Nickel(ii)-methyl complexes adopting unusual seesaw geometries.
Hill, Ethan A.; Zhao, Norman; Filatov, Alexander S.; Anderson, John S.; Chemical communications (Cambridge, England) 56 (2020) 7861–7864; doi:10.1039/c9cc09249h

data_7125849
_publ_section_title
;
 Nickel(ii)-methyl complexes adopting unusual seesaw geometries.
;
_journal_issue                   57
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7861
_journal_page_last               7864
_journal_paper_doi               10.1039/c9cc09249h
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C27 H38 B Cl N6 Ni'
_chemical_formula_sum            'C27 H38 B Cl N6 Ni'
_chemical_formula_weight         551.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2019-11-27 deposited with the CCDC.	2020-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.925(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6383(16)
_cell_length_b                   17.821(3)
_cell_length_c                   16.177(3)
_cell_measurement_reflns_used    7750
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.87
_cell_measurement_theta_min      2.29
_cell_volume                     2777.1(8)
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25048
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.074
_diffrn_reflns_theta_max         25.074
_diffrn_reflns_theta_min         2.286
_diffrn_source                   'micro-focus X-ray tube'
_diffrn_source_type              'INCOATEC ImuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0782 before and 0.0590 after correction. 
The Ratio of minimum to maximum transmission is 0.9034. 
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       prism
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0456P)^2^+1.4255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3761
_reflns_number_total             4930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09249h2.cif
_cod_data_source_block           1a_tBuNiCl
_cod_depositor_comments
'Adding full bibliography for 7125849--7125850.cif.'
_cod_original_cell_volume        2777.0(8)
_cod_database_code               7125849
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.694
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H4(0.026) H5(0.021) H6(0.021) H7(0.03) H8(0.023) H9(0.023)
 H11A(0.042) H11B(0.042) H11C(0.042) H12B(0.043) H12A(0.043) H12C(0.043)
 H13A(0.051) H13B(0.051) H13C(0.051) H15A(0.04) H15B(0.04) H15C(0.04)
 H16A(0.046) H16B(0.046) H16C(0.046) H17A(0.053) H17B(0.053) H17C(0.053)
 H19A(0.037) H19B(0.037) H19C(0.037) H20A(0.036) H20B(0.036) H20C(0.036)
 H21A(0.038) H21B(0.038) H21C(0.038) H23(0.025) H24(0.034) H25(0.035)
 H26(0.033) H27(0.025)
 Fixed X: H4(0.592254) H5(0.941454) H6(0.606581) H7(0.419154) H8(0.988106)
 H9(0.435128) H11A(0.432458) H11B(0.280489) H11C(0.377734) H12B(0.090429)
 H12A(0.134744) H12C(0.191248) H13A(0.213612) H13B(0.183309) H13C(0.335419)
 H15A(0.59371) H15B(0.662837) H15C(0.741776) H16A(0.711068) H16B(0.655244)
 H16C(0.573914) H17A(0.951241) H17B(0.880573) H17C(0.939784) H19A(0.135375)
 H19B(0.107282) H19C(0.210387) H20A(0.401405) H20B(0.298351) H20C(0.44375)
 H21A(0.32453) H21B(0.178205) H21C(0.20211) H23(0.878234) H24(1.015131)
 H25(0.965836) H26(0.77228) H27(0.636148)
 Fixed Y: H4(0.530455) H5(0.691229) H6(0.584921) H7(0.563166) H8(0.825991)
 H9(0.653215) H11A(0.775159) H11B(0.811244) H11C(0.811537) H12B(0.740674)
 H12A(0.666104) H12C(0.746036) H13A(0.614849) H13B(0.691849) H13C(0.655801)
 H15A(0.902769) H15B(0.984217) H15C(0.912719) H16A(0.936748) H16B(1.002543)
 H16C(0.924342) H17A(0.935844) H17B(1.010995) H17C(0.949923) H19A(0.724663)
 H19B(0.811628) H19C(0.787511) H20A(0.865527) H20B(0.890423) H20C(0.85178)
 H21A(0.755787) H21B(0.793987) H21C(0.706794) H23(0.605519) H24(0.49924)
 H25(0.394592) H26(0.395545) H27(0.502521)
 Fixed Z: H4(0.682679) H5(0.547655) H6(0.383152) H7(0.785236) H8(0.568723)
 H9(0.295416) H11A(0.830506) H11B(0.8233) H11C(0.745037) H12B(0.736264)
 H12A(0.688757) H12C(0.659874) H13A(0.826412) H13B(0.873405) H13C(0.878754)
 H15A(0.678308) H15B(0.686138) H15C(0.724776) H16A(0.473407) H16B(0.530839)
 H16C(0.524789) H17A(0.646296) H17B(0.610796) H17C(0.5486) H19A(0.4284)
 H19B(0.409713) H19C(0.484656) H20A(0.425384) H20B(0.350735) H20C(0.331777)
 H21A(0.24676) H21B(0.264414) H21C(0.283801) H23(0.647068) H24(0.660027)
 H25(0.578059) H26(0.487731) H27(0.474085)
;
_shelx_res_checksum              69571
_olex2_submission_special_instructions 'No special instructions were received'