Bis(benzo-15-crown-5-κ^5^<i>O</i>)barium tetrakis(isothiocyanato-κ<i>N</i>)cobaltate(II)
Cao, Zhiqiang; Liu, Kai; Niu, Meiju; Wang, Daqi; Acta Crystallographica Section E 66 (2010) m68–; doi:10.1107/S1600536809053471

data_2224604
_publ_section_title
;
 Bis(benzo-15-crown-5-\k^5^<i>O</i>)barium
 tetrakis(isothiocyanato-\k<i>N</i>)cobaltate(II)
;
_journal_coeditor_code           CV2669
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m68
_journal_paper_doi               10.1107/S1600536809053471
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ba (C14 H20 O5)2] [Co (N C S)4]'
_chemical_formula_moiety         'C28 H40 Ba O10 2+, C4 Co N4 S4 2-'
_chemical_formula_sum            'C32 H40 Ba Co N4 O10 S4'
_chemical_formula_weight         965.19
_chemical_name_systematic
;
Bis(benzo-15-crown-5-\k^5^<i>O</i>)barium
tetrakis(isothiocyanato-\k<i>N</i>)cobaltate(II)
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.5772(13)
_cell_length_b                   12.5772(13)
_cell_length_c                   23.758(3)
_cell_measurement_reflns_used    2944
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.6525
_cell_measurement_theta_min      2.537
_cell_volume                     3254.7(6)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            14488
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  0.6742
_exptl_absorpt_correction_T_min  0.5594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1461
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.680
_refine_diff_density_min         -1.384
_refine_ls_abs_structure_details 'Flack (1983), 1623 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      2.363
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1148P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.1960
_reflns_number_gt                2749
_reflns_number_total             3786
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv2669.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2224604
_cod_database_fobs_code          2224604