Simultaneous nitrosylation and N-nitrosation of a Ni-thiolate model complex of Ni-containing SOD.
Truong, Phan T.; Broering, Ellen P.; Dzul, Stephen P.; Chakraborty, Indranil; Stemmler, Timothy L.; Harrop, Todd C.; Chemical science 9 (2018) 8567–8574; doi:10.1039/c8sc03321h

data_1549959
_publ_section_title
;
 Simultaneous nitrosylation and N-nitrosation of a Ni-thiolate model
 complex of Ni-containing SOD.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              8567
_journal_page_last               8574
_journal_paper_doi               10.1039/c8sc03321h
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety
'2(C14 H6 F6 N4 Ni O2 S2), 3(C8 H20 N), C3 H6 N0.5, C4 N0.5, C4 H10 O'
_chemical_formula_sum            'C63 H88 F12 N12 Ni2 O5 S4'
_chemical_formula_weight         1567.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-09
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-07-12 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                112.8160(10)
_cell_angle_beta                 92.7190(10)
_cell_angle_gamma                91.167(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3985(6)
_cell_length_b                   16.8518(9)
_cell_length_c                   18.0347(9)
_cell_measurement_reflns_used    9562
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.43
_cell_volume                     3745.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest PHOTON 100 CMOS'
_diffrn_measurement_method       'Phi\Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15409
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.458
_diffrn_reflns_theta_min         1.968
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.745373
_exptl_absorpt_correction_T_min  0.579933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER TWINABS'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       plate
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.254
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         15409
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      4.031
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+11.0518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.2002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11647
_reflns_number_total             15409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03321h2.cif
_cod_data_source_block           twin5
_cod_depositor_comments
'Adding full bibliography for 1549958--1549959.cif.'
_cod_database_code               1549959
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.862
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5089(14)
 0.4911(14)
2. 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
3. Restrained distances
 C55-C56
 1.5 with sigma of 0.02
 N12-C54
 1.45 with sigma of 0.02
 C59-C61
 1.45 with sigma of 0.02
 C62-C63
 1.45 with sigma of 0.02
 C62-C64
 1.54 with sigma of 0.02
 O5-C67
 1.46 with sigma of 0.02
 O5-C66
 1.53 with sigma of 0.02
 C65-C66
 1.78 with sigma of 0.02
 C67-C68
 1.65 with sigma of 0.02
 N12-C54 \\sim N12-C56 \\sim N12-C48
 with sigma of 0.02
 N13-C60 \\sim N13-C61 \\sim N13-C63 \\sim N13-C64
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(F3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C55) = Uanis(C56)
Uanis(C53) = Uanis(C54)
Uanis(C68) = Uanis(C67)
Uanis(F7') = Uanis(F7)
Uanis(F11) = Uanis(F12')
Uanis(F1) = Uanis(F1')
Uanis(F3) = Uanis(F3')
Uanis(F2) = Uanis(F2')
Uanis(F8') = Uanis(F8)
Uanis(F9) = Uanis(F9')
Uanis(F9') = Uanis(F8)
Uanis(F7) = Uanis(F8')
Uanis(F12) = Uanis(F10')
Uanis(C64) = Uanis(C62)
Uanis(C60) = Uanis(C63)
5. Same fragment restrains
{F1', F2', F3'} sigma for 1-2: 0.02, 1-3: 0.04
as
{F1, F2, F3}
{F7', F8', F9'} sigma for 1-2: 0.02, 1-3: 0.04
as
{F7, F8, F9}
{F10', F11', F12'} sigma for 1-2: 0.02, 1-3: 0.04
as
{F10, F11, F12}
6. Others
 Sof(F1')=Sof(F2')=Sof(F3')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F7')=Sof(F8')=Sof(F9')=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(2)
 Sof(F10')=Sof(F11')=Sof(F12')=1-FVAR(3)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(3)
 Fixed Sof: C54(0.5) C56(0.5) C60(0.5) C61(0.5) C63(0.5) C64(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C18(H18A,H18B), C20(H20A,H20B), C22(H22A,H22B), C24(H24A,
 H24B), C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B), C46(H46A,H46B),
 C48(H48A,H48B), C50(H50A,H50B), C52(H52A,H52B), C66(H66A,H66B), C67(H67A,H67B)
7.b Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,
 H29B,H29C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C),
 C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C65(H65A,H65B,
 H65C), C68(H68A,H68B,H68C)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C10(H10), C12(H12), C13(H13), C33(H33), C35(H35),
 C36(H36), C40(H40), C42(H42), C43(H43)
;
_shelx_res_checksum              3979
_olex2_submission_special_instructions 'No special instructions were received'