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_1542583
_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         'C16 H11 Fe3 N O7 S2'
_chemical_formula_sum            'C16 H11 Fe3 N O7 S2'
_chemical_formula_weight         560.93
_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             2014-05-27
_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                94.504(10)
_cell_angle_beta                 108.019(10)
_cell_angle_gamma                93.687(10)
_cell_formula_units_Z            2
_cell_length_a                   7.7263(14)
_cell_length_b                   11.203(2)
_cell_length_c                   11.900(2)
_cell_measurement_reflns_used    6152
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.538
_cell_measurement_theta_min      2.705
_cell_volume                     972.2(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.992
_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_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4458
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.575
_diffrn_reflns_theta_min         1.809
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.463
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1049 before and 0.0797 after correction.
 The Ratio of minimum to maximum transmission is 0.78.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 38923 reflections, Rint = 0.0693
 (18429 with I > 3sig(I), Rint = 0.0587)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4458
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0425P)^2^+0.1252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4016
_reflns_number_total             4458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00213g3.cif
_cod_data_source_block           cn
_cod_depositor_comments
'Adding full bibliography for 1542583--1542586.cif.'
_cod_original_cell_volume        972.3(3)
_cod_database_code               1542583
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.757
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C3-C2A \\sim C3-C2 \\sim C2-C1 \\sim C2A-C1
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C2A)
4. Others
 Sof(H1BC)=Sof(H1BD)=Sof(H3BC)=Sof(H3BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C2(H2A,H2B), C3(H3AA,H3AB), C3(H3BC,H3BD),
 C2A(H2AA,H2AB)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14)
;
_shelx_res_checksum              32927