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_7010968
_publ_section_title
;
 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 KCN in refluxing water, recrystallized 
from aqueous ethanol.
;
_chemical_formula_analytical     'C12 H19 Co K3 N8 O9.50 '
_chemical_formula_moiety         '3(K +), C12 H6 N8 O4 Co 3-, 5.5(H2 O)'
_chemical_formula_structural     'K3, (Co (C10 H8 N6 O4) 2(C N), 5.5(H2 O)'
_chemical_formula_sum            'C12 H19 Co K3 N8 O9.5'
_chemical_formula_weight         603.56
_chemical_melting_point          527
_chemical_name_common            K~3~[Co(bbphen)(CN)~2~].5.5H~2~O
_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'
_audit_creation_date             'Mon Feb 22 11:25:41 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                112.19(1)
_cell_angle_beta                 114.59(2)
_cell_angle_gamma                79.37(2)
_cell_formula_units_Z            2
_cell_length_a                   11.126(3)
_cell_length_b                   12.813(2)
_cell_length_c                   9.737(2)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      11.8
_cell_measurement_theta_min      11.1
_cell_volume                     1168.1(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/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 AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.00858
_diffrn_orient_matrix_UB_12      -0.08328
_diffrn_orient_matrix_UB_13      -0.03489
_diffrn_orient_matrix_UB_21      -0.04338
_diffrn_orient_matrix_UB_22      -0.00342
_diffrn_orient_matrix_UB_23      -0.11444
_diffrn_orient_matrix_UB_31      0.08845
_diffrn_orient_matrix_UB_32      -0.01282
_diffrn_orient_matrix_UB_33      -0.00847
_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  0.014
_diffrn_reflns_av_sigmaI/netI    0.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5151
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         0.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        -4.07
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   Coppens_numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             614.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.05
_refine_diff_density_min         -1.02
_refine_ls_abs_structure_details centrosymmetric
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.716
_refine_ls_hydrogen_treatment
'noref except for Hatoms of solvated molecules which were not included'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4873
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.0020
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo^2^) + 0.00040(Fo^2^)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1801
_reflns_number_gt                4024
_reflns_number_total             4873
_reflns_threshold_expression     'F^2^ 2 \s(F^2^)'
_cod_data_source_file            b106001p.txt
_cod_data_source_block           K3[Co(bbphen)(CN)2]
_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 
;
_cod_original_cell_volume        1168.2(5)
_cod_original_formula_sum        'C12 H19 Co K3 N8 O9.50 '
_cod_database_code               7010968