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_7010967
_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 PPh~4~[Co(bbphen)], PPh~4~Cl, and excess of KCN in 
refluxing chloroform, recrystallized from acetonitrile.
;
_chemical_formula_analytical     'C63 H56 Co N9 O5 P2 '
_chemical_formula_moiety
'2(C24 H20 P 1+) C11 H8 N7 O4 Co 2-,2(C2 H3 N),H2 O'
_chemical_formula_structural
'2(P(C6 H5)4),(Co (C10 H8 N6 O4)(C N)),2(C2 H3 N),(H2 O)'
_chemical_formula_sum            'C63 H56 Co N9 O5 P2'
_chemical_formula_weight         1140.07
_chemical_melting_point          485
_chemical_name_common            (PPh~4~)~2~[Co(bbphen)(CN)].2CH~3~CN.H~2~O
_chemical_name_systematic
;
Tetraphenylphosphonium Cyano(o-phenylenebis(biuretato))cobaltate(III) 
Diacetonitrile Unihydrate Solvate
;
_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             'Sat Feb 20 14:20:32 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                96.82(3)
_cell_angle_beta                 101.26(2)
_cell_angle_gamma                101.25(2)
_cell_formula_units_Z            2
_cell_length_a                   13.579(3)
_cell_length_b                   16.696(5)
_cell_length_c                   13.047(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      12.0
_cell_measurement_theta_min      11.0
_cell_volume                     2807.2(14)
_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      -0.04280
_diffrn_orient_matrix_UB_12      -0.02581
_diffrn_orient_matrix_UB_13      -0.07206
_diffrn_orient_matrix_UB_21      0.04937
_diffrn_orient_matrix_UB_22      -0.03629
_diffrn_orient_matrix_UB_23      -0.00845
_diffrn_orient_matrix_UB_31      -0.04083
_diffrn_orient_matrix_UB_32      -0.04299
_diffrn_orient_matrix_UB_33      0.03179
_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  0.134
_diffrn_reflns_av_sigmaI/netI    0.234
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10812
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        -1.10
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1188.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.82
_refine_diff_density_min         -0.86
_refine_ls_abs_structure_details centrosymmetric
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_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     721
_refine_ls_number_reflns         10442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2415
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.0070
_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          0.1264
_refine_ls_wR_factor_ref         0.1585
_reflns_number_gt                4352
_reflns_number_total             10442
_reflns_threshold_expression     'F^2^ 2 \s(F^2^)'
_cod_data_source_file            b106001p.txt
_cod_data_source_block           '[PPh4]2[Co(bbphen)(CN)]'
_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        2807(1)
_cod_original_formula_sum        'C63 H56 Co N9 O5 P2 '
_cod_database_code               7010967