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_4344635
_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         'C61 H50 Fe N2 O2 P2'
_chemical_formula_sum            'C61 H50 Fe N2 O2 P2'
_chemical_formula_weight         960.82
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 98.3580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1826(6)
_cell_length_b                   20.0251(8)
_cell_length_c                   17.0084(8)
_cell_measurement_reflns_used    24658
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      3.05
_cell_volume                     4779.2(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_publication_material  'BRUKER SHELXTL'
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_laue_measured_fraction_full 0.988
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24194
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         3.077
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.644234
_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    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         8332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+4.0937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6971
_reflns_number_total             8332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01733_si_001.cif
_cod_data_source_block           GDP320
_cod_database_code               4344635
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2013-4
_shelx_res_checksum              1467
_shelx_hkl_checksum              59226