#------------------------------------------------------------------------------
#$Date: 2019-09-08 06:42:15 +0300 (Sun, 08 Sep 2019) $
#$Revision: 218078 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021765.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_2021765
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 H37 N2 P2)], 0.5C2 H2 Cl2'
_chemical_formula_moiety 'C44 H37 Br N2 Ni P2, C0.5 H Cl'
_chemical_formula_sum 'C44.5 H38 Br Cl N2 Ni P2'
_chemical_formula_weight 836.78
_chemical_name_systematic
;(2,6-Bis{[(triphenyl-\l^5^-phosphanylidene)imino]methyl}phenyl-\k^3^N,C^1^,N')bromidonickel(II)
dichlorometahne hemisolvate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_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 90
_cell_angle_beta 97.421(5)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 28.319(13)
_cell_length_b 11.655(5)
_cell_length_c 23.593(10)
_cell_measurement_reflns_used 8496
_cell_measurement_temperature 170
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 1.7
_cell_volume 7722(6)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2009)
;
_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 170
_diffrn_detector 'Rigaku XtaLAB area detector'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Rigaku Mini template'
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_radiation_monochromator 'Graphite Monochromator'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0842
_diffrn_reflns_av_unetI/netI 0.0745
_diffrn_reflns_limit_h_max 36
_diffrn_reflns_limit_h_min -36
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 40203
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 27.510
_diffrn_reflns_theta_min 1.892
_diffrn_source 'Sealed Tube'
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 1.724
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.671
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(REQAB; Rigaku, 1998)
;
_exptl_crystal_colour 'clear reddish orange'
_exptl_crystal_density_diffrn 1.440
_exptl_crystal_density_method "'not measured"
_exptl_crystal_description block
_exptl_crystal_F_000 3432
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.37
_exptl_crystal_size_min 0.18
_refine_diff_density_max 0.438
_refine_diff_density_min -0.667
_refine_ls_extinction_coef 0.00011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.070
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 466
_refine_ls_number_reflns 8846
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.070
_refine_ls_R_factor_all 0.0836
_refine_ls_R_factor_gt 0.0529
_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^)+(0.0234P)^2^+15.3313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0964
_refine_ls_wR_factor_ref 0.1114
_reflns_number_gt 6363
_reflns_number_total 8846
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jx3045sup1.cif
_cod_data_source_block x634
_cod_original_formula_sum 'C44.50 H38 Br Cl N2 Ni P2'
_cod_database_code 2021765
_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_estimated_absorpt_t_min 0.560
_shelx_estimated_absorpt_t_max 0.747
_shelx_hkl_file
;
0 0 2 0.23 1.45
0 0 -3 1.34 0.70
0 0 3 -0.76 1.39
0 0 -3 1.51 0.70
0 0 4 612.34 27.78
0 0 -4 618.26 26.80
0 0 -4 553.92 24.01
0 0 5 8.60 3.49
0 0 -5 2.56 1.86
0 0 -5 5.11 1.92
0 0 6 -5.99 3.25
0 0 -6 1.69 1.63
0 0 -6 -0.29 2.03
0 0 7 11.16 4.07
0 0 -7 -1.80 1.92
0 0 -7 -1.16 1.98
0 0 8 217.62 23.37
0 0 -8 200.88 8.78
0 0 -8 190.76 8.60
0 0 9 -1.69 3.66
0 0 -9 0.81 0.76
0 0 -9 2.03 1.34
0 0 10 355.95 28.66
0 0 -10 302.07 18.83
0 0 -10 292.25 18.89
0 0 -11 5.17 1.28
0 0 -11 -2.50 3.14
0 0 12 110.44 20.87
0 0 -12 128.40 22.26
0 0 -12 140.60 23.95
0 0 13 25.11 11.86
0 0 -13 2.32 1.45
0 0 -13 3.49 1.69
0 0 14 1405.20 68.18
0 0 -14 1461.70 69.92
0 0 -14 1535.40 74.69
0 0 15 20.52 7.44
0 0 -15 9.42 3.55
0 0 -15 8.83 4.30
0 0 16 1308.25 62.08
0 0 -16 1433.10 65.74
0 0 -16 1532.32 70.56
0 0 17 11.04 8.43
0 0 -17 9.18 6.74
0 0 -17 3.84 3.89
0 0 18 396.87 44.58
0 0 -18 451.27 32.67
0 0 -18 470.69 34.47
0 0 19 4.71 4.24
0 0 -19 -4.82 3.08
0 0 -19 -11.45 4.07
0 0 20 15.52 11.04
0 0 -20 40.34 10.81
0 0 -20 53.53 14.36
0 0 21 -5.93 7.90
0 0 -21 9.94 5.11
0 0 -21 -3.49 4.13
0 0 22 20.40 10.99
0 0 -22 -2.96 2.96
0 0 -22 14.01 7.03
0 0 23 -1.80 4.88
0 0 -23 3.95 3.72
0 0 -23 8.02 6.10
0 0 24 47.08 16.62
0 0 -24 53.47 13.95
0 0 -24 29.70 4.42
0 0 25 2.85 4.71
0 0 -25 12.44 8.83
0 0 -25 5.64 4.65
0 0 26 143.68 22.44
0 0 -26 124.04 20.81
0 0 -26 132.52 24.59
0 0 27 0.52 7.03
0 0 -27 6.80 5.87
0 0 28 74.22 26.21
0 0 29 -10.17 9.18
0 0 30 20.92 13.54
0 -2 0 406.17 24.47
0 2 0 416.69 24.99
0 -2 -1 257.61 15.64
0 2 1 279.87 16.68
0 -2 1 286.38 17.73
0 -2 -1 276.55 20.98
0 2 -1 282.95 17.09
0 2 1 268.07 16.45
0 2 -2 38.42 4.88
0 -2 -2 38.77 4.94
0 -2 2 41.27 5.23
0 2 2 38.59 4.36
0 -2 2 50.34 6.57
0 -2 -2 50.74 6.51
0 2 -2 38.59 5.64
0 2 2 48.36 6.28
0 -2 3 630.59 27.09
0 2 3 635.53 27.49
0 -2 -3 621.00 27.03
0 2 -3 660.40 28.66
0 2 -3 654.30 28.19
0 2 3 667.44 11.33
0 -2 4 3.20 1.74
0 2 4 10.58 3.78
0 -2 -4 8.08 3.20
0 2 -4 1.34 1.45
0 2 -4 9.88 3.43
0 2 4 7.61 2.62
0 -2 5 837.51 30.86
0 2 5 861.28 31.85
0 -2 -5 865.81 31.62
0 2 -5 896.50 32.78
0 2 -5 832.45 30.34
0 2 5 901.97 32.84
0 -2 6 2161.80 53.94
0 2 6 2138.32 53.65
0 -2 -6 2179.41 66.09
0 2 -6 2176.39 53.71
0 2 -6 2131.00 52.25
0 2 6 2249.22 55.16
0 -2 7 378.15 24.18
0 2 7 396.00 28.54
0 -2 -7 390.36 24.41
0 2 -7 444.65 6.80
0 2 -7 389.84 24.24
0 2 7 405.30 24.59
0 -2 8 1.45 3.60
0 2 8 4.94 2.67
0 -2 -8 0.87 1.05
0 2 -8 -0.58 2.27
0 2 -8 4.18 1.45
0 2 8 3.08 2.03
0 -2 9 1417.93 13.89
0 2 9 1458.79 38.13
0 -2 -9 1463.44 36.97
0 -2 -9 1391.66 12.26
0 2 -9 1494.95 57.54
0 -2 10 688.30 52.54
0 2 10 683.48 52.54
0 -2 -10 655.87 49.81
0 2 -10 722.60 396.29
0 -2 -10 665.29 51.09
0 2 -10 674.64 52.08
0 -2 11 436.74 48.18
0 2 11 366.99 45.69
0 -2 -11 362.64 30.28
0 2 -11 358.62 28.89
0 -2 -11 386.76 31.45
0 2 -11 342.35 50.16
0 -2 12 1878.80 86.84
0 2 12 1908.38 92.01
0 -2 -12 1941.40 89.10
0 2 -12 1859.38 85.56
0 -2 -12 2012.71 93.17
0 2 -12 1927.45 90.09
0 -2 13 95.79 13.95
0 2 13 98.23 14.24
0 -2 -13 98.93 15.69
0 2 -13 97.94 17.38
0 -2 -13 118.98 21.22
0 2 -13 89.05 17.03
0 -2 14 639.36 33.19
0 2 14 614.14 37.72
0 -2 -14 644.48 32.03
0 2 -14 629.83 31.50
0 -2 -14 625.36 32.55
0 2 -14 634.31 37.32
0 -2 15 114.85 18.83
0 2 15 100.44 15.40
0 -2 -15 111.25 16.10
0 2 -15 96.37 16.33
0 -2 -15 133.80 18.08
0 -2 16 192.45 19.06
0 2 16 216.22 18.02
0 -2 -16 210.76 22.61
0 2 -16 212.38 22.03
0 -2 -16 211.45 20.05
0 2 -16 183.50 21.74
0 -2 17 105.79 15.87
0 2 17 88.23 12.09
0 -2 -17 94.45 17.55
0 2 -17 98.29 13.83
0 -2 -17 93.58 13.08
0 2 -17 78.99 10.69
0 -2 18 105.38 20.11
0 2 18 161.70 27.55
0 -2 -18 87.48 17.38
0 2 -18 81.90 14.76
0 -2 -18 172.34 27.78
0 2 -18 78.58 16.68
0 -2 19 430.76 51.27
0 2 19 458.19 47.08
0 -2 -19 446.16 27.26
0 2 -19 443.14 33.42
0 -2 -19 468.94 35.63
0 2 -19 520.67 32.38
0 -2 20 10.64 7.21
0 2 20 2.27 6.22
0 -2 -20 10.58 4.94
0 2 -20 -1.98 2.44
0 -2 -20 -2.44 3.78
0 2 -20 5.99 1.86
0 -2 21 155.95 33.25
0 2 21 158.50 33.65
0 -2 -21 147.52 27.20
0 2 -21 146.76 28.02
0 -2 -21 168.33 29.24
0 2 -21 138.68 25.81
0 -2 22 75.74 17.26
0 2 22 59.81 20.63
0 -2 -22 72.71 16.10
0 2 -22 63.36 20.75
0 -2 -22 61.73 19.01
0 2 -22 63.01 21.45
0 -2 23 99.16 21.80
0 2 23 79.51 18.19
0 -2 -23 80.62 19.18
0 2 -23 85.50 19.30
0 -2 -23 73.00 17.38
0 2 -23 88.41 17.79
0 2 24 22.44 7.21
0 -2 24 9.53 8.31
0 -2 -24 12.67 7.21
0 2 -24 5.93 6.74
0 -2 -24 0.70 5.00
0 2 -24 11.39 6.68
0 2 25 42.14 15.81
0 -2 25 40.22 14.94
0 -2 -25 31.39 11.28
0 2 -25 39.93 14.59
0 -2 -25 35.75 12.73
0 2 -25 37.72 14.12
0 2 26 12.21 9.53
0 -2 26 24.64 13.89
0 -2 -26 9.24 6.80
0 2 -26 11.97 8.78
0 -2 -26 11.51 8.54
0 2 -26 10.00 8.25
0 -2 27 22.49 11.62
0 2 27 15.87 10.40
0 2 -27 1.86 3.20
0 -2 -27 7.03 5.93
0 2 -27 -6.34 4.24
0 -2 28 37.32 15.46
0 2 28 79.11 27.78
0 -2 29 21.33 15.34
0 2 29 28.25 15.34
0 -2 30 103.75 29.12
0 2 30 109.16 29.64
0 -4 0 63.24 9.76
0 4 0 69.75 8.95
0 -4 1 262.20 25.75
0 -4 -1 232.67 7.27
0 4 -1 231.33 5.29
0 4 1 241.04 16.10
0 4 2 34.93 4.13
0 -4 2 36.85 3.25
0 -4 2 40.51 6.22
0 -4 -2 35.51 5.87
0 4 -2 45.57 6.57
0 4 2 42.37 6.16
0 -4 3 2052.18 49.75
0 4 3 2058.46 50.22
0 -4 3 1918.50 48.07
0 -4 -3 2036.37 50.74
0 4 -3 2063.17 51.15
0 4 3 1979.82 54.11
0 -4 4 301.14 18.31
0 4 4 304.28 19.41
0 -4 4 320.67 21.39
0 -4 -4 300.73 24.12
0 4 -4 279.34 17.67
0 -4 5 1040.88 38.77
0 4 5 1037.92 40.16
0 -4 5 1046.29 38.94
0 -4 -5 1009.38 39.58
0 4 -5 1029.32 38.13
0 4 5 1076.45 39.52
0 -4 6 4.48 2.21
0 4 6 7.90 2.73
0 -4 -6 4.59 1.92
0 4 -6 5.70 2.32
0 4 -6 7.38 2.91
0 4 6 8.14 2.96
0 -4 7 2352.16 107.06
0 4 7 2432.25 117.00
0 -4 -7 2396.22 110.44
0 4 -7 2340.65 106.95
0 4 -7 2399.41 109.51
0 4 7 2481.95 113.05
0 -4 8 291.32 30.57
0 4 8 347.99 36.73
0 -4 -8 383.62 42.55
0 4 -8 272.14 22.44
0 4 -8 292.25 34.64
0 4 8 280.85 22.84
0 -4 9 320.96 38.77
0 4 9 292.83 34.29
0 4 -9 292.77 26.62
0 4 -9 314.80 25.46
0 4 9 324.39 26.21
0 -4 10 94.57 17.32
0 4 10 119.62 18.31
0 -4 -10 90.62 51.09
0 4 -10 103.46 17.84
0 4 -10 117.58 20.87
0 4 10 100.90 17.79
0 -4 11 731.14 36.04
0 4 11 758.98 39.52
0 -4 -11 820.54 40.34
0 4 -11 754.91 37.14
0 4 -11 759.04 37.78
0 4 11 726.08 36.44
0 -4 12 101.77 14.12
0 4 12 130.49 101.72
0 -4 -12 123.46 96.37
0 4 -12 102.12 15.46
0 4 -12 123.40 96.31
0 4 12 104.68 14.82
0 -4 13 32.08 7.44
0 4 13 44.12 9.82
0 -4 -13 45.39 9.24
0 4 -13 50.16 10.69
0 4 -13 28.36 11.16
0 4 13 36.73 7.15
0 -4 14 165.94 16.39
0 4 14 191.23 24.41
0 -4 -14 158.74 17.79
0 4 -14 174.72 17.55
0 -4 -14 148.86 19.65
0 4 -14 166.82 15.64
0 -4 15 8.20 7.61
0 4 15 6.22 5.29
0 -4 -15 5.23 3.78
0 4 -15 -4.71 3.95
0 -4 -15 17.50 7.44
0 4 -15 7.61 5.23
0 -4 16 18.08 7.73
0 4 16 31.39 14.59
0 -4 -16 17.26 7.03
0 4 -16 8.66 5.99
0 -4 -16 18.02 6.92
0 4 -16 27.61 10.99
0 -4 17 50.92 17.73
0 4 17 1.39 3.02
0 -4 -17 11.39 3.49
0 4 -17 13.66 2.91
0 -4 -17 -6.16 4.59
0 4 -17 6.28 3.25
0 -4 18 261.27 240.98
0 4 18 312.76 31.10
0 -4 -18 250.86 39.47
0 4 -18 226.86 32.32
0 -4 -18 257.61 26.39
0 4 -18 238.95 34.12
0 -4 19 278.24 36.73
0 4 19 254.00 36.27
0 -4 -19 303.58 29.76
0 4 -19 286.43 39.52
0 -4 -19 285.21 35.40
0 4 -19 259.70 43.42
0 -4 20 60.45 19.82
0 -4 -20 35.16 13.66
0 4 -20 42.31 17.09
0 -4 -20 69.52 22.20
0 4 -20 57.43 19.12
0 -4 21 249.58 43.94
0 4 21 265.16 33.13
0 -4 -21 225.46 35.16
0 4 -21 237.32 36.68
0 -4 -21 240.63 32.67
0 4 -21 244.18 32.32
0 -4 22 -2.09 6.92
0 4 22 -1.34 4.42
0 -4 -22 -4.24 4.48
0 4 -22 -8.66 4.94
0 -4 -22 -4.01 4.82
0 4 -22 -7.56 5.46
0 -4 23 131.53 28.13
0 4 23 126.59 28.19
0 -4 -23 121.83 28.36
0 4 -23 111.48 25.05
0 -4 -23 157.11 17.38
0 4 -23 108.87 26.21
0 -4 24 -7.79 6.74
0 4 24 12.50 8.49
0 -4 -24 8.37 6.68
0 4 -24 1.05 2.96
0 -4 -24 1.74 2.79
0 4 -24 -3.31 4.71
0 -4 25 54.81 19.70
0 4 25 35.46 17.61
0 -4 -25 6.57 5.70
0 4 -25 11.10 8.49
0 -4 -25 34.29 14.18
0 4 -25 6.57 5.87
0 -4 26 8.20 7.03
0 4 26 1.22 6.45
0 4 -26 9.01 7.56
0 -4 -26 2.79 3.49
0 4 -26 6.68 5.75
0 -4 27 14.47 13.48
0 4 27 11.68 9.88
0 4 -27 10.06 8.66
0 -4 -27 6.80 5.64
0 4 -27 2.67 5.06
0 -4 28 -5.41 8.66
0 4 28 15.64 16.33
0 4 29 12.73 11.51
0 -4 29 9.07 5.41
0 -6 0 3.49 8.78
0 6 0 -4.42 3.25
0 -6 1 232.50 38.71
0 -6 -1 251.97 40.69
0 6 -1 260.40 21.16
0 6 1 237.49 30.98
0 6 2 1.10 0.52
0 -6 2 -9.88 14.59
0 -6 -2 -2.56 13.89
0 6 -2 -4.36 3.08
0 6 2 4.77 1.92
0 6 3 13.95 6.28
0 -6 3 21.39 17.09
0 -6 -3 -4.42 17.09
0 6 -3 18.08 8.37
0 6 3 15.46 7.27
0 6 4 219.53 20.05
0 -6 4 202.79 26.62
0 -6 4 155.60 31.27
0 -6 -4 186.46 35.98
0 6 -4 223.89 25.57
0 6 4 226.74 27.43
0 -6 5 13.37 6.04
0 6 5 11.62 5.29
0 -6 5 48.42 14.53
0 -6 -5 39.87 12.26
0 6 -5 15.00 7.09
0 6 5 8.54 4.48
0 -6 6 22.44 7.44
0 6 6 17.67 5.93
0 -6 -6 49.11 16.04
0 6 -6 18.31 6.34
0 6 6 10.11 4.07
0 -6 7 220.75 13.60
0 6 7 267.78 23.42
0 -6 7 205.87 33.42
0 -6 -7 221.86 29.64
0 6 -7 238.95 29.47
0 6 7 230.69 25.05
0 -6 8 584.67 28.71
0 6 8 537.07 44.35
0 -6 8 556.25 429.94
0 -6 -8 545.67 42.37
0 6 -8 530.32 40.98
0 6 8 506.14 39.12
0 -6 9 538.17 41.21
0 6 9 485.45 40.34
0 -6 9 431.74 36.33
0 -6 -9 452.49 35.34
0 6 -9 485.57 45.63
0 6 9 463.48 36.27
0 -6 10 237.55 7.27
0 6 10 261.38 29.00
0 -6 10 268.77 36.56
0 -6 -10 260.74 28.42
0 6 -10 254.12 32.96
0 6 10 257.78 28.71
0 -6 11 419.89 32.20
0 6 11 507.54 33.19
0 -6 11 436.74 33.48
0 -6 -11 403.09 36.50
0 6 -11 447.79 34.35
0 6 11 407.10 47.14
0 -6 12 119.27 15.98
0 6 12 112.06 15.87
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-33 -3 -8 11.45 10.58
-33 3 -8 -1.10 6.68
-33 -5 12 24.99 15.05
-33 5 12 2.79 5.00
33 -5 -12 1.28 3.08
33 5 -12 -3.43 5.41
-33 -5 11 29.82 18.60
-33 5 11 -9.82 7.96
33 -5 -11 6.45 7.85
33 5 -11 -11.33 5.70
-33 -5 10 17.26 11.51
-33 5 10 9.30 3.55
33 -5 -10 2.67 6.28
33 5 -10 10.17 9.18
-33 -5 9 7.85 7.90
-33 5 9 -2.96 7.03
33 -5 -9 -17.96 7.73
33 5 -9 8.95 8.95
-33 -5 8 12.21 8.95
-33 5 8 -0.29 4.77
33 -5 -8 0.58 5.06
33 5 -8 7.32 7.27
-33 -5 7 -4.42 7.03
-33 5 7 8.49 8.20
33 -5 -7 4.24 5.99
33 5 -7 9.65 7.50
-33 -5 6 33.01 17.44
-33 5 6 -10.75 6.57
33 -5 -6 -9.01 6.97
33 5 -6 2.03 3.20
-33 -5 5 3.25 6.63
-33 5 5 -10.11 6.63
33 -5 -5 -7.67 6.92
-33 5 4 9.65 8.08
33 5 -4 24.06 12.79
33 -5 -4 40.11 19.99
-33 5 3 16.80 9.94
33 5 -3 10.11 8.72
33 -5 -3 -10.29 5.70
-33 5 2 14.36 10.11
33 5 -2 12.67 9.47
33 -5 -2 10.64 9.07
33 5 -1 54.52 22.32
33 -5 -1 49.06 19.94
-33 -5 1 40.63 21.68
-33 5 1 52.08 21.51
33 5 0 13.48 9.82
33 -5 0 3.02 5.52
-33 -5 0 -8.78 6.92
-33 5 0 8.14 7.96
33 5 1 31.74 15.58
33 -5 1 37.14 18.83
-33 -5 -1 38.54 19.76
-33 5 -1 34.64 17.26
33 5 2 -0.12 7.03
33 -5 2 13.95 10.29
-33 -5 -2 16.16 11.28
-33 5 -2 17.90 11.39
33 5 3 17.15 11.04
33 -5 3 5.70 6.16
-33 -5 -3 6.92 7.44
-33 5 -3 24.35 14.59
33 5 4 26.04 15.52
33 -5 4 15.75 10.81
-33 -5 -4 23.31 15.11
-33 5 -4 9.42 3.60
33 5 5 -19.24 6.63
33 -5 5 -0.87 5.81
-33 -5 -5 -1.69 4.48
-33 5 -5 -9.71 6.10
-34 0 15 7.03 7.21
34 0 -15 2.62 5.58
-34 0 14 41.44 18.08
34 0 -14 14.18 9.36
-34 0 13 5.17 6.45
34 0 -13 0.93 4.18
-34 0 12 85.56 20.98
34 0 -12 61.90 56.79
-34 0 11 12.67 9.42
34 0 -11 8.78 8.14
-34 0 10 14.94 10.69
34 0 -10 6.68 6.68
-34 0 9 12.55 10.40
34 0 -9 -0.81 5.81
-34 0 8 47.84 20.87
34 0 -8 24.94 12.44
-34 0 7 19.99 11.39
34 0 -7 16.27 8.20
-34 0 6 189.25 36.27
34 0 -6 177.05 38.54
-34 0 5 7.38 6.57
34 0 -5 -0.76 4.24
34 0 -4 36.56 15.23
34 0 -3 3.14 4.48
34 0 -2 56.26 19.59
34 0 -1 -1.16 6.97
-34 0 1 1.86 3.14
34 0 0 41.67 21.33
-34 0 0 35.98 18.19
34 0 1 25.23 12.44
-34 0 -1 -12.55 5.29
34 0 2 -2.44 6.28
-34 0 -2 2.62 5.23
34 0 3 -12.50 6.34
-34 0 -3 -1.86 6.10
34 0 4 -0.12 6.34
-34 0 -4 -0.81 6.68
34 0 5 12.96 9.65
-34 0 -5 -12.55 7.38
34 0 6 49.64 20.69
-34 0 -6 38.65 18.13
34 0 7 -21.97 6.63
-34 0 -7 12.73 10.81
-34 -2 14 17.20 11.97
-34 2 14 19.36 12.61
34 -2 -14 29.59 15.98
34 2 -14 28.66 14.82
-34 -2 13 41.91 17.96
-34 2 13 93.93 26.62
34 -2 -13 104.27 28.25
34 2 -13 108.81 29.00
-34 -2 12 13.25 10.93
-34 2 12 6.68 6.68
34 -2 -12 -6.86 4.94
34 2 -12 7.03 6.63
-34 -2 11 11.45 9.07
-34 2 11 39.76 19.99
34 -2 -11 22.15 11.80
34 2 -11 15.29 11.22
-34 -2 10 18.83 11.80
-34 2 10 13.48 10.11
34 -2 -10 -2.38 7.15
34 2 -10 10.46 9.71
-34 -2 9 25.34 12.73
-34 2 9 37.37 19.18
34 -2 -9 28.13 14.59
34 2 -9 15.98 11.04
-34 -2 8 23.37 11.39
-34 2 8 10.75 9.18
34 -2 -8 27.03 14.07
34 2 -8 25.23 12.73
-34 -2 7 26.74 12.50
-34 2 7 24.47 11.62
34 -2 -7 10.87 8.89
34 2 -7 7.61 7.21
-34 -2 6 66.09 27.84
-34 2 6 67.77 28.31
34 -2 -6 52.08 21.91
34 2 -6 39.47 19.88
-34 2 5 -4.07 6.68
34 -2 -5 6.51 6.86
34 2 -4 24.18 14.18
34 -2 -4 22.38 7.85
34 2 -3 -0.87 7.15
34 -2 -3 4.18 6.63
34 2 -2 18.72 13.25
34 -2 -2 15.52 12.50
34 2 -1 11.62 10.00
34 -2 -1 20.34 12.96
-34 -2 1 24.99 13.19
34 2 0 19.36 12.15
34 -2 0 15.00 11.16
-34 -2 0 11.45 9.47
-34 2 0 7.09 6.97
34 2 1 51.79 20.87
34 -2 1 57.31 23.89
-34 -2 -1 52.08 22.73
-34 2 -1 45.69 24.41
34 2 2 20.87 13.14
34 -2 2 9.01 7.44
-34 -2 -2 20.81 14.12
-34 2 -2 18.95 13.60
34 2 3 65.10 18.48
34 -2 3 58.12 24.47
-34 -2 -3 55.51 24.41
-34 2 -3 39.93 20.98
34 2 4 12.26 9.07
34 -2 4 19.47 12.15
-34 -2 -4 50.39 21.10
-34 2 -4 24.53 12.73
34 2 5 24.06 15.64
34 -2 5 24.24 14.41
-34 -2 -5 21.16 13.72
-34 2 -5 12.21 10.93
34 2 6 4.94 6.28
34 -2 6 13.48 11.39
-34 -2 -6 -0.41 4.94
-34 2 -6 -2.73 7.03
34 2 7 8.20 6.63
34 -2 7 -2.96 6.16
-34 2 -7 23.37 14.24
-34 -4 12 19.06 12.03
-34 4 12 7.03 8.72
-34 -4 11 44.17 19.12
-34 4 11 50.04 21.22
34 -4 -11 44.29 19.94
34 4 -11 47.02 19.70
-34 -4 10 4.71 6.16
-34 4 10 2.32 7.09
34 -4 -10 2.91 5.87
34 4 -10 0.29 2.44
-34 -4 9 72.71 19.01
-34 4 9 94.51 26.04
34 -4 -9 86.20 24.41
34 4 -9 52.20 22.84
-34 -4 8 29.53 15.05
-34 4 8 24.30 13.72
34 -4 -8 4.82 5.64
34 4 -8 25.81 13.83
-34 -4 7 87.42 20.11
-34 4 7 46.62 19.76
34 -4 -7 69.98 19.24
34 4 -7 45.63 19.59
-34 -4 6 5.52 7.15
-34 4 6 4.71 6.34
34 -4 -6 2.44 3.14
-34 -4 5 -5.81 6.57
-34 4 5 21.45 20.69
34 -4 -5 14.01 10.81
-34 4 4 8.66 9.36
34 4 -4 21.27 13.08
34 -4 -4 16.97 10.11
-34 4 3 -15.75 7.61
34 4 -3 -0.52 6.68
34 4 -2 15.40 11.57
34 -4 -2 29.47 16.27
34 4 -1 39.00 20.52
34 -4 -1 75.21 17.90
34 4 0 6.97 7.61
34 -4 0 0.58 4.71
-34 -4 0 -9.76 6.45
-34 4 0 -5.23 4.82
34 4 1 54.40 22.49
34 -4 1 29.53 15.00
-34 -4 -1 44.00 19.82
-34 4 -1 54.69 22.55
34 4 2 18.02 12.03
34 -4 2 -3.55 3.72
-34 -4 -2 13.83 5.64
-34 4 -2 20.87 12.50
34 4 3 42.95 18.43
34 -4 3 38.94 17.20
-34 -4 -3 39.35 16.97
-34 4 -3 44.06 19.24
34 4 4 6.10 6.45
34 -4 4 0.52 7.09
-34 -4 -4 -6.39 7.27
-34 4 -4 -4.82 5.70
-35 -1 12 42.84 18.31
-35 1 12 25.69 15.52
35 -1 -12 31.21 16.16
35 1 -12 16.51 12.15
-35 -1 11 16.39 11.51
-35 1 11 -11.92 8.14
35 -1 -11 -14.07 7.09
35 1 -11 -1.98 5.81
-35 -1 10 33.13 18.43
-35 1 10 40.86 18.31
35 -1 -10 8.25 3.25
35 1 -10 1.51 3.49
-35 -1 9 4.24 6.74
-35 1 9 22.32 12.67
35 -1 -9 12.90 9.36
35 1 -9 1.51 2.85
-35 -1 8 -3.55 7.90
-35 1 8 15.40 10.99
35 -1 -8 9.76 8.66
35 1 -8 -3.60 4.77
-35 -1 7 36.73 19.53
-35 1 7 20.52 13.37
35 -1 -7 4.01 4.71
35 1 -7 3.08 6.04
-35 -1 6 21.85 14.18
-35 1 6 16.74 10.69
35 -1 -6 -5.93 4.77
-35 -1 5 24.01 13.02
-35 1 5 -3.78 7.50
35 1 -4 4.88 6.10
35 -1 -4 8.60 8.72
35 1 -3 15.52 11.33
35 -1 -3 19.18 11.68
35 1 -2 31.91 16.45
35 -1 -2 28.54 15.52
35 1 -1 23.77 13.25
35 -1 -1 9.71 10.29
35 1 0 14.53 11.10
35 -1 0 -5.46 5.52
35 1 1 6.45 6.92
35 -1 1 -2.91 6.97
-35 -1 -1 7.56 7.38
-35 1 -1 10.69 9.01
35 1 2 11.92 8.43
35 -1 2 5.17 7.85
-35 -1 -2 -4.13 5.81
-35 1 -2 7.03 7.67
35 1 3 6.16 7.32
35 -1 3 3.37 4.88
-35 -1 -3 -2.44 5.93
-35 1 -3 0.81 3.66
35 1 4 -0.06 7.21
35 -1 4 5.17 3.66
-35 -1 -4 16.39 11.28
-35 1 -4 3.84 5.58
35 1 5 30.69 15.75
35 -1 5 -4.30 7.61
-35 -1 -5 1.80 5.00
-35 1 -5 -3.66 6.28
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-35 3 10 32.72 16.33
35 -3 -10 0.99 5.29
35 3 -10 5.29 6.34
-35 -3 9 31.33 16.45
-35 3 9 11.10 12.32
35 -3 -9 17.44 13.83
35 3 -9 15.23 9.65
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-35 3 8 7.44 5.29
35 -3 -8 23.83 14.12
35 3 -8 4.42 5.06
-35 -3 7 -4.42 8.08
-35 3 7 -14.47 8.25
35 -3 -7 -2.09 6.34
-35 -3 6 27.14 16.80
-35 3 6 12.44 10.81
35 -3 -6 9.24 8.89
-35 -3 5 16.27 10.40
-35 3 5 23.48 12.85
35 -3 -5 28.07 15.23
-35 3 4 16.45 10.99
35 3 -4 5.87 7.09
35 3 -3 -0.41 6.45
35 3 -2 41.04 16.91
35 -3 -2 67.19 17.03
35 3 -1 38.42 16.33
35 -3 -1 7.85 3.78
35 3 0 25.81 15.34
35 -3 0 38.54 17.03
35 3 1 14.65 9.24
35 -3 1 -8.78 5.87
-35 -3 -1 9.36 3.31
35 3 2 36.39 9.88
35 -3 2 26.85 8.37
-35 -3 -2 16.33 11.22
-35 3 -2 31.45 16.10
35 3 3 86.43 22.78
35 -3 3 71.32 17.67
-35 -3 -3 82.30 24.76
-35 3 -3 57.60 24.82
-36 0 10 -2.62 8.54
-36 0 9 -0.87 4.30
36 0 -9 -7.56 5.17
-36 0 8 15.93 11.39
36 0 -8 22.90 13.83
-36 0 7 10.06 9.82
-36 0 6 -8.14 7.79
-36 0 5 9.07 3.08
36 0 -4 19.76 11.86
36 0 -3 5.99 6.57
36 0 -2 39.29 17.44
36 0 -1 -8.54 6.57
36 0 0 19.24 11.92
36 0 1 13.95 8.95
36 0 2 10.52 10.23
-36 -2 8 14.36 9.53
-36 2 8 2.15 4.24
36 -2 -8 -0.58 5.99
-36 -2 7 10.58 9.59
-36 2 7 16.97 11.39
36 -2 -7 7.56 4.77
-36 -2 6 9.88 4.77
-36 2 6 8.43 3.95
-36 -2 5 18.31 11.80
36 2 -4 10.00 9.76
36 2 -3 48.77 20.87
36 -2 -3 43.30 18.89
36 2 -2 29.88 16.39
36 -2 -2 25.57 15.87
36 2 -1 16.91 12.32
36 -2 -1 38.59 16.33
36 2 0 -1.16 7.09
36 -2 0 15.29 11.57
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 13041
_shelx_res_file
;
x634.res created by SHELXL-2014/7
TITL x634_a.res in C2/c
REM Old TITL X634 in C2/c #15
REM SHELXT solution in C2/c
REM R1 0.142, Rweak 0.009, Alpha 0.050, Orientation as input
REM Formula found by SHELXT: C87 N6 P4 Cl2 Br4
CELL 0.71073 28.3189 11.6551 23.593 90 97.421 90
ZERR 8 0.0129 0.0052 0.0104 0 0.005 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Br Cl N Ni P
UNIT 356 304 8 8 16 8 16
L.S. 10
PLAN 5
SIZE 0.18 0.37 0.38
TEMP -103.15
BOND $H
LIST 6
MORE -1
CONF
fmap 2 53
acta 52
OMIT 0 0 2
OMIT -1 1 1
REM
REM
REM
WGHT 0.023400 15.331301
EXTI 0.000113
FVAR 0.13123
BR1 3 0.394490 0.212106 0.469422 11.00000 0.04435 0.03115 =
0.02967 -0.00124 0.01306 0.00805
NI1 6 0.372672 0.341369 0.539792 11.00000 0.02703 0.02449 =
0.02217 -0.00171 0.00534 0.00222
P1 7 0.390335 0.104270 0.604198 11.00000 0.02993 0.02654 =
0.02723 0.00035 0.00624 0.00329
P2 7 0.359002 0.461157 0.418552 11.00000 0.02617 0.03040 =
0.02364 0.00072 0.00508 -0.00007
CL1 4 0.522749 0.301611 0.699210 11.00000 0.08410 0.09456 =
0.05619 -0.00244 0.03296 0.00632
N1 5 0.378656 0.239576 0.605532 11.00000 0.03183 0.02824 =
0.02463 0.00034 0.00668 0.00447
N2 5 0.358832 0.467112 0.486711 11.00000 0.03209 0.02740 =
0.02466 -0.00081 0.00566 0.00056
C2 1 0.371704 0.420061 0.651676 11.00000 0.02490 0.03146 =
0.02520 -0.00206 0.00702 0.00174
C39 1 0.315857 0.364887 0.378908 11.00000 0.02801 0.03409 =
0.02438 -0.00711 0.00569 0.00332
C27 1 0.339720 0.598615 0.386723 11.00000 0.02848 0.03393 =
0.02262 0.00245 0.00055 0.00060
C6 1 0.357025 0.563928 0.576665 11.00000 0.02582 0.02739 =
0.02917 -0.00723 0.00461 0.00146
C9 1 0.383286 0.036012 0.671932 11.00000 0.04412 0.02536 =
0.03242 -0.00015 0.01038 0.00468
C5 1 0.354664 0.649233 0.617845 11.00000 0.03648 0.02487 =
0.03395 -0.00460 0.00429 0.00146
AFIX 43
H5 2 0.348913 0.726849 0.606739 11.00000 -1.20000
AFIX 0
C28 1 0.291771 0.628992 0.383986 11.00000 0.02870 0.03755 =
0.02941 0.00119 0.00153 -0.00046
AFIX 43
H28 2 0.270001 0.578230 0.398529 11.00000 -1.20000
AFIX 0
C26 1 0.468444 -0.042631 0.597611 11.00000 0.03583 0.03486 =
0.03082 0.00193 0.00193 0.00455
AFIX 43
H26 2 0.448807 -0.103525 0.607610 11.00000 -1.20000
AFIX 0
C21 1 0.450609 0.068712 0.592567 11.00000 0.02830 0.03622 =
0.02591 -0.00327 0.00500 0.00366
C33 1 0.417365 0.437415 0.396615 11.00000 0.02614 0.03628 =
0.02899 0.00655 0.00849 0.00320
C7 1 0.381963 0.295657 0.662425 11.00000 0.03946 0.03242 =
0.02370 -0.00062 0.00472 0.00536
AFIX 23
H7A 2 0.414232 0.285452 0.683558 11.00000 -1.20000
H7B 2 0.358482 0.261887 0.685268 11.00000 -1.20000
AFIX 0
C22 1 0.480306 0.157400 0.578923 11.00000 0.03831 0.02926 =
0.03606 -0.00355 0.00472 0.00431
AFIX 43
H22 2 0.468592 0.233828 0.575903 11.00000 -1.20000
AFIX 0
C4 1 0.360873 0.618706 0.675461 11.00000 0.04527 0.03409 =
0.03349 -0.01389 0.00946 0.00611
AFIX 43
H4 2 0.359207 0.676378 0.703588 11.00000 -1.20000
AFIX 0
C3 1 0.369467 0.505486 0.692683 11.00000 0.04038 0.03926 =
0.02508 -0.00603 0.00478 0.00571
AFIX 43
H3 2 0.373787 0.486506 0.732173 11.00000 -1.20000
AFIX 0
C16 1 0.302418 0.081061 0.540781 11.00000 0.03032 0.03572 =
0.03905 -0.00906 0.00883 -0.00140
AFIX 43
H16 2 0.295256 0.149180 0.560074 11.00000 -1.20000
AFIX 0
C40 1 0.307308 0.377874 0.319572 11.00000 0.03431 0.05133 =
0.02737 -0.00553 0.00400 -0.00087
AFIX 43
H40 2 0.324318 0.434575 0.301549 11.00000 -1.20000
AFIX 0
C8 1 0.352810 0.581860 0.513321 11.00000 0.03747 0.02095 =
0.02779 -0.00284 0.00402 0.00111
AFIX 23
H8A 2 0.321245 0.614493 0.498974 11.00000 -1.20000
H8B 2 0.377716 0.635544 0.503818 11.00000 -1.20000
AFIX 0
C29 1 0.275826 0.732785 0.360164 11.00000 0.03398 0.04244 =
0.03258 0.00011 -0.00480 0.00604
AFIX 43
H29 2 0.243203 0.753209 0.358542 11.00000 -1.20000
AFIX 0
C38 1 0.425445 0.371888 0.349408 11.00000 0.03305 0.04125 =
0.04088 0.00174 0.01074 0.00170
AFIX 43
H38 2 0.399517 0.335693 0.326699 11.00000 -1.20000
AFIX 0
C23 1 0.526562 0.134792 0.569793 11.00000 0.03325 0.04307 =
0.04350 -0.00194 0.00866 -0.00297
AFIX 43
H23 2 0.546664 0.195599 0.560804 11.00000 -1.20000
AFIX 0
C20 1 0.357585 -0.066067 0.522978 11.00000 0.04224 0.02817 =
0.03419 -0.00040 0.00172 0.00651
AFIX 43
H20 2 0.388266 -0.100037 0.530223 11.00000 -1.20000
AFIX 0
C1 1 0.365294 0.450816 0.593817 11.00000 0.02423 0.02900 =
0.02627 -0.00260 0.00167 -0.00037
C15 1 0.347889 0.033176 0.551909 11.00000 0.03298 0.02884 =
0.02896 0.00419 0.00582 -0.00279
C32 1 0.370966 0.673138 0.364208 11.00000 0.03441 0.04397 =
0.04394 0.00705 0.00870 -0.00362
AFIX 43
H32 2 0.403562 0.652942 0.365185 11.00000 -1.20000
AFIX 0
C44 1 0.289813 0.283375 0.404576 11.00000 0.03288 0.03775 =
0.03460 -0.00872 0.00685 0.00104
AFIX 43
H44 2 0.294768 0.273644 0.444885 11.00000 -1.20000
AFIX 0
C25 1 0.514752 -0.064577 0.588064 11.00000 0.04056 0.03787 =
0.04001 0.00108 0.00586 0.01594
AFIX 43
H25 2 0.526814 -0.140674 0.591363 11.00000 -1.20000
AFIX 0
C30 1 0.307422 0.806869 0.338694 11.00000 0.05438 0.03525 =
0.04246 0.01016 -0.00392 -0.00077
AFIX 43
H30 2 0.296575 0.878510 0.322794 11.00000 -1.20000
AFIX 0
C34 1 0.456036 0.491153 0.428403 11.00000 0.03148 0.05247 =
0.03552 0.00656 0.00151 -0.00059
AFIX 43
H34 2 0.450964 0.536239 0.460615 11.00000 -1.20000
AFIX 0
C31 1 0.354607 0.776440 0.340447 11.00000 0.05082 0.04294 =
0.05217 0.02080 0.00701 -0.00385
AFIX 43
H31 2 0.376095 0.826909 0.325187 11.00000 -1.20000
AFIX 0
C19 1 0.323294 -0.116010 0.483871 11.00000 0.05338 0.02828 =
0.03820 -0.00581 0.00048 0.00024
AFIX 43
H19 2 0.330573 -0.183533 0.464176 11.00000 -1.20000
AFIX 0
C37 1 0.471620 0.359362 0.335439 11.00000 0.04955 0.05550 =
0.05439 0.00831 0.02510 0.01076
AFIX 43
H37 2 0.477025 0.313714 0.303543 11.00000 -1.20000
AFIX 0
C17 1 0.267537 0.030601 0.501952 11.00000 0.03266 0.04445 =
0.04489 -0.00625 0.00967 -0.00289
AFIX 43
H17 2 0.236624 0.063468 0.495194 11.00000 -1.20000
AFIX 0
C42 1 0.249129 0.229353 0.312542 11.00000 0.03329 0.05739 =
0.05198 -0.03174 0.00014 -0.00350
AFIX 43
H42 2 0.226398 0.182714 0.290084 11.00000 -1.20000
AFIX 0
C43 1 0.256452 0.215944 0.371235 11.00000 0.03430 0.03964 =
0.06149 -0.01351 0.01089 -0.00451
AFIX 43
H43 2 0.238616 0.160400 0.388909 11.00000 -1.20000
AFIX 0
C14 1 0.338756 -0.001463 0.682818 11.00000 0.06007 0.04581 =
0.04067 0.00101 0.01473 -0.01000
AFIX 43
H14 2 0.311911 0.007649 0.654569 11.00000 -1.20000
AFIX 0
C18 1 0.277942 -0.067691 0.473135 11.00000 0.04043 0.04435 =
0.04538 -0.00882 0.00392 -0.01290
AFIX 43
H18 2 0.254337 -0.102115 0.446178 11.00000 -1.20000
AFIX 0
C24 1 0.543576 0.023765 0.573737 11.00000 0.03237 0.05344 =
0.04123 -0.00721 0.00900 0.00918
AFIX 43
H24 2 0.575183 0.007970 0.566589 11.00000 -1.20000
AFIX 0
C41 1 0.274456 0.309480 0.286592 11.00000 0.04366 0.07124 =
0.03311 -0.01783 -0.00355 0.00383
AFIX 43
H41 2 0.269531 0.318122 0.246220 11.00000 -1.20000
AFIX 0
C10 1 0.421752 0.024430 0.714733 11.00000 0.05968 0.05321 =
0.03265 0.00626 0.01015 0.01526
AFIX 43
H10 2 0.452316 0.051219 0.708392 11.00000 -1.20000
AFIX 0
C36 1 0.509481 0.412954 0.367725 11.00000 0.03193 0.06544 =
0.06243 0.02157 0.01887 0.00881
AFIX 43
H36 2 0.540829 0.403653 0.358160 11.00000 -1.20000
AFIX 0
C13 1 0.333322 -0.052515 0.735186 11.00000 0.09389 0.04782 =
0.04654 -0.00045 0.03367 -0.02099
AFIX 43
H13 2 0.302850 -0.078890 0.742132 11.00000 -1.20000
AFIX 0
C35 1 0.501749 0.480187 0.413999 11.00000 0.02859 0.06710 =
0.05452 0.01264 0.00485 -0.00195
AFIX 43
H35 2 0.527605 0.518571 0.435747 11.00000 -1.20000
AFIX 0
C11 1 0.415677 -0.026082 0.766652 11.00000 0.09687 0.06324 =
0.03219 0.00795 0.01045 0.03227
AFIX 43
H11 2 0.442152 -0.033943 0.795521 11.00000 -1.20000
AFIX 0
C12 1 0.371573 -0.064778 0.776518 11.00000 0.12932 0.03327 =
0.04471 0.00776 0.03555 0.00850
AFIX 43
H12 2 0.367686 -0.099934 0.811948 11.00000 -1.20000
AFIX 0
C45 1 0.500000 0.389153 0.750000 10.50000 0.06257 0.06582 =
0.05519 0.00000 0.02079 0.00000
AFIX 23
H45A 2 0.525573 0.438905 0.769138 10.50000 -1.20000
H45B 2 0.474428 0.438907 0.730862 10.50000 -1.20000
AFIX 0
HKLF 4
REM x634_a.res in C2/c
REM R1 = 0.0529 for 6363 Fo > 4sig(Fo) and 0.0836 for all 8846 data
REM 466 parameters refined using 0 restraints
END
WGHT 0.0234 15.3510
REM Highest difference peak 0.438, deepest hole -0.667, 1-sigma level 0.089
Q1 1 0.3620 0.2026 0.6025 11.00000 0.05 0.44
Q2 1 0.3806 0.2333 0.5221 11.00000 0.05 0.36
Q3 1 0.4166 0.1208 0.5068 11.00000 0.05 0.36
Q4 1 0.3431 0.4600 0.4617 11.00000 0.05 0.34
Q5 1 0.3849 0.1240 0.4990 11.00000 0.05 0.32
;
_shelx_res_checksum 2060
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Br Br1 0.39449(2) 0.21211(3) 0.46942(2) 0.03433(12) Uani d 1
Ni Ni1 0.37267(2) 0.34137(4) 0.53979(2) 0.02438(12) Uani d 1
P P1 0.39034(3) 0.10427(8) 0.60420(4) 0.0277(2) Uani d 1
P P2 0.35900(3) 0.46116(8) 0.41855(4) 0.0266(2) Uani d 1
Cl Cl1 0.52275(6) 0.30161(14) 0.69921(6) 0.0762(4) Uani d 1
N N1 0.37866(11) 0.2396(3) 0.60553(12) 0.0280(7) Uani d 1
N N2 0.35883(11) 0.4671(2) 0.48671(13) 0.0279(7) Uani d 1
C C2 0.37170(12) 0.4201(3) 0.65168(15) 0.0269(8) Uani d 1
C C39 0.31586(13) 0.3649(3) 0.37891(15) 0.0286(8) Uani d 1
C C27 0.33972(13) 0.5986(3) 0.38672(15) 0.0286(8) Uani d 1
C C6 0.35703(12) 0.5639(3) 0.57666(16) 0.0274(8) Uani d 1
C C9 0.38329(14) 0.0360(3) 0.67193(17) 0.0335(9) Uani d 1
C C5 0.35466(13) 0.6492(3) 0.61784(16) 0.0318(9) Uani d 1
H H5 0.3489 0.7268 0.6067 0.038 Uiso calc 1
C C28 0.29177(13) 0.6290(3) 0.38399(16) 0.0321(9) Uani d 1
H H28 0.2700 0.5782 0.3985 0.038 Uiso calc 1
C C26 0.46844(14) -0.0426(3) 0.59761(16) 0.0340(9) Uani d 1
H H26 0.4488 -0.1035 0.6076 0.041 Uiso calc 1
C C21 0.45061(13) 0.0687(3) 0.59257(16) 0.0300(8) Uani d 1
C C33 0.41737(13) 0.4374(3) 0.39662(16) 0.0300(8) Uani d 1
C C7 0.38196(14) 0.2957(3) 0.66242(15) 0.0318(9) Uani d 1
H H7A 0.4142 0.2855 0.6836 0.038 Uiso calc 1
H H7B 0.3585 0.2619 0.6853 0.038 Uiso calc 1
C C22 0.48031(14) 0.1574(3) 0.57892(17) 0.0346(9) Uani d 1
H H22 0.4686 0.2338 0.5759 0.041 Uiso calc 1
C C4 0.36087(14) 0.6187(3) 0.67546(17) 0.0372(10) Uani d 1
H H4 0.3592 0.6764 0.7036 0.045 Uiso calc 1
C C3 0.36947(14) 0.5055(3) 0.69268(16) 0.0349(9) Uani d 1
H H3 0.3738 0.4865 0.7322 0.042 Uiso calc 1
C C16 0.30242(13) 0.0811(3) 0.54078(17) 0.0346(9) Uani d 1
H H16 0.2953 0.1492 0.5601 0.042 Uiso calc 1
C C40 0.30731(14) 0.3779(4) 0.31957(17) 0.0377(10) Uani d 1
H H40 0.3243 0.4346 0.3015 0.045 Uiso calc 1
C C8 0.35281(14) 0.5819(3) 0.51332(15) 0.0288(8) Uani d 1
H H8A 0.3212 0.6145 0.4990 0.035 Uiso calc 1
H H8B 0.3777 0.6355 0.5038 0.035 Uiso calc 1
C C29 0.27583(14) 0.7328(3) 0.36016(17) 0.0371(9) Uani d 1
H H29 0.2432 0.7532 0.3585 0.045 Uiso calc 1
C C38 0.42544(14) 0.3719(3) 0.34941(18) 0.0379(10) Uani d 1
H H38 0.3995 0.3357 0.3267 0.045 Uiso calc 1
C C23 0.52656(14) 0.1348(4) 0.56979(18) 0.0396(10) Uani d 1
H H23 0.5467 0.1956 0.5608 0.048 Uiso calc 1
C C20 0.35759(15) -0.0661(3) 0.52298(16) 0.0351(9) Uani d 1
H H20 0.3883 -0.1000 0.5302 0.042 Uiso calc 1
C C1 0.36529(12) 0.4508(3) 0.59382(15) 0.0266(8) Uani d 1
C C15 0.34789(13) 0.0332(3) 0.55191(16) 0.0301(8) Uani d 1
C C32 0.37097(15) 0.6731(4) 0.36421(18) 0.0405(10) Uani d 1
H H32 0.4036 0.6529 0.3652 0.049 Uiso calc 1
C C44 0.28981(13) 0.2834(3) 0.40458(17) 0.0349(9) Uani d 1
H H44 0.2948 0.2736 0.4449 0.042 Uiso calc 1
C C25 0.51475(14) -0.0646(4) 0.58806(17) 0.0394(10) Uani d 1
H H25 0.5268 -0.1407 0.5914 0.047 Uiso calc 1
C C30 0.30742(16) 0.8069(4) 0.33869(18) 0.0449(11) Uani d 1
H H30 0.2966 0.8785 0.3228 0.054 Uiso calc 1
C C34 0.45604(14) 0.4912(4) 0.42840(18) 0.0401(10) Uani d 1
H H34 0.4510 0.5362 0.4606 0.048 Uiso calc 1
C C31 0.35461(16) 0.7764(4) 0.3404(2) 0.0486(12) Uani d 1
H H31 0.3761 0.8269 0.3252 0.058 Uiso calc 1
C C19 0.32329(15) -0.1160(3) 0.48387(18) 0.0404(10) Uani d 1
H H19 0.3306 -0.1835 0.4642 0.049 Uiso calc 1
C C37 0.47162(16) 0.3594(4) 0.3354(2) 0.0515(12) Uani d 1
H H37 0.4770 0.3137 0.3035 0.062 Uiso calc 1
C C17 0.26754(15) 0.0306(4) 0.50195(18) 0.0403(10) Uani d 1
H H17 0.2366 0.0635 0.4952 0.048 Uiso calc 1
C C42 0.24913(15) 0.2294(4) 0.3125(2) 0.0480(12) Uani d 1
H H42 0.2264 0.1827 0.2901 0.058 Uiso calc 1
C C43 0.25645(15) 0.2159(4) 0.3712(2) 0.0447(11) Uani d 1
H H43 0.2386 0.1604 0.3889 0.054 Uiso calc 1
C C14 0.33876(17) -0.0015(4) 0.68282(19) 0.0481(11) Uani d 1
H H14 0.3119 0.0076 0.6546 0.058 Uiso calc 1
C C18 0.27794(15) -0.0677(4) 0.47313(19) 0.0435(11) Uani d 1
H H18 0.2543 -0.1021 0.4462 0.052 Uiso calc 1
C C24 0.54358(15) 0.0238(4) 0.57374(18) 0.0420(10) Uani d 1
H H24 0.5752 0.0080 0.5666 0.050 Uiso calc 1
C C41 0.27446(16) 0.3095(4) 0.28659(19) 0.0501(12) Uani d 1
H H41 0.2695 0.3181 0.2462 0.060 Uiso calc 1
C C10 0.42175(17) 0.0244(4) 0.71473(18) 0.0481(12) Uani d 1
H H10 0.4523 0.0512 0.7084 0.058 Uiso calc 1
C C36 0.50948(16) 0.4130(4) 0.3677(2) 0.0521(13) Uani d 1
H H36 0.5408 0.4037 0.3582 0.063 Uiso calc 1
C C13 0.3333(2) -0.0525(4) 0.7352(2) 0.0606(15) Uani d 1
H H13 0.3029 -0.0789 0.7421 0.073 Uiso calc 1
C C35 0.50175(15) 0.4802(4) 0.4140(2) 0.0501(12) Uani d 1
H H35 0.5276 0.5186 0.4357 0.060 Uiso calc 1
C C11 0.4157(2) -0.0261(4) 0.7667(2) 0.0639(16) Uani d 1
H H11 0.4422 -0.0339 0.7955 0.077 Uiso calc 1
C C12 0.3716(2) -0.0648(4) 0.7765(2) 0.0670(17) Uani d 1
H H12 0.3677 -0.0999 0.8119 0.080 Uiso calc 1
C C45 0.5000 0.3892(6) 0.7500 0.0600(19) Uani d 1
H H45A 0.5256 0.4389 0.7691 0.072 Uiso calc 0.5
H H45B 0.4744 0.4389 0.7309 0.072 Uiso calc 0.5
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 0.0443(2) 0.0312(2) 0.0297(2) 0.00805(17) 0.01306(18) -0.00124(16)
Ni1 0.0270(2) 0.0245(3) 0.0222(2) 0.00222(19) 0.00534(19) -0.00171(18)
P1 0.0299(5) 0.0265(5) 0.0272(5) 0.0033(4) 0.0062(4) 0.0004(4)
P2 0.0262(5) 0.0304(5) 0.0236(5) -0.0001(4) 0.0051(4) 0.0007(4)
Cl1 0.0841(10) 0.0946(12) 0.0562(8) 0.0063(8) 0.0330(8) -0.0024(8)
N1 0.0318(17) 0.0282(17) 0.0246(16) 0.0045(13) 0.0067(14) 0.0003(13)
N2 0.0321(17) 0.0274(17) 0.0247(16) 0.0006(13) 0.0057(14) -0.0008(13)
C2 0.0249(18) 0.031(2) 0.0252(19) 0.0017(15) 0.0070(16) -0.0021(15)
C39 0.0280(19) 0.034(2) 0.0244(19) 0.0033(15) 0.0057(16) -0.0071(15)
C27 0.0285(19) 0.034(2) 0.0226(18) 0.0006(16) 0.0006(16) 0.0025(15)
C6 0.0258(19) 0.027(2) 0.029(2) 0.0015(15) 0.0046(16) -0.0072(15)
C9 0.044(2) 0.025(2) 0.032(2) 0.0047(17) 0.0104(19) -0.0002(16)
C5 0.036(2) 0.025(2) 0.034(2) 0.0015(16) 0.0043(18) -0.0046(16)
C28 0.029(2) 0.038(2) 0.029(2) -0.0005(16) 0.0015(17) 0.0012(16)
C26 0.036(2) 0.035(2) 0.031(2) 0.0046(17) 0.0019(18) 0.0019(17)
C21 0.028(2) 0.036(2) 0.026(2) 0.0037(16) 0.0050(16) -0.0033(16)
C33 0.0261(19) 0.036(2) 0.029(2) 0.0032(16) 0.0085(17) 0.0065(16)
C7 0.039(2) 0.032(2) 0.0237(19) 0.0054(17) 0.0047(17) -0.0006(16)
C22 0.038(2) 0.029(2) 0.036(2) 0.0043(17) 0.0047(19) -0.0035(17)
C4 0.045(2) 0.034(2) 0.033(2) 0.0061(18) 0.009(2) -0.0139(17)
C3 0.040(2) 0.039(2) 0.025(2) 0.0057(18) 0.0048(18) -0.0060(17)
C16 0.030(2) 0.036(2) 0.039(2) -0.0014(17) 0.0088(18) -0.0091(18)
C40 0.034(2) 0.051(3) 0.027(2) -0.0009(19) 0.0040(18) -0.0055(18)
C8 0.037(2) 0.0210(19) 0.028(2) 0.0011(15) 0.0040(17) -0.0028(15)
C29 0.034(2) 0.042(3) 0.033(2) 0.0060(18) -0.0048(18) 0.0001(18)
C38 0.033(2) 0.041(2) 0.041(2) 0.0017(18) 0.0107(19) 0.0017(19)
C23 0.033(2) 0.043(3) 0.043(3) -0.0030(18) 0.009(2) -0.0019(19)
C20 0.042(2) 0.028(2) 0.034(2) 0.0065(17) 0.0017(19) -0.0004(16)
C1 0.0242(18) 0.029(2) 0.0263(19) -0.0004(15) 0.0017(16) -0.0026(15)
C15 0.033(2) 0.029(2) 0.029(2) -0.0028(16) 0.0058(17) 0.0042(15)
C32 0.034(2) 0.044(3) 0.044(3) -0.0036(18) 0.009(2) 0.0071(19)
C44 0.033(2) 0.038(2) 0.035(2) 0.0010(17) 0.0068(18) -0.0087(18)
C25 0.041(2) 0.038(2) 0.040(2) 0.0159(19) 0.006(2) 0.0011(18)
C30 0.054(3) 0.035(2) 0.042(3) -0.001(2) -0.004(2) 0.0102(19)
C34 0.031(2) 0.052(3) 0.036(2) -0.0006(19) 0.0015(19) 0.0066(19)
C31 0.051(3) 0.043(3) 0.052(3) -0.004(2) 0.007(2) 0.021(2)
C19 0.053(3) 0.028(2) 0.038(2) 0.0002(19) 0.000(2) -0.0058(17)
C37 0.050(3) 0.056(3) 0.054(3) 0.011(2) 0.025(3) 0.008(2)
C17 0.033(2) 0.044(3) 0.045(3) -0.0029(18) 0.010(2) -0.006(2)
C42 0.033(2) 0.057(3) 0.052(3) -0.004(2) 0.000(2) -0.032(2)
C43 0.034(2) 0.040(3) 0.061(3) -0.0045(19) 0.011(2) -0.014(2)
C14 0.060(3) 0.046(3) 0.041(3) -0.010(2) 0.015(2) 0.001(2)
C18 0.040(2) 0.044(3) 0.045(3) -0.013(2) 0.004(2) -0.009(2)
C24 0.032(2) 0.053(3) 0.041(2) 0.0092(19) 0.009(2) -0.007(2)
C41 0.044(3) 0.071(4) 0.033(2) 0.004(2) -0.004(2) -0.018(2)
C10 0.060(3) 0.053(3) 0.033(2) 0.015(2) 0.010(2) 0.006(2)
C36 0.032(2) 0.065(3) 0.062(3) 0.009(2) 0.019(2) 0.022(3)
C13 0.094(4) 0.048(3) 0.047(3) -0.021(3) 0.034(3) 0.000(2)
C35 0.029(2) 0.067(3) 0.055(3) -0.002(2) 0.005(2) 0.013(2)
C11 0.097(4) 0.063(4) 0.032(3) 0.032(3) 0.010(3) 0.008(2)
C12 0.129(5) 0.033(3) 0.045(3) 0.008(3) 0.036(4) 0.008(2)
C45 0.063(5) 0.066(5) 0.055(4) 0.000 0.021(4) 0.000
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'
Cl Cl 0.1484 0.1585 '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'
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
N1 Ni1 Br1 . 99.58(9)
N2 Ni1 Br1 . 94.42(9)
N2 Ni1 N1 . 165.67(12)
C1 Ni1 Br1 . 170.89(11)
C1 Ni1 N1 . 82.87(15)
C1 Ni1 N2 . 83.76(15)
N1 P1 C9 . 111.38(16)
N1 P1 C21 . 115.24(17)
N1 P1 C15 . 109.97(17)
C21 P1 C9 . 104.21(18)
C15 P1 C9 . 105.08(18)
C15 P1 C21 . 110.37(18)
N2 P2 C39 . 116.75(17)
N2 P2 C27 . 109.52(16)
N2 P2 C33 . 114.30(17)
C27 P2 C39 . 100.61(17)
C33 P2 C39 . 109.51(18)
C33 P2 C27 . 104.58(17)
P1 N1 Ni1 . 125.36(17)
C7 N1 Ni1 . 116.2(2)
C7 N1 P1 . 117.3(2)
P2 N2 Ni1 . 125.97(17)
C8 N2 Ni1 . 115.5(2)
C8 N2 P2 . 118.2(2)
C3 C2 C7 . 126.9(3)
C3 C2 C1 . 118.8(3)
C1 C2 C7 . 114.3(3)
C40 C39 P2 . 117.7(3)
C44 C39 P2 . 123.7(3)
C44 C39 C40 . 118.5(4)
C28 C27 P2 . 118.7(3)
C32 C27 P2 . 122.3(3)
C32 C27 C28 . 119.1(4)
C5 C6 C8 . 126.1(3)
C1 C6 C5 . 119.6(3)
C1 C6 C8 . 114.3(3)
C14 C9 P1 . 120.3(3)
C14 C9 C10 . 118.6(4)
C10 C9 P1 . 121.0(3)
C6 C5 H5 . 120.5
C4 C5 C6 . 119.0(4)
C4 C5 H5 . 120.5
C27 C28 H28 . 119.9
C29 C28 C27 . 120.3(4)
C29 C28 H28 . 119.9
C21 C26 H26 . 120.0
C25 C26 H26 . 120.0
C25 C26 C21 . 120.0(4)
C26 C21 P1 . 122.6(3)
C26 C21 C22 . 119.2(4)
C22 C21 P1 . 118.2(3)
C38 C33 P2 . 124.1(3)
C34 C33 P2 . 117.3(3)
C34 C33 C38 . 118.5(4)
N1 C7 C2 . 106.6(3)
N1 C7 H7A . 110.4
N1 C7 H7B . 110.4
C2 C7 H7A . 110.4
C2 C7 H7B . 110.4
H7A C7 H7B . 108.6
C21 C22 H22 . 119.8
C23 C22 C21 . 120.4(4)
C23 C22 H22 . 119.8
C5 C4 H4 . 119.3
C3 C4 C5 . 121.4(3)
C3 C4 H4 . 119.3
C2 C3 H3 . 120.1
C4 C3 C2 . 119.7(4)
C4 C3 H3 . 120.1
C15 C16 H16 . 119.5
C17 C16 H16 . 119.5
C17 C16 C15 . 121.0(4)
C39 C40 H40 . 119.4
C41 C40 C39 . 121.1(4)
C41 C40 H40 . 119.4
N2 C8 C6 . 107.2(3)
N2 C8 H8A . 110.3
N2 C8 H8B . 110.3
C6 C8 H8A . 110.3
C6 C8 H8B . 110.3
H8A C8 H8B . 108.5
C28 C29 H29 . 120.0
C28 C29 C30 . 120.0(4)
C30 C29 H29 . 120.0
C33 C38 H38 . 120.0
C33 C38 C37 . 120.1(4)
C37 C38 H38 . 120.0
C22 C23 H23 . 120.0
C24 C23 C22 . 119.9(4)
C24 C23 H23 . 120.0
C15 C20 H20 . 119.5
C19 C20 H20 . 119.5
C19 C20 C15 . 120.9(4)
C2 C1 Ni1 . 119.2(3)
C6 C1 Ni1 . 119.2(3)
C6 C1 C2 . 121.5(3)
C16 C15 P1 . 117.4(3)
C20 C15 P1 . 124.1(3)
C20 C15 C16 . 118.5(4)
C27 C32 H32 . 120.0
C31 C32 C27 . 120.1(4)
C31 C32 H32 . 120.0
C39 C44 H44 . 120.0
C39 C44 C43 . 120.0(4)
C43 C44 H44 . 120.0
C26 C25 H25 . 119.9
C24 C25 C26 . 120.3(4)
C24 C25 H25 . 119.9
C29 C30 H30 . 120.1
C31 C30 C29 . 119.9(4)
C31 C30 H30 . 120.1
C33 C34 H34 . 119.3
C35 C34 C33 . 121.4(4)
C35 C34 H34 . 119.3
C32 C31 H31 . 119.7
C30 C31 C32 . 120.6(4)
C30 C31 H31 . 119.7
C20 C19 H19 . 119.9
C20 C19 C18 . 120.2(4)
C18 C19 H19 . 119.9
C38 C37 H37 . 119.8
C36 C37 C38 . 120.4(4)
C36 C37 H37 . 119.8
C16 C17 H17 . 120.1
C18 C17 C16 . 119.8(4)
C18 C17 H17 . 120.1
C43 C42 H42 . 119.8
C41 C42 H42 . 119.8
C41 C42 C43 . 120.4(4)
C44 C43 H43 . 119.8
C42 C43 C44 . 120.4(4)
C42 C43 H43 . 119.8
C9 C14 H14 . 119.9
C9 C14 C13 . 120.2(5)
C13 C14 H14 . 119.9
C19 C18 H18 . 120.2
C17 C18 C19 . 119.6(4)
C17 C18 H18 . 120.2
C23 C24 C25 . 120.2(4)
C23 C24 H24 . 119.9
C25 C24 H24 . 119.9
C40 C41 H41 . 120.2
C42 C41 C40 . 119.6(4)
C42 C41 H41 . 120.2
C9 C10 H10 . 119.8
C11 C10 C9 . 120.4(5)
C11 C10 H10 . 119.8
C37 C36 H36 . 120.0
C37 C36 C35 . 120.0(4)
C35 C36 H36 . 120.0
C14 C13 H13 . 119.8
C12 C13 C14 . 120.5(5)
C12 C13 H13 . 119.8
C34 C35 H35 . 120.2
C36 C35 C34 . 119.6(4)
C36 C35 H35 . 120.2
C10 C11 H11 . 119.8
C12 C11 C10 . 120.4(5)
C12 C11 H11 . 119.8
C13 C12 C11 . 119.8(5)
C13 C12 H12 . 120.1
C11 C12 H12 . 120.1
Cl1 C45 Cl1 2_656 109.1(4)
Cl1 C45 H45A . 109.9
Cl1 C45 H45A 2_656 109.9
Cl1 C45 H45B . 109.9
Cl1 C45 H45B 2_656 109.9
H45A C45 H45B . 108.3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Br1 Ni1 . 2.3818(9)
Ni1 N1 . 1.943(3)
Ni1 N2 . 1.935(3)
Ni1 C1 . 1.834(4)
P1 N1 . 1.612(3)
P1 C9 . 1.819(4)
P1 C21 . 1.812(4)
P1 C15 . 1.808(4)
P2 N2 . 1.610(3)
P2 C39 . 1.825(4)
P2 C27 . 1.823(4)
P2 C33 . 1.816(4)
Cl1 C45 . 1.758(4)
N1 C7 . 1.485(4)
N2 C8 . 1.497(4)
C2 C7 . 1.494(5)
C2 C3 . 1.395(5)
C2 C1 . 1.400(5)
C39 C40 . 1.398(5)
C39 C44 . 1.389(5)
C27 C28 . 1.397(5)
C27 C32 . 1.393(5)
C6 C5 . 1.398(5)
C6 C8 . 1.498(5)
C6 C1 . 1.390(5)
C9 C14 . 1.389(6)
C9 C10 . 1.393(6)
C5 H5 . 0.9500
C5 C4 . 1.394(5)
C28 H28 . 0.9500
C28 C29 . 1.385(5)
C26 H26 . 0.9500
C26 C21 . 1.392(5)
C26 C25 . 1.383(5)
C21 C22 . 1.396(5)
C33 C38 . 1.394(5)
C33 C34 . 1.394(5)
C7 H7A . 0.9900
C7 H7B . 0.9900
C22 H22 . 0.9500
C22 C23 . 1.380(5)
C4 H4 . 0.9500
C4 C3 . 1.393(5)
C3 H3 . 0.9500
C16 H16 . 0.9500
C16 C15 . 1.397(5)
C16 C17 . 1.388(5)
C40 H40 . 0.9500
C40 C41 . 1.385(6)
C8 H8A . 0.9900
C8 H8B . 0.9900
C29 H29 . 0.9500
C29 C30 . 1.386(6)
C38 H38 . 0.9500
C38 C37 . 1.397(6)
C23 H23 . 0.9500
C23 C24 . 1.380(6)
C20 H20 . 0.9500
C20 C15 . 1.388(5)
C20 C19 . 1.379(5)
C32 H32 . 0.9500
C32 C31 . 1.383(6)
C44 H44 . 0.9500
C44 C43 . 1.392(5)
C25 H25 . 0.9500
C25 C24 . 1.383(6)
C30 H30 . 0.9500
C30 C31 . 1.378(6)
C34 H34 . 0.9500
C34 C35 . 1.386(6)
C31 H31 . 0.9500
C19 H19 . 0.9500
C19 C18 . 1.395(6)
C37 H37 . 0.9500
C37 C36 . 1.382(7)
C17 H17 . 0.9500
C17 C18 . 1.383(6)
C42 H42 . 0.9500
C42 C43 . 1.382(6)
C42 C41 . 1.369(6)
C43 H43 . 0.9500
C14 H14 . 0.9500
C14 C13 . 1.398(6)
C18 H18 . 0.9500
C24 H24 . 0.9500
C41 H41 . 0.9500
C10 H10 . 0.9500
C10 C11 . 1.390(6)
C36 H36 . 0.9500
C36 C35 . 1.384(7)
C13 H13 . 0.9500
C13 C12 . 1.368(8)
C35 H35 . 0.9500
C11 H11 . 0.9500
C11 C12 . 1.376(8)
C12 H12 . 0.9500
C45 Cl1 2_656 1.758(4)
C45 H45A . 0.9900
C45 H45B . 0.9900
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
Ni1 N1 C7 C2 9.0(4)
Ni1 N2 C8 C6 -3.0(4)
P1 N1 C7 C2 177.6(2)
P1 C9 C14 C13 -179.2(3)
P1 C9 C10 C11 178.9(4)
P1 C21 C22 C23 179.8(3)
P2 N2 C8 C6 -176.5(2)
P2 C39 C40 C41 -178.8(3)
P2 C39 C44 C43 177.9(3)
P2 C27 C28 C29 179.9(3)
P2 C27 C32 C31 179.9(3)
P2 C33 C38 C37 179.3(3)
P2 C33 C34 C35 -178.4(3)
N1 Ni1 C1 C2 6.4(3)
N1 Ni1 C1 C6 -178.4(3)
N1 P1 C9 C14 84.7(4)
N1 P1 C9 C10 -92.6(4)
N1 P1 C21 C26 171.4(3)
N1 P1 C21 C22 -7.6(4)
N1 P1 C15 C16 -28.8(3)
N1 P1 C15 C20 152.0(3)
N2 Ni1 C1 C2 -178.8(3)
N2 Ni1 C1 C6 -3.6(3)
N2 P2 C39 C40 165.0(3)
N2 P2 C39 C44 -12.1(4)
N2 P2 C27 C28 -72.2(3)
N2 P2 C27 C32 109.0(3)
N2 P2 C33 C38 144.3(3)
N2 P2 C33 C34 -37.5(4)
C39 P2 N2 Ni1 62.6(3)
C39 P2 N2 C8 -124.6(3)
C39 P2 C27 C28 51.4(3)
C39 P2 C27 C32 -127.5(3)
C39 P2 C33 C38 11.2(4)
C39 P2 C33 C34 -170.7(3)
C39 C40 C41 C42 1.4(7)
C39 C44 C43 C42 0.2(6)
C27 P2 N2 Ni1 176.07(19)
C27 P2 N2 C8 -11.2(3)
C27 P2 C39 C40 46.7(3)
C27 P2 C39 C44 -130.5(3)
C27 P2 C33 C38 -95.9(4)
C27 P2 C33 C34 82.2(3)
C27 C28 C29 C30 0.3(6)
C27 C32 C31 C30 0.0(7)
C6 C5 C4 C3 0.2(6)
C9 P1 N1 Ni1 -170.7(2)
C9 P1 N1 C7 21.9(3)
C9 P1 C21 C26 49.0(4)
C9 P1 C21 C22 -129.9(3)
C9 P1 C15 C16 91.1(3)
C9 P1 C15 C20 -88.0(4)
C9 C14 C13 C12 0.9(7)
C9 C10 C11 C12 -0.3(7)
C5 C6 C8 N2 178.5(3)
C5 C6 C1 Ni1 -175.6(3)
C5 C6 C1 C2 -0.5(5)
C5 C4 C3 C2 -0.4(6)
C28 C27 C32 C31 1.1(6)
C28 C29 C30 C31 0.8(7)
C26 C21 C22 C23 0.9(6)
C26 C25 C24 C23 1.1(6)
C21 P1 N1 Ni1 70.9(3)
C21 P1 N1 C7 -96.5(3)
C21 P1 C9 C14 -150.4(3)
C21 P1 C9 C10 32.3(4)
C21 P1 C15 C16 -157.1(3)
C21 P1 C15 C20 23.8(4)
C21 C26 C25 C24 0.3(6)
C21 C22 C23 C24 0.5(6)
C33 P2 N2 Ni1 -67.0(3)
C33 P2 N2 C8 105.8(3)
C33 P2 C39 C40 -63.1(3)
C33 P2 C39 C44 119.7(3)
C33 P2 C27 C28 164.9(3)
C33 P2 C27 C32 -13.9(4)
C33 C38 C37 C36 -0.9(7)
C33 C34 C35 C36 -1.1(7)
C7 C2 C3 C4 178.0(4)
C7 C2 C1 Ni1 -2.8(4)
C7 C2 C1 C6 -177.9(3)
C22 C23 C24 C25 -1.4(7)
C3 C2 C7 N1 178.0(4)
C3 C2 C1 Ni1 175.4(3)
C3 C2 C1 C6 0.3(5)
C16 C17 C18 C19 0.7(7)
C40 C39 C44 C43 0.7(6)
C8 C6 C5 C4 -177.9(4)
C8 C6 C1 Ni1 2.8(4)
C8 C6 C1 C2 177.8(3)
C29 C30 C31 C32 -0.9(7)
C38 C33 C34 C35 -0.2(6)
C38 C37 C36 C35 -0.4(7)
C20 C19 C18 C17 0.0(7)
C1 C2 C7 N1 -4.0(4)
C1 C2 C3 C4 0.1(6)
C1 C6 C5 C4 0.2(6)
C1 C6 C8 N2 0.3(4)
C15 P1 N1 Ni1 -54.6(3)
C15 P1 N1 C7 138.0(3)
C15 P1 C9 C14 -34.3(4)
C15 P1 C9 C10 148.4(3)
C15 P1 C21 C26 -63.3(4)
C15 P1 C21 C22 117.7(3)
C15 C16 C17 C18 -0.9(6)
C15 C20 C19 C18 -0.6(6)
C32 C27 C28 C29 -1.2(6)
C44 C39 C40 C41 -1.5(6)
C25 C26 C21 P1 179.8(3)
C25 C26 C21 C22 -1.2(6)
C34 C33 C38 C37 1.2(6)
C19 C20 C15 P1 179.6(3)
C19 C20 C15 C16 0.4(6)
C37 C36 C35 C34 1.5(7)
C17 C16 C15 P1 -178.9(3)
C17 C16 C15 C20 0.3(6)
C43 C42 C41 C40 -0.5(7)
C14 C9 C10 C11 1.5(6)
C14 C13 C12 C11 0.3(8)
C41 C42 C43 C44 -0.3(7)
C10 C9 C14 C13 -1.8(6)
C10 C11 C12 C13 -0.6(8)
_cod_database_fobs_code 2021765