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_4129508
_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, 0.65(C H2 Cl2), 3(C F3 O3 S), 0.5(C4 H10 O), 0.5(O)'
_chemical_formula_sum            'C89.65 H66.3 Cl1.3 F9 Fe4 N13 O15 S3'
_chemical_formula_weight         2102.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
HELXL-2014,
and manual edit
;
_cell_angle_alpha                76.679(2)
_cell_angle_beta                 72.463(2)
_cell_angle_gamma                83.139(2)
_cell_formula_units_Z            4
_cell_length_a                   17.9136(12)
_cell_length_b                   20.5955(14)
_cell_length_c                   26.4341(19)
_cell_measurement_reflns_used    9029
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.53
_cell_measurement_theta_min      2.30
_cell_volume                     9035.9(11)
_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      100.05
_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  0.0793
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            271002
_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         26.022
_diffrn_reflns_theta_min         2.177
_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    0.829
_exptl_absorpt_correction_T_max  0.7456
_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 0.0997 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.9427.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4281
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.070
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2739
_refine_ls_number_reflns         35588
_refine_ls_number_restraints     1089
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.0941
_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^)+(0.1096P)^2^+79.9331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2421
_refine_ls_wR_factor_ref         0.2650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25602
_reflns_number_total             35588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b07397_si_004.cif
_cod_data_source_block           p14225_f
_cod_original_cell_volume        9036.0(11)
_cod_original_formula_sum        'C89.65 H66.30 Cl1.30 F9 Fe4 N13 O15 S3'
_cod_database_code               4129508
_shelxl_version_number           2014-2
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.872
_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
 S109-O111 = O200_$1-C101_$1
 1.411 with sigma of 0.02
 O200-C102
 1.411 with sigma of 0.02
 C100-C101
 1.517 with sigma of 0.02
 C102-C103
 1.517 with sigma of 0.02
 C101-C102
 2.3409 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C109) = Uanis(S109)
4. Rigid body (RIGU) restrains
 S112, F121, F120, F119, O120, O119, O118, C112
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O200, C101, C100, C102, C103
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S111, F118, F115, F117, O115, O117, O116, C111
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O201
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S110, F113, F114, F112, O114, O112, O113, C110, S109, F110, F111, F109, O110,
 O111, O109, C109, S108, F106, F107, F108, O107, O106, O108, C108
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl3, Cl4, C105, S114, F126, F125, F127, O124, O126, O125, C114
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Same fragment restrains
{Cl0A, Cl2, C104} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl3, Cl4, C105}
{S106, F102, F100, F101, O102, O100, O101, C106} sigma for 1-2: 0.02, 1-3: 0.04
as
{S107, F103, F105, F104, O105, O103, O104, C107}
{S106, F102, F100, F101, O102, O100, O101, C106} sigma for 1-2: 0.02, 1-3: 0.04
as
{S115, F129, F128, F130, O129, O127, O128, C115}
{S106, F102, F100, F101, O102, O100, O101, C106} sigma for 1-2: 0.02, 1-3: 0.04
as
{S112, F121, F120, F119, O120, O119, O118, C112}
{S106, F102, F100, F101, O102, O100, O101, C106} sigma for 1-2: 0.02, 1-3: 0.04
as
{S113, F123, F124, F122, O121, O122, O123, C113}
{S106, F102, F100, F101, O102, O100, O101, C106} sigma for 1-2: 0.01, 1-3: 0.01
as
{S114, F126, F125, F127, O124, O126, O125, C114}
{S106, F102, F100, F101, O102, O100, O101, C106} sigma for 1-2: 0.02, 1-3: 0.04
as
{S111, F118, F115, F117, O115, O117, O116, C111}
{S106, F102, F100, F101, O102, O100, O101, C106} sigma for 1-2: 0.02, 1-3: 0.04
as
{S110, F113, F114, F112, O114, O112, O113, C110}
{S106, F102, F100, F101, O102, O100, O101, C106} sigma for 1-2: 0.02, 1-3: 0.04
as
{S109, F110, F111, F109, O110, O111, O109, C109}
{S106, F102, F100, F101, O102, O100, O101, C106} sigma for 1-2: 0.02, 1-3: 0.04
as
{S108, F106, F107, F108, O107, O106, O108, C108}
6. Others
 1*[Sof(S108)+Sof(F106)+Sof(F107)+Sof(F108)+Sof(O107)+Sof(O106)+Sof(O108)+
 Sof(C108)]+1*[Sof(S110)+Sof(F113)+Sof(F114)+Sof(F112)+Sof(O114)+Sof(O112)+
 Sof(O113)+Sof(C110)]+1*[Sof(S109)+Sof(F110)+Sof(F111)+Sof(F109)+Sof(O110)+
 Sof(O111)+Sof(O109)+Sof(C109)]+1*[Sof(S111)+Sof(F118)+Sof(F115)+Sof(F117)+
 Sof(O115)+Sof(O117)+Sof(O116)+Sof(C111)]=2 with esd of 0.000001
 1*[Sof(S109)+Sof(F110)+Sof(F111)+Sof(F109)+Sof(O110)+Sof(O111)+Sof(O109)+
 Sof(C109)]+1*[Sof(S111)+Sof(F118)+Sof(F115)+Sof(F117)+Sof(O115)+Sof(O117)+
 Sof(O116)+Sof(C111)]=1 with esd of 0.000001
 1*[Sof(S108)+Sof(F106)+Sof(F107)+Sof(F108)+Sof(O107)+Sof(O106)+Sof(O108)+
 Sof(C108)]+1*[Sof(S110)+Sof(F113)+Sof(F114)+Sof(F112)+Sof(O114)+Sof(O112)+
 Sof(O113)+Sof(C110)]=1 with esd of 0.000001
 1*[Sof(S115)+Sof(F129)+Sof(F128)+Sof(F130)+Sof(O129)+Sof(O127)+Sof(O128)+
 Sof(C115)]+1*[Sof(S114)+Sof(F126)+Sof(F125)+Sof(F127)+Sof(O124)+Sof(O126)+
 Sof(O125)+Sof(C114)]=1 with esd of 0.000001
 1*[Sof(S115)+Sof(F129)+Sof(F128)+Sof(F130)+Sof(O129)+Sof(O127)+Sof(O128)+
 Sof(C115)]+1*[Sof(Cl3)+Sof(Cl4)+Sof(C105)+Sof(H10M)+Sof(H10N)]=1 with esd of
 0.000001
 Sof(S112)=Sof(F121)=Sof(F120)=Sof(F119)=Sof(O120)=Sof(O119)=Sof(O118)=
 Sof(C112)=1-FVAR(1)
 Sof(S113)=Sof(F123)=Sof(F124)=Sof(F122)=Sof(O121)=Sof(O122)=Sof(O123)=
 Sof(C113)=FVAR(1)
 Sof(S108)=Sof(F106)=Sof(F107)=Sof(F108)=Sof(O107)=Sof(O106)=Sof(O108)=
 Sof(C108)=FVAR(2)
 Sof(S110)=Sof(F113)=Sof(F114)=Sof(F112)=Sof(O114)=Sof(O112)=Sof(O113)=
 Sof(C110)=FVAR(3)
 Sof(S109)=Sof(F110)=Sof(F111)=Sof(F109)=Sof(O110)=Sof(O111)=Sof(O109)=
 Sof(C109)=FVAR(4)
 Sof(S111)=Sof(F118)=Sof(F115)=Sof(F117)=Sof(O115)=Sof(O117)=Sof(O116)=
 Sof(C111)=FVAR(5)
 Sof(S115)=Sof(F129)=Sof(F128)=Sof(F130)=Sof(O129)=Sof(O127)=Sof(O128)=
 Sof(C115)=FVAR(6)
 Sof(S114)=Sof(F126)=Sof(F125)=Sof(F127)=Sof(O124)=Sof(O126)=Sof(O125)=
 Sof(C114)=FVAR(7)
 Sof(Cl3)=Sof(Cl4)=Sof(C105)=Sof(H10M)=Sof(H10N)=FVAR(8)
7.a Secondary CH2 refined with riding coordinates:
 C104(H10K,H10L), C105(H10M,H10N), C101(H10A,H10B), C102(H10F,H10G)
7.b Me refined with riding coordinates:
 C100(H10C,H10D,H10E), C103(H10H,H10I,H10J)
7.c Aromatic/amide H refined with riding coordinates:
 C51A(H51A), C52A(H52A), C81A(H81A), C59A(H59A), C4A(H4A), C54A(H54A),
 C2A(H2A), C6A(H6A), C71A(H71A), C24A(H24A), C68A(H68A), C58A(H58A), C53A(H53A),
  C63A(H63A), C69A(H69A), C41A(H41A), C62A(H62A), C44A(H44A), C72A(H72A),
 C25A(H25A), C90A(H90A), C89A(H89A), C33A(H33A), C16A(H16A), C13A(H13A),
 C88A(H88A), C75A(H75A), C76A(H76A), C14A(H14A), C49A(H49A), C34A(H34A),
 C15A(H15A), C46A(H46A), C78A(H78A), C87A(H87A), C86A(H86A), C48A(H48A),
 C98A(H98A), C47A(H47A), C96A(H96A), C95A(H95A), C23A(H23A), C26A(H26A),
 C56A(H56A), C57A(H57A), C82A(H82A), C61A(H61A), C66A(H66A), C64A(H64A),
 C67A(H67A), C36A(H36A), C43A(H43A), C91A(H91A), C79A(H79A), C85A(H85A),
 C35A(H35A), C42A(H42A), C77A(H77A), C94A(H94A), C97A(H97A), C2(H2), C26(H26),
 C24(H24), C6(H6), C44(H44), C51(H51), C69(H69), C49(H49), C16(H16), C15(H15),
 C71(H71), C41(H41), C46(H46), C34(H34), C33(H33), C57(H57), C59(H59), C43(H43),
  C53(H53), C81(H81), C14(H14), C64(H64), C66(H66), C61(H61), C42(H42),
 C68(H68), C75(H75), C82(H82), C92(H92), C91(H91), C67(H67), C76(H76), C63(H63),
  C78(H78), C98(H98), C97(H97), C89(H89), C88(H88), C96(H96), C4(H4), C23(H23),
 C36(H36), C35(H35), C25(H25), C56(H56), C72(H72), C54(H54), C52(H52), C48(H48),
  C58(H58), C13(H13), C47(H47), C79(H79), C99(H99), C77(H77), C62(H62),
 C85(H85), C95(H95), C86(H86), C87(H87)
;
_shelx_res_checksum              32685
_shelx_hkl_checksum              46758
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'