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_4132474
_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, F6 P'
_chemical_formula_sum            'C63 H46 Cu F6 N9 P Zn'
_chemical_formula_weight         1202.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-11-29
_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                 90.768(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.550(2)
_cell_length_b                   31.109(8)
_cell_length_c                   19.849(5)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      23.662
_cell_measurement_theta_min      2.216
_cell_volume                     5896(2)
_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 2014/5 (Sheldrick, 2014)'
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66386
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        19.998
_diffrn_reflns_theta_max         19.998
_diffrn_reflns_theta_min         1.663
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.861
_exptl_absorpt_correction_T_max  0.5614
_exptl_absorpt_correction_T_min  0.4653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0729 before and 0.0565 after correction. The Ratio of minimum to maximum transmission is 0.8288. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       plate
_exptl_crystal_F_000             2460
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         5491
_refine_ls_number_restraints     512
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0220P)^2^+35.0860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1240
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4952
_reflns_number_total             5491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04189_si_005.cif
_cod_data_source_block           znnccupf6_sq
_cod_original_cell_volume        5897(2)
_cod_database_code               4132474
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.763
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C17-C16 \\sim C17A-C16
 with sigma of 0.02
 C39-C38 \\sim C39A-C38
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C17A \\sim C18A
\\sim C19A \\sim C20A \\sim C21A \\sim C22A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C39A \\sim C40A
\\sim C41A \\sim C42A \\sim C43A \\sim C44A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C39A) = Uanis(C39)
Uanis(C17) = Uanis(C17A)
Uanis(C22A) = Uanis(C22)
4. Rigid body (RIGU) restrains
 C17, C18, C19, C20, C21, C22, C17A, C18A, C19A, C20A, C21A, C22A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C39, C40, C41, C42, C43, C44, C39A, C40A, C41A, C42A, C43A, C44A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=
 Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C39A)=Sof(C40A)=Sof(H40A)=
 Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=Sof(H43A)=Sof(C44A)=
 Sof(H44A)=1-FVAR(1)
 Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=
 Sof(H21)=Sof(C22)=Sof(H22)=Sof(C39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=
 Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C57(H57A,H57B), C63(H63A,H63B)
6.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), C18A(H18A),
 C19A(H19A), C20A(H20A), C21A(H21A), C22A(H22A), 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), C40A(H40A), C41A(H41A), C42A(H42A), C43A(H43A),
 C44A(H44A), C46(H46), C47(H47), C48(H48), C49(H49), C52(H52), C53(H53),
 C54(H54), C55(H55), C58(H58), C59(H59), C60(H60), C61(H61)
6.c Fitted hexagon refined as free rotating group:
 C17(C18,C19,C20,C21,C22), C17A(C18A,C19A,C20A,C21A,C22A), C39(C40,C41,C42,C43,
 C44), C39A(C40A,C41A,C42A,C43A,C44A)
;
_shelx_res_checksum              83759
_shelx_hkl_checksum              8546
_shelx_fab_checksum              84795
_olex2_submission_special_instructions 'No special instructions were received'