Nitric oxide activation by distal redox modulation in tetranuclear iron nitrosyl complexes.
de Ruiter, Graham; Thompson, Niklas B.; Lionetti, Davide; Agapie, Theodor; Journal of the American Chemical Society 137 (2015) 14094–14106; doi:10.1021/jacs.5b07397

data_4129513
_publ_section_title
;
 Nitric oxide activation by distal redox modulation in tetranuclear iron
 nitrosyl complexes.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14094
_journal_page_last               14106
_journal_paper_doi               10.1021/jacs.5b07397
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
'C84 H60 Fe4 N13 O5, C F3 O3 S, 1.5(C4 H10 O)'
_chemical_formula_sum            'C91 H75 F3 Fe4 N13 O9.5 S'
_chemical_formula_weight         1815.10
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
SHELXL-2014,
and manual edit
;
_cell_angle_alpha                90
_cell_angle_beta                 98.2302(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1605(7)
_cell_length_b                   29.0785(17)
_cell_length_c                   22.8070(13)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      2.28
_cell_volume                     7981.7(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT-2014/4 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            126756
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.027
_diffrn_reflns_theta_min         2.197
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatech I\mS HB'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0729 before and 0.0619 after correction.
The Ratio of minimum to maximum transmission is 0.9614.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3740
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         15691
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0361P)^2^+18.5903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11081
_reflns_number_total             15691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b07397_si_002.cif
_cod_data_source_block           p14163_f
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__computing_cell_refinement' was replaced with
'_computing_cell_refinement'.

Automatic conversion script
Id: cif_correct_tags 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_formula_sum        'C91 H75 F3 Fe4 N13 O9.50 S'
_cod_database_code               4129513
_shelxl_version_number           2014-2
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.841
_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
2. Restrained distances
 C101-C100
 1.517 with sigma of 0.002
 H10N-H10I
 2.2 with sigma of 0.005
 H10I-H10O
 2.2 with sigma of 0.005
 H10Q-H10I
 2.2 with sigma of 0.005
 H10N-H10J
 2.2 with sigma of 0.005
 C102-C101 \\sim C106_$1-C105_$1
 with sigma of 0.0001
 C103-C100 \\sim C107_$1-C104_$1
 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(C104) \\sim Ueq, Uanis(O101) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq, : with sigma of 0.01 and sigma
for terminal atoms of 0.1
4. Rigid body (RIGU) restrains
 C106, O101, C105, C104, H10N, H10O, H10P, H10Q, C107, H10K, H10L, H10M, H10R,
 H10S, H10T
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Same fragment restrains
{O100, C100, C101, C102, C103} sigma for 1-2: 0.01, 1-3: 0.01
as
{O101, C104, C105, C106, C107}
6. Others
 Fixed Sof: O101(0.5) C104(0.5) H10K(0.5) H10L(0.5) H10M(0.5) C105(0.5)
 H10N(0.5) H10O(0.5) C106(0.5) H10P(0.5) H10Q(0.5) C107(0.5) H10R(0.5)
 H10S(0.5) H10T(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C101(H10D,H10E), C102(H10F,H10G), C105(H10N,H10O), C106(H10P,H10Q)
7.b Me refined with riding coordinates:
 C100(H10A,H10B,H10C), C103(H10H,H10I,H10J), C104(H10K,H10L,H10M), C107(H10R,
 H10S,H10T)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C13(H13), C14(H14), C15(H15), C16(H16), C23(H23),
 C24(H24), C25(H25), C26(H26), C33(H33), C34(H34), C35(H35), C36(H36), C41(H41),
  C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49),
 C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59),
  C61(H61), C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68),
 C69(H69), C71(H71), C72(H72), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79),
  C81(H81), C82(H82), C85(H85), C86(H86), C87(H87), C88(H88), C89(H89),
 C91(H91), C92(H92), C95(H95), C96(H96), C97(H97), C98(H98), C99(H99)
;
_shelx_res_checksum              5966
_shelx_hkl_checksum              93557
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'