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_1547618
_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         'C62 H57 N4 Ni P S2, 2(C6 H6)'
_chemical_formula_sum            'C74 H69 N4 Ni P S2'
_chemical_formula_weight         1168.13
_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                 95.324(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9016(19)
_cell_length_b                   16.642(2)
_cell_length_c                   28.249(5)
_cell_measurement_reflns_used    4753
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      31.1
_cell_volume                     6039.1(16)
_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 0.991
_diffrn_measured_fraction_theta_max 0.989
_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  0.0266
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            39966
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.381
_diffrn_reflns_theta_min         6.608
_exptl_absorpt_coefficient_mu    1.720
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         10959
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0971P)^2^+7.2977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9650
_reflns_number_total             10959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03882h2.cif
_cod_data_source_block           0607kf
_cod_database_code               1547618
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.714
_shelx_estimated_absorpt_t_max   0.950
_shelx_res_checksum              9954