0.03428 -0.01216 -0.00620 -0.00481
AFIX 23
H7A 2 0.950539 0.460088 0.876224 11.00000 -1.20000
H7B 2 0.809206 0.508386 0.882740 11.00000 -1.20000
AFIX 0
C8 1 0.724556 0.418651 0.574591 11.00000 0.05128 0.04798 =
0.02843 -0.00189 -0.00454 -0.02252
AFIX 23
H8A 2 0.654528 0.456661 0.541751 11.00000 -1.20000
H8B 2 0.781596 0.391634 0.532966 11.00000 -1.20000
AFIX 0
C9 1 0.746153 0.177810 1.009505 11.00000 0.02428 0.02446 =
0.03007 -0.00609 -0.00706 0.00203
H9 2 0.667831 0.172432 0.995169 11.00000 0.00896
C10 1 0.831101 0.116171 0.956364 11.00000 0.04700 0.02787 =
0.02829 -0.00955 0.00003 -0.00019
AFIX 23
H10A 2 0.826842 0.145492 0.892120 11.00000 -1.20000
H10B 2 0.922965 0.117598 0.970053 11.00000 -1.20000
AFIX 0
C11 1 0.781638 0.007902 0.980815 11.00000 0.05784 0.03369 =
0.05811 -0.02413 0.00129 -0.00309
AFIX 23
H11A 2 0.693243 0.006186 0.960917 11.00000 -1.20000
H11B 2 0.839611 -0.030675 0.949413 11.00000 -1.20000
AFIX 0
C12 1 0.777946 -0.039341 1.081420 11.00000 0.06587 0.02260 =
0.05413 -0.00662 0.00169 -0.00134
AFIX 23
H12A 2 0.867505 -0.043693 1.100487 11.00000 -1.20000
H12B 2 0.742083 -0.106738 1.094830 11.00000 -1.20000
AFIX 0
C13 1 0.692900 0.021830 1.133395 11.00000 0.04833 0.03213 =
0.03628 -0.00265 0.00490 -0.00938
AFIX 23
H13A 2 0.601651 0.021245 1.118223 11.00000 -1.20000
H13B 2 0.694886 -0.008282 1.197695 11.00000 -1.20000
AFIX 0
C14 1 0.742758 0.129365 1.111122 11.00000 0.04030 0.03141 =
0.02834 -0.00583 0.00133 -0.00004
AFIX 23
H14A 2 0.831230 0.130416 1.131075 11.00000 -1.20000
H14B 2 0.684939 0.167472 1.143092 11.00000 -1.20000
AFIX 0
C15 1 0.965836 0.299834 1.018045 11.00000 0.02573 0.02581 =
0.03402 -0.00914 -0.00124 -0.00146
C16 1 0.988704 0.285663 1.108150 11.00000 0.02999 0.03649 =
0.03774 -0.01483 -0.00926 0.00283
AFIX 43
H16 2 0.919655 0.293970 1.149286 11.00000 -1.20000
AFIX 0
C17 1 1.114432 0.259041 1.137667 11.00000 0.04148 0.04099 =
0.05472 -0.01586 -0.02374 0.00400
AFIX 43
H17 2 1.128942 0.248740 1.198318 11.00000 -1.20000
AFIX 0
C18 1 1.215758 0.248255 1.076951 11.00000 0.03195 0.03277 =
0.07512 -0.01682 -0.01871 0.00098
AFIX 43
H18 2 1.298897 0.228706 1.096896 11.00000 -1.20000
AFIX 0
C19 1 1.197008 0.265795 0.986826 11.00000 0.02410 0.02941 =
0.08263 -0.01615 0.00870 -0.00171
AFIX 43
H19 2 1.268066 0.260715 0.945941 11.00000 -1.20000
AFIX 0
C20 1 1.071127 0.291321 0.956307 11.00000 0.03052 0.02694 =
0.04511 -0.01331 0.00497 -0.00734
AFIX 43
H20 2 1.057942 0.302490 0.895368 11.00000 -1.20000
AFIX 0
C21 1 0.697061 0.372489 1.048379 11.00000 0.02582 0.02860 =
0.01670 -0.00549 0.00086 -0.00203
C22 1 0.560267 0.353675 1.059552 11.00000 0.03241 0.03090 =
0.03151 -0.01075 -0.00387 -0.00187
AFIX 43
H22 2 0.525537 0.303596 1.037641 11.00000 -1.20000
AFIX 0
C23 1 0.476305 0.409327 1.103119 11.00000 0.02850 0.04335 =
0.03148 -0.01003 -0.00183 0.00454
AFIX 43
H23 2 0.385745 0.395314 1.111469 11.00000 -1.20000
AFIX 0
C24 1 0.525867 0.485262 1.134177 11.00000 0.04118 0.02989 =
0.03194 -0.00657 -0.00160 0.00790
AFIX 43
H24 2 0.468722 0.522922 1.162579 11.00000 -1.20000
AFIX 0
C25 1 0.660164 0.505302 1.123095 11.00000 0.05562 0.02475 =
0.03177 -0.01278 -0.00378 -0.00166
AFIX 43
H25 2 0.693786 0.556183 1.144469 11.00000 -1.20000
AFIX 0
C26 1 0.745943 0.449299 1.079788 11.00000 0.03573 0.02620 =
0.03354 -0.00847 -0.00060 -0.00607
AFIX 43
H26 2 0.836438 0.463558 1.071935 11.00000 -1.20000
AFIX 0
C27 1 0.578228 0.130449 0.671434 11.00000 0.03007 0.03125 =
0.02958 -0.01328 -0.00169 0.00069
AFIX 13
H27 2 0.519503 0.111957 0.727144 11.00000 -1.20000
AFIX 0
C28 1 0.718937 0.101505 0.698168 11.00000 0.03586 0.04152 =
0.03813 -0.01406 -0.01029 0.00855
AFIX 23
H28A 2 0.780628 0.116708 0.644684 11.00000 -1.20000
H28B 2 0.745118 0.140116 0.738373 11.00000 -1.20000
AFIX 0
C29 1 0.724217 -0.009816 0.745136 11.00000 0.06532 0.04542 =
0.06084 -0.01792 -0.02712 0.02203
AFIX 23
H29A 2 0.668380 -0.023522 0.801333 11.00000 -1.20000
H29B 2 0.814534 -0.027691 0.759562 11.00000 -1.20000
AFIX 0
C30 1 0.677783 -0.073971 0.686245 11.00000 0.08588 0.03869 =
0.06199 -0.01916 -0.02516 0.02400
AFIX 23
H30A 2 0.739832 -0.066378 0.633378 11.00000 -1.20000
H30B 2 0.677081 -0.143843 0.719859 11.00000 -1.20000
AFIX 0
C31 1 0.540456 -0.044840 0.656550 11.00000 0.07512 0.03331 =
0.04663 -0.01975 -0.00731 0.00332
AFIX 23
H31A 2 0.476272 -0.060850 0.708688 11.00000 -1.20000
H31B 2 0.517259 -0.082895 0.615133 11.00000 -1.20000
AFIX 0
C32 1 0.534926 0.066681 0.610338 11.00000 0.04224 0.03403 =
0.03091 -0.01044 -0.00733 0.00019
AFIX 23
H32A 2 0.445042 0.084298 0.594657 11.00000 -1.20000
H32B 2 0.592539 0.081266 0.554896 11.00000 -1.20000
AFIX 0
C33 1 0.389875 0.297110 0.652844 11.00000 0.02807 0.03787 =
0.02122 -0.00545 -0.00636 -0.00143
C34 1 0.362682 0.395233 0.655644 11.00000 0.05044 0.03361 =
0.04506 -0.01372 -0.01293 0.00548
AFIX 43
H34 2 0.431899 0.441524 0.644144 11.00000 -1.20000
AFIX 0
C35 1 0.235078 0.425545 0.675136 11.00000 0.05573 0.06565 =
0.05128 -0.03097 -0.02141 0.03225
AFIX 43
H35 2 0.219064 0.491522 0.676516 11.00000 -1.20000
AFIX 0
C36 1 0.132755 0.358039 0.692341 11.00000 0.04192 0.08364 =
0.04094 -0.01968 -0.01118 0.03190
AFIX 43
H36 2 0.046760 0.378140 0.705112 11.00000 -1.20000
AFIX 0
C37 1 0.156804 0.260656 0.690786 11.00000 0.02994 0.07448 =
0.05354 -0.01522 0.00034 -0.00240
AFIX 43
H37 2 0.086881 0.214885 0.703485 11.00000 -1.20000
AFIX 0
C38 1 0.284882 0.229282 0.670390 11.00000 0.03042 0.04365 =
0.05140 -0.01242 0.00249 -0.00232
AFIX 43
H38 2 0.299808 0.163319 0.668562 11.00000 -1.20000
AFIX 0
C39 1 0.570852 0.282539 0.502262 11.00000 0.03415 0.02918 =
0.02743 -0.00892 -0.00582 -0.00782
C40 1 0.689883 0.259226 0.460407 11.00000 0.03767 0.03836 =
0.03339 -0.00919 -0.00307 -0.00379
AFIX 43
H40 2 0.761971 0.238100 0.494375 11.00000 -1.20000
AFIX 0
C41 1 0.701649 0.267315 0.368283 11.00000 0.04819 0.04762 =
0.03051 -0.00849 0.00575 -0.00951
AFIX 43
H41 2 0.781187 0.250797 0.340973 11.00000 -1.20000
AFIX 0
C42 1 0.595933 0.299730 0.317089 11.00000 0.06902 0.04378 =
0.02583 -0.00623 -0.00560 -0.00847
AFIX 43
H42 2 0.603746 0.305138 0.255363 11.00000 -1.20000
AFIX 0
C43 1 0.479159 0.323921 0.358060 11.00000 0.06362 0.04583 =
0.03760 -0.00648 -0.02210 -0.00528
AFIX 43
H43 2 0.408044 0.346315 0.323476 11.00000 -1.20000
AFIX 0
C44 1 0.465118 0.315579 0.450411 11.00000 0.04201 0.02996 =
0.03152 -0.00390 -0.00509 -0.00014
AFIX 43
H44 2 0.385171 0.332092 0.477221 11.00000 -1.20000
AFIX 0
PART 1
C90 1 0.924403 -0.050751 0.445757 21.00000 0.09839 0.19838 =
0.15117 -0.09135 0.00022 -0.03475
AFIX 23
H90A 2 0.972479 -0.109909 0.439016 21.00000 -1.20000
H90B 2 0.839288 -0.072576 0.478288 21.00000 -1.20000
AFIX 0
C91 1 0.901413 0.013488 0.354907 21.00000 0.10265 0.22343 =
0.16790 -0.07197 -0.01289 -0.05923
AFIX 137
H91A 2 0.985203 0.033850 0.321520 21.00000 -1.50000
H91B 2 0.852294 0.071637 0.360919 21.00000 -1.50000
H91C 2 0.851849 -0.023412 0.323436 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C90A 1 0.946992 0.063996 0.425657 -21.00000 0.13161 0.17759 =
0.13497 -0.09814 -0.00870 -0.01389
AFIX 23
H90C 2 1.016541 0.086992 0.377659 -21.00000 -1.20000
H90D 2 0.908642 0.121984 0.442281 -21.00000 -1.20000
AFIX 0
C91A 1 0.839037 0.007445 0.392590 -21.00000 0.13464 0.15966 =
0.17957 -0.09149 -0.03304 -0.00484
AFIX 137
H91D 2 0.838474 0.031222 0.328172 -21.00000 -1.50000
H91E 2 0.753841 0.018902 0.420428 -21.00000 -1.50000
H91F 2 0.857670 -0.062952 0.408610 -21.00000 -1.50000
AFIX 0
HKLF 4
REM x95777res_a.res in P-1
REM R1 = 0.0540 for 6137 Fo > 4sig(Fo) and 0.0989 for all 9359 data
REM 500 parameters refined using 78 restraints
END
WGHT 0.0356 0.0000
REM Highest difference peak 0.755, deepest hole -0.617, 1-sigma level 0.096
Q1 1 0.7522 -0.1953 0.4745 11.00000 0.05 0.75
Q2 1 0.6586 -0.1211 1.0707 11.00000 0.05 0.69
Q3 1 0.3770 0.1574 0.6984 11.00000 0.05 0.64
Q4 1 0.9803 0.4181 0.9011 11.00000 0.05 0.61
Q5 1 0.2159 0.1604 0.7520 11.00000 0.05 0.59
Q6 1 0.7360 0.3736 0.5392 11.00000 0.05 0.54
;
_shelx_res_checksum 16658
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.52473(4) 0.23279(3) 0.85085(3) 0.03128(12) Uani d 1 . .
Ni Ni1 0.70581(5) 0.34300(4) 0.77095(3) 0.02380(13) Uani d 1 . .
P P1 0.79918(10) 0.30788(8) 0.97946(7) 0.0236(2) Uani d 1 . .
P P2 0.55928(10) 0.26562(8) 0.62436(7) 0.0258(2) Uani d 1 . .
O O1 1.0000 0.0000 0.5000 0.165(4) Uani d 1 . .
N N1 0.8002(3) 0.3640(2) 0.8732(2) 0.0258(7) Uani d 1 . .
N N2 0.6667(3) 0.3362(3) 0.6497(2) 0.0291(8) Uani d 1 . .
C C1 0.8020(4) 0.4539(3) 0.7078(3) 0.0253(9) Uani d 1 . .
C C2 0.8734(4) 0.5075(3) 0.7533(2) 0.0245(9) Uani d 1 . .
C C3 0.9469(4) 0.5909(3) 0.7056(3) 0.0344(10) Uani d 1 . .
H H3 0.9957 0.6262 0.7360 0.041 Uiso calc 1 . .
C C4 0.9473(4) 0.6216(4) 0.6121(3) 0.0406(12) Uani d 1 . .
H H4 0.9957 0.6781 0.5800 0.049 Uiso calc 1 . .
C C5 0.8757(4) 0.5684(4) 0.5662(3) 0.0388(11) Uani d 1 . .
H H5 0.8768 0.5890 0.5035 0.047 Uiso calc 1 . .
C C6 0.8025(4) 0.4842(3) 0.6143(3) 0.0306(10) Uani d 1 . .
C C7 0.8631(4) 0.4653(3) 0.8537(3) 0.0307(10) Uani d 1 . .
H H7A 0.9505 0.4601 0.8762 0.037 Uiso calc 1 . .
H H7B 0.8092 0.5084 0.8827 0.037 Uiso calc 1 . .
C C8 0.7246(5) 0.4187(4) 0.5746(3) 0.0438(12) Uani d 1 . .
H H8A 0.6545 0.4567 0.5418 0.053 Uiso calc 1 . .
H H8B 0.7816 0.3916 0.5330 0.053 Uiso calc 1 . .
C C9 0.7462(4) 0.1778(3) 1.0095(3) 0.0262(9) Uani d 1 . .
H H9 0.668(3) 0.172(3) 0.995(2) 0.009(9) Uiso d 1 . .
C C10 0.8311(4) 0.1162(3) 0.9564(3) 0.0341(10) Uani d 1 . .
H H10A 0.8268 0.1455 0.8921 0.041 Uiso calc 1 . .
H H10B 0.9230 0.1176 0.9701 0.041 Uiso calc 1 . .
C C11 0.7816(5) 0.0079(4) 0.9808(3) 0.0479(13) Uani d 1 . .
H H11A 0.6932 0.0062 0.9609 0.057 Uiso calc 1 . .
H H11B 0.8396 -0.0307 0.9494 0.057 Uiso calc 1 . .
C C12 0.7779(5) -0.0393(3) 1.0814(3) 0.0485(13) Uani d 1 . .
H H12A 0.8675 -0.0437 1.1005 0.058 Uiso calc 1 . .
H H12B 0.7421 -0.1067 1.0948 0.058 Uiso calc 1 . .
C C13 0.6929(5) 0.0218(3) 1.1334(3) 0.0404(11) Uani d 1 . .
H H13A 0.6017 0.0212 1.1182 0.049 Uiso calc 1 . .
H H13B 0.6949 -0.0083 1.1977 0.049 Uiso calc 1 . .
C C14 0.7428(4) 0.1294(3) 1.1111(3) 0.0339(10) Uani d 1 . .
H H14A 0.8312 0.1304 1.1311 0.041 Uiso calc 1 . .
H H14B 0.6849 0.1675 1.1431 0.041 Uiso calc 1 . .
C C15 0.9658(4) 0.2998(3) 1.0180(3) 0.0283(9) Uani d 1 . .
C C16 0.9887(4) 0.2857(3) 1.1082(3) 0.0334(10) Uani d 1 . .
H H16 0.9197 0.2940 1.1493 0.040 Uiso calc 1 . .
C C17 1.1144(5) 0.2590(4) 1.1377(3) 0.0440(12) Uani d 1 . .
H H17 1.1289 0.2487 1.1983 0.053 Uiso calc 1 . .
C C18 1.2158(5) 0.2483(4) 1.0770(4) 0.0453(12) Uani d 1 . .
H H18 1.2989 0.2287 1.0969 0.054 Uiso calc 1 . .
C C19 1.1970(4) 0.2658(3) 0.9868(4) 0.0458(13) Uani d 1 . .
H H19 1.2681 0.2607 0.9459 0.055 Uiso calc 1 . .
C C20 1.0711(4) 0.2913(3) 0.9563(3) 0.0338(10) Uani d 1 . .
H H20 1.0579 0.3025 0.8954 0.041 Uiso calc 1 . .
C C21 0.6971(4) 0.3725(3) 1.0484(2) 0.0239(9) Uani d 1 . .
C C22 0.5603(4) 0.3537(3) 1.0596(3) 0.0310(10) Uani d 1 . .
H H22 0.5255 0.3036 1.0376 0.037 Uiso calc 1 . .
C C23 0.4763(4) 0.4093(3) 1.1031(3) 0.0345(10) Uani d 1 . .
H H23 0.3857 0.3953 1.1115 0.041 Uiso calc 1 . .
C C24 0.5259(4) 0.4853(3) 1.1342(3) 0.0348(10) Uani d 1 . .
H H24 0.4687 0.5229 1.1626 0.042 Uiso calc 1 . .
C C25 0.6602(5) 0.5053(3) 1.1231(3) 0.0363(11) Uani d 1 . .
H H25 0.6938 0.5562 1.1445 0.044 Uiso calc 1 . .
C C26 0.7459(4) 0.4493(3) 1.0798(3) 0.0318(10) Uani d 1 . .
H H26 0.8364 0.4636 1.0719 0.038 Uiso calc 1 . .
C C27 0.5782(4) 0.1304(3) 0.6714(3) 0.0293(9) Uani d 1 . .
H H27 0.5195 0.1120 0.7271 0.035 Uiso calc 1 . .
C C28 0.7189(4) 0.1015(4) 0.6982(3) 0.0375(11) Uani d 1 . .
H H28A 0.7806 0.1167 0.6447 0.045 Uiso calc 1 . .
H H28B 0.7451 0.1401 0.7384 0.045 Uiso calc 1 . .
C C29 0.7242(6) -0.0098(4) 0.7451(4) 0.0554(14) Uani d 1 . .
H H29A 0.6684 -0.0235 0.8013 0.066 Uiso calc 1 . .
H H29B 0.8145 -0.0277 0.7596 0.066 Uiso calc 1 . .
C C30 0.6778(6) -0.0740(4) 0.6862(4) 0.0602(16) Uani d 1 . .
H H30A 0.7398 -0.0664 0.6334 0.072 Uiso calc 1 . .
H H30B 0.6771 -0.1438 0.7199 0.072 Uiso calc 1 . .
C C31 0.5405(5) -0.0448(4) 0.6565(3) 0.0498(13) Uani d 1 . .
H H31A 0.4763 -0.0609 0.7087 0.060 Uiso calc 1 . .
H H31B 0.5173 -0.0829 0.6151 0.060 Uiso calc 1 . .
C C32 0.5349(5) 0.0667(3) 0.6103(3) 0.0351(10) Uani d 1 . .
H H32A 0.4450 0.0843 0.5947 0.042 Uiso calc 1 . .
H H32B 0.5925 0.0813 0.5549 0.042 Uiso calc 1 . .
C C33 0.3899(4) 0.2971(3) 0.6528(3) 0.0292(9) Uani d 1 . .
C C34 0.3627(5) 0.3952(4) 0.6556(3) 0.0419(12) Uani d 1 . .
H H34 0.4319 0.4415 0.6441 0.050 Uiso calc 1 . .
C C35 0.2351(5) 0.4255(5) 0.6751(3) 0.0540(15) Uani d 1 . .
H H35 0.2191 0.4915 0.6765 0.065 Uiso calc 1 . .
C C36 0.1328(5) 0.3580(5) 0.6923(3) 0.0547(15) Uani d 1 . .
H H36 0.0468 0.3781 0.7051 0.066 Uiso calc 1 . .
C C37 0.1568(5) 0.2607(5) 0.6908(3) 0.0531(14) Uani d 1 . .
H H37 0.0869 0.2149 0.7035 0.064 Uiso calc 1 . .
C C38 0.2849(4) 0.2293(4) 0.6704(3) 0.0421(12) Uani d 1 . .
H H38 0.2998 0.1633 0.6686 0.051 Uiso calc 1 . .
C C39 0.5709(4) 0.2825(3) 0.5023(3) 0.0297(10) Uani d 1 . .
C C40 0.6899(4) 0.2592(3) 0.4604(3) 0.0364(11) Uani d 1 . .
H H40 0.7620 0.2381 0.4944 0.044 Uiso calc 1 . .
C C41 0.7016(5) 0.2673(4) 0.3683(3) 0.0428(12) Uani d 1 . .
H H41 0.7812 0.2508 0.3410 0.051 Uiso calc 1 . .
C C42 0.5959(5) 0.2997(4) 0.3171(3) 0.0465(13) Uani d 1 . .
H H42 0.6037 0.3051 0.2554 0.056 Uiso calc 1 . .
C C43 0.4792(5) 0.3239(4) 0.3581(3) 0.0488(13) Uani d 1 . .
H H43 0.4080 0.3463 0.3235 0.059 Uiso calc 1 . .
C C44 0.4651(5) 0.3156(3) 0.4504(3) 0.0351(10) Uani d 1 . .
H H44 0.3852 0.3321 0.4772 0.042 Uiso calc 1 . .
C C90 0.9244(16) -0.0508(14) 0.4458(10) 0.141(6) Uani d 0.575(11) A 1
H H90A 0.9725 -0.1099 0.4390 0.169 Uiso calc 0.575(11) A 1
H H90B 0.8393 -0.0726 0.4783 0.169 Uiso calc 0.575(11) A 1
C C91 0.9014(19) 0.0135(19) 0.3549(10) 0.160(9) Uani d 0.575(11) A 1
H H91A 0.9852 0.0339 0.3215 0.240 Uiso calc 0.575(11) A 1
H H91B 0.8523 0.0716 0.3609 0.240 Uiso calc 0.575(11) A 1
H H91C 0.8518 -0.0234 0.3234 0.240 Uiso calc 0.575(11) A 1
C C90A 0.947(2) 0.0640(15) 0.4257(12) 0.137(7) Uani d 0.425(11) A 2
H H90C 1.0165 0.0870 0.3777 0.165 Uiso calc 0.425(11) A 2
H H90D 0.9086 0.1220 0.4423 0.165 Uiso calc 0.425(11) A 2
C C91A 0.839(2) 0.007(2) 0.3926(16) 0.148(10) Uani d 0.425(11) A 2
H H91D 0.8385 0.0312 0.3282 0.222 Uiso calc 0.425(11) A 2
H H91E 0.7538 0.0189 0.4204 0.222 Uiso calc 0.425(11) A 2
H H91F 0.8577 -0.0630 0.4086 0.222 Uiso calc 0.425(11) A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br1 0.0286(2) 0.0377(3) 0.0273(2) -0.00738(19) -0.00101(17) -0.00807(18)
Ni1 0.0251(3) 0.0243(3) 0.0222(3) -0.0026(2) -0.0017(2) -0.0063(2)
P1 0.0242(5) 0.0253(6) 0.0216(5) -0.0008(4) -0.0014(4) -0.0067(4)
P2 0.0264(6) 0.0281(6) 0.0234(5) -0.0008(5) -0.0037(4) -0.0069(4)
O1 0.162(9) 0.186(11) 0.164(9) -0.059(8) -0.033(7) -0.069(8)
N1 0.0326(19) 0.0206(19) 0.0234(17) -0.0059(15) -0.0025(15) -0.0038(14)
N2 0.0331(19) 0.030(2) 0.0223(18) -0.0065(16) -0.0045(15) -0.0022(15)
C1 0.026(2) 0.023(2) 0.028(2) -0.0019(17) -0.0031(17) -0.0064(17)
C2 0.029(2) 0.022(2) 0.023(2) -0.0007(17) -0.0008(17) -0.0074(17)
C3 0.041(3) 0.030(3) 0.033(2) -0.008(2) -0.002(2) -0.0093(19)
C4 0.042(3) 0.038(3) 0.035(3) -0.016(2) 0.001(2) 0.002(2)
C5 0.044(3) 0.044(3) 0.026(2) -0.014(2) -0.004(2) -0.002(2)
C6 0.031(2) 0.034(3) 0.025(2) -0.0065(19) -0.0031(18) -0.0047(18)
C7 0.037(2) 0.024(2) 0.034(2) -0.0048(19) -0.0062(19) -0.0122(18)
C8 0.051(3) 0.048(3) 0.028(2) -0.023(2) -0.005(2) -0.002(2)
C9 0.024(2) 0.024(2) 0.030(2) 0.0020(18) -0.0071(18) -0.0061(17)
C10 0.047(3) 0.028(3) 0.028(2) 0.000(2) 0.000(2) -0.0096(19)
C11 0.058(3) 0.034(3) 0.058(3) -0.003(2) 0.001(3) -0.024(2)
C12 0.066(4) 0.023(3) 0.054(3) -0.001(2) 0.002(3) -0.007(2)
C13 0.048(3) 0.032(3) 0.036(3) -0.009(2) 0.005(2) -0.003(2)
C14 0.040(3) 0.031(3) 0.028(2) 0.000(2) 0.0013(19) -0.0058(19)
C15 0.026(2) 0.026(2) 0.034(2) -0.0015(18) -0.0012(18) -0.0091(18)
C16 0.030(2) 0.036(3) 0.038(2) 0.003(2) -0.0093(19) -0.015(2)
C17 0.041(3) 0.041(3) 0.055(3) 0.004(2) -0.024(2) -0.016(2)
C18 0.032(3) 0.033(3) 0.075(4) 0.001(2) -0.019(3) -0.017(3)
C19 0.024(2) 0.029(3) 0.083(4) -0.002(2) 0.009(3) -0.016(3)
C20 0.031(2) 0.027(3) 0.045(3) -0.0073(19) 0.005(2) -0.013(2)
C21 0.026(2) 0.029(2) 0.0167(19) -0.0020(17) 0.0009(16) -0.0055(16)
C22 0.032(2) 0.031(3) 0.032(2) -0.0019(19) -0.0039(19) -0.0108(19)
C23 0.029(2) 0.043(3) 0.031(2) 0.005(2) -0.0018(19) -0.010(2)
C24 0.041(3) 0.030(3) 0.032(2) 0.008(2) -0.002(2) -0.0066(19)
C25 0.056(3) 0.025(3) 0.032(2) -0.002(2) -0.004(2) -0.0128(19)
C26 0.036(2) 0.026(2) 0.034(2) -0.0061(19) -0.0006(19) -0.0085(19)
C27 0.030(2) 0.031(3) 0.030(2) 0.0007(19) -0.0017(18) -0.0133(19)
C28 0.036(3) 0.042(3) 0.038(3) 0.009(2) -0.010(2) -0.014(2)
C29 0.065(4) 0.045(4) 0.061(3) 0.022(3) -0.027(3) -0.018(3)
C30 0.086(4) 0.039(3) 0.062(4) 0.024(3) -0.025(3) -0.019(3)
C31 0.075(4) 0.033(3) 0.047(3) 0.003(3) -0.007(3) -0.020(2)
C32 0.042(3) 0.034(3) 0.031(2) 0.000(2) -0.007(2) -0.010(2)
C33 0.028(2) 0.038(3) 0.021(2) -0.0014(19) -0.0064(17) -0.0054(18)
C34 0.050(3) 0.034(3) 0.045(3) 0.005(2) -0.013(2) -0.014(2)
C35 0.056(3) 0.066(4) 0.051(3) 0.032(3) -0.021(3) -0.031(3)
C36 0.042(3) 0.084(5) 0.041(3) 0.032(3) -0.011(2) -0.020(3)
C37 0.030(3) 0.074(4) 0.054(3) -0.002(3) 0.000(2) -0.015(3)
C38 0.030(2) 0.044(3) 0.051(3) -0.002(2) 0.002(2) -0.012(2)
C39 0.034(2) 0.029(2) 0.027(2) -0.0078(19) -0.0058(18) -0.0089(18)
C40 0.038(3) 0.038(3) 0.033(2) -0.004(2) -0.003(2) -0.009(2)
C41 0.048(3) 0.048(3) 0.031(3) -0.010(2) 0.006(2) -0.008(2)
C42 0.069(4) 0.044(3) 0.026(2) -0.008(3) -0.006(2) -0.006(2)
C43 0.064(4) 0.046(3) 0.038(3) -0.005(3) -0.022(3) -0.006(2)
C44 0.042(3) 0.030(3) 0.032(2) 0.000(2) -0.005(2) -0.0039(19)
C90 0.098(11) 0.198(15) 0.151(11) -0.035(10) 0.000(9) -0.091(10)
C91 0.103(14) 0.223(19) 0.168(12) -0.059(15) -0.013(11) -0.072(12)
C90A 0.132(14) 0.178(14) 0.135(13) -0.014(11) -0.009(10) -0.098(10)
C91A 0.135(18) 0.16(2) 0.18(2) -0.005(15) -0.033(15) -0.091(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 Ni1 Br1 . . 101.36(9)
N2 Ni1 Br1 . . 95.61(10)
N2 Ni1 N1 . . 162.01(13)
C1 Ni1 Br1 . . 162.67(13)
C1 Ni1 N1 . . 82.51(15)
C1 Ni1 N2 . . 83.05(15)
N1 P1 C9 . . 114.88(18)
N1 P1 C15 . . 111.38(18)
N1 P1 C21 . . 111.90(18)
C9 P1 C15 . . 102.7(2)
C21 P1 C9 . . 108.06(18)
C21 P1 C15 . . 107.30(18)
N2 P2 C27 . . 116.16(19)
N2 P2 C33 . . 113.08(19)
N2 P2 C39 . . 109.66(18)
C33 P2 C27 . . 107.6(2)
C33 P2 C39 . . 104.91(19)
C39 P2 C27 . . 104.55(19)
C90 O1 C90 2_756 . 180.0
C90A O1 C90A . 2_756 180.0
P1 N1 Ni1 . . 134.54(19)
C7 N1 Ni1 . . 113.2(2)
C7 N1 P1 . . 110.6(2)
P2 N2 Ni1 . . 127.39(19)
C8 N2 Ni1 . . 115.0(3)
C8 N2 P2 . . 116.5(3)
C2 C1 Ni1 . . 120.1(3)
C2 C1 C6 . . 120.3(4)
C6 C1 Ni1 . . 119.6(3)
C1 C2 C7 . . 113.9(3)
C3 C2 C1 . . 120.2(4)
C3 C2 C7 . . 125.9(4)
C2 C3 H3 . . 120.2
C2 C3 C4 . . 119.6(4)
C4 C3 H3 . . 120.2
C3 C4 H4 . . 119.8
C3 C4 C5 . . 120.4(4)
C5 C4 H4 . . 119.8
C4 C5 H5 . . 120.1
C4 C5 C6 . . 119.7(4)
C6 C5 H5 . . 120.1
C1 C6 C5 . . 119.7(4)
C1 C6 C8 . . 114.5(4)
C5 C6 C8 . . 125.8(4)
N1 C7 C2 . . 107.2(3)
N1 C7 H7A . . 110.3
N1 C7 H7B . . 110.3
C2 C7 H7A . . 110.3
C2 C7 H7B . . 110.3
H7A C7 H7B . . 108.5
N2 C8 C6 . . 107.8(3)
N2 C8 H8A . . 110.1
N2 C8 H8B . . 110.1
C6 C8 H8A . . 110.1
C6 C8 H8B . . 110.1
H8A C8 H8B . . 108.5
P1 C9 H9 . . 111(2)
C10 C9 P1 . . 111.6(3)
C10 C9 H9 . . 104(2)
C14 C9 P1 . . 112.7(3)
C14 C9 H9 . . 106(2)
C14 C9 C10 . . 110.9(4)
C9 C10 H10A . . 109.5
C9 C10 H10B . . 109.5
H10A C10 H10B . . 108.1
C11 C10 C9 . . 110.5(3)
C11 C10 H10A . . 109.5
C11 C10 H10B . . 109.5
C10 C11 H11A . . 109.3
C10 C11 H11B . . 109.3
H11A C11 H11B . . 107.9
C12 C11 C10 . . 111.7(4)
C12 C11 H11A . . 109.3
C12 C11 H11B . . 109.3
C11 C12 H12A . . 109.5
C11 C12 H12B . . 109.5
C11 C12 C13 . . 110.9(4)
H12A C12 H12B . . 108.1
C13 C12 H12A . . 109.5
C13 C12 H12B . . 109.5
C12 C13 H13A . . 109.4
C12 C13 H13B . . 109.4
H13A C13 H13B . . 108.0
C14 C13 C12 . . 111.0(4)
C14 C13 H13A . . 109.4
C14 C13 H13B . . 109.4
C9 C14 H14A . . 109.5
C9 C14 H14B . . 109.5
C13 C14 C9 . . 110.8(3)
C13 C14 H14A . . 109.5
C13 C14 H14B . . 109.5
H14A C14 H14B . . 108.1
C16 C15 P1 . . 122.5(3)
C16 C15 C20 . . 119.3(4)
C20 C15 P1 . . 117.4(3)
C15 C16 H16 . . 119.7
C15 C16 C17 . . 120.6(4)
C17 C16 H16 . . 119.7
C16 C17 H17 . . 120.2
C18 C17 C16 . . 119.5(4)
C18 C17 H17 . . 120.2
C17 C18 H18 . . 119.5
C17 C18 C19 . . 121.0(5)
C19 C18 H18 . . 119.5
C18 C19 H19 . . 119.9
C18 C19 C20 . . 120.1(4)
C20 C19 H19 . . 119.9
C15 C20 C19 . . 119.4(4)
C15 C20 H20 . . 120.3
C19 C20 H20 . . 120.3
C22 C21 P1 . . 118.2(3)
C26 C21 P1 . . 122.5(3)
C26 C21 C22 . . 118.7(4)
C21 C22 H22 . . 119.9
C23 C22 C21 . . 120.3(4)
C23 C22 H22 . . 119.9
C22 C23 H23 . . 119.7
C24 C23 C22 . . 120.6(4)
C24 C23 H23 . . 119.7
C23 C24 H24 . . 120.1
C25 C24 C23 . . 119.9(4)
C25 C24 H24 . . 120.1
C24 C25 H25 . . 120.0
C24 C25 C26 . . 120.1(4)
C26 C25 H25 . . 120.0
C21 C26 C25 . . 120.5(4)
C21 C26 H26 . . 119.8
C25 C26 H26 . . 119.8
P2 C27 H27 . . 106.6
C28 C27 P2 . . 112.9(3)
C28 C27 H27 . . 106.6
C28 C27 C32 . . 109.6(3)
C32 C27 P2 . . 114.0(3)
C32 C27 H27 . . 106.6
C27 C28 H28A . . 109.6
C27 C28 H28B . . 109.6
H28A C28 H28B . . 108.2
C29 C28 C27 . . 110.1(4)
C29 C28 H28A . . 109.6
C29 C28 H28B . . 109.6
C28 C29 H29A . . 109.3
C28 C29 H29B . . 109.3
C28 C29 C30 . . 111.8(4)
H29A C29 H29B . . 107.9
C30 C29 H29A . . 109.3
C30 C29 H29B . . 109.3
C29 C30 H30A . . 109.3
C29 C30 H30B . . 109.3
H30A C30 H30B . . 107.9
C31 C30 C29 . . 111.7(4)
C31 C30 H30A . . 109.3
C31 C30 H30B . . 109.3
C30 C31 H31A . . 109.5
C30 C31 H31B . . 109.5
C30 C31 C32 . . 110.7(4)
H31A C31 H31B . . 108.1
C32 C31 H31A . . 109.5
C32 C31 H31B . . 109.5
C27 C32 H32A . . 109.3
C27 C32 H32B . . 109.3
C31 C32 C27 . . 111.6(4)
C31 C32 H32A . . 109.3
C31 C32 H32B . . 109.3
H32A C32 H32B . . 108.0
C34 C33 P2 . . 118.2(3)
C38 C33 P2 . . 123.6(4)
C38 C33 C34 . . 118.2(4)
C33 C34 H34 . . 119.2
C35 C34 C33 . . 121.6(5)
C35 C34 H34 . . 119.2
C34 C35 H35 . . 120.2
C36 C35 C34 . . 119.7(5)
C36 C35 H35 . . 120.2
C35 C36 H36 . . 120.0
C35 C36 C37 . . 120.0(5)
C37 C36 H36 . . 120.0
C36 C37 H37 . . 119.6
C36 C37 C38 . . 120.9(5)
C38 C37 H37 . . 119.6
C33 C38 C37 . . 119.7(5)
C33 C38 H38 . . 120.2
C37 C38 H38 . . 120.2
C40 C39 P2 . . 118.4(3)
C44 C39 P2 . . 122.5(3)
C44 C39 C40 . . 119.1(4)
C39 C40 H40 . . 119.8
C41 C40 C39 . . 120.4(4)
C41 C40 H40 . . 119.8
C40 C41 H41 . . 119.9
C42 C41 C40 . . 120.3(5)
C42 C41 H41 . . 119.9
C41 C42 H42 . . 120.3
C43 C42 C41 . . 119.4(4)
C43 C42 H42 . . 120.3
C42 C43 H43 . . 119.4
C42 C43 C44 . . 121.2(5)
C44 C43 H43 . . 119.4
C39 C44 C43 . . 119.7(4)
C39 C44 H44 . . 120.2
C43 C44 H44 . . 120.2
O1 C90 H90A . . 108.9
O1 C90 H90B . . 108.9
H90A C90 H90B . . 107.7
C91 C90 O1 . . 113.5(13)
C91 C90 H90A . . 108.9
C91 C90 H90B . . 108.9
C90 C91 H91A . . 109.5
C90 C91 H91B . . 109.5
C90 C91 H91C . . 109.5
H91A C91 H91B . . 109.5
H91A C91 H91C . . 109.5
H91B C91 H91C . . 109.5
O1 C90A H90C . . 109.9
O1 C90A H90D . . 109.9
O1 C90A C91A . . 109.1(15)
H90C C90A H90D . . 108.3
C91A C90A H90C . . 109.9
C91A C90A H90D . . 109.9
C90A C91A H91D . . 109.5
C90A C91A H91E . . 109.5
C90A C91A H91F . . 109.5
H91D C91A H91E . . 109.5
H91D C91A H91F . . 109.5
H91E C91A H91F . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Br1 Ni1 . 2.4344(7)
Ni1 N1 . 1.990(3)
Ni1 N2 . 1.964(3)
Ni1 C1 . 1.833(4)
P1 N1 . 1.616(3)
P1 C9 . 1.815(4)
P1 C15 . 1.823(4)
P1 C21 . 1.811(4)
P2 N2 . 1.607(3)
P2 C27 . 1.834(4)
P2 C33 . 1.808(4)
P2 C39 . 1.826(4)
O1 C90 . 1.482(12)
O1 C90 2_756 1.482(12)
O1 C90A . 1.392(16)
O1 C90A 2_756 1.392(16)
N1 C7 . 1.495(5)
N2 C8 . 1.484(5)
C1 C2 . 1.387(5)
C1 C6 . 1.388(5)
C2 C3 . 1.385(5)
C2 C7 . 1.498(5)
C3 H3 . 0.9300
C3 C4 . 1.390(6)
C4 H4 . 0.9300
C4 C5 . 1.390(6)
C5 H5 . 0.9300
C5 C6 . 1.393(6)
C6 C8 . 1.485(6)
C7 H7A . 0.9700
C7 H7B . 0.9700
C8 H8A . 0.9700
C8 H8B . 0.9700
C9 H9 . 0.85(3)
C9 C10 . 1.537(5)
C9 C14 . 1.530(5)
C10 H10A . 0.9700
C10 H10B . 0.9700
C10 C11 . 1.527(6)
C11 H11A . 0.9700
C11 H11B . 0.9700
C11 C12 . 1.513(7)
C12 H12A . 0.9700
C12 H12B . 0.9700
C12 C13 . 1.521(6)
C13 H13A . 0.9700
C13 H13B . 0.9700
C13 C14 . 1.521(6)
C14 H14A . 0.9700
C14 H14B . 0.9700
C15 C16 . 1.387(5)
C15 C20 . 1.393(5)
C16 H16 . 0.9300
C16 C17 . 1.396(6)
C17 H17 . 0.9300
C17 C18 . 1.363(6)
C18 H18 . 0.9300
C18 C19 . 1.372(7)
C19 H19 . 0.9300
C19 C20 . 1.400(6)
C20 H20 . 0.9300
C21 C22 . 1.399(5)
C21 C26 . 1.389(5)
C22 H22 . 0.9300
C22 C23 . 1.386(5)
C23 H23 . 0.9300
C23 C24 . 1.378(6)
C24 H24 . 0.9300
C24 C25 . 1.377(6)
C25 H25 . 0.9300
C25 C26 . 1.397(6)
C26 H26 . 0.9300
C27 H27 . 0.9800
C27 C28 . 1.531(6)
C27 C32 . 1.537(5)
C28 H28A . 0.9700
C28 H28B . 0.9700
C28 C29 . 1.523(7)
C29 H29A . 0.9700
C29 H29B . 0.9700
C29 C30 . 1.526(6)
C30 H30A . 0.9700
C30 H30B . 0.9700
C30 C31 . 1.512(7)
C31 H31A . 0.9700
C31 H31B . 0.9700
C31 C32 . 1.523(6)
C32 H32A . 0.9700
C32 H32B . 0.9700
C33 C34 . 1.392(6)
C33 C38 . 1.389(6)
C34 H34 . 0.9300
C34 C35 . 1.384(6)
C35 H35 . 0.9300
C35 C36 . 1.366(7)
C36 H36 . 0.9300
C36 C37 . 1.371(8)
C37 H37 . 0.9300
C37 C38 . 1.397(6)
C38 H38 . 0.9300
C39 C40 . 1.392(6)
C39 C44 . 1.386(6)
C40 H40 . 0.9300
C40 C41 . 1.388(6)
C41 H41 . 0.9300
C41 C42 . 1.379(7)
C42 H42 . 0.9300
C42 C43 . 1.371(7)
C43 H43 . 0.9300
C43 C44 . 1.391(6)
C44 H44 . 0.9300
C90 H90A . 0.9700
C90 H90B . 0.9700
C90 C91 . 1.482(16)
C91 H91A . 0.9600
C91 H91B . 0.9600
C91 H91C . 0.9600
C90A H90C . 0.9700
C90A H90D . 0.9700
C90A C91A . 1.544(17)
C91A H91D . 0.9600
C91A H91E . 0.9600
C91A H91F . 0.9600
_cod_database_fobs_code 2021766