Substitution reactions of iron(ii) carbamoyl-thioether complexes related to mono-iron hydrogenase
Xie, Zhu-Lin; Durgaprasad, Gummadi; Ali, Azim K.; Rose, Michael J.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01696D

data_7043646
_publ_section_title
;
 Substitution reactions of iron(ii) carbamoyl-thioether complexes related
 to mono-iron hydrogenase
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01696D
_journal_year                    2017
_chemical_formula_moiety         'C25 H24 N2 Fe Cl4 O3 S2'
_chemical_formula_sum            'C16.33 H15.33 Cl2 Fe0.67 N1.33 O2 S1.33'
_chemical_formula_weight         413.18
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.091(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   17.0361(6)
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_cell_length_c                   26.0871(9)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.7280
_cell_measurement_theta_min      3.3540
_cell_volume                     6333.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.27t (Agilent, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.27t (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.27t (Agilent, 2015)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type
'Agilent SuperNova Dual with AtlasS2 detector'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            22169
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.182
_diffrn_reflns_theta_min         3.388
_diffrn_source                   'microfocus sealed tube'
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_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.27t (Agilent, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.050
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_refine_diff_density_max         0.638
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6220
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0719
_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^)+(0.0970P)^2^+17.2923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1838
_refine_ls_wR_factor_ref         0.2048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4551
_reflns_number_total             6220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01696d2.cif
_cod_data_source_block           2g
_cod_database_code               7043646
_shelx_estimated_absorpt_t_min   0.113
_shelx_estimated_absorpt_t_max   0.804
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2013-4
_shelx_res_checksum              75032
_shelx_fab_checksum              17638