Crystal structure of (6,9-diacetyl-5,10,15,20-tetraphenylsecochlorinato)nickel(II)
Sharma, Meenakshi; Brückner, Christian; Zeller, Matthias; Acta Crystallographica Section E Crystallographic Communications 80 (2024) –; doi:10.1107/S2056989024004717

data_2023141
_publ_section_title
;
 Crystal structure of
 (6,9-diacetyl-5,10,15,20-tetraphenylsecochlorinato)nickel(II)
;
_journal_coeditor_code           YY2012
_journal_issue                   6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024004717
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Ni (C46 H32 N4 O2)]'
_chemical_formula_moiety         'C46 H32 N4 Ni O2'
_chemical_formula_sum            'C46 H32 N4 Ni O2'
_chemical_formula_weight         731.46
_chemical_name_systematic
;
(6,9-Diacetyl-5,10,15,20-tetraphenylsecochlorinato)nickel(II)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                72.0900(18)
_cell_angle_beta                 69.6031(19)
_cell_angle_gamma                74.6737(18)
_cell_formula_units_Z            4
_cell_length_a                   14.1382(5)
_cell_length_b                   15.3202(5)
_cell_length_c                   18.3835(7)
_cell_measurement_reflns_used    9410
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.0606
_cell_measurement_theta_min      2.2418
_cell_volume                     3495.8(2)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2020)
;
_computing_data_collection
;
APEX4 v2022.10-1 (Bruker, 2022)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2020)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b),
<i>ShelXle</i> Rev1573 (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS D8 Quest'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            226909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.200
_diffrn_reflns_theta_min         1.916
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.416
_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     959
_refine_ls_number_reflns         26754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+1.6735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                19735
_reflns_number_total             26754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yy2012.cif
_cod_data_source_block           I
_cod_database_code               2023141
_shelx_estimated_absorpt_t_min   0.869
_shelx_estimated_absorpt_t_max   0.920
_shelx_hkl_checksum              67541
_shelx_res_checksum              26168