Co(iii) complexes of (1,3-selenazol-2-yl)hydrazones and their sulphur analogues.
Filipović, Nenad R; Elshaflu, Hana; Grubišić, Sonja; Jovanović, Ljiljana S; Rodić, Marko; Novaković, Irena; Malešević, Aleksandar; Djordjević, Ivana S; Li, Haidong; Šojić, Nešo; Marinković, Aleksandar; Todorović, Tamara R; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2910–2924; doi:10.1039/c6dt04785h

data_7041949
_publ_section_title
;
 Co(iii) complexes of (1,3-selenazol-2-yl)hydrazones and their sulphur
 analogues.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2910
_journal_page_last               2924
_journal_paper_doi               10.1039/c6dt04785h
_journal_volume                  46
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_compound_source        synthetic
_chemical_formula_moiety         'C32 H26 Co N8 O2 S2 1+, B F4 1-'
_chemical_formula_sum            'C32 H26 B Co F4 N8 O2 S2'
_chemical_formula_weight         764.47
_chemical_melting_point          ?
_chemical_name_systematic
'Bis(1-(4-(4-methoxyphenyl)thiazol-2-yl)-2-(pyridin-2-ylmethylene)hydrazin- 1-ide-cobalt(III) tetrafluoridoborate'
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      152
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_creation_date             2016-10-06T15:20:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-12-16 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   9.2130(2)
_cell_length_b                   9.2130(2)
_cell_length_c                   33.5153(7)
_cell_measurement_reflns_used    7702
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.007
_cell_measurement_theta_min      2.824
_cell_volume                     2463.63(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury CSD (Macrae et al., 2008)'
_computing_publication_material  'SHELXLE (H\"ubschle et al., 2011)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.328
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
        List of Runs (angles in degrees, time in seconds):
  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -19.00  10.00   1.00   40.00    --  -18.39 -99.00  60.00   29
  2  \w    -53.00  45.00   1.00   40.00    --   19.01 -37.00 -90.00   98
  3  \w     18.00  59.00   1.00   40.00    --   19.01 -99.00-180.00   41
  4  \w     36.00  61.00   1.00   40.00    --   19.01 178.00 -60.00   25
  5  \w     -7.00  85.00   1.00   40.00    --   19.01  37.00  90.00   92
  6  \w    -21.00  40.00   1.00   40.00    --   19.01 -57.00 120.00   61
  7  \w    -11.00  30.00   1.00   40.00    --   19.01  77.00 -60.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass fiber'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0361612
_diffrn_orient_matrix_UB_12      -0.0204752
_diffrn_orient_matrix_UB_13      -0.0193173
_diffrn_orient_matrix_UB_21      0.0590851
_diffrn_orient_matrix_UB_22      -0.0240513
_diffrn_orient_matrix_UB_23      -0.0057618
_diffrn_orient_matrix_UB_31      -0.0557241
_diffrn_orient_matrix_UB_32      -0.0830997
_diffrn_orient_matrix_UB_33      0.0064273
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            19412
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         29.032
_diffrn_reflns_theta_min         2.553
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.95322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             1170
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.119
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Refined as a 4-component inversion twin:
 TWIN -1 0 0 0 -1 0 0 0 1 -4
 BASF   0.53672   0.44223   0.01664

 0.53672     0.03062     0.000   BASF  1 
 0.44223     0.03218     0.000   BASF  2 
 0.01664     0.03056     0.000   BASF  3

 The total amount of rotated-and-inverted structure, x-, is deduced by 
 summing the volume fractions corresponding to twin laws of determinant -1,
 (BASF 2 + BASF 3) which is the equivalent of the Flack x parameter for 
 multiply twinned crystals. 
 (Flack and Bernardinelli, Acta Cryst. (1999). A55, 908--915)
;
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4013
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1160P)^2^+0.2809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1519
_reflns_Friedel_coverage         0.713
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                3864
_reflns_number_total             4013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04785h2.cif
_cod_data_source_block           2-S
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7041947--7041951.cif.
;
_cod_original_cell_volume        2463.63(12)
_cod_original_sg_symbol_Hall     'P 31 2"''
_cod_database_code               7041949
_cell_oxdiff_length_a            9.2112(4)
_cell_oxdiff_length_b            9.2115(3)
_cell_oxdiff_length_c            33.5224(11)
_cell_oxdiff_angle_alpha         90.000(3)
_cell_oxdiff_angle_beta          89.998(3)
_cell_oxdiff_angle_gamma         119.985(4)
_cell_oxdiff_volume              2463.63(16)
_cell_oxdiff_measurement_reflns_used 7699
_oxdiff_exptl_absorpt_empirical_full_min 0.95
_oxdiff_exptl_absorpt_empirical_full_max 1.068
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_reflns_odcompleteness_completeness 99.8
_reflns_odcompleteness_theta     26.32
_reflns_odcompleteness_iscentric 1
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              47627