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_4129512
_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, 2(C F3 O3 S), C4 H10 O, C H2 Cl2, H2 O'
_chemical_formula_sum            'C91 H74 Cl2 F6 Fe4 N13 O13 S2'
_chemical_formula_weight         2030.05
_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   mixed
_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                 96.5282(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.0449(10)
_cell_length_b                   16.4976(6)
_cell_length_c                   24.0586(10)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.36
_cell_volume                     9087.4(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            296321
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.600
_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    0.813
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1053 before and 0.0549 after correction.
The Ratio of minimum to maximum transmission is 0.8999.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4156
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.713
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1210
_refine_ls_number_reflns         20815
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0713
_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^)+(0.1190P)^2^+35.3511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.2197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17100
_reflns_number_total             20815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b07397_si_003.cif
_cod_data_source_block           p14221_f
_cod_database_code               4129512
_shelxl_version_number           2014-2
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.854
_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, All O(H,H) groups
2. Restrained distances
 Cl3-C101 \\sim Cl4-C101
 with sigma of 0.02
 Cl3-Cl4 \\sim Cl2-Cl1
 with sigma of 0.02
 Cl2-C100 \\sim Cl1-C100 \\sim Cl3-C101 \\sim Cl4-C101
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C102) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.1
4. Rigid body (RIGU) restrains
 S2, O104, O105, O106, C107, F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C100, Cl1, Cl2, H10M, H10N
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C101, H10K, H10L, Cl3, Cl4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O100, C104, H10A, H10B, C105, H10H, H10I, H10J, C103, C102, H10F, H10G, H10C,
 H10D, H10E
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C101(0.5) H10K(0.5) H10L(0.5) Cl3(0.5) Cl4(0.5) Cl1(0.5) Cl2(0.5)
 C100(0.5) H10M(0.5) H10N(0.5)
6.a Free rotating group:
 O107(H10O,H10P)
6.b Secondary CH2 refined with riding coordinates:
 C104(H10A,H10B), C101(H10K,H10L), C103(H10F,H10G), C100(H10M,H10N)
6.c Me refined with riding coordinates:
 C102(H10C,H10D,H10E), C105(H10H,H10I,H10J)
6.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C59(H59), C58(H58), C2(H2), C16(H16), C54(H54), C81(H81), C56(H56),
 C4(H4), C64(H64), C82(H82), C44(H44), C49(H49), C51(H51), C14(H14), C71(H71),
 C36(H36), C57(H57), C63(H63), C72(H72), C15(H15), C47(H47), C61(H61), C23(H23),
  C41(H41), C48(H48), C53(H53), C46(H46), C52(H52), C79(H79), C91(H91),
 C13(H13), C75(H75), C98(H98), C99(H99), C78(H78), C35(H35), C42(H42), C69(H69),
  C66(H66), C26(H26), C62(H62), C92(H92), C76(H76), C24(H24), C89(H89),
 C33(H33), C97(H97), C43(H43), C96(H96), C77(H77), C34(H34), C25(H25), C95(H95),
  C88(H88), C85(H85), C67(H67), C68(H68), C86(H86), C87(H87)
;
_shelx_res_checksum              39035
_shelx_hkl_checksum              55607
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'