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_4347063
_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            'C54.95 H40.68 Cl1.03 N2 O Pd S'
_chemical_formula_weight         919.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                62.24(3)
_cell_angle_beta                 81.23(3)
_cell_angle_gamma                89.46(4)
_cell_formula_units_Z            2
_cell_length_a                   10.635(3)
_cell_length_b                   14.695(4)
_cell_length_c                   15.144(5)
_cell_measurement_reflns_used    7608
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.93
_cell_measurement_theta_min      3.07
_cell_volume                     2064.7(12)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.34
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16434
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.076
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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)
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         7640
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+1.3850P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6035
_reflns_number_total             7640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02684_si_002.cif
_cod_data_source_block           '[Pd(SBzc-CHO)]'
_cod_database_code               4347063
_shelx_estimated_absorpt_t_min   0.810
_shelx_estimated_absorpt_t_max   0.958
_shelxl_version_number           2013-2
_shelx_res_checksum              1803
_shelx_hkl_checksum              74776