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_1542585
_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
'C19 H19 Fe3 N4 O6 S2, B1 F4, 0.6(C2 H3 N), 0.72(H2 O)'
_chemical_formula_sum            'C20.2 H22.23 B F4 Fe3 N4.6 O6.72 S2'
_chemical_formula_weight         755.40
_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   mixed
_audit_creation_date             2014-08-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2016-01-14 deposited with the CCDC.
2016-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                76.988(2)
_cell_angle_beta                 85.341(2)
_cell_angle_gamma                81.750(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4593(5)
_cell_length_b                   11.6085(6)
_cell_length_c                   12.2560(6)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      30.015
_cell_measurement_theta_min      2.502
_cell_volume                     1433.02(12)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.938
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46532
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.797
_diffrn_reflns_theta_min         1.970
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.717
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0768 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.8236.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       block
_exptl_crystal_F_000             761
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.038
_refine_diff_density_max         2.007
_refine_diff_density_min         -1.856
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         8411
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0908P)^2^+2.8479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6833
_reflns_number_total             8411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00213g3.cif
_cod_data_source_block           8314
_cod_depositor_comments
'Adding full bibliography for 1542583--1542586.cif.'
_cod_original_formula_sum        'C20.20 H22.23 B F4 Fe3 N4.60 O6.72 S2'
_cod_database_code               1542585
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Shared sites
{B1S, B1T}
3. Restrained distances
 C2E-C1E
 1.54 with sigma of 0.005
 N1E-C2E
 1.1 with sigma of 0.005
 F1-B1S \\sim F1A-B1T \\sim F3A-B1T \\sim F2-B1S \\sim F2A-B1T \\sim F3-B1S
\\sim F4A-B1T \\sim F4-B1S
 with sigma of 0.005
 F1-F2 \\sim F2-F3 \\sim F3-F4 \\sim F4-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim
F3A-F4A \\sim F4A-F1A \\sim F1A-F3A
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(N1E) = Uanis(C1E) = Uanis(C2E)
Uanis(B1S) = Uanis(F1) = Uanis(F2) = Uanis(F3) = Uanis(F4) = Uanis(B1T) =
Uanis(F1A) = Uanis(F2A) = Uanis(F3A) = Uanis(F4A)
5. Others
 Sof(B1T)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=1-FVAR(1)
 Sof(B1S)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1)
 Sof(O7A)=Sof(H7AA)=Sof(H7AB)=FVAR(2)
 Fixed Sof: N1E(0.6) C1E(0.6) H1EA(0.6) H1EB(0.6) H1EC(0.6) C2E(0.6)
6.a Riding coordinates:
 O7A(H7AA,H7AB)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
6.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C1E(H1EA,H1EB,H1EC)
;
_shelx_res_checksum              66186