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_4347061
_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            'C52 H35 Cl3 N2 O0.9 Pd2 S'
_chemical_formula_weight         1053.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 102.23(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.086(3)
_cell_length_b                   28.335(6)
_cell_length_c                   16.858(4)
_cell_measurement_reflns_used    4463
_cell_measurement_temperature    79.9(4)
_cell_measurement_theta_max      28.93
_cell_measurement_theta_min      2.68
_cell_volume                     6109(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      79.9(4)
_diffrn_detector_area_resol_mean 10.34
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_av_unetI/netI     0.1736
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22967
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.681
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.34a (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       paralleleppiped
_exptl_crystal_F_000             2109
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
;
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         11156
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0868
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1076P)^2^+4.8230P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2121
_refine_ls_wR_factor_ref         0.2408
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6001
_reflns_number_total             11156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02684_si_002.cif
_cod_data_source_block           PdSAz
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C52 H35 Cl3 N2 O0.90 Pd2 S'
_cod_database_code               4347061
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2013-2
_shelx_res_checksum              39712
_shelx_hkl_checksum              90886