The influence of phosphine ligand substituted [2Fe2S] model complexes as electro-catalyst on proton reduction
Zhang, Xia; Ma, Xiaoyuan; Zhang, Tianyong; Li, Bin; Jiang, Shuang; Zhang, Guanghui; Hai, Li; Wang, Jingchao; Shao, Xiao; RSC Advances 8 (2018) 42262–; doi:10.1039/C8RA08016J

data_7232028
_publ_section_title
;
 The influence of phosphine ligand substituted [2Fe2S] model complexes as
 electro-catalyst on proton reduction
;
_journal_issue                   74
_journal_name_full               'RSC Advances'
_journal_page_first              42262
_journal_paper_doi               10.1039/C8RA08016J
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C12 H17 Fe2 O5 P S2'
_chemical_formula_sum            'C12 H17 Fe2 O5 P S2'
_chemical_formula_weight         448.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-23
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2017-01-08 deposited with the CCDC.
2018-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.9678(4)
_cell_length_b                   11.62457(18)
_cell_length_c                   12.7424(2)
_cell_measurement_reflns_used    25834
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      30.9750
_cell_measurement_theta_min      1.6990
_cell_volume                     3550.23(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 PILT
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -105.00  75.00   0.50    4.00    --  -15.00  45.00   0.00  360
  2  \w   -105.00  75.00   0.50    4.00    --  -15.00  45.00  90.00  360
  3  \w   -105.00  75.00   0.50    4.00    --  -15.00  45.00 180.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Xtalab P200'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0128086000
_diffrn_orient_matrix_UB_12      -0.0469364000
_diffrn_orient_matrix_UB_13      -0.0261477000
_diffrn_orient_matrix_UB_21      0.0263035000
_diffrn_orient_matrix_UB_22      -0.0275396000
_diffrn_orient_matrix_UB_23      -0.0044462000
_diffrn_orient_matrix_UB_31      -0.0044572000
_diffrn_orient_matrix_UB_32      -0.0275935000
_diffrn_orient_matrix_UB_33      0.0489449000
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0096
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45269
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         1.699
_diffrn_source                   'Rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         4586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0170
_refine_ls_R_factor_gt           0.0157
_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^)+(0.0220P)^2^+1.2030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0410
_refine_ls_wR_factor_ref         0.0415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4365
_reflns_number_total             4586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra08016j1.cif
_cod_data_source_block           m20160623g
_cod_original_cell_volume        3550.25(10)
_cod_database_code               7232028
_chemical_oxdiff_formula         'C12 H17 Fe2 O5 P S2'
_shelx_estimated_absorpt_t_max   0.743
_shelx_estimated_absorpt_t_min   0.628
_reflns_odcompleteness_completeness 92.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              33073
_shelx_shelxl_version_number     2014/8
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.473
_oxdiff_exptl_absorpt_empirical_full_min 0.690