Cyanide Docking and Linkage Isomerism in Models for the Artificial [FeFe]-Hydrogenase Maturation Process.
Sil, Debangsu; Martinez, Zachary; Ding, Shengda; Bhuvanesh, Nattamai; Darensbourg, Donald J.; Hall, Michael B.; Darensbourg, Marcetta Y.; Journal of the American Chemical Society 140 (2018) 9904–9911; doi:10.1021/jacs.8b04189

data_4132475
_publ_section_title
;
 Cyanide Docking and Linkage Isomerism in Models for the Artificial
 [FeFe]-Hydrogenase Maturation Process.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9904
_journal_page_last               9911
_journal_paper_doi               10.1021/jacs.8b04189
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C63 H46 Cu N9 Zn, C H2 Cl2'
_chemical_formula_sum            'C64 H48 Cl2 Cu N9 Zn'
_chemical_formula_weight         1142.92
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.583(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1151(6)
_cell_length_b                   18.5419(8)
_cell_length_c                   19.9898(8)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      25.009
_cell_measurement_theta_min      2.421
_cell_volume                     5231.5(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            64165
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.067
_diffrn_reflns_theta_max         25.067
_diffrn_reflns_theta_min         2.422
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  0.5618
_exptl_absorpt_correction_T_min  0.4925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0943 before and 0.0678 after correction. The Ratio of minimum to maximum transmission is 0.8766. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.194
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         9250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0284P)^2^+12.7834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6882
_reflns_number_total             9250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04189_si_004.cif
_cod_data_source_block           ds
_cod_database_code               4132475
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.799
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C57(H57A,H57B), C58(H58A,H58B), C3S(H3SA,H3SB)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36),
 C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48),
  C49(H49), C52(H52), C53(H53), C54(H54), C55(H55), C61(H61), C62(H62),
 C63(H63), C64(H64)
;
_shelx_res_checksum              85978
_shelx_hkl_checksum              26144
_olex2_submission_special_instructions 'No special instructions were received'