Iron Hydride Detection and Intramolecular Hydride Transfer in a Synthetic Model of Mono-Iron Hydrogenase with a CNS Chelate.
Durgaprasad, Gummadi; Xie, Zhu-Lin; Rose, Michael J.; Inorganic chemistry 55 (2016) 386–389; doi:10.1021/acs.inorgchem.5b01733

data_4344634
_publ_section_title
;
 Iron Hydride Detection and Intramolecular Hydride Transfer in a Synthetic
 Model of Mono-Iron Hydrogenase with a CNS Chelate.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              386
_journal_page_last               389
_journal_paper_doi               10.1021/acs.inorgchem.5b01733
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'2 C12 H9 N2 O, 2 Fe, 2 C H3 S, 4 C O, 1.5 C6 H5 F'
_chemical_formula_sum            'C39 H31.5 F1.5 Fe2 N4 O6 S2'
_chemical_formula_weight         856.50
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 90.928(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.9479(6)
_cell_length_b                   18.8950(6)
_cell_length_c                   18.6299(5)
_cell_measurement_reflns_used    11342
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      75.1
_cell_measurement_theta_min      3.8
_cell_volume                     8076.9(4)
_computing_cell_refinement
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
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'CrysAlisPro V 1.171.37.31, Agilent Technologies'
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'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'Shelxl-2013, Sheldrick, G. M.'
_computing_structure_solution
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
'Agilent SuperNova Dual with AtlasS2 detector'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18490
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         69.984
_diffrn_reflns_theta_min         3.830
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    7.204
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       prism
_exptl_crystal_F_000             3512
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         7568
_refine_ls_number_restraints     335
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+3.2208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6048
_reflns_number_total             7568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01733_si_001.cif
_cod_data_source_block           GDP288
_cod_original_formula_sum        'C39 H31.50 F1.50 Fe2 N4 O6 S2'
_cod_database_code               4344634
_shelx_estimated_absorpt_t_min   0.313
_shelx_estimated_absorpt_t_max   0.715
_shelxl_version_number           2013-4
_shelx_res_checksum              40961
_shelx_hkl_checksum              49415
_shelx_fab_checksum              23618