#------------------------------------------------------------------------------ #$Date: 2019-09-08 06:42:15 +0300 (Sun, 08 Sep 2019) $ #$Revision: 218078 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021767.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_2021767 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 H61 N2 P2)]' _chemical_formula_moiety 'C44 H61 Br N2 Ni P2' _chemical_formula_sum 'C44 H61 Br N2 Ni P2' _chemical_formula_weight 818.50 _chemical_name_systematic (2,6-Bis{[(dicyclohexylphenyl-\l^5^-phosphanylidene)imino]methyl}phenyl-\k^3^N,C^1^,N')bromidonickel(II) _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 93.740(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.9686(12) _cell_length_b 10.4728(5) _cell_length_c 17.5599(9) _cell_measurement_reflns_used 6324 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.3810 _cell_measurement_theta_min 2.2360 _cell_volume 4031.5(4) _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 293(2) _diffrn_detector 'Rigaku XtaLAB area detector' _diffrn_detector_area_resol_mean 13.6612 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku XtaLAB mini' _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 0.0807 _diffrn_reflns_av_unetI/netI 0.0662 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 41828 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.484 _diffrn_reflns_theta_min 1.858 _diffrn_source 'Sealed Tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.585 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.86615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (REQAB; Rigaku, 1998) ; _exptl_crystal_colour 'clear dark red' _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method "'not measured" _exptl_crystal_description plate _exptl_crystal_F_000 1728 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.112 _refine_diff_density_min -1.135 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 455 _refine_ls_number_reflns 9264 _refine_ls_number_restraints 52 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0554 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+6.6008P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1368 _refine_ls_wR_factor_ref 0.1620 _reflns_number_gt 6380 _reflns_number_total 9264 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jx3045sup1.cif _cod_data_source_block x964b77res _cod_database_code 2021767 _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 0.86615 _shelx_estimated_absorpt_t_max 1.00000 _shelx_hkl_file ; -2 0 0 4978.37 46.50 3 0 0 73.33 6.98 -3 0 0 61.14 6.61 -4 0 0 2018.41 31.84 4 0 0 2212.48 32.91 4 0 0 2122.58 43.23 -4 0 0 2105.31 43.50 5 0 0 2245.56 49.21 -5 0 0 2237.27 49.82 5 0 0 2295.64 37.45 6 0 0 123.64 16.52 -6 0 0 126.61 13.15 6 0 0 117.71 9.32 -7 0 0 2381.10 60.21 7 0 0 2404.06 60.48 7 0 0 2483.32 45.89 -8 0 0 203.46 18.96 8 0 0 215.44 20.00 8 0 0 188.89 13.78 9 0 0 474.37 22.81 9 0 0 442.85 29.62 -9 0 0 485.40 31.06 10 0 0 47.96 12.32 -10 0 0 59.87 12.69 10 0 0 50.33 8.12 11 0 0 2157.71 71.31 -11 0 0 2040.05 69.84 11 0 0 2168.62 52.96 12 0 0 703.91 42.81 -12 0 0 589.35 39.25 12 0 0 554.78 27.91 13 0 0 1829.76 52.30 -13 0 0 1839.94 72.26 13 0 0 1939.79 73.16 14 0 0 221.41 25.91 -14 0 0 231.51 27.23 14 0 0 232.25 19.42 -15 0 0 36.35 9.22 15 0 0 43.03 9.42 15 0 0 14.05 7.90 16 0 0 15.00 5.85 16 0 0 19.93 8.10 -16 0 0 11.66 9.88 -17 0 0 6.07 12.25 17 0 0 11.78 4.71 17 0 0 11.20 9.59 18 0 0 -0.07 6.44 18 0 0 1.71 3.93 -18 0 0 -11.91 11.51 19 0 0 110.27 15.64 -19 0 0 103.97 19.52 19 0 0 107.78 20.79 20 0 0 68.21 17.78 -20 0 0 30.52 14.34 21 0 0 -4.76 6.88 -21 0 0 9.49 15.30 22 0 0 102.05 21.15 -22 0 0 109.29 26.35 -23 0 0 113.85 27.47 23 0 0 134.03 26.01 24 0 0 265.33 38.03 -24 0 0 313.34 43.13 -25 0 0 296.94 44.77 25 0 0 305.09 43.50 26 0 0 347.78 46.67 -26 0 0 362.59 49.18 27 0 0 205.29 37.03 -27 0 0 220.41 40.57 -28 0 0 -1.05 12.03 28 0 0 4.49 11.30 0 1 0 3.90 1.44 0 1 0 4.56 1.59 1 1 0 2612.42 31.64 1 1 0 2573.12 31.06 2 1 0 1892.83 33.74 -2 1 0 1894.07 29.49 2 -1 0 1931.03 35.59 -2 -1 0 1772.70 29.84 3 1 0 209.83 12.95 -3 -1 0 194.94 11.44 3 -1 0 214.17 9.34 -3 1 0 216.00 12.08 3 -1 0 206.12 12.66 -3 1 0 218.32 9.88 4 -1 0 18.93 3.90 -4 1 0 10.88 3.15 -4 -1 0 19.00 4.34 4 1 0 8.42 3.49 4 -1 0 17.17 3.29 5 1 0 1.12 3.29 -5 1 0 4.95 2.93 5 -1 0 8.32 3.81 -5 -1 0 19.61 5.54 5 -1 0 11.22 4.61 -6 1 0 136.91 12.71 6 -1 0 161.50 13.86 -6 -1 0 145.54 13.98 6 -1 0 140.76 12.17 6 1 0 134.59 14.91 7 -1 0 211.92 16.44 7 -1 0 240.47 17.71 7 1 0 230.71 10.25 -7 -1 0 240.37 18.91 7 1 0 213.88 19.13 -7 1 0 226.85 19.49 8 1 0 173.40 9.98 8 -1 0 125.61 13.78 -8 -1 0 150.30 16.42 -8 1 0 187.94 19.54 8 1 0 142.18 16.61 8 -1 0 147.89 14.91 -9 -1 0 609.08 34.45 9 -1 0 635.75 31.18 9 1 0 647.60 38.23 -9 1 0 654.39 37.69 9 -1 0 600.79 31.67 9 1 0 663.22 20.88 -10 1 0 931.69 46.86 10 -1 0 891.34 38.30 10 -1 0 914.49 41.16 10 1 0 950.40 48.13 -10 -1 0 980.36 44.84 10 1 0 964.48 26.91 -11 1 0 76.19 15.39 11 1 0 61.09 13.32 11 -1 0 61.96 10.90 11 -1 0 52.01 11.08 -11 -1 0 73.31 13.61 11 1 0 52.94 6.86 12 1 0 1749.33 71.14 12 -1 0 1818.42 57.79 -12 -1 0 1689.12 66.11 12 1 0 1728.20 40.40 -12 1 0 1843.42 71.33 12 -1 0 1708.61 62.14 13 1 0 35.08 6.49 -13 1 0 28.27 11.73 13 -1 0 30.98 9.88 13 1 0 36.62 12.91 -13 -1 0 40.30 12.71 13 -1 0 31.30 8.64 14 1 0 413.87 21.39 -14 -1 0 430.19 36.28 14 -1 0 400.99 33.01 14 -1 0 420.82 29.66 14 1 0 426.70 37.91 -14 1 0 457.44 38.50 -15 -1 0 434.05 37.91 15 -1 0 430.85 35.52 15 -1 0 404.53 29.79 -15 1 0 452.63 40.23 15 1 0 389.67 21.49 15 1 0 486.13 42.03 16 1 0 6.15 2.49 16 1 0 16.91 10.00 -16 1 0 23.35 11.22 16 -1 0 -1.83 4.85 16 -1 0 22.08 8.37 -16 -1 0 34.35 13.88 17 -1 0 173.77 25.49 -17 -1 0 171.53 26.40 17 1 0 130.35 13.32 17 1 0 126.32 21.61 -17 1 0 169.99 25.35 17 -1 0 127.27 17.66 18 1 0 381.20 39.96 18 -1 0 323.07 27.96 -18 1 0 366.52 38.79 18 -1 0 348.81 35.13 -18 -1 0 345.95 38.45 19 1 0 11.73 9.66 19 -1 0 14.93 6.61 19 -1 0 31.49 13.47 -19 1 0 19.81 5.76 -20 -1 0 17.25 13.88 20 -1 0 1.02 3.93 20 -1 0 9.71 9.10 20 1 0 4.73 7.59 -20 1 0 -5.05 11.78 21 -1 0 67.50 12.37 21 -1 0 99.09 20.83 -21 -1 0 91.21 22.27 21 1 0 73.16 21.22 -21 1 0 57.28 15.17 22 1 0 33.52 14.27 -22 -1 0 41.77 17.27 -22 1 0 11.93 8.64 22 -1 0 27.69 12.00 -23 -1 0 69.50 22.37 23 -1 0 66.75 19.59 23 1 0 82.31 22.30 -23 1 0 51.99 17.27 24 1 0 263.96 39.30 -24 -1 0 272.38 39.50 -24 1 0 225.85 37.98 24 -1 0 274.13 38.08 -25 1 0 152.84 31.15 25 1 0 133.74 31.03 25 -1 0 111.37 25.49 -25 -1 0 126.91 30.64 26 -1 0 38.54 18.52 -26 1 0 50.96 21.57 26 1 0 73.58 24.62 -26 -1 0 47.21 20.30 -27 1 0 46.45 24.32 -27 -1 0 18.96 16.81 27 -1 0 9.17 10.83 27 1 0 14.95 13.47 -28 1 0 15.17 7.78 -28 -1 0 10.08 15.34 28 -1 0 8.49 11.91 0 -2 0 1813.98 38.74 0 -2 0 1685.56 29.98 0 -2 0 1844.79 35.59 -1 2 0 -3.85 3.51 -1 -2 0 3.39 1.76 1 -2 0 1.15 3.22 -1 -2 0 -2.00 2.05 1 -2 0 3.85 1.76 -1 -2 0 0.61 2.39 -2 2 0 45.28 6.66 2 -2 0 36.72 3.93 -2 -2 0 40.20 5.15 -2 -2 0 48.35 5.83 2 -2 0 32.18 6.22 -2 -2 0 41.86 5.78 -3 -2 0 50.84 5.12 3 -2 0 50.67 8.07 -3 -2 0 42.86 6.20 3 2 0 38.89 5.90 -3 2 0 47.91 6.66 3 -2 0 53.26 4.85 -4 2 0 485.89 21.74 4 2 0 469.05 24.05 4 -2 0 512.67 16.98 4 2 0 463.20 13.00 4 -2 0 433.31 24.20 -4 -2 0 466.03 21.74 -5 -2 0 1403.62 40.52 5 2 0 1348.22 43.74 5 2 0 1345.39 20.05 5 2 0 1362.27 22.25 5 -2 0 1326.51 43.69 5 -2 0 1313.11 30.13 -5 2 0 1322.56 38.11 6 -2 0 2428.23 45.13 6 2 0 2464.05 63.40 -6 -2 0 2399.57 57.01 6 -2 0 2324.29 60.38 -6 2 0 2292.42 54.38 -7 -2 0 2083.04 56.77 7 -2 0 2077.72 46.11 7 -2 0 2165.06 60.67 -7 2 0 2081.72 56.50 7 2 0 2125.95 63.50 -8 2 0 1349.27 49.13 8 -2 0 1311.67 49.18 -8 -2 0 1303.19 47.42 8 2 0 1422.77 55.11 8 -2 0 1288.04 39.23 9 -2 0 -0.39 2.98 -9 -2 0 3.37 3.54 9 2 0 -2.95 6.12 -9 2 0 5.98 4.29 9 -2 0 4.66 6.22 10 -2 0 45.52 8.29 -10 2 0 38.96 5.15 10 2 0 53.94 13.30 -10 -2 0 69.45 13.52 11 2 0 338.05 31.25 -11 2 0 316.63 28.45 -11 -2 0 320.07 27.74 11 -2 0 284.55 22.25 11 2 0 318.75 11.08 11 -2 0 351.42 27.25 12 -2 0 7.64 4.27 12 2 0 -1.39 5.54 12 2 0 2.34 1.37 -12 -2 0 0.73 4.20 12 -2 0 -0.61 4.03 13 -2 0 30.96 8.54 13 -2 0 21.69 8.59 13 2 0 16.32 7.66 -13 2 0 24.52 5.54 -13 -2 0 25.74 9.25 14 -2 0 84.87 15.15 -14 -2 0 107.93 18.96 14 -2 0 89.78 15.42 -14 2 0 136.30 21.66 15 -2 0 5.85 5.73 -15 2 0 1.78 7.93 15 2 0 12.56 9.69 15 -2 0 2.05 5.64 -15 -2 0 6.37 7.68 16 -2 0 95.58 16.27 16 2 0 92.53 22.15 -16 2 0 102.97 21.35 -16 -2 0 103.53 19.91 16 -2 0 74.19 14.86 -17 -2 0 299.92 35.28 17 2 0 374.47 40.69 17 -2 0 343.95 31.88 17 -2 0 305.07 30.69 -17 2 0 352.88 39.59 18 2 0 196.90 30.54 -18 2 0 168.26 27.69 -18 -2 0 168.57 27.52 18 -2 0 153.08 21.81 18 -2 0 150.15 23.96 -19 -2 0 522.36 48.33 19 -2 0 510.87 41.03 19 -2 0 532.82 42.89 -19 2 0 657.46 53.96 19 2 0 605.84 54.13 20 2 0 -6.07 9.03 20 -2 0 16.69 11.32 -20 2 0 17.83 10.22 -20 -2 0 5.90 8.44 20 -2 0 -2.46 7.68 21 2 0 33.93 14.52 -21 2 0 59.01 15.54 21 -2 0 50.69 13.61 -21 -2 0 60.01 19.03 21 -2 0 56.77 14.64 22 -2 0 42.50 14.08 22 2 0 43.20 18.81 -22 2 0 31.15 11.54 -22 -2 0 26.10 12.12 22 -2 0 32.08 12.88 23 2 0 14.64 13.05 23 -2 0 3.98 6.73 23 -2 0 9.56 8.64 -23 -2 0 16.05 10.66 -23 2 0 14.86 10.81 24 2 0 39.89 18.05 -24 2 0 33.42 13.27 -24 -2 0 42.16 16.98 24 -2 0 11.91 6.88 25 -2 0 91.04 21.57 -25 -2 0 103.27 27.32 25 2 0 81.51 23.79 -25 2 0 94.68 22.81 -26 -2 0 8.44 8.86 -26 2 0 -17.25 21.52 26 -2 0 -10.15 11.64 26 2 0 4.49 12.25 27 -2 0 13.15 12.61 27 2 0 12.76 15.03 -27 2 0 -11.83 13.17 -27 -2 0 -16.59 18.25 28 2 0 92.04 31.42 -28 -2 0 51.57 24.32 -28 2 0 55.79 23.61 0 -3 0 2.17 1.85 0 -3 0 -4.64 3.66 0 -3 0 0.68 2.61 1 -3 0 1397.94 31.23 -1 -3 0 1438.78 35.72 1 -3 0 1476.52 45.16 -1 -3 0 1475.22 41.03 -1 -3 0 1478.93 39.79 -1 3 0 1375.20 37.98 2 -3 0 853.14 22.79 -2 -3 0 842.82 31.03 2 -3 0 836.60 35.45 -2 -3 0 893.39 29.93 -2 -3 0 899.20 30.32 -2 3 0 890.80 30.37 -3 -3 0 814.18 30.91 3 -3 0 771.07 35.47 -3 -3 0 861.09 27.76 -3 -3 0 715.47 29.76 -3 3 0 773.85 29.18 3 -3 0 761.51 21.54 4 -3 0 410.33 27.05 -4 3 0 426.80 22.25 -4 -3 0 438.44 19.00 4 3 0 379.47 23.74 -4 -3 0 419.68 23.00 4 -3 0 402.40 16.13 5 3 0 1876.16 33.98 -5 3 0 1904.61 49.84 5 -3 0 1863.89 36.52 -5 -3 0 1930.64 51.50 5 -3 0 1820.47 57.92 5 3 0 1983.28 57.28 6 3 0 675.63 35.59 6 3 0 646.14 18.42 -6 3 0 672.46 31.25 6 -3 0 663.31 23.27 6 -3 0 690.37 37.06 -6 -3 0 668.56 32.28 7 3 0 2301.45 32.15 7 -3 0 2245.63 46.21 -7 -3 0 2306.94 63.21 7 3 0 2343.63 70.38 7 -3 0 2181.28 67.80 -7 3 0 2221.80 59.65 8 3 0 368.76 29.08 -8 3 0 383.52 26.91 8 -3 0 394.89 21.22 -8 -3 0 375.20 26.69 8 3 0 368.45 11.56 8 -3 0 382.38 29.35 9 -3 0 110.41 11.98 9 3 0 107.39 19.13 -9 -3 0 82.75 13.83 -9 3 0 114.34 16.47 9 -3 0 94.92 15.03 -10 -3 0 1.78 4.37 -10 3 0 -0.98 5.12 10 3 0 -1.32 7.32 10 -3 0 12.66 11.44 10 -3 0 0.46 3.44 -11 -3 0 -3.37 3.37 11 -3 0 10.44 6.37 -11 3 0 -2.22 4.54 11 -3 0 4.83 4.20 11 3 0 4.34 5.32 -12 -3 0 214.73 24.37 12 3 0 185.31 25.81 -12 3 0 201.70 23.79 12 -3 0 209.97 19.64 12 -3 0 187.85 22.59 13 -3 0 162.67 17.86 -13 3 0 151.33 21.08 13 -3 0 190.09 23.88 13 3 0 194.48 26.93 -13 -3 0 181.70 23.08 14 -3 0 338.73 27.42 14 -3 0 357.00 33.37 -14 -3 0 357.22 34.45 14 3 0 374.45 38.64 -14 3 0 357.18 35.81 15 -3 0 9.42 6.10 -15 -3 0 1.29 4.29 15 3 0 17.13 5.66 -15 3 0 23.05 14.44 15 -3 0 10.49 5.03 -16 -3 0 402.33 38.18 16 -3 0 343.61 33.54 -16 3 0 427.87 42.30 16 -3 0 332.15 29.45 16 3 0 401.18 42.03 17 -3 0 -2.68 4.95 17 -3 0 -6.73 8.00 -17 -3 0 -12.42 6.98 17 3 0 -2.98 9.27 18 3 0 277.28 37.96 -18 3 0 253.45 34.64 18 -3 0 226.02 28.35 18 -3 0 244.76 28.03 -18 -3 0 251.05 32.28 19 -3 0 100.88 20.57 -19 3 0 116.37 25.62 19 3 0 124.00 25.52 -19 -3 0 123.22 22.25 19 -3 0 98.53 18.54 20 3 0 150.94 29.52 -20 3 0 132.59 23.03 20 -3 0 111.39 20.30 20 -3 0 121.05 20.59 -20 -3 0 119.68 22.10 21 -3 0 -4.03 8.07 21 -3 0 17.54 11.47 21 3 0 -2.17 9.71 -21 -3 0 7.66 11.78 -21 3 0 10.42 11.91 22 3 0 74.06 19.57 22 -3 0 93.02 19.88 -22 -3 0 73.53 16.42 -22 3 0 78.97 18.00 22 -3 0 82.68 18.81 -23 3 0 2.32 11.93 23 3 0 -7.34 10.37 23 -3 0 0.32 6.42 -23 -3 0 -14.91 13.34 23 -3 0 -5.95 7.32 -24 3 0 10.10 7.07 24 3 0 16.93 17.42 24 -3 0 -0.41 6.66 24 -3 0 3.46 8.22 -24 -3 0 -15.27 16.91 25 3 0 17.42 13.54 -25 -3 0 0.95 11.76 -25 3 0 -16.86 16.76 25 -3 0 -5.05 8.29 -26 -3 0 -6.29 17.30 26 -3 0 30.10 15.49 -26 3 0 -17.93 18.88 26 3 0 6.00 9.37 -27 3 0 -5.76 15.08 -27 -3 0 -6.61 11.91 27 3 0 14.30 12.51 0 -4 0 43.96 8.29 0 -4 0 36.15 7.05 0 -4 0 35.54 6.64 1 -4 0 155.13 11.83 -1 -4 0 138.18 12.27 -1 -4 0 155.52 14.71 1 -4 0 134.66 15.74 -1 4 0 189.33 15.32 -1 -4 0 132.03 14.22 -2 -4 0 5.39 4.27 -2 -4 0 2.37 2.66 2 -4 0 3.29 5.00 2 -4 0 7.68 2.61 -2 4 0 4.64 3.12 -2 -4 0 -6.88 4.22 -3 -4 0 138.98 14.42 -3 4 0 119.05 13.44 -3 -4 0 142.67 13.81 3 -4 0 137.32 16.47 3 -4 0 145.89 10.81 -3 -4 0 143.30 14.78 4 4 0 387.06 25.83 4 -4 0 371.96 17.10 -4 4 0 354.37 22.81 -4 -4 0 370.45 21.20 -4 -4 0 369.59 23.98 4 -4 0 359.69 28.32 5 -4 0 7.42 8.00 -5 -4 0 7.78 3.20 -5 -4 0 3.81 3.95 -5 4 0 10.00 3.73 5 4 0 -3.07 6.27 -6 -4 0 681.64 35.93 6 4 0 673.95 24.37 6 -4 0 650.46 23.74 -6 4 0 705.01 34.10 6 4 0 706.13 39.03 6 -4 0 648.99 39.89 7 4 0 306.82 27.25 -7 -4 0 282.87 24.15 -7 4 0 305.48 23.71 8 4 0 471.00 17.91 8 4 0 510.01 36.76 -8 4 0 524.31 32.35 8 -4 0 448.05 35.01 -8 -4 0 470.93 32.01 8 -4 0 474.18 22.66 -9 -4 0 309.60 26.37 9 -4 0 308.92 30.27 -9 4 0 325.07 26.86 9 4 0 308.73 13.37 9 -4 0 330.39 19.91 9 4 0 301.60 29.35 10 -4 0 88.51 17.42 10 4 0 65.31 5.34 10 -4 0 66.36 9.54 10 4 0 52.47 12.54 -10 4 0 66.43 12.61 -10 -4 0 75.63 13.64 -11 -4 0 20.05 7.44 11 -4 0 10.64 3.59 -11 4 0 24.93 10.08 11 4 0 17.22 7.27 11 -4 0 20.49 10.34 12 -4 0 -3.66 4.32 12 4 0 6.64 7.17 -12 -4 0 -6.39 9.93 12 -4 0 4.12 7.17 -12 4 0 -1.51 5.39 13 4 0 -10.49 10.15 -13 -4 0 -3.10 5.27 -13 4 0 0.68 7.34 13 -4 0 -9.88 10.39 13 -4 0 3.12 2.95 14 -4 0 -0.07 7.64 -14 4 0 -4.54 9.73 -14 -4 0 -0.07 4.56 14 4 0 -2.05 10.95 14 -4 0 1.37 4.03 15 -4 0 -1.17 10.05 -15 4 0 -9.27 9.71 -15 -4 0 -0.20 4.93 15 -4 0 13.03 8.47 16 4 0 33.50 12.25 16 -4 0 26.47 8.32 -16 -4 0 30.25 13.93 -16 4 0 36.25 13.73 16 -4 0 38.54 10.71 17 -4 0 421.87 33.47 -17 -4 0 389.13 40.03 17 4 0 452.34 48.74 17 -4 0 431.02 40.57 -17 4 0 464.66 47.52 -18 -4 0 -7.83 13.03 18 -4 0 11.44 9.27 -18 4 0 9.05 15.44 18 4 0 4.42 13.42 18 -4 0 3.90 6.37 19 4 0 402.26 47.99 -19 4 0 408.58 46.60 -19 -4 0 352.00 39.84 19 -4 0 379.98 40.28 19 -4 0 347.90 32.32 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-22 32.49 16.88 -7 0 22 31.67 15.25 6 0 -22 -8.51 8.86 -6 0 22 -6.29 7.49 5 0 -22 10.17 8.98 -5 0 22 34.64 16.35 4 0 -22 27.42 18.22 -4 0 22 10.25 7.61 3 0 -22 7.73 10.64 -3 0 22 13.08 13.86 2 0 -22 8.07 8.68 -2 0 22 9.51 8.86 1 0 -22 22.37 17.71 -1 0 22 -17.44 16.71 0 0 -22 117.51 28.49 0 0 22 67.84 21.91 -1 0 -22 95.48 26.10 1 0 22 116.05 26.49 -2 0 -22 363.35 50.30 2 0 22 318.29 42.91 -3 0 -22 0.90 11.42 3 0 22 11.12 14.15 -4 0 -22 141.18 28.45 4 0 22 200.31 34.81 -5 0 -22 -11.81 18.35 5 0 22 -4.00 7.51 8 -1 -22 34.93 17.86 8 1 -22 56.33 21.71 -8 -1 22 36.13 16.71 7 -1 -22 30.52 13.86 7 1 -22 51.84 21.39 -7 -1 22 15.08 11.03 6 -1 -22 -12.47 9.61 -6 -1 22 8.12 8.20 -6 1 22 -8.10 10.71 5 -1 -22 29.32 17.10 5 1 -22 48.25 26.57 -5 -1 22 37.52 17.05 -5 1 22 20.91 8.25 4 -1 -22 58.01 25.10 4 1 -22 32.96 21.44 -4 -1 22 36.47 16.15 -4 1 22 34.98 13.81 3 1 -22 -8.78 18.22 -3 -1 22 8.20 7.59 -3 1 22 6.46 7.83 2 -1 -22 -6.71 11.78 2 1 -22 3.71 8.90 -2 -1 22 0.98 9.34 -2 1 22 -15.08 12.81 1 -1 -22 82.24 27.42 1 1 -22 23.86 17.88 -1 -1 22 36.54 12.05 -1 1 22 46.13 15.05 0 -1 -22 58.89 24.83 0 1 -22 24.20 12.56 0 -1 22 36.18 15.52 0 1 22 31.30 16.03 -1 -1 -22 103.90 29.18 -1 1 -22 58.55 17.76 1 -1 22 98.05 23.13 1 1 22 76.43 21.79 -2 -1 -22 94.90 30.25 -2 1 -22 49.89 17.83 2 -1 22 71.36 24.69 2 1 22 64.67 21.25 -3 -1 -22 106.36 31.81 -3 1 -22 58.21 18.64 3 -1 22 85.75 26.42 3 1 22 67.21 22.79 -4 -1 -22 35.76 21.49 -4 1 -22 5.54 10.66 4 -1 22 12.61 11.27 4 1 22 19.59 10.39 -5 -1 -22 14.20 14.73 -5 1 -22 -3.85 14.13 5 -1 22 1.95 11.64 5 1 22 -1.49 8.25 8 -2 -22 2.81 12.25 -8 -2 22 11.37 13.25 8 2 -22 25.15 15.86 7 -2 -22 -4.51 9.95 -7 -2 22 -1.56 9.71 7 2 -22 6.17 11.95 6 -2 -22 2.88 13.10 -6 -2 22 4.46 10.47 6 2 -22 13.47 10.00 5 -2 -22 126.78 32.49 -5 -2 22 67.26 20.76 5 2 -22 71.21 22.61 4 -2 -22 32.93 17.59 -4 -2 22 53.74 19.64 4 2 -22 57.55 18.71 3 -2 -22 72.21 23.44 -3 -2 22 78.99 20.54 3 2 -22 61.04 23.10 -3 2 22 86.56 22.81 2 -2 -22 7.95 11.91 2 2 -22 -20.64 16.69 -2 -2 22 -7.32 8.68 -2 2 22 -10.39 10.51 1 -2 -22 15.08 17.61 1 2 -22 1.85 14.42 -1 -2 22 25.08 15.59 -1 2 22 -3.15 9.66 0 -2 -22 27.62 16.83 0 2 -22 58.72 23.00 0 -2 22 27.52 13.00 0 2 22 33.74 13.71 -1 -2 -22 24.25 17.35 -1 2 -22 14.25 15.34 1 -2 22 3.95 12.98 1 2 22 0.90 12.64 -2 -2 -22 14.91 15.17 -2 2 -22 15.10 11.44 2 -2 22 16.08 11.88 2 2 22 24.98 15.59 -3 -2 -22 20.57 16.88 -3 2 -22 3.12 13.12 3 -2 22 -7.34 10.25 3 2 22 19.37 14.17 -4 -2 -22 40.42 19.98 -4 2 -22 41.40 19.30 4 -2 22 -0.73 10.54 4 2 22 6.59 7.56 5 -3 -22 -3.51 9.73 -5 -3 22 4.12 10.34 5 3 -22 -0.15 9.69 4 -3 -22 107.29 27.08 -4 -3 22 129.47 29.23 4 3 -22 116.42 29.71 3 -3 -22 33.67 12.88 -3 -3 22 31.91 17.54 3 3 -22 15.08 11.54 2 -3 -22 18.30 16.13 -2 -3 22 -24.08 16.13 2 3 -22 20.05 15.81 1 -3 -22 15.91 9.73 -1 -3 22 24.05 11.03 1 3 -22 30.20 17.81 0 -3 -22 12.12 16.49 0 -3 22 -1.56 12.49 0 3 -22 -4.49 10.27 -1 -3 -22 6.83 10.88 1 -3 22 1.83 7.90 -1 3 -22 5.83 14.15 1 3 22 9.49 7.90 -2 -3 -22 18.35 17.44 2 -3 22 -3.56 14.91 -2 3 -22 7.66 8.10 2 3 22 -1.00 11.61 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 55384 _shelx_res_file ; x964b77res.res created by SHELXL-2014/7 TITL x964b77res_a.res in P2(1)/c REM Old TITL x964b 77res in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.118, Rweak 0.003, Alpha 0.061, Orientation as input REM Formula found by SHELXT: C44 N2 P2 Ni2 CELL 0.71073 21.9686 10.4728 17.5599 90 93.74 90 ZERR 4 0.0012 0.0005 0.0009 0 0.005 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Br N Ni P UNIT 176 244 4 8 4 8 DELU C10 C11 C12 C13 C14 SIMU C10 C11 C12 C13 C14 RIGU C10 > C14 L.S. 5 PLAN 5 LIST 6 fmap 2 53 acta REM REM REM WGHT 0.069200 6.600800 FVAR 0.27583 BR1 3 0.182812 0.703763 0.750358 11.00000 0.03444 0.03355 = 0.03976 -0.00610 0.00044 0.00182 NI1 5 0.266099 0.587443 0.698395 11.00000 0.01931 0.02189 = 0.02128 -0.00263 0.00286 -0.00278 P1 6 0.152966 0.401001 0.634775 11.00000 0.01772 0.02107 = 0.01921 -0.00188 0.00202 -0.00164 P2 6 0.349393 0.733134 0.830356 11.00000 0.02052 0.02256 = 0.02325 -0.00252 0.00183 -0.00222 N1 4 0.224218 0.434902 0.652078 11.00000 0.01665 0.02249 = 0.02508 -0.00500 0.00461 -0.00002 N2 4 0.329782 0.703768 0.742227 11.00000 0.02702 0.02640 = 0.02218 -0.00342 0.00249 -0.00821 C1 1 0.328475 0.535741 0.641162 11.00000 0.01957 0.03114 = 0.01986 0.00162 0.00109 -0.00385 C2 1 0.322983 0.424538 0.598343 11.00000 0.02037 0.02757 = 0.02126 0.00045 0.00156 0.00131 C3 1 0.369826 0.389136 0.552655 11.00000 0.02485 0.03703 = 0.03184 -0.00802 0.00422 0.00196 AFIX 43 H3 2 0.366621 0.314442 0.524031 11.00000 -1.20000 AFIX 0 C4 1 0.421158 0.465654 0.550065 11.00000 0.02567 0.04772 = 0.03486 -0.00142 0.01105 0.00300 AFIX 43 H4 2 0.452485 0.441229 0.520015 11.00000 -1.20000 AFIX 0 C5 1 0.426416 0.578041 0.591649 11.00000 0.02220 0.04868 = 0.02839 0.00379 0.00381 -0.00705 AFIX 43 H5 2 0.460653 0.629594 0.588720 11.00000 -1.20000 AFIX 0 C6 1 0.379876 0.613309 0.638016 11.00000 0.02417 0.03047 = 0.02215 0.00259 0.00292 -0.00189 C7 1 0.265924 0.351701 0.608774 11.00000 0.02438 0.02515 = 0.02911 -0.00663 0.00528 0.00119 AFIX 23 H7A 2 0.275213 0.273751 0.637021 11.00000 -1.20000 H7B 2 0.246365 0.329003 0.559513 11.00000 -1.20000 AFIX 0 C8 1 0.378082 0.728266 0.688570 11.00000 0.02254 0.03559 = 0.02627 0.00026 0.00208 -0.01198 AFIX 23 H8A 2 0.417228 0.740544 0.716452 11.00000 -1.20000 H8B 2 0.368537 0.804177 0.658470 11.00000 -1.20000 AFIX 0 C9 1 0.105547 0.434036 0.714178 11.00000 0.02011 0.03165 = 0.02059 -0.00253 0.00380 -0.00115 C15 1 0.116333 0.476599 0.549609 11.00000 0.01778 0.02544 = 0.02119 0.00039 0.00004 -0.00371 AFIX 13 H15 2 0.076459 0.435918 0.539423 11.00000 -1.20000 AFIX 0 C16 1 0.105096 0.620930 0.561956 11.00000 0.04021 0.02335 = 0.02880 -0.00048 -0.00551 -0.00145 AFIX 23 H16A 2 0.080276 0.632542 0.605134 11.00000 -1.20000 H16B 2 0.143773 0.663760 0.573326 11.00000 -1.20000 AFIX 0 C17 1 0.072740 0.680201 0.490544 11.00000 0.04547 0.02757 = 0.03597 0.00346 -0.01058 -0.00053 AFIX 23 H17A 2 0.032417 0.642981 0.482296 11.00000 -1.20000 H17B 2 0.067864 0.771186 0.498499 11.00000 -1.20000 AFIX 0 C18 1 0.108112 0.658721 0.420202 11.00000 0.04431 0.04934 = 0.03336 0.01717 -0.01213 -0.01388 AFIX 23 H18A 2 0.085037 0.692662 0.375753 11.00000 -1.20000 H18B 2 0.146590 0.704252 0.425906 11.00000 -1.20000 AFIX 0 C19 1 0.120287 0.518019 0.408168 11.00000 0.03281 0.05877 = 0.02208 0.00693 0.00127 -0.00537 AFIX 23 H19A 2 0.145405 0.507753 0.365155 11.00000 -1.20000 H19B 2 0.081939 0.474271 0.396165 11.00000 -1.20000 AFIX 0 C20 1 0.152508 0.457593 0.478976 11.00000 0.02902 0.03960 = 0.02473 0.00154 0.00369 -0.00037 AFIX 23 H20A 2 0.192635 0.495451 0.487916 11.00000 -1.20000 H20B 2 0.157820 0.366946 0.470207 11.00000 -1.20000 AFIX 0 C21 1 0.143675 0.230277 0.620910 11.00000 0.02182 0.02338 = 0.02100 -0.00121 0.00411 -0.00346 C22 1 0.103233 0.176390 0.564468 11.00000 0.02986 0.03258 = 0.02395 -0.00133 0.00237 -0.00462 AFIX 43 H22 2 0.082880 0.228545 0.528286 11.00000 -1.20000 AFIX 0 C23 1 0.093611 0.044912 0.562678 11.00000 0.03210 0.02898 = 0.03161 -0.00200 -0.00137 -0.01008 AFIX 43 H23 2 0.067255 0.009334 0.524861 11.00000 -1.20000 AFIX 0 C24 1 0.123047 -0.032599 0.616805 11.00000 0.04179 0.02283 = 0.03598 -0.00328 0.00900 -0.00857 AFIX 43 H24 2 0.115826 -0.120103 0.615923 11.00000 -1.20000 AFIX 0 C25 1 0.163301 0.019032 0.672478 11.00000 0.02906 0.02693 = 0.03408 0.00718 0.00844 0.00137 AFIX 43 H25 2 0.183207 -0.033529 0.708811 11.00000 -1.20000 AFIX 0 C26 1 0.173684 0.148953 0.673696 11.00000 0.02481 0.02986 = 0.02545 -0.00225 0.00236 -0.00240 AFIX 43 H26 2 0.201345 0.182995 0.710598 11.00000 -1.20000 AFIX 0 C27 1 0.297439 0.659696 0.894644 11.00000 0.02131 0.02780 = 0.01993 -0.00369 0.00340 -0.00042 AFIX 13 H27 2 0.255960 0.685399 0.877181 11.00000 -1.20000 AFIX 0 C28 1 0.300414 0.513076 0.889172 11.00000 0.03353 0.02999 = 0.03159 -0.00097 0.00704 -0.00648 AFIX 23 H28A 2 0.289502 0.486729 0.837106 11.00000 -1.20000 H28B 2 0.341771 0.484679 0.902490 11.00000 -1.20000 AFIX 0 C29 1 0.256994 0.450977 0.942760 11.00000 0.03860 0.03185 = 0.03944 0.00021 0.01154 -0.00678 AFIX 23 H29A 2 0.215313 0.472798 0.926152 11.00000 -1.20000 H29B 2 0.261066 0.358892 0.940040 11.00000 -1.20000 AFIX 0 C30 1 0.269873 0.493910 1.024670 11.00000 0.03691 0.04516 = 0.03653 0.00903 0.00850 0.00377 AFIX 23 H30A 2 0.310485 0.466796 1.042801 11.00000 -1.20000 H30B 2 0.240819 0.454555 1.056722 11.00000 -1.20000 AFIX 0 C31 1 0.265147 0.638644 1.030252 11.00000 0.03521 0.04767 = 0.02315 0.00050 0.00643 0.00209 AFIX 23 H31A 2 0.274891 0.664806 1.082622 11.00000 -1.20000 H31B 2 0.223554 0.664677 1.016171 11.00000 -1.20000 AFIX 0 C32 1 0.308509 0.705603 0.978018 11.00000 0.03435 0.03462 = 0.02476 -0.00314 0.00380 -0.00021 AFIX 23 H32A 2 0.350384 0.687846 0.995799 11.00000 -1.20000 H32B 2 0.302287 0.797186 0.980287 11.00000 -1.20000 AFIX 0 C33 1 0.353414 0.903399 0.852327 11.00000 0.02279 0.02440 = 0.02762 0.00118 -0.00120 -0.00040 AFIX 13 H33 2 0.364512 0.912539 0.907019 11.00000 -1.20000 AFIX 0 C34 1 0.290605 0.964003 0.835900 11.00000 0.02813 0.02802 = 0.04202 -0.00509 -0.00171 0.00379 AFIX 23 H34A 2 0.277221 0.949373 0.782884 11.00000 -1.20000 H34B 2 0.261556 0.923190 0.867349 11.00000 -1.20000 AFIX 0 C35 1 0.291296 1.106915 0.851676 11.00000 0.04259 0.03073 = 0.04843 -0.00694 -0.00722 0.00849 AFIX 23 H35A 2 0.251286 1.142073 0.837596 11.00000 -1.20000 H35B 2 0.299907 1.121151 0.905892 11.00000 -1.20000 AFIX 0 C36 1 0.338505 1.175897 0.807897 11.00000 0.07318 0.02437 = 0.05804 0.00137 -0.01323 0.00673 AFIX 23 H36A 2 0.339448 1.265426 0.822078 11.00000 -1.20000 H36B 2 0.327483 1.170277 0.753605 11.00000 -1.20000 AFIX 0 C37 1 0.401475 1.117219 0.825062 11.00000 0.05111 0.03080 = 0.05248 -0.00037 0.00136 -0.00836 AFIX 23 H37A 2 0.430625 1.159354 0.794341 11.00000 -1.20000 H37B 2 0.414203 1.131305 0.878335 11.00000 -1.20000 AFIX 0 C38 1 0.401651 0.974264 0.808415 11.00000 0.03488 0.03117 = 0.03834 -0.00141 0.00158 -0.00464 AFIX 23 H38A 2 0.441703 0.939598 0.822816 11.00000 -1.20000 H38B 2 0.393433 0.960568 0.754084 11.00000 -1.20000 AFIX 0 C39 1 0.423517 0.663652 0.858055 11.00000 0.02323 0.03072 = 0.03223 0.00462 0.00559 -0.00091 C40 1 0.439635 0.550352 0.821984 11.00000 0.03583 0.03614 = 0.03722 -0.00036 0.01144 0.00906 AFIX 43 H40 2 0.414589 0.517583 0.781923 11.00000 -1.20000 AFIX 0 C41 1 0.493008 0.486982 0.846050 11.00000 0.04169 0.04588 = 0.05679 0.00791 0.01663 0.01946 AFIX 43 H41 2 0.503537 0.411800 0.821977 11.00000 -1.20000 AFIX 0 C42 1 0.530309 0.534476 0.905068 11.00000 0.03176 0.06429 = 0.08550 0.02798 0.00287 0.01665 AFIX 43 H42 2 0.565874 0.491196 0.920907 11.00000 -1.20000 AFIX 0 C43 1 0.515247 0.646393 0.941085 11.00000 0.03572 0.05604 = 0.06757 0.01653 -0.01600 -0.00814 AFIX 43 H43 2 0.540771 0.678784 0.980803 11.00000 -1.20000 AFIX 0 C44 1 0.462243 0.709833 0.917915 11.00000 0.02755 0.03692 = 0.04975 -0.00418 -0.00424 -0.00341 AFIX 43 H44 2 0.452136 0.784703 0.942620 11.00000 -1.20000 AFIX 0 C10 1 0.133439 0.379788 0.789428 11.00000 0.02670 0.04405 = 0.02057 0.00329 0.00472 0.00125 AFIX 23 H10A 2 0.136420 0.287635 0.785557 11.00000 -1.20000 H10B 2 0.174280 0.413638 0.799412 11.00000 -1.20000 AFIX 0 C11 1 0.094422 0.414579 0.855257 11.00000 0.03495 0.06629 = 0.02391 -0.00090 0.00775 0.00133 AFIX 23 H11A 2 0.093637 0.506620 0.861288 11.00000 -1.20000 H11B 2 0.112223 0.377808 0.902279 11.00000 -1.20000 AFIX 0 C12 1 0.029377 0.364887 0.840000 11.00000 0.03450 0.08955 = 0.03031 0.00279 0.01401 -0.00475 AFIX 23 H12A 2 0.004901 0.389679 0.881582 11.00000 -1.20000 H12B 2 0.029886 0.272374 0.837447 11.00000 -1.20000 AFIX 0 C13 1 0.000986 0.418886 0.764945 11.00000 0.02481 0.10027 = 0.03221 -0.00834 0.00951 0.00000 AFIX 23 H13A 2 -0.039692 0.384054 0.755227 11.00000 -1.20000 H13B 2 -0.002577 0.510895 0.769172 11.00000 -1.20000 AFIX 0 C14 1 0.039407 0.386459 0.698512 11.00000 0.02137 0.06006 = 0.02723 -0.00458 0.00427 -0.00127 AFIX 23 H14A 2 0.021663 0.425935 0.652271 11.00000 -1.20000 H14B 2 0.039506 0.294738 0.690837 11.00000 -1.20000 AFIX 0 H9 2 0.104375 0.532985 0.714667 11.00000 0.02916 HKLF 4 REM x964b77res_a.res in P2(1)/c REM R1 = 0.0554 for 6380 Fo > 4sig(Fo) and 0.0931 for all 9264 data REM 455 parameters refined using 52 restraints END WGHT 0.0691 6.6108 REM Highest difference peak 1.112, deepest hole -1.135, 1-sigma level 0.109 Q1 1 0.0995 0.5800 0.8046 11.00000 0.05 0.61 Q2 1 0.2608 1.0063 0.6989 11.00000 0.05 0.58 Q3 1 0.2644 0.8191 0.7006 11.00000 0.05 0.56 Q4 1 0.1824 0.4790 0.7529 11.00000 0.05 0.55 Q5 1 0.3416 0.7362 0.7861 11.00000 0.05 0.52 ; _shelx_res_checksum 29405 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.18281(2) 0.70376(4) 0.75036(3) 0.03600(14) Uani d 1 Ni Ni1 0.26610(2) 0.58744(5) 0.69840(3) 0.02076(13) Uani d 1 P P1 0.15297(4) 0.40100(9) 0.63478(5) 0.0193(2) Uani d 1 P P2 0.34939(5) 0.73313(10) 0.83036(6) 0.0221(2) Uani d 1 N N1 0.22422(14) 0.4349(3) 0.65208(18) 0.0213(7) Uani d 1 N N2 0.32978(16) 0.7038(3) 0.74223(18) 0.0252(7) Uani d 1 C C1 0.32847(18) 0.5357(4) 0.6412(2) 0.0235(8) Uani d 1 C C2 0.32298(18) 0.4245(4) 0.5983(2) 0.0231(8) Uani d 1 C C3 0.36983(19) 0.3891(4) 0.5527(2) 0.0311(10) Uani d 1 H H3 0.3666 0.3144 0.5240 0.037 Uiso calc 1 C C4 0.4212(2) 0.4657(5) 0.5501(3) 0.0357(10) Uani d 1 H H4 0.4525 0.4412 0.5200 0.043 Uiso calc 1 C C5 0.4264(2) 0.5780(5) 0.5916(2) 0.0330(10) Uani d 1 H H5 0.4607 0.6296 0.5887 0.040 Uiso calc 1 C C6 0.37988(18) 0.6133(4) 0.6380(2) 0.0255(9) Uani d 1 C C7 0.26592(18) 0.3517(4) 0.6088(2) 0.0261(9) Uani d 1 H H7A 0.2752 0.2738 0.6370 0.031 Uiso calc 1 H H7B 0.2464 0.3290 0.5595 0.031 Uiso calc 1 C C8 0.37808(19) 0.7283(4) 0.6886(2) 0.0281(9) Uani d 1 H H8A 0.4172 0.7405 0.7165 0.034 Uiso calc 1 H H8B 0.3685 0.8042 0.6585 0.034 Uiso calc 1 C C9 0.10555(18) 0.4340(4) 0.7142(2) 0.0240(8) Uani d 1 C C15 0.11633(17) 0.4766(4) 0.5496(2) 0.0215(8) Uani d 1 H H15 0.0765 0.4359 0.5394 0.026 Uiso calc 1 C C16 0.1051(2) 0.6209(4) 0.5620(2) 0.0311(10) Uani d 1 H H16A 0.0803 0.6325 0.6051 0.037 Uiso calc 1 H H16B 0.1438 0.6638 0.5733 0.037 Uiso calc 1 C C17 0.0727(2) 0.6802(4) 0.4905(3) 0.0369(11) Uani d 1 H H17A 0.0324 0.6430 0.4823 0.044 Uiso calc 1 H H17B 0.0679 0.7712 0.4985 0.044 Uiso calc 1 C C18 0.1081(2) 0.6587(5) 0.4202(3) 0.0430(12) Uani d 1 H H18A 0.0850 0.6927 0.3758 0.052 Uiso calc 1 H H18B 0.1466 0.7043 0.4259 0.052 Uiso calc 1 C C19 0.1203(2) 0.5180(5) 0.4082(2) 0.0379(11) Uani d 1 H H19A 0.1454 0.5078 0.3652 0.045 Uiso calc 1 H H19B 0.0819 0.4743 0.3962 0.045 Uiso calc 1 C C20 0.1525(2) 0.4576(5) 0.4790(2) 0.0310(10) Uani d 1 H H20A 0.1926 0.4955 0.4879 0.037 Uiso calc 1 H H20B 0.1578 0.3669 0.4702 0.037 Uiso calc 1 C C21 0.14367(18) 0.2303(4) 0.6209(2) 0.0219(8) Uani d 1 C C22 0.1032(2) 0.1764(4) 0.5645(2) 0.0288(9) Uani d 1 H H22 0.0829 0.2285 0.5283 0.035 Uiso calc 1 C C23 0.0936(2) 0.0449(4) 0.5627(3) 0.0310(10) Uani d 1 H H23 0.0673 0.0093 0.5249 0.037 Uiso calc 1 C C24 0.1230(2) -0.0326(4) 0.6168(3) 0.0333(10) Uani d 1 H H24 0.1158 -0.1201 0.6159 0.040 Uiso calc 1 C C25 0.1633(2) 0.0190(4) 0.6725(3) 0.0297(9) Uani d 1 H H25 0.1832 -0.0335 0.7088 0.036 Uiso calc 1 C C26 0.17368(19) 0.1490(4) 0.6737(2) 0.0267(9) Uani d 1 H H26 0.2013 0.1830 0.7106 0.032 Uiso calc 1 C C27 0.29744(18) 0.6597(4) 0.8946(2) 0.0229(8) Uani d 1 H H27 0.2560 0.6854 0.8772 0.028 Uiso calc 1 C C28 0.3004(2) 0.5131(4) 0.8892(3) 0.0315(10) Uani d 1 H H28A 0.2895 0.4867 0.8371 0.038 Uiso calc 1 H H28B 0.3418 0.4847 0.9025 0.038 Uiso calc 1 C C29 0.2570(2) 0.4510(5) 0.9428(3) 0.0362(11) Uani d 1 H H29A 0.2153 0.4728 0.9262 0.043 Uiso calc 1 H H29B 0.2611 0.3589 0.9400 0.043 Uiso calc 1 C C30 0.2699(2) 0.4939(5) 1.0247(3) 0.0393(11) Uani d 1 H H30A 0.3105 0.4668 1.0428 0.047 Uiso calc 1 H H30B 0.2408 0.4546 1.0567 0.047 Uiso calc 1 C C31 0.2651(2) 0.6386(5) 1.0303(2) 0.0351(10) Uani d 1 H H31A 0.2749 0.6648 1.0826 0.042 Uiso calc 1 H H31B 0.2236 0.6647 1.0162 0.042 Uiso calc 1 C C32 0.3085(2) 0.7056(4) 0.9780(2) 0.0312(10) Uani d 1 H H32A 0.3504 0.6878 0.9958 0.037 Uiso calc 1 H H32B 0.3023 0.7972 0.9803 0.037 Uiso calc 1 C C33 0.35341(18) 0.9034(4) 0.8523(2) 0.0251(8) Uani d 1 H H33 0.3645 0.9125 0.9070 0.030 Uiso calc 1 C C34 0.2906(2) 0.9640(4) 0.8359(3) 0.0329(10) Uani d 1 H H34A 0.2772 0.9494 0.7829 0.039 Uiso calc 1 H H34B 0.2616 0.9232 0.8673 0.039 Uiso calc 1 C C35 0.2913(2) 1.1069(4) 0.8517(3) 0.0410(12) Uani d 1 H H35A 0.2513 1.1421 0.8376 0.049 Uiso calc 1 H H35B 0.2999 1.1212 0.9059 0.049 Uiso calc 1 C C36 0.3385(3) 1.1759(5) 0.8079(3) 0.0526(15) Uani d 1 H H36A 0.3394 1.2654 0.8221 0.063 Uiso calc 1 H H36B 0.3275 1.1703 0.7536 0.063 Uiso calc 1 C C37 0.4015(2) 1.1172(5) 0.8251(3) 0.0449(12) Uani d 1 H H37A 0.4306 1.1594 0.7943 0.054 Uiso calc 1 H H37B 0.4142 1.1313 0.8783 0.054 Uiso calc 1 C C38 0.4017(2) 0.9743(4) 0.8084(3) 0.0348(10) Uani d 1 H H38A 0.4417 0.9396 0.8228 0.042 Uiso calc 1 H H38B 0.3934 0.9606 0.7541 0.042 Uiso calc 1 C C39 0.42352(19) 0.6637(4) 0.8581(2) 0.0286(9) Uani d 1 C C40 0.4396(2) 0.5504(4) 0.8220(3) 0.0360(11) Uani d 1 H H40 0.4146 0.5176 0.7819 0.043 Uiso calc 1 C C41 0.4930(2) 0.4870(5) 0.8460(3) 0.0475(13) Uani d 1 H H41 0.5035 0.4118 0.8220 0.057 Uiso calc 1 C C42 0.5303(3) 0.5345(6) 0.9051(4) 0.0606(17) Uani d 1 H H42 0.5659 0.4912 0.9209 0.073 Uiso calc 1 C C43 0.5152(2) 0.6464(6) 0.9411(3) 0.0540(15) Uani d 1 H H43 0.5408 0.6788 0.9808 0.065 Uiso calc 1 C C44 0.4622(2) 0.7098(5) 0.9179(3) 0.0384(11) Uani d 1 H H44 0.4521 0.7847 0.9426 0.046 Uiso calc 1 C C10 0.1334(2) 0.3798(5) 0.7894(2) 0.0303(9) Uani d 1 H H10A 0.1364 0.2876 0.7856 0.036 Uiso calc 1 H H10B 0.1743 0.4136 0.7994 0.036 Uiso calc 1 C C11 0.0944(2) 0.4146(6) 0.8553(3) 0.0415(12) Uani d 1 H H11A 0.0936 0.5066 0.8613 0.050 Uiso calc 1 H H11B 0.1122 0.3778 0.9023 0.050 Uiso calc 1 C C12 0.0294(2) 0.3649(7) 0.8400(3) 0.0509(14) Uani d 1 H H12A 0.0049 0.3897 0.8816 0.061 Uiso calc 1 H H12B 0.0299 0.2724 0.8374 0.061 Uiso calc 1 C C13 0.0010(2) 0.4189(7) 0.7649(3) 0.0521(15) Uani d 1 H H13A -0.0397 0.3841 0.7552 0.063 Uiso calc 1 H H13B -0.0026 0.5109 0.7692 0.063 Uiso calc 1 C C14 0.03941(19) 0.3865(5) 0.6985(3) 0.0361(11) Uani d 1 H H14A 0.0217 0.4259 0.6523 0.043 Uiso calc 1 H H14B 0.0395 0.2947 0.6908 0.043 Uiso calc 1 H H9 0.104(2) 0.533(4) 0.715(2) 0.029(12) Uiso d 1 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 0.0344(3) 0.0336(3) 0.0398(3) 0.00182(19) 0.00044(19) -0.0061(2) Ni1 0.0193(3) 0.0219(3) 0.0213(3) -0.0028(2) 0.00286(19) -0.0026(2) P1 0.0177(5) 0.0211(5) 0.0192(5) -0.0016(4) 0.0020(4) -0.0019(4) P2 0.0205(5) 0.0226(5) 0.0233(5) -0.0022(4) 0.0018(4) -0.0025(4) N1 0.0167(16) 0.0225(16) 0.0251(17) 0.0000(13) 0.0046(13) -0.0050(13) N2 0.0270(18) 0.0264(18) 0.0222(17) -0.0082(14) 0.0025(14) -0.0034(14) C1 0.0196(19) 0.031(2) 0.0199(19) -0.0039(17) 0.0011(15) 0.0016(16) C2 0.0204(19) 0.028(2) 0.0213(19) 0.0013(16) 0.0016(15) 0.0004(16) C3 0.025(2) 0.037(2) 0.032(2) 0.0020(19) 0.0042(17) -0.0080(19) C4 0.026(2) 0.048(3) 0.035(2) 0.003(2) 0.0111(19) -0.001(2) C5 0.022(2) 0.049(3) 0.028(2) -0.007(2) 0.0038(17) 0.004(2) C6 0.024(2) 0.030(2) 0.022(2) -0.0019(17) 0.0029(16) 0.0026(17) C7 0.024(2) 0.025(2) 0.029(2) 0.0012(17) 0.0053(16) -0.0066(17) C8 0.023(2) 0.036(2) 0.026(2) -0.0120(18) 0.0021(16) 0.0003(18) C9 0.020(2) 0.032(2) 0.0206(19) -0.0011(17) 0.0038(15) -0.0025(17) C15 0.0178(19) 0.025(2) 0.0212(19) -0.0037(16) 0.0000(15) 0.0004(16) C16 0.040(3) 0.023(2) 0.029(2) -0.0014(19) -0.0055(19) -0.0005(18) C17 0.045(3) 0.028(2) 0.036(3) -0.001(2) -0.011(2) 0.0035(19) C18 0.044(3) 0.049(3) 0.033(3) -0.014(2) -0.012(2) 0.017(2) C19 0.033(2) 0.059(3) 0.022(2) -0.005(2) 0.0013(18) 0.007(2) C20 0.029(2) 0.040(2) 0.025(2) -0.0004(19) 0.0037(17) 0.0015(19) C21 0.022(2) 0.0234(19) 0.0210(19) -0.0035(16) 0.0041(15) -0.0012(16) C22 0.030(2) 0.033(2) 0.024(2) -0.0046(19) 0.0024(17) -0.0013(18) C23 0.032(2) 0.029(2) 0.032(2) -0.0101(19) -0.0014(18) -0.0020(18) C24 0.042(3) 0.023(2) 0.036(2) -0.0086(19) 0.009(2) -0.0033(19) C25 0.029(2) 0.027(2) 0.034(2) 0.0014(18) 0.0084(18) 0.0072(18) C26 0.025(2) 0.030(2) 0.025(2) -0.0024(17) 0.0024(16) -0.0023(17) C27 0.021(2) 0.028(2) 0.0199(19) -0.0004(16) 0.0034(15) -0.0037(16) C28 0.034(2) 0.030(2) 0.032(2) -0.0065(19) 0.0070(19) -0.0010(19) C29 0.039(3) 0.032(2) 0.039(3) -0.007(2) 0.012(2) 0.000(2) C30 0.037(3) 0.045(3) 0.037(3) 0.004(2) 0.009(2) 0.009(2) C31 0.035(3) 0.048(3) 0.023(2) 0.002(2) 0.0064(18) 0.000(2) C32 0.034(2) 0.035(2) 0.025(2) -0.0002(19) 0.0038(18) -0.0031(18) C33 0.023(2) 0.024(2) 0.028(2) -0.0004(16) -0.0012(16) 0.0012(17) C34 0.028(2) 0.028(2) 0.042(3) 0.0038(19) -0.0017(19) -0.005(2) C35 0.043(3) 0.031(2) 0.048(3) 0.008(2) -0.007(2) -0.007(2) C36 0.073(4) 0.024(2) 0.058(3) 0.007(3) -0.013(3) 0.001(2) C37 0.051(3) 0.031(2) 0.052(3) -0.008(2) 0.001(2) 0.000(2) C38 0.035(3) 0.031(2) 0.038(3) -0.005(2) 0.002(2) -0.001(2) C39 0.023(2) 0.031(2) 0.032(2) -0.0009(18) 0.0056(17) 0.0046(18) C40 0.036(3) 0.036(2) 0.037(3) 0.009(2) 0.011(2) 0.000(2) C41 0.042(3) 0.046(3) 0.057(3) 0.019(2) 0.017(3) 0.008(3) C42 0.032(3) 0.064(4) 0.085(5) 0.017(3) 0.003(3) 0.028(4) C43 0.036(3) 0.056(3) 0.068(4) -0.008(3) -0.016(3) 0.017(3) C44 0.028(2) 0.037(3) 0.050(3) -0.003(2) -0.004(2) -0.004(2) C10 0.027(2) 0.044(3) 0.021(2) 0.0013(19) 0.0047(16) 0.0033(18) C11 0.035(2) 0.066(3) 0.024(2) 0.001(2) 0.0078(18) -0.001(2) C12 0.034(2) 0.090(4) 0.030(2) -0.005(3) 0.0140(19) 0.003(3) C13 0.025(2) 0.100(5) 0.032(2) 0.000(3) 0.0095(18) -0.008(3) C14 0.021(2) 0.060(3) 0.027(2) -0.001(2) 0.0043(16) -0.005(2) 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' 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 N1 Ni1 Br1 102.53(9) N2 Ni1 Br1 94.37(10) N2 Ni1 N1 162.16(14) C1 Ni1 Br1 164.55(13) C1 Ni1 N1 83.17(15) C1 Ni1 N2 81.94(16) N1 P1 C9 114.13(18) N1 P1 C15 115.32(18) N1 P1 C21 109.95(18) C9 P1 C15 107.41(18) C21 P1 C9 102.96(19) C21 P1 C15 106.07(18) N2 P2 C27 112.03(18) N2 P2 C33 113.35(19) N2 P2 C39 111.06(19) C33 P2 C27 107.71(18) C39 P2 C27 104.52(19) C39 P2 C33 107.69(19) P1 N1 Ni1 132.07(19) C7 N1 Ni1 113.0(2) C7 N1 P1 113.1(3) P2 N2 Ni1 129.2(2) C8 N2 Ni1 112.1(2) C8 N2 P2 114.8(3) C2 C1 Ni1 120.2(3) C2 C1 C6 120.6(4) C6 C1 Ni1 119.1(3) C1 C2 C3 119.6(4) C1 C2 C7 114.1(3) C3 C2 C7 126.4(4) C4 C3 C2 119.8(4) C5 C4 C3 120.9(4) C4 C5 C6 119.5(4) C1 C6 C5 119.6(4) C1 C6 C8 113.1(4) C5 C6 C8 127.3(4) C2 C7 N1 108.1(3) N2 C8 C6 106.5(3) C10 C9 P1 111.9(3) C10 C9 C14 110.7(4) C14 C9 P1 112.3(3) C16 C15 P1 111.9(3) C20 C15 P1 112.5(3) C20 C15 C16 109.7(3) C17 C16 C15 110.5(3) C18 C17 C16 111.8(4) C19 C18 C17 111.2(4) C18 C19 C20 111.5(4) C19 C20 C15 111.6(4) C22 C21 P1 123.4(3) C26 C21 P1 118.0(3) C26 C21 C22 118.3(4) C23 C22 C21 120.1(4) C24 C23 C22 120.2(4) C23 C24 C25 120.4(4) C26 C25 C24 119.6(4) C25 C26 C21 121.5(4) C28 C27 P2 110.5(3) C28 C27 C32 111.4(3) C32 C27 P2 112.9(3) C29 C28 C27 110.8(4) C30 C29 C28 111.9(4) C29 C30 C31 110.3(4) C30 C31 C32 111.6(4) C31 C32 C27 111.0(4) C34 C33 P2 109.6(3) C34 C33 C38 110.3(4) C38 C33 P2 113.0(3) C35 C34 C33 112.1(4) C36 C35 C34 112.1(4) C35 C36 C37 110.5(4) C38 C37 C36 111.8(4) C37 C38 C33 111.5(4) C40 C39 P2 117.8(3) C44 C39 P2 123.6(3) C44 C39 C40 118.3(4) C41 C40 C39 120.0(5) C42 C41 C40 120.5(5) C41 C42 C43 120.3(5) C44 C43 C42 119.8(5) C43 C44 C39 121.1(5) C11 C10 C9 110.6(4) C10 C11 C12 110.5(4) C11 C12 C13 110.4(4) C14 C13 C12 111.3(4) C13 C14 C9 110.7(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 Ni1 2.4253(7) Ni1 N1 1.991(3) Ni1 N2 1.973(3) Ni1 C1 1.833(4) P1 N1 1.614(3) P1 C9 1.827(4) P1 C15 1.831(4) P1 C21 1.814(4) P2 N2 1.609(3) P2 C27 1.827(4) P2 C33 1.825(4) P2 C39 1.821(4) N1 C7 1.506(5) N2 C8 1.487(5) C1 C2 1.387(6) C1 C6 1.395(6) C2 C3 1.396(6) C2 C7 1.489(6) C3 C4 1.387(6) C4 C5 1.386(7) C5 C6 1.398(6) C6 C8 1.498(6) C9 C10 1.529(6) C9 C14 1.544(6) C15 C16 1.549(6) C15 C20 1.529(5) C16 C17 1.532(6) C17 C18 1.518(7) C18 C19 1.515(7) C19 C20 1.527(6) C21 C22 1.405(6) C21 C26 1.393(6) C22 C23 1.393(6) C23 C24 1.379(6) C24 C25 1.385(6) C25 C26 1.380(6) C27 C28 1.540(6) C27 C32 1.545(5) C28 C29 1.528(6) C29 C30 1.516(7) C30 C31 1.523(7) C31 C32 1.534(6) C33 C34 1.529(6) C33 C38 1.541(6) C34 C35 1.522(6) C35 C36 1.514(8) C36 C37 1.526(8) C37 C38 1.525(6) C39 C40 1.401(6) C39 C44 1.395(6) C40 C41 1.389(7) C41 C42 1.372(8) C42 C43 1.382(9) C43 C44 1.379(7) C10 C11 1.527(6) C11 C12 1.528(7) C12 C13 1.529(7) C13 C14 1.522(6) _cod_database_fobs_code 2021767