Effective stabilization of a planar phosphorus(III) center embedded in a porphyrin-based fused aromatic skeleton
Osuka, Atsuhiro; Fujimoto, Keisuke; Chem. Sci.  (2017) –; doi:10.1039/C7SC03882H

data_1547617
_publ_section_title
;
 Effective stabilization of a planar phosphorus(III) center embedded in a
 porphyrin-based fused aromatic skeleton
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03882H
_journal_year                    2017
_chemical_formula_moiety         'C128 H114 N8 P2 Ni2, 4(C H Cl3)'
_chemical_formula_sum            'C132 H118 Cl12 N8 Ni2 P2'
_chemical_formula_weight         2421.10
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-01 deposited with the CCDC.
2017-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.009(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6212(19)
_cell_length_b                   16.587(2)
_cell_length_c                   27.567(4)
_cell_measurement_reflns_used    5364
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      25.7
_cell_volume                     5749.1(14)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            37277
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.332
_diffrn_reflns_theta_min         6.670
_exptl_absorpt_coefficient_mu    3.670
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.983
_refine_diff_density_min         -1.436
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         10386
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0723
_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^)+(0.1478P)^2^+6.6858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2098
_refine_ls_wR_factor_ref         0.2218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8519
_reflns_number_total             10386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03882h2.cif
_cod_data_source_block           0603kf
_cod_depositor_comments
;

2019-08-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C66 H59 Cl6 N4 Ni P'
_cod_original_formula_weight         1210.55
_cod_original_formula_moiety         'C64 H57 N4 P Ni, 2(C H Cl3)'
_cod_original_formula_units_Z            4
_cod_database_code               1547617
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.473
_shelx_estimated_absorpt_t_max   0.930
_shelx_res_checksum              66280