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_7041947
_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_compound_source        synthetic
_chemical_formula_moiety         'C32 H26 Co N8 O2 Se2, B F4, O H2'
_chemical_formula_sum            'C32 H26 B Co F4 N8 O3 Se2'
_chemical_formula_weight         874.27
_chemical_melting_point          ?
_chemical_name_systematic
'Bis(1-(4-(4-methoxyphenyl)-1,3-selenazol-2-yl)-2- (pyridin-2-ylmethylene)hydrazin-1-ide-cobalt(III) tetrafluoridoborate hydrate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_creation_date             2016-06-15T11:06:26-00:00
_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                99.814(3)
_cell_angle_beta                 96.688(3)
_cell_angle_gamma                104.417(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1149(3)
_cell_length_b                   11.9728(5)
_cell_length_c                   13.9147(5)
_cell_measurement_reflns_used    7157
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.815
_cell_measurement_theta_min      2.663
_cell_volume                     1742.49(11)
_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      294(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 16.328
_diffrn_detector_type            'Sapphire3 (Oxford Diffraction)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.888
_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    -25.00  23.00   1.00   12.00    --  -18.54 -99.00  30.00   48
  2  \w    -80.00 -22.00   1.00   12.00    --  -18.54 131.00 170.00   58
  3  \w     -7.00  92.00   1.00   12.00    --   19.17  37.00  30.00   99
  4  \w    -11.00  89.00   1.00   12.00    --   19.17  77.00 120.00  100
  5  \w    -54.00  63.00   1.00   12.00    --   19.17 -19.00-180.00  117
  6  \w    -83.00 -26.00   1.00   12.00    --  -18.54 137.00 -13.00   57
  7  \w    -25.00  23.00   1.00   12.00    --  -18.54 -99.00-150.00   48
  8  \w     35.00  95.00   1.00   12.00    --   19.17 178.00  90.00   60
  9  \w     -2.00  88.00   1.00   12.00    --   19.17  57.00-120.00   90
 10  \w    -50.00  41.00   1.00   12.00    --   19.17 -57.00  90.00   91
 11  \w    -53.00  45.00   1.00   12.00    --   19.17 -37.00   0.00   98
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Gemini S (Oxford Diffraction)'
_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      0.0073716
_diffrn_orient_matrix_UB_12      0.0343845
_diffrn_orient_matrix_UB_13      -0.0367919
_diffrn_orient_matrix_UB_21      0.0227422
_diffrn_orient_matrix_UB_22      0.0520191
_diffrn_orient_matrix_UB_23      0.0374009
_diffrn_orient_matrix_UB_31      0.0624001
_diffrn_orient_matrix_UB_32      -0.0046275
_diffrn_orient_matrix_UB_33      0.0000696
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.039
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30249
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         29.114
_diffrn_reflns_theta_min         2.572
_diffrn_source                   'fine focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) (Oxford Diffraction)'
_exptl_absorpt_coefficient_mu    2.649
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_correction_T_min  0.361
_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. Reid.
        (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            red
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       prism
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.678
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         8296
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0566P)^2^+1.4045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0
_reflns_number_gt                6244
_reflns_number_total             8296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04785h2.cif
_cod_data_source_block           2-Se
_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_database_code               7041947
_cell_oxdiff_length_a            11.1149(3)
_cell_oxdiff_length_b            11.9728(4)
_cell_oxdiff_length_c            13.9147(5)
_cell_oxdiff_angle_alpha         99.814(3)
_cell_oxdiff_angle_beta          96.688(3)
_cell_oxdiff_angle_gamma         104.417(3)
_cell_oxdiff_volume              1742.50(10)
_cell_oxdiff_measurement_reflns_used 7157
_oxdiff_exptl_absorpt_empirical_full_min 0.938
_oxdiff_exptl_absorpt_empirical_full_max 1.055
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_theta     26.32
_reflns_odcompleteness_iscentric 1
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              19219