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_1542586
_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
'C44 H54 Fe3 N O3 P4 S2, C32 H12 B F24, C4 H9 O'
_chemical_formula_sum            'C80 H75 B F24 Fe3 N O4 P4 S2'
_chemical_formula_weight         1936.77
_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   mixed
_audit_creation_date             2015-02-23
_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                92.828(5)
_cell_angle_beta                 94.410(5)
_cell_angle_gamma                99.584(5)
_cell_formula_units_Z            2
_cell_length_a                   13.352(5)
_cell_length_b                   13.623(5)
_cell_length_c                   24.074(8)
_cell_measurement_reflns_used    8323
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      23.424
_cell_measurement_theta_min      2.208
_cell_volume                     4296(3)
_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 0.845
_diffrn_measured_fraction_theta_max 0.989
_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_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.845
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.845
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.850
_diffrn_reflns_theta_min         2.138
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.622
_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 0.0859 before and 0.0648 after correction.
 The Ratio of minimum to maximum transmission is 0.83.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 184721 reflections, Rint = 0.1148
 (43813 with I > 3sig(I), Rint = 0.0616)
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       block
_exptl_crystal_F_000             1970
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.070
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1080
_refine_ls_number_reflns         13129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0790
_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^)+(0.1273P)^2^+8.0032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2135
_refine_ls_wR_factor_ref         0.2317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9068
_reflns_number_total             13129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00213g3.cif
_cod_data_source_block           twin4
_cod_depositor_comments
'Adding full bibliography for 1542583--1542586.cif.'
_cod_database_code               1542586
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.899
_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 Fe(H) groups
2.a Riding coordinates:
 Fe3(H)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C2S(H2SA,H2SB)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C2C(H2C), C4C(H4C), C6C(H6C), C10C(H10C), C12C(H12C), C14C(H14C),
 C18C(H18C), C20C(H20C), C22C(H22C), C26C(H26C), C28C(H28C), C30C(H30C),
 C4S(H4S)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C1S(H1SA,H1SB,H1SC), C5S(H5SA,
 H5SB,H5SC)
;
_shelx_res_checksum              54153
_olex2_submission_special_instructions 'No special instructions were received'