Modeling the Signatures of Hydrides in Metalloenzymes: ENDOR Analysis of a Di-iron Fe(μ-NH)(μ-H)Fe Core
R. Adam Kinney; Caroline T. Saouma; Jonas C. Peters; Brian M. Hoffman; Journal of the American Chemical Society 134 (2012) 12637–12647; doi:10.1021/ja303739g

data_4118394
_publ_section_title
;
 Modeling the Signatures of Hydrides in Metalloenzymes: ENDOR Analysis of
 a Di-iron Fe(\m-NH)(\m-H)Fe Core
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12637
_journal_page_last               12647
_journal_paper_doi               10.1021/ja303739g
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C90 H84 B2 Fe2 N P6, 3(C4 H8 O)'
_chemical_formula_sum            'C102 H108 B2 Fe2 N O3 P6'
_chemical_formula_weight         1715.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.173(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2692(19)
_cell_length_b                   14.4294(16)
_cell_length_c                   36.797(4)
_cell_measurement_reflns_used    7400
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      2.3
_cell_volume                     8444.0(16)
_computing_cell_refinement       'SAINT V6.45A (Bruker, 2007)'
_computing_data_collection       'Bruker SMART v5.054 (Bruker, 2007)'
_computing_data_reduction        'SAINT V6.45A (Bruker, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w scans at 5 \f settings'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            154350
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         31.55
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dichroic olive/brown'
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       plate
_exptl_crystal_F_000             3612
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         25383
_refine_ls_number_restraints     505
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+7.4971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1607
_reflns_number_gt                16264
_reflns_number_total             25383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303739g_si_002.cif
_cod_data_source_block           car12ma1
_cod_original_cell_volume        8444.0(17)
_cod_database_code               4118394