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_7043516
_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            'C67 H83 Fe3 K2 N O29 S'
_chemical_formula_weight         1644.14
_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                93.487(3)
_cell_angle_beta                 90.553(3)
_cell_angle_gamma                115.373(4)
_cell_formula_units_Z            2
_cell_length_a                   14.1536(11)
_cell_length_b                   15.8852(13)
_cell_length_c                   20.497(2)
_cell_measurement_reflns_used    13954
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     4152.9(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 AFC12 Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60703
_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         3.039
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.717
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       needle
_exptl_crystal_F_000             1712
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.072
_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     931
_refine_ls_number_reflns         19025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0459P)^2^+1.7054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13954
_reflns_number_total             19025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01506b2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;

2018-01-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         822.07
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C33.50 H41.50 Fe1.50 K N0.50 O14.50 S0.50'
_cod_database_code               7043516
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              39004
_shelx_fab_checksum              78141