Synthesis and interconversions of reduced, alkali‒metal supported iron‒sulfur‒carbonyl complexes
Shupp, J. Patrick; Rose, Amber R.; Rose, Michael J.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01506B

data_7043517
_publ_section_title
;
 Synthesis and interconversions of reduced, alkali--metal supported
 iron--sulfur--carbonyl complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01506B
_journal_year                    2017
_chemical_formula_sum            'C72 H90 Fe5 K2 O33 S4'
_chemical_formula_weight         1969.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-04-15 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                92.417(3)
_cell_angle_beta                 96.261(3)
_cell_angle_gamma                115.604(3)
_cell_formula_units_Z            2
_cell_length_a                   14.8881(13)
_cell_length_b                   15.2863(13)
_cell_length_c                   20.8167(18)
_cell_measurement_reflns_used    19338
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     4225.7(6)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku ADC12 Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            68085
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.005
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.119
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       plate
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.340
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         19338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+22.3407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1992
_refine_ls_wR_factor_ref         0.2120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15302
_reflns_number_total             19338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01506b2.cif
_cod_data_source_block           shelx
_cod_database_code               7043517
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              90468