Synthetic and Structural Studies on Linear and Macrocyclic Pd- and Pt-Bridged Butterfly Fe/S Cluster Complexes
Song, Li-Cheng; Zhang, Long-Duo; Liu, Bei-Bei; Ding, Shu-Da; Chen, Hao; Xu, Xiu-Fang; Fan, Gui-Lan; Organometallics 36 (2017) 1419–; doi:10.1021/acs.organomet.7b00117

data_4089262
_publ_section_title
;
 Synthetic and Structural Studies on Linear and Macrocyclic Pd- and
 Pt-Bridged Butterfly Fe/S Cluster Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1419
_journal_paper_doi               10.1021/acs.organomet.7b00117
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C52 H34 Fe4 O12 P2 Pd S6'
_chemical_formula_sum            'C52 H34 Fe4 O12 P2 Pd S6'
_chemical_formula_weight         1434.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 124.423(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.363(3)
_cell_length_b                   14.7490(13)
_cell_length_c                   27.309(2)
_cell_measurement_reflns_used    19950
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      1.20
_cell_volume                     11749.3(17)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            53730
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.940
_diffrn_reflns_theta_min         1.396
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    1.589
_exptl_absorpt_correction_T_max  0.698
_exptl_absorpt_correction_T_min  0.558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5744
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_platon_squeeze_details
;
;
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         14038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0260P)^2^+28.7534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12223
_reflns_number_total             14038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00117_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        11749.3(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4089262
_shelx_estimated_absorpt_t_min   0.683
_shelx_estimated_absorpt_t_max   0.721
_shelxl_version_number           2013-3
_shelx_res_checksum              36387
_shelx_hkl_checksum              61493