Structural and HER studies of diphosphine-monothiolate complexes [Fe2(CO)4(μ-naphthalene-2-thiolate)2(μ-dppe)] and [Fe2(CO)4(μ-naphthalene-2-thiolate)2(μ-DPEPhos)]
Faujdar, Hemlata; Spannenberg, Anke; Kaur-Ghumaan, Sandeep; Inorganica Chimica Acta 501 (2020) 119227–; doi:10.1016/j.ica.2019.119227

data_1565592
_publ_section_title
;
 Structural and HER studies of diphosphine-monothiolate complexes
 [Fe2(CO)4(\m-naphthalene-2-thiolate)2(\m-dppe)] and
 [Fe2(CO)4(\m-naphthalene-2-thiolate)2(\m-DPEPhos)]
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119227
_journal_paper_doi               10.1016/j.ica.2019.119227
_journal_volume                  501
_journal_year                    2020
_chemical_formula_sum            'C50 H38 Fe2 O4 P2 S2'
_chemical_formula_weight         940.56
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.1797(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9602(4)
_cell_length_b                   11.0683(3)
_cell_length_c                   20.8501(5)
_cell_measurement_reflns_used    3635
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.29
_cell_measurement_theta_min      4.26
_cell_volume                     4357.68(18)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         microfocus
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32848
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        66.707
_diffrn_reflns_theta_max         66.707
_diffrn_reflns_theta_min         2.340
_exptl_absorpt_coefficient_mu    7.292
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.24
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       needle
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         7566
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0655P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5867
_reflns_number_total             7566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-501-119227.cif
_cod_data_source_block           AX1577
_cod_original_cell_volume        4357.67(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565592
_shelx_shelxl_version_number     2014/7