Structural and spectroscopic comparisons of the square-planar four-coordinate [o-phenylenebis(biuretato)]cobaltate(III) complex and the five-coordinate mono- and six-coordinate dicyano adducts
Takashi Yagi; Hiroshi Hanai; Takashi Komorita; Takayoshi Suzuki; Sumio Kaizaki; J. Chem. Soc., Dalton Trans.  (2002) 1126–1131; doi:10.1039/b106001p

data_7010966
_publ_section_title
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 Structural and spectroscopic comparisons of the square-planar
 four-coordinate [o-phenylenebis(biuretato)]cobaltate(III) complex and
 the five-coordinate mono- and six-coordinate dicyano adducts
;
_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1126
_journal_page_last               1131
_journal_paper_doi               10.1039/b106001p
_journal_year                    2002
_chemical_compound_source
;
Prepared from K[Co(bbphen)] and cryptand[2,2,2] in water,recrystallized from 
a mixture of dimethylsulfoxide and water.
;
_chemical_formula_analytical     'C28 H44 Co K N8 O10'
_chemical_formula_moiety         'C18 H36 K N2 O6 1+, C10 H8 N6 O4 Co 1-'
_chemical_formula_structural     '(K (C18 H36 N2 O6)), (Co (C10 H8 N6 O4))'
_chemical_formula_sum            'C28 H44 Co K N8 O10'
_chemical_formula_weight         750.73
_chemical_melting_point          476
_chemical_name_common            '[K(crypt)][Co(bbphen)]'
_chemical_name_systematic
;
4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8,8,8]hexacosane pottassium 
(o-phenylenebis(biuretato))cobaltate(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Wed Mar  3 12:48:11 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 93.92(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.540(2)
_cell_length_b                   16.692(4)
_cell_length_c                   15.317(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.9
_cell_volume                     3453.7(11)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    'ORTEP in teXsan'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.03951
_diffrn_orient_matrix_UB_12      0.03291
_diffrn_orient_matrix_UB_13      -0.04435
_diffrn_orient_matrix_UB_21      -0.06258
_diffrn_orient_matrix_UB_22      -0.02195
_diffrn_orient_matrix_UB_23      0.02161
_diffrn_orient_matrix_UB_31      -0.00159
_diffrn_orient_matrix_UB_32      0.04499
_diffrn_orient_matrix_UB_33      0.04300
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_sigmaI/netI    0.087
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10456
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        -3.49
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   Coppens_numerical
_exptl_crystal_colour            red-purple
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.91
_refine_ls_abs_structure_details Centrosymmetric
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.270
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     433
_refine_ls_number_reflns         10074
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo^2^) + 0.00090(Fo^2^)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                5910
_reflns_number_total             10074
_reflns_threshold_expression     'F^2^ > 2.0 \s(F^2^)'
_cod_data_source_file            b106001p.txt
_cod_data_source_block           '[K(crypt)][Co(bbphen)]'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_reflns_observed_expression' tag replaced with
'_reflns_threshold_expression' tag as specified in the replacement
file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

'_atom_site_calc_flags'
tag replaced with '_atom_site_calc_flag' tag as specified in the
replacement file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

'_atom_type_scat_imag'
tag replaced with '_atom_type_scat_dispersion_imag' tag as specified
in the replacement file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 3137 2015-03-23 15:08:43Z antanas 
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_cod_original_cell_volume        3453(1)
_cod_database_code               7010966