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_7043649
_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         'C82 H53 B F24 Fe N2 O2 P2 S'
_chemical_formula_sum            'C82 H53 B F24 Fe N2 O2 P2 S'
_chemical_formula_weight         1714.92
_chemical_name_systematic
;
 ?
;
_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-2013
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                87.007(2)
_cell_angle_beta                 70.413(2)
_cell_angle_gamma                68.967(2)
_cell_formula_units_Z            2
_cell_length_a                   14.5766(10)
_cell_length_b                   17.7215(13)
_cell_length_c                   18.8505(13)
_cell_measurement_reflns_used    13783
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4244
_cell_measurement_theta_min      1.7122
_cell_volume                     4269.1(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60121
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.995
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0649P)^2^+3.8687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14935
_reflns_number_total             19294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01696d2.cif
_cod_data_source_block           3b
_cod_database_code               7043649
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.936
_shelxl_version_number           2013-4
_shelx_res_checksum              78732
_shelx_fab_checksum              70694