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_4129511
_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, 1.14(C4 H10 O), 2(C F3 O3 S), 2.86(C2 H3 N)'
_chemical_formula_sum            'C96.69 H79.66 F6 Fe4 N14.87 O11.13 S2'
_chemical_formula_weight         2029.43
_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             2015-07-08
_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                 95.4328(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.4372(11)
_cell_length_b                   30.6281(15)
_cell_length_c                   24.9731(12)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      2.34
_cell_volume                     18607.5(15)
_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
_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 0.998
_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  0.0709
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            266264
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         2.229
_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    0.737
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1177 before and 0.0594 after correction.
The Ratio of minimum to maximum transmission is 0.9429.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             8343
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.718
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1396
_refine_ls_number_reflns         21287
_refine_ls_number_restraints     249
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0864P)^2^+83.7107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16220
_reflns_number_total             21287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b07397_si_001.cif
_cod_data_source_block           p14147_f
_cod_database_code               4129511
_shelxl_version_number           2014-2
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.867
_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
 C304-C305
 1.458 with sigma of 0.02
 C305-N302
 1.157 with sigma of 0.02
 C304-N302
 2.615 with sigma of 0.02
 C208-C209
 1.517 with sigma of 0.02
 C211-C210
 1.517 with sigma of 0.02
 C209-O200
 1.411 with sigma of 0.02
 O200-C210
 1.411 with sigma of 0.02
 C208-O200
 2.3756 with sigma of 0.02
 O200-C211
 2.3756 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C204) = Uanis(C205)
Uanis(C202) = Uanis(C203)
4. Rigid body (RIGU) restrains
 C401, F403, F405, F404, S401, O404, O403, O405, S402, O407, O406, C402, F406,
 F408, O408, F407
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N303, C307, C306, H30J, H30K, H30L
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O201, C200, H20P, H20Q, H20R, C201, H20S, H20T, C202, C203, H20W, H20X, H20Y
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C307, N303, C306, H30J, H30K, H30L
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Same fragment restrains
{C400, F400, F401, F402, S400, O402, O400, O401} sigma for 1-2: 0.02, 1-3: 0.04
as
{C401, F403, F405, F404, S401, O404, O403, O405}
{C400, F400, F401, F402, S400, O402, O400, O401} sigma for 1-2: 0.02, 1-3: 0.04
as
{C402, F406, F408, F407, S402, O407, O408, O406}
{N302, C305, C304} sigma for 1-2: 0.02, 1-3: 0.04
as
{N300, C301, C300}
{N302, C305, C304} sigma for 1-2: 0.02, 1-3: 0.04
as
{N301, C303, C302}
{C208, C209, O200, C210, C211} sigma for 1-2: 0.02, 1-3: 0.04
as
{C207, C206, O202, C205, C204}
{C208, C209, O200, C210, C211} sigma for 1-2: 0.02, 1-3: 0.04
as
{C200, C201, O201, C202, C203}
{N302, C305, C304} sigma for 1-2: 0.02, 1-3: 0.04
as
{N303, C307, C306}
6. Others
 Sof(C402)=Sof(F406)=Sof(F408)=Sof(F407)=Sof(S402)=Sof(O407)=Sof(O408)=
 Sof(O406)=1-FVAR(1)
 Sof(C401)=Sof(F403)=Sof(F405)=Sof(F404)=Sof(S401)=Sof(O404)=Sof(O403)=
 Sof(O405)=FVAR(1)
 Sof(C200)=Sof(H20P)=Sof(H20Q)=Sof(H20R)=Sof(C201)=Sof(H20S)=Sof(H20T)=
 Sof(O201)=Sof(C202)=Sof(H20U)=Sof(H20V)=Sof(C203)=Sof(H20W)=Sof(H20X)=
 Sof(H20Y)=1-FVAR(2)
 Sof(C207)=Sof(H20F)=Sof(H20G)=Sof(H20H)=Sof(C206)=Sof(H20I)=Sof(H20J)=
 Sof(O202)=Sof(C205)=Sof(H20K)=Sof(H20L)=Sof(C204)=Sof(H20M)=Sof(H20N)=
 Sof(H20O)=Sof(N303)=Sof(C307)=Sof(C306)=Sof(H30J)=Sof(H30K)=Sof(H30L)=0.5*
 FVAR(3)
 Fixed Sof: C208(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C209(0.5) H20D(0.5)
 H20E(0.5) O200(0.5) C210(0.5) H21A(0.5) H21B(0.5) C211(0.5) H21C(0.5)
 H21D(0.5) H21E(0.5) N301(0.5) C303(0.5) C302(0.5) H30G(0.5) H30H(0.5) H30I(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C209(H20D,H20E), C210(H21A,H21B), C206(H20I,H20J), C205(H20K,H20L), C201(H20S,
 H20T), C202(H20U,H20V)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C52(H52), C51(H51), C2(H2), C71(H71), C16(H16), C53(H53),
 C66(H66), C26(H26), C13(H13), C36(H36), C14(H14), C61(H61), C82(H82), C63(H63),
  C15(H15), C23(H23), C81(H81), C24(H24), C54(H54), C41(H41), C72(H72),
 C62(H62), C79(H79), C91(H91), C33(H33), C42(H42), C44(H44), C92(H92), C46(H46),
  C69(H69), C25(H25), C85(H85), C49(H49), C99(H99), C64(H64), C77(H77),
 C35(H35), C43(H43), C75(H75), C78(H78), C34(H34), C67(H67), C68(H68), C76(H76),
  C59(H59), C98(H98), C96(H96), C86(H86), C56(H56), C48(H48), C95(H95),
 C47(H47), C89(H89), C57(H57), C97(H97), C58(H58), C88(H88), C87(H87)
7.c Idealised Me refined as rotating group:
 C208(H20A,H20B,H20C), C211(H21C,H21D,H21E), C304(H30A,H30B,H30C), C300(H30D,
 H30E,H30F), C302(H30G,H30H,H30I), C207(H20F,H20G,H20H), C204(H20M,H20N,H20O),
 C200(H20P,H20Q,H20R), C203(H20W,H20X,H20Y), C306(H30J,H30K,H30L)
;
_shelx_res_checksum              45278
_shelx_hkl_checksum              59760
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'