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_4129509
_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 N12 O4, B F4, 2(C4 H10 O)'
_chemical_formula_sum            'C92 H80 B F4 Fe4 N12 O6'
_chemical_formula_weight         1759.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-07
_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                 113.5582(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.1338(10)
_cell_length_b                   17.6952(4)
_cell_length_c                   25.3732(6)
_cell_measurement_reflns_used    9543
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.51
_cell_measurement_theta_min      2.77
_cell_volume                     16517.6(7)
_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 0.982
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1195
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            161510
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.779
_diffrn_reflns_theta_min         2.771
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.115
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.4986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1453 before and 0.0924 after correction.
The Ratio of minimum to maximum transmission is 0.6611.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             7272
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.701
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         17491
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0750
_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^)+(0.0913P)^2^+141.3511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.2040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12935
_reflns_number_total             17491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b07397_si_005.cif
_cod_data_source_block           p15116_f
_cod_database_code               4129509
_shelxl_version_number           2014-2
_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
 C103-C102
 1.517 with sigma of 0.002
 O100-C101
 1.411 with sigma of 0.002
 O100-C102
 1.411 with sigma of 0.002
 C102-C101
 2.309 with sigma of 0.002
 C103-C100
 4.7431 with sigma of 0.002
 O100-C101 \\sim O100-C102 \\sim O300-C302 \\sim O200-C201 \\sim O300-C301
\\sim O200-C202 \\sim O400-
 C401 \\sim O400-C402
 with sigma of 0.02
 C101-C100 \\sim C302-C303 \\sim C401-C400 \\sim C102-C103 \\sim C202-C203
\\sim C402-C403 \\sim C301-
 C300 \\sim C201-C200
 with sigma of 0.02
 O100-C103 \\sim O400-C403 \\sim O200-C200 \\sim O300-C300 \\sim O100-C100
\\sim O300-C303 \\sim O400-
 C400 \\sim O200-C203
 with sigma of 0.04
 C102-C101 \\sim C201-C202 \\sim C301-C302 \\sim C402-C401
 with sigma of 0.04
 O100-C101 \\sim O100-C102 \\sim O300-C302 \\sim O200-C201 \\sim O300-C301
\\sim O200-C202 \\sim O400-
 C401 \\sim O400-C402
 with sigma of 0.02
 C302-C303 \\sim C102-C103 \\sim C202-C203 \\sim C402-C403 \\sim C301-C300
\\sim C201-C200 \\sim C401-
 C400 \\sim C101-C100
 with sigma of 0.02
 O200-C200 \\sim O400-C400 \\sim O200-C203 \\sim O300-C300 \\sim O100-C100
\\sim O300-C303 \\sim O100-
 C103 \\sim O400-C403
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C401) \\sim Ueq, Uanis(O400) \\sim Ueq, Uanis(C402) \\sim Ueq,
Uanis(C403) \\sim Ueq, Uanis(C400) \\sim Ueq, : with sigma of 0.01 and sigma
for terminal atoms of 0.1
Uanis(C27) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.05
Uanis(C102) \\sim Ueq, Uanis(O100) \\sim Ueq, Uanis(C101) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C100) \\sim Ueq, : with sigma of 0.001 and sigma
for terminal atoms of 0.1
Uanis(C200) = Uanis(C201)
Uanis(C401) = Uanis(C400)
Uanis(C101) = Uanis(C100)
4. Rigid body (RIGU) restrains
 O300, C301, C302, C300, C303, O200, C201, C202, C200, C203, O400, C402, C401,
 C403, C400
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C102, O100, C101, H10A, H10B, C103, H10F, H10G, C100, H10C, H10D, H10E, H10H,
 H10I, H10J
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Same fragment restrains
{O100, C102, C103, C101, C100} sigma for 1-2: 0.02, 1-3: 0.04
as
{O200, C201, C200, C202, C203}
{O100, C102, C103, C101, C100} sigma for 1-2: 0.02, 1-3: 0.04
as
{O400, C402, C403, C401, C400}
{O100, C102, C103, C101, C100} sigma for 1-2: 0.02, 1-3: 0.04
as
{O300, C301, C300, C302, C303}
6. Others
 Sof(O300)=Sof(C301)=Sof(H30A)=Sof(H30B)=Sof(C300)=Sof(H30C)=Sof(H30D)=
 Sof(H30E)=Sof(C302)=Sof(H30F)=Sof(H30G)=Sof(C303)=Sof(H30H)=Sof(H30I)=
 Sof(H30J)=1-FVAR(1)
 Sof(O200)=Sof(C201)=Sof(H20A)=Sof(H20B)=Sof(C200)=Sof(H20C)=Sof(H20D)=
 Sof(H20E)=Sof(C202)=Sof(H20F)=Sof(H20G)=Sof(C203)=Sof(H20H)=Sof(H20I)=
 Sof(H20J)=Sof(O400)=Sof(C402)=Sof(H40A)=Sof(H40B)=Sof(C403)=Sof(H40C)=
 Sof(H40D)=Sof(H40E)=Sof(C401)=Sof(H40F)=Sof(H40G)=Sof(C400)=Sof(H40H)=
 Sof(H40I)=Sof(H40J)=0.5*FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C102(H10A,H10B), C101(H10F,H10G), C201(H20A,H20B), C202(H20F,H20G), C402(H40A,
 H40B), C401(H40F,H40G), C301(H30A,H30B), C302(H30F,H30G)
7.b Me refined with riding coordinates:
 C103(H10C,H10D,H10E), C100(H10H,H10I,H10J), C200(H20C,H20D,H20E), C203(H20H,
 H20I,H20J), C403(H40C,H40D,H40E), C400(H40H,H40I,H40J), C300(H30C,H30D,H30E),
 C303(H30H,H30I,H30J)
7.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C61(H61), C4(H4), C25(H25), C99(H99), C51(H51), C66(H66),
 C92(H92), C56(H56), C63(H63), C64(H64), C34(H34), C82(H82), C69(H69), C96(H96),
  C44(H44), C91(H91), C41(H41), C79(H79), C71(H71), C77(H77), C68(H68),
 C88(H88), C26(H26), C98(H98), C72(H72), C59(H59), C35(H35), C67(H67), C89(H89),
  C86(H86), C87(H87), C58(H58), C49(H49), C46(H46), C13(H13), C76(H76),
 C48(H48), C57(H57), C47(H47), C16(H16), C75(H75), C24(H24), C43(H43), C62(H62),
  C23(H23), C81(H81), C95(H95), C52(H52), C33(H33), C85(H85), C97(H97),
 C36(H36), C42(H42), C78(H78), C54(H54), C53(H53), C15(H15), C14(H14)
;
_shelx_res_checksum              66415
_shelx_hkl_checksum              98311
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'