Diiron Bridged-Thiolate Complexes That Bind N2 at the Fe(II)Fe(II), Fe(II)Fe(I), and Fe(I)Fe(I) Redox States.
Creutz, Sidney E.; Peters, Jonas C.; Journal of the American Chemical Society 137 (2015) 7310–7313; doi:10.1021/jacs.5b04738

data_4123805
_publ_section_title
;
 Diiron Bridged-Thiolate Complexes That Bind N2 at the Fe(II)Fe(II),
 Fe(II)Fe(I), and Fe(I)Fe(I) Redox States.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7310
_journal_page_last               7313
_journal_paper_doi               10.1021/jacs.5b04738
_journal_volume                  137
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_sum            'C55 H76 Fe2 O2 P4 S Si2'
_chemical_formula_weight         1092.97
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6501(4)
_cell_length_b                   19.5046(7)
_cell_length_c                   20.8033(6)
_cell_measurement_temperature    100(2)
_cell_volume                     5538.7(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_unetI/netI     0.1274
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            117711
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.289
_diffrn_reflns_theta_min         2.306
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  .7471
_exptl_absorpt_correction_T_min  .6890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1578 before and 0.1113 after correction.
The Ratio of minimum to maximum transmission is 0.8425.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_refine_diff_density_max         2.202
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 5897 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         26729
_refine_ls_number_restraints     761
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1359
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0581P)^2^+2.2781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.856
_reflns_friedel_fraction_full    0.999
_reflns_friedel_fraction_max     0.996
_reflns_number_gt                16732
_reflns_number_total             26729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04738_si_002.cif
_cod_data_source_block           compound13
_cod_depositor_comments
'Adding full bibliography for 4123801--4123807.cif.'
_cod_database_code               4123805
_shelxl_version_number           2013-3
_shelx_res_checksum              76105
_shelx_hkl_checksum              14865