Crystal structure of tetracarbonyl-{μ-[N-(diphenylphosphanyl)-N,P,P-triphenylphosphinous amide]}-bis[μ-(phenylmethanethiolato)]diiron (Fe–Fe), C48H39Fe2NO4P2S2
Gao, Xin-Ping; Lü, Shuang; Li, Qian-Li; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 607–609; doi:10.1515/ncrs-2023-0115

data_8107509
_publ_section_title
;
 Crystal structure of
 tetracarbonyl-{\m-[N-(diphenylphosphanyl)-N,P,P-triphenylphosphinous
 amide]}-bis[\m-(phenylmethanethiolato)]diiron (Fe--Fe), C48H39Fe2NO4P2S2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              607
_journal_page_last               609
_journal_paper_doi               10.1515/ncrs-2023-0115
_journal_volume                  238
_journal_year                    2023
_chemical_formula_sum            'C48 H39 Fe2 N O4 P2 S2'
_chemical_formula_weight         931.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 108.297(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4073(11)
_cell_length_b                   16.9013(14)
_cell_length_c                   11.8261(12)
_cell_measurement_reflns_used    5840
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.1235
_cell_measurement_theta_min      2.1635
_cell_volume                     2164.8(4)
_computing_cell_refinement       'SAINT (BRUKER, 2009) [1]'
_computing_data_collection       'APEX2 (BRUKER, 2009) [1]'
_computing_data_reduction        'SADABS (BRUKER, 2009) [1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009) [4]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [4]'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018) [3]'
_computing_structure_solution    'ShelXS (Sheldrick, 2008) [2]'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10927
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.018
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_min         2.164
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
; 
 Flack x determined using 2698 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.022(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7335
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0232P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_full    0.917
_reflns_Friedel_fraction_max     0.917
_reflns_number_gt                6467
_reflns_number_total             7335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0115_suppl_001.cif
_cod_data_source_block           d
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               8107509
_shelx_estimated_absorpt_t_min   0.718
_shelx_estimated_absorpt_t_max   0.886
_shelx_res_checksum              86378
_shelx_hkl_checksum              77839