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_7041951
_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_formula_sum            'C32 H26 B Co F4 N8 Se2'
_chemical_formula_weight         826.27
_chemical_name_systematic
'Bis(2-(pyridin-2-ylmethylene)-1-(4-(p-tolyl)-1,3-selenazol-2-yl)hydrazin-1- ide-cobalt(III) tetrafluoridoborate'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-21T15:21:24-00:00
_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                90
_cell_formula_units_Z            4
_cell_length_a                   9.8772(2)
_cell_length_b                   15.1645(4)
_cell_length_c                   22.6936(4)
_cell_measurement_reflns_used    9710
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.572
_cell_measurement_theta_min      2.996
_cell_volume                     3399.11(13)
_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_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      294(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 0.93
_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    -54.00  92.00   1.00   25.00    --   19.17   0.00   0.00  146
  2  \w     32.00  96.00   1.00   25.00    --   19.17-178.00 -60.00   64
  3  \w    -79.00 -40.00   1.00   25.00    --  -18.39 130.00 -14.00   39
  4  \w    -25.00  24.00   1.00   25.00    --  -18.39 -99.00 -60.00   49
  5  \w    -50.00  41.00   1.00   25.00    --   19.17 -57.00 -60.00   91
  6  \w    -11.00  89.00   1.00   25.00    --   19.17  77.00  60.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0514301
_diffrn_orient_matrix_UB_12      -0.0293656
_diffrn_orient_matrix_UB_13      0.0095312
_diffrn_orient_matrix_UB_21      -0.0406032
_diffrn_orient_matrix_UB_22      0.0363975
_diffrn_orient_matrix_UB_23      0.0085562
_diffrn_orient_matrix_UB_31      -0.0293984
_diffrn_orient_matrix_UB_32      0.0011147
_diffrn_orient_matrix_UB_33      -0.0285027
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.93
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33384
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         29.078
_diffrn_reflns_theta_min         2.62
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.705
_exptl_absorpt_correction_T_max  0.592
_exptl_absorpt_correction_T_min  0.422
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       prism
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.453
_exptl_crystal_size_mid          0.337
_exptl_crystal_size_min          0.239
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 2379 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         8168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0510P)^2^+0.7642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.735
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     0.856
_reflns_number_gt                6391
_reflns_number_total             8168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04785h2.cif
_cod_data_source_block           3-Se
_cod_depositor_comments
'Adding full bibliography for 7041947--7041951.cif.'
_cod_database_code               7041951
_cell_oxdiff_length_a            9.8762(2)
_cell_oxdiff_length_b            15.1625(4)
_cell_oxdiff_length_c            22.6988(4)
_cell_oxdiff_angle_alpha         89.9906(18)
_cell_oxdiff_angle_beta          90.0085(17)
_cell_oxdiff_angle_gamma         89.994(2)
_cell_oxdiff_volume              3399.11(14)
_cell_oxdiff_measurement_reflns_used 9710
_oxdiff_exptl_absorpt_empirical_full_min 0.962
_oxdiff_exptl_absorpt_empirical_full_max 1.037
_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              86831