Cyanide-bridged iron complexes as biomimetics of tri-iron arrangements in maturases of the H cluster of the di-iron hydrogenase
Lunsford, Allen M.; Beto, Christopher C.; Ding, Shengda; Erdem, Özlen F.; Wang, Ning; Bhuvanesh, Nattamai; Hall, Michael B.; Darensbourg, Marcetta Y.; Chem. Sci. 7 (2016) 3710–; doi:10.1039/C6SC00213G

data_1542584
_publ_section_title
;
 Cyanide-bridged iron complexes as biomimetics of tri-iron arrangements in
 maturases of the H cluster of the di-iron hydrogenase
;
_journal_issue                   6
_journal_name_full               'Chem. Sci.'
_journal_page_first              3710
_journal_paper_doi               10.1039/C6SC00213G
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C40 H35 Fe3 N O5 P2 S2'
_chemical_formula_sum            'C40 H35 Fe3 N O5 P2 S2'
_chemical_formula_weight         903.30
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-03-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.22 svn.r3046 for OlexSys, GUI svn.r4928)
;
_audit_update_record
;
2016-01-14 deposited with the CCDC.
2016-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                105.449(5)
_cell_angle_beta                 100.216(5)
_cell_angle_gamma                110.921(4)
_cell_formula_units_Z            2
_cell_length_a                   11.3103(15)
_cell_length_b                   12.9416(18)
_cell_length_c                   15.479(2)
_cell_measurement_reflns_used    9645
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      27.777
_cell_measurement_theta_min      2.487
_cell_volume                     1944.2(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            87852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.898
_diffrn_reflns_theta_min         2.023
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.339
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0671 before and 0.0493 after correction.
The Ratio of minimum to maximum transmission is 0.8762.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         9112
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0406P)^2^+2.8009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7750
_reflns_number_total             9112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00213g3.cif
_cod_data_source_block           pdtisomer
_cod_depositor_comments
'Adding full bibliography for 1542583--1542586.cif.'
_cod_database_code               1542584
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.824
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C36, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C18, C19, C20, C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B), C1(H1A,H1B), C3(H3A,H3B), C2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C28(H28), C14(H14), C34(H34), C30(H30), C33(H33),
 C26(H26), C27(H27), C15(H15), C31(H31), C18(H18), C13(H13), C36(H36), C32(H32),
  C22(H22), C16(H16), C12(H12), C19(H19), C38(H38), C37(H37), C40(H40),
 C20(H20), C21(H21), C39(H39)
;
_shelx_res_checksum              19051
_olex2_submission_special_instructions 'No special instructions were received'