Ni(II) 10-Phosphacorrole: A Porphyrin Analogue Containing Phosphorus at the Meso Position.
Omori, Hiroto; Hiroto, Satoru; Takeda, Youhei; Fliegl, Heike; Minakata, Satoshi; Shinokubo, Hiroshi; Journal of the American Chemical Society 141 (2019) 4800–4805; doi:10.1021/jacs.8b13169

data_4129029
_publ_section_title
;
 Ni(II) 10-Phosphacorrole: A Porphyrin Analogue Containing Phosphorus at
 the Meso Position.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4800
_journal_page_last               4805
_journal_paper_doi               10.1021/jacs.8b13169
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C91 H83 Cl3 N8 Ni2 P2'
_chemical_formula_sum            'C91 H83 Cl3 N8 Ni2 P2'
_chemical_formula_weight         1574.36
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                100.329(2)
_cell_angle_beta                 115.508(2)
_cell_angle_gamma                101.094(2)
_cell_formula_units_Z            2
_cell_length_a                   16.0007(10)
_cell_length_b                   16.1997(10)
_cell_length_c                   17.7476(12)
_cell_measurement_reflns_used    171
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      24.3938
_cell_measurement_theta_min      2.7159
_cell_volume                     3891.7(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  ImuS
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25866
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.105
_diffrn_reflns_theta_min         2.151
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.310
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1095
_refine_ls_number_reflns         13132
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0569P)^2^+6.5265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11824
_reflns_number_total             13132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13169_si_002.cif
_cod_data_source_block           shino150807oh_0m_a
_cod_database_code               4129029
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.727
_shelx_estimated_absorpt_t_max   0.817
_shelxl_version_number           2014-3
_shelx_res_checksum              45748
_shelx_hkl_checksum              59935