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_4129027
_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_sum            'C47 H45 Au Cl3 N4 Ni P'
_chemical_formula_weight         1058.86
_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
_cell_angle_alpha                98.6560(10)
_cell_angle_beta                 107.3330(10)
_cell_angle_gamma                113.7310(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7696(6)
_cell_length_b                   13.2248(6)
_cell_length_c                   15.5398(7)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.25
_cell_volume                     2180.75(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
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_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15242
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.069
_diffrn_reflns_theta_min         2.495
_exptl_absorpt_coefficient_mu    4.050
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         7349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0202
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+1.8074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7180
_reflns_number_total             7349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13169_si_004.cif
_cod_data_source_block           oomori20161215_0m_a_a
_cod_original_cell_volume        2180.75(17)
_cod_database_code               4129027
_shelx_estimated_absorpt_t_min   0.257
_shelx_estimated_absorpt_t_max   0.823
_shelxl_version_number           2014-3
_shelx_res_checksum              52928
_shelx_hkl_checksum              66489