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_4129510
_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, 0.89(C H2 Cl2), 3(C F3 O3 S), 0.55(C4 H10 O)'
_chemical_formula_sum            'C90.1 H67.3 Cl1.78 F9 Fe4 N12 O13.55 S3'
_chemical_formula_weight         2088.54
_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             2015-05-18
_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                99.6189(19)
_cell_angle_beta                 94.3724(19)
_cell_angle_gamma                93.4051(18)
_cell_formula_units_Z            2
_cell_length_a                   15.4560(7)
_cell_length_b                   15.4962(7)
_cell_length_c                   19.2923(10)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.40
_cell_measurement_theta_min      2.42
_cell_volume                     4530.2(4)
_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      100.03
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.998
_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  0.0651
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            242554
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.577
_diffrn_reflns_theta_min         2.388
_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    0.838
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0933 before and 0.0549 after correction.
The Ratio of minimum to maximum transmission is 0.9234.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2127
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.146
_refine_diff_density_max         2.627
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1549
_refine_ls_number_reflns         32996
_refine_ls_number_restraints     708
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0740
_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^)+(0.1114P)^2^+12.8628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23072
_reflns_number_total             32996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b07397_si_006.cif
_cod_data_source_block           p15147_f
_cod_original_formula_sum        'C90.10 H67.30 Cl1.78 F9 Fe4 N12 O13.55 S3'
_cod_database_code               4129510
_shelxl_version_number           2014-2
_shelx_estimated_absorpt_t_max   0.887
_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
 H67-H10T
 2.2 with sigma of 0.01
 H68-H10L
 2.2 with sigma of 0.01
 H10S_$1-H25
 2.3 with sigma of 0.01
 H68-H10R_$1
 2.3 with sigma of 0.01
 O100-C102
 1.41 with sigma of 0.01
 O100-C101
 1.41 with sigma of 0.01
 C101-C100
 1.57 with sigma of 0.01
 C103-C102
 1.57 with sigma of 0.01
 C103-O100
 2.3456 with sigma of 0.01
 O100-C100
 2.3456 with sigma of 0.01
 C102-C101
 2.3409 with sigma of 0.01
 C103-C100
 4.7431 with sigma of 0.01
 H68-H10P_$1
 2.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C108) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.1
Uanis(C106) \\sim Ueq, Uanis(O101) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C104) \\sim Ueq, Uanis(C107) \\sim Ueq, : with sigma of 0.01 and sigma
for terminal atoms of 0.1
Uanis(O101) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.1
4. Rigid body (RIGU) restrains
 S203, F211, F209, F210, O209, O210, O211, C203
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S204, F212, F213, F214, O214, O212, O213, C204
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S205, F215, F216, F217, O215, O216, O217, C205
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S201, F203, F205, F204, O205, O203, O204, C201
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S202, F208, F206, F207, O206, O208, O207, C202
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl1, Cl2, C206
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl3, Cl4, C108, Cl5, Cl6, C109
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O100, C101, C102, C100, H10D, H10E, H10F, H10G, C103, H10A, H10B, H10C, H10H,
 H10I, H10J
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O101, C105, C106, C104, H10N, H10O, H10P, H10Q, C107, H10K, H10L, H10M, H10R,
 H10S, H10T
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Same fragment restrains
{Cl4, Cl3, C108} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl1, Cl2, C206}
{Cl3, Cl4, C108} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl5, Cl6, C109}
{S200, F202, F200, F201, O201, O200, O202, C200} sigma for 1-2: 0.02, 1-3: 0.04
as
{S201, F203, F205, F204, O205, O203, O204, C201}
{S200, F202, F200, F201, O201, O200, O202, C200} sigma for 1-2: 0.02, 1-3: 0.04
as
{S203, F211, F209, F210, O209, O210, O211, C203}
{S200, F202, F200, F201, O201, O200, O202, C200} sigma for 1-2: 0.02, 1-3: 0.04
as
{S205, F215, F216, F217, O215, O216, O217, C205}
{S200, F202, F200, F201, O201, O200, O202, C200} sigma for 1-2: 0.02, 1-3: 0.04
as
{S204, F212, F213, F214, O214, O212, O213, C204}
{S200, F202, F200, F201, O201, O200, O202, C200} sigma for 1-2: 0.02, 1-3: 0.04
as
{S202, F208, F206, F207, O206, O208, O207, C202}
{O100, C100, C101, C102, C103} sigma for 1-2: 0.01, 1-3: 0.01
as
{O101, C104, C105, C106, C107}
6. Others
 1*[Sof(O100)+Sof(C100)+Sof(H10A)+Sof(H10B)+Sof(H10C)+Sof(C101)+Sof(H10D)+
 Sof(H10E)+Sof(C102)+Sof(H10F)+Sof(H10G)+Sof(C103)+Sof(H10H)+Sof(H10I)+
 Sof(H10J)]+1*[Sof(Cl5)+Sof(Cl6)+Sof(C109)+Sof(H10W)+Sof(H10X)]+1*[Sof(Cl3)+
 Sof(Cl4)+Sof(C108)+Sof(H10U)+Sof(H10V)]=1 with esd of 0
 1*[Sof(Cl1)+Sof(Cl2)+Sof(C206)+Sof(H20A)+Sof(H20B)]+1*[Sof(S205)+Sof(F215)+
 Sof(F216)+Sof(F217)+Sof(O215)+Sof(O216)+Sof(O217)+Sof(C205)]+1*[Sof(O101)+
 Sof(C104)+Sof(H10K)+Sof(H10L)+Sof(H10M)+Sof(C105)+Sof(H10N)+Sof(H10O)+
 Sof(C106)+Sof(H10P)+Sof(H10Q)+Sof(C107)+Sof(H10R)+Sof(H10S)+Sof(H10T)]=1 with
 esd of 0.000001
 1*[Sof(O101)+Sof(C104)+Sof(H10K)+Sof(H10L)+Sof(H10M)+Sof(C105)+Sof(H10N)+
 Sof(H10O)+Sof(C106)+Sof(H10P)+Sof(H10Q)+Sof(C107)+Sof(H10R)+Sof(H10S)+
 Sof(H10T)]+1*[Sof(S203)+Sof(F211)+Sof(F209)+Sof(F210)+Sof(O209)+Sof(O210)+
 Sof(O211)+Sof(C203)]+1*[Sof(S204)+Sof(F212)+Sof(F213)+Sof(F214)+Sof(O214)+
 Sof(O212)+Sof(O213)+Sof(C204)]=1 with esd of 0.000001
 1*[Sof(S205)+Sof(F215)+Sof(F216)+Sof(F217)+Sof(O215)+Sof(O216)+Sof(O217)+
 Sof(C205)]+1*[Sof(S203)+Sof(F211)+Sof(F209)+Sof(F210)+Sof(O209)+Sof(O210)+
 Sof(O211)+Sof(C203)]+1*[Sof(S204)+Sof(F212)+Sof(F213)+Sof(F214)+Sof(O214)+
 Sof(O212)+Sof(O213)+Sof(C204)]=1 with esd of 0.000001
 Sof(S202)=Sof(F208)=Sof(F206)=Sof(F207)=Sof(O206)=Sof(O208)=Sof(O207)=
 Sof(C202)=1-FVAR(1)
 Sof(S201)=Sof(F203)=Sof(F205)=Sof(F204)=Sof(O205)=Sof(O203)=Sof(O204)=
 Sof(C201)=FVAR(1)
 Sof(O100)=Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C101)=Sof(H10D)=
 Sof(H10E)=Sof(C102)=Sof(H10F)=Sof(H10G)=Sof(C103)=Sof(H10H)=Sof(H10I)=
 Sof(H10J)=FVAR(2)
 Sof(Cl5)=Sof(Cl6)=Sof(C109)=Sof(H10W)=Sof(H10X)=FVAR(3)
 Sof(Cl3)=Sof(Cl4)=Sof(C108)=Sof(H10U)=Sof(H10V)=FVAR(4)
 Sof(Cl1)=Sof(Cl2)=Sof(C206)=Sof(H20A)=Sof(H20B)=FVAR(5)
 Sof(S205)=Sof(F215)=Sof(F216)=Sof(F217)=Sof(O215)=Sof(O216)=Sof(O217)=
 Sof(C205)=FVAR(6)
 Sof(O101)=Sof(C104)=Sof(H10K)=Sof(H10L)=Sof(H10M)=Sof(C105)=Sof(H10N)=
 Sof(H10O)=Sof(C106)=Sof(H10P)=Sof(H10Q)=Sof(C107)=Sof(H10R)=Sof(H10S)=
 Sof(H10T)=0.5*FVAR(8)
 Sof(S203)=Sof(F211)=Sof(F209)=Sof(F210)=Sof(O209)=Sof(O210)=Sof(O211)=
 Sof(C203)=FVAR(8)
 Sof(S204)=Sof(F212)=Sof(F213)=Sof(F214)=Sof(O214)=Sof(O212)=Sof(O213)=
 Sof(C204)=FVAR(9)
7.a Secondary CH2 refined with riding coordinates:
 C206(H20A,H20B), C108(H10U,H10V), C109(H10W,H10X), 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:
 C13(H13), C6(H6), C44(H44), C41(H41), C15(H15), C56(H56), C43(H43), C51(H51),
 C26(H26), C71(H71), C58(H58), C42(H42), C72(H72), C14(H14), C46(H46), C57(H57),
  C91(H91), C36(H36), C53(H53), C33(H33), C95(H95), C49(H49), C52(H52),
 C61(H61), C24(H24), C25(H25), C82(H82), C99(H99), C96(H96), C75(H75), C79(H79),
  C35(H35), C69(H69), C76(H76), C97(H97), C89(H89), C62(H62), C78(H78),
 C66(H66), C87(H87), C88(H88), C68(H68), C67(H67), C4(H4), C2(H2), C59(H59),
 C16(H16), C48(H48), C92(H92), C23(H23), C64(H64), C81(H81), C47(H47), C54(H54),
  C63(H63), C34(H34), C77(H77), C98(H98), C85(H85), C86(H86)
;
_shelx_res_checksum              6605
_shelx_hkl_checksum              55774
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'