Oxalate- and Squarate-Biimidazole Supramolecular Synthons: Hydrogen-Bonded Networks Based on [Co(H2biimidazole)3]3+
Borel, Cédric; Larsson, Krister; Håkansson, Mikael; Olsson, Björn E.; Bond, Andrew D.; Öhrström, Lars; Crystal Growth & Design 9 (2009) 2821–; doi:10.1021/cg900075j

data_4509453
_publ_section_title
;
 Oxalate- and Squarate-Biimidazole Supramolecular Synthons:
 Hydrogen-Bonded Networks Based on [Co(H2biimidazole)3]3+
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2821
_journal_paper_doi               10.1021/cg900075j
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety         'C18 H18 Co N12 3+, 3(C4 H O4 -), 2(H2 O)'
_chemical_formula_sum            'C30 H25 Co N12 O14'
_chemical_formula_weight         836.55
_chemical_name_systematic
;
trisbiimdazolecobalt(III)tris(3-hydroxycyclobut-3-ene-1,2-dion-4-olate)hydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                118.386(1)
_cell_angle_beta                 100.462(1)
_cell_angle_gamma                99.392(1)
_cell_formula_units_Z            2
_cell_length_a                   10.1255(9)
_cell_length_b                   13.9169(5)
_cell_length_c                   14.6328(5)
_cell_measurement_reflns_used    7732
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.71
_cell_volume                     1708.10(18)
_computing_cell_refinement       'SAINT v.7.06a (Bruker, 2003)'
_computing_data_collection       'APEX2 v.1.0-22 (Bruker Nonius, 2004)'
_computing_data_reduction        'SAINT v.7.06a'
_computing_molecular_graphics    'SHELXTL v.6.10'
_computing_publication_material  'SHELXTL v.6.10'
_computing_structure_refinement  'SHELXTL v.6.10'
_computing_structure_solution    'SHELXTL v.6.10 (Sheldrick, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker-Nonius X8APEX-II CCD'
_diffrn_measurement_method       'thin-slice \w and \f 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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37915
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         3.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS v.2.10 (Sheldrick, 2003)
 Ratio of minimum to maximum apparent transmission:  0.831434
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         9476
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0497P)^2^+0.3444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                8216
_reflns_number_total             9476
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cg900075jsup1.cif
_cod_data_source_block           3
_cod_original_cell_volume        1708.10(17)
_cod_database_code               4509453