Non-sterical stabilization of one-electron-oxidized NiSalen complex by thiophene core
Lukyanov, Daniil A.; Vereshchagin, Anatoliy A.; Sizov, Vladimir V.; Kalnin, Arseniy Y.; Novoselova, Julia V.; Alekseeva, Elena V.; Levin, Oleg V.; New Journal of Chemistry 45 (2021) 14425–14431; doi:10.1039/D1NJ02443D

data_7060859
_publ_section_title
;
 Non-sterical stabilization of one-electron-oxidized NiSalen complex by
 thiophene core
;
_journal_issue                   32
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14425
_journal_page_last               14431
_journal_paper_doi               10.1039/D1NJ02443D
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C12 H10 N2 Ni O2 S2'
_chemical_formula_sum            'C12 H10 N2 Ni O2 S2'
_chemical_formula_weight         337.05
_chemical_name_systematic        '[Ni(ThioSalEn)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2021-04-23 deposited with the CCDC.	2021-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.068(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6136(6)
_cell_length_b                   7.44583(19)
_cell_length_c                   19.8695(7)
_cell_measurement_reflns_used    8075
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.8920
_cell_measurement_theta_min      2.9640
_cell_volume                     2533.60(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -95.00  -20.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241  -38.0000 -120.0000 75

  2 omega  -64.00   51.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241   19.0000 -120.0000 115

  3 omega    4.00   36.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       23.5178   57.0000 -150.0000 32

  4 omega   60.00   99.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       23.5178 -178.0000 -180.0000 39

  5 omega  -90.00  -53.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241  -57.0000  150.0000 37

  6 omega  -65.00  -39.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241  126.0000  104.0000 26

  7 omega   14.00   71.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       23.5178   57.0000 -120.0000 57

  8 omega   58.00   92.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       23.5178   57.0000  150.0000 34

  9 omega   14.00   47.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       23.5178   57.0000  150.0000 33

 10 omega   -3.00   37.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       23.5178  -77.0000  -90.0000 40

 11 omega  -41.00  -15.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       23.5178  -77.0000  -90.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0274609000
_diffrn_orient_matrix_UB_12      -0.0190168000
_diffrn_orient_matrix_UB_13      0.0156845000
_diffrn_orient_matrix_UB_21      0.0292311000
_diffrn_orient_matrix_UB_22      0.0146732000
_diffrn_orient_matrix_UB_23      0.0354243000
_diffrn_orient_matrix_UB_31      -0.0103006000
_diffrn_orient_matrix_UB_32      0.0921611000
_diffrn_orient_matrix_UB_33      -0.0024023000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25015
_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         27.500
_diffrn_reflns_theta_min         2.954
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.857
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description       needle
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0347P)^2^+3.5179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5173
_reflns_number_total             5810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02443d3.cif
_cod_data_source_block           103-245-4914_dal002
_cod_depositor_comments          'Adding full bibliography for 7060859.cif.'
_cod_original_cell_volume        2533.59(15)
_cod_database_code               7060859
_chemical_oxdiff_formula         'C12 H10 N2 O2 S2 Ni'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C26(H26A,H26B), C32(H32A,H32B), C1B(H1BA,H1BB)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C11(H11), C17(H17), C25(H25), C27(H27), C15(H15), C13(H13),
 C18(H18), C1A(H1A), C1D(H1D), C2(H2)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'