Palladium(II), Ruthenium(II), and Ruthenium(III) Complexes of 23-Thiaazuliporphyrin: The Case of Coordination-Induced Contraction.
Białek, Michał J; Latos-Grażyński, Lechosław; Inorganic chemistry 55 (2016) 1758–1769; doi:10.1021/acs.inorgchem.5b02684

data_4347062
_publ_section_title
;
 Palladium(II), Ruthenium(II), and Ruthenium(III) Complexes of
 23-Thiaazuliporphyrin: The Case of Coordination-Induced Contraction.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1758
_journal_page_last               1769
_journal_paper_doi               10.1021/acs.inorgchem.5b02684
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C57 H43 Cl9 N2 O Ru S'
_chemical_formula_weight         1224.11
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.31(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.995(2)
_cell_length_b                   20.962(4)
_cell_length_c                   23.410(8)
_cell_measurement_reflns_used    8403
_cell_measurement_temperature    100.1(4)
_cell_measurement_theta_max      28.81
_cell_measurement_theta_min      2.70
_cell_volume                     5324(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.1(4)
_diffrn_detector_area_resol_mean 10.35
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23673
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.702
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark gold'
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       plate
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.093
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         10465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0339P)^2^+9.2166P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8552
_reflns_number_total             10465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02684_si_002.cif
_cod_data_source_block           '[Ru(SAz)Cl(CO)]'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347062
_shelx_estimated_absorpt_t_min   0.852
_shelx_estimated_absorpt_t_max   0.984
_shelxl_version_number           2013-2
_shelx_res_checksum              28825
_shelx_hkl_checksum              28073