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_1547620
_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         'C68 H57 N4 Ni O P S2, 3.641(C Cl4)'
_chemical_formula_sum            'C71.65 H57 Cl14.59 N4 Ni O P S2'
_chemical_formula_weight         1660.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                96.635(3)
_cell_angle_beta                 103.033(7)
_cell_angle_gamma                104.706(2)
_cell_formula_units_Z            2
_cell_length_a                   14.070(3)
_cell_length_b                   15.707(3)
_cell_length_c                   18.170(3)
_cell_measurement_reflns_used    3219
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      25.2
_cell_volume                     3719.8(12)
_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 0.970
_diffrn_measured_fraction_theta_max 0.966
_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  0.0669
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48771
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.491
_diffrn_reflns_theta_min         6.538
_exptl_absorpt_coefficient_mu    6.295
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.162
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         13223
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0674
_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^)+(0.1315P)^2^+2.7840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.1989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9994
_reflns_number_total             13223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03882h2.cif
_cod_data_source_block           1028kf
_cod_database_code               1547620
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.272
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              96899