#------------------------------------------------------------------------------
#$Date: 2025-08-18 17:33:07 +0200 (Mon 18 de Aug de 2025) $
#$Revision: 301779 $
#$URL: svn://www.crystallography.net/cod/cif/1/54/99/1549958.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1549958
loop_
_publ_author_name
'Truong, Phan T.'
'Broering, Ellen P.'
'Dzul, Stephen P.'
'Chakraborty, Indranil'
'Stemmler, Timothy L.'
'Harrop, Todd C.'
_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_sum            'C30 H46 F6 N8 Ni2 O4 S2'
_chemical_formula_weight         878.28
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-06-19 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.9760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.2608(14)
_cell_length_b                   10.7528(6)
_cell_length_c                   17.4230(10)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.26
_cell_volume                     3848.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'OMEGA SCAN'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30284
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.500
_diffrn_reflns_theta_min         1.983
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.426
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5892
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0772P)²+8.1826P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4865
_reflns_number_total             5892
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc03321h2.cif
_cod_data_source_block           j1
_cod_depositor_comments
'Adding full bibliography for 1549958--1549959.cif.'
_cod_database_code               1549958
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.744
_shelx_estimated_absorpt_t_max   0.893
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.07424(2) 0.55581(3) 0.21290(2) 0.02648(10) Uani 1 1 d D . . . .
S1 S -0.01049(3) 0.53312(6) 0.14403(4) 0.02886(13) Uani 1 1 d . . . . .
N1 N -0.09719(10) 0.37926(19) 0.18472(13) 0.0276(4) Uani 1 1 d . . . . .
N2 N -0.1171(6) 0.6826(9) 0.2059(12) 0.0302(18) Uani 0.65(7) 1 d D U P A 1
O1 O -0.1376(10) 0.7841(13) 0.2024(11) 0.065(3) Uani 0.65(7) 1 d D U P A 1
N2' N -0.1249(13) 0.671(2) 0.185(2) 0.038(4) Uani 0.35(7) 1 d D U P A 2
O1' O -0.162(3) 0.751(4) 0.175(3) 0.076(9) Uani 0.35(7) 1 d D U P A 2
C1 C -0.01872(12) 0.3700(2) 0.13187(15) 0.0308(5) Uani 1 1 d . . . . .
C2 C -0.06141(11) 0.3053(2) 0.15424(15) 0.0284(4) Uani 1 1 d . . . . .
C3 C -0.06574(14) 0.1769(3) 0.14712(19) 0.0374(6) Uani 1 1 d . . . . .
H3 H -0.0946 0.1333 0.1621 0.045 Uiso 1 1 calc R U . . .
C4 C -0.02802(17) 0.1115(3) 0.1181(2) 0.0488(7) Uani 1 1 d . . . . .
C5 C 0.01368(16) 0.1744(3) 0.0951(2) 0.0505(8) Uani 1 1 d . . . . .
H5 H 0.0388 0.1298 0.0742 0.061 Uiso 1 1 calc R U . . .
C6 C 0.01847(14) 0.3017(3) 0.1025(2) 0.0415(6) Uani 1 1 d . . . . .
H6 H 0.0476 0.3442 0.0875 0.050 Uiso 1 1 calc R U . . .
C7 C -0.0355(3) -0.0256(4) 0.1070(4) 0.0808(16) Uani 1 1 d D . . . .
F1 F -0.0804(7) -0.0425(15) 0.0171(9) 0.079(3) Uani 0.51(3) 1 d D U P B 1
F2 F 0.0161(8) -0.086(2) 0.1275(14) 0.101(5) Uani 0.51(3) 1 d D U P B 1
F3 F -0.0722(8) -0.0753(7) 0.1388(13) 0.072(4) Uani 0.51(3) 1 d D U P B 1
F1' F -0.0836(7) -0.0683(18) 0.0354(13) 0.098(5) Uani 0.49(3) 1 d D U P B 2
F2' F 0.0192(7) -0.081(2) 0.1069(12) 0.077(4) Uani 0.49(3) 1 d D U P B 2
F3' F -0.0365(15) -0.0801(7) 0.1798(14) 0.102(5) Uani 0.49(3) 1 d D U P B 2
N4 N 0.20636(10) 0.5301(2) 0.10365(14) 0.0306(4) Uani 1 1 d . . . . .
C8 C 0.27706(16) 0.5738(3) 0.2659(2) 0.0471(7) Uani 1 1 d . . . . .
H8A H 0.3184 0.6126 0.3063 0.071 Uiso 1 1 calc R U . . .
H8B H 0.2777 0.4857 0.2807 0.071 Uiso 1 1 calc R U . . .
H8C H 0.2412 0.6156 0.2700 0.071 Uiso 1 1 calc R U . . .
C9 C 0.26753(16) 0.5852(3) 0.1742(2) 0.0500(8) Uani 1 1 d . . . . .
H9A H 0.2685 0.6746 0.1613 0.060 Uiso 1 1 calc R U . . .
H9B H 0.3051 0.5452 0.1720 0.060 Uiso 1 1 calc R U . . .
C10 C 0.25709(17) 0.5180(4) 0.0012(2) 0.0566(9) Uani 1 1 d . . . . .
H10A H 0.2484 0.5415 -0.0576 0.085 Uiso 1 1 calc R U . . .
H10B H 0.2622 0.4276 0.0078 0.085 Uiso 1 1 calc R U . . .
H10C H 0.2971 0.5587 0.0437 0.085 Uiso 1 1 calc R U . . .
C11 C 0.20087(16) 0.5586(3) 0.0160(2) 0.0423(6) Uani 1 1 d . . . . .
H11A H 0.1954 0.6496 0.0067 0.051 Uiso 1 1 calc R U . . .
H11B H 0.1607 0.5188 -0.0288 0.051 Uiso 1 1 calc R U . . .
C12 C 0.16108(14) 0.3142(3) 0.04178(18) 0.0380(6) Uani 1 1 d . . . . .
H12A H 0.1668 0.2253 0.0557 0.057 Uiso 1 1 calc R U . . .
H12B H 0.1679 0.3301 -0.0087 0.057 Uiso 1 1 calc R U . . .
H12C H 0.1169 0.3395 0.0284 0.057 Uiso 1 1 calc R U . . .
C13 C 0.20962(14) 0.3874(3) 0.11823(18) 0.0372(5) Uani 1 1 d . . . . .
H13A H 0.2539 0.3583 0.1327 0.045 Uiso 1 1 calc R U . . .
H13B H 0.2025 0.3698 0.1689 0.045 Uiso 1 1 calc R U . . .
C14 C 0.13785(18) 0.7174(3) 0.1034(2) 0.0500(7) Uani 1 1 d . . . . .
H14A H 0.0980 0.7400 0.1059 0.075 Uiso 1 1 calc R U . . .
H14B H 0.1356 0.7489 0.0493 0.075 Uiso 1 1 calc R U . . .
H14C H 0.1755 0.7540 0.1531 0.075 Uiso 1 1 calc R U . . .
C15 C 0.14495(15) 0.5743(3) 0.1064(2) 0.0391(6) Uani 1 1 d . . . . .
H15A H 0.1457 0.5431 0.1603 0.047 Uiso 1 1 calc R U . . .
H15B H 0.1064 0.5381 0.0565 0.047 Uiso 1 1 calc R U . . .
N3 N -0.14348(10) 0.3188(2) 0.19024(15) 0.0341(4) Uani 1 1 d . . . . .
O2 O -0.17548(9) 0.3834(2) 0.21811(13) 0.0395(4) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
N2' Ni1 N1 126.0(12) .
N2 Ni1 N1 133.6(5) .
N2' Ni1 S1 118.3(10) .
N2 Ni1 S1 123.8(5) .
N1 Ni1 S1 86.21(6) .
N2' Ni1 S1 122.0(13) 2
N2 Ni1 S1 109.8(6) 2
N1 Ni1 S1 99.10(6) 2
S1 Ni1 S1 96.66(2) 2
C1 S1 Ni1 96.14(8) .
C1 S1 Ni1 102.68(8) 2
Ni1 S1 Ni1 82.07(2) 2
N3 N1 C2 113.5(2) .
N3 N1 Ni1 126.90(17) .
C2 N1 Ni1 119.63(15) .
O1 N2 Ni1 167.8(12) .
O1' N2' Ni1 170(2) .
C2 C1 C6 118.5(2) .
C2 C1 S1 120.53(19) .
C6 C1 S1 120.9(2) .
C3 C2 C1 119.9(2) .
C3 C2 N1 124.1(2) .
C1 C2 N1 116.0(2) .
C2 C3 C4 120.3(3) .
C3 C4 C5 120.3(3) .
C3 C4 C7 119.5(3) .
C5 C4 C7 120.1(3) .
C6 C5 C4 119.7(3) .
C5 C6 C1 121.3(3) .
F2 C7 F3 112.9(12) .
F1' C7 F2' 102.7(10) .
F1' C7 F3' 110.2(8) .
F2' C7 F3' 102.9(11) .
F1' C7 C4 117.9(10) .
F2 C7 C4 115.7(11) .
F3 C7 C4 113.8(4) .
F2' C7 C4 111.7(10) .
F3' C7 C4 110.2(5) .
F2 C7 F1 110.8(11) .
F3 C7 F1 97.1(8) .
C4 C7 F1 104.5(8) .
C9 N4 C11 110.4(2) .
C9 N4 C15 113.1(2) .
C11 N4 C15 109.5(2) .
C9 N4 C13 107.6(2) .
C11 N4 C13 110.0(2) .
C15 N4 C13 106.1(2) .
N4 C9 C8 116.6(3) .
N4 C11 C10 116.5(3) .
C12 C13 N4 114.5(2) .
N4 C15 C14 113.3(2) .
O2 N3 N1 114.2(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2' 1.621(11) .
Ni1 N2 1.659(7) .
Ni1 N1 1.971(2) .
Ni1 S1 2.3169(7) .
Ni1 S1 2.3555(7) 2
S1 C1 1.767(3) .
S1 Ni1 2.3555(7) 2
N1 N3 1.299(3) .
N1 C2 1.422(3) .
N2 O1 1.182(8) .
N2' O1' 1.162(12) .
C1 C2 1.409(3) .
C1 C6 1.401(4) .
C2 C3 1.386(4) .
C3 C4 1.392(4) .
C4 C5 1.387(5) .
C4 C7 1.486(5) .
C5 C6 1.374(4) .
C7 F1' 1.307(13) .
C7 F2 1.258(18) .
C7 F3 1.330(8) .
C7 F2' 1.405(16) .
C7 F3' 1.408(12) .
C7 F1 1.429(15) .
N4 C9 1.499(4) .
N4 C11 1.503(4) .
N4 C15 1.527(4) .
N4 C13 1.551(4) .
C8 C9 1.510(5) .
C10 C11 1.511(5) .
C12 C13 1.503(4) .
C14 C15 1.545(4) .
N3 O2 1.269(3) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139052457
