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_4509454
_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+, C2 O4 2-, Cl -, 5.5(H2 O)
;
_chemical_formula_sum            'C20 H29 Cl Co N12 O9.5'
_chemical_formula_weight         683.93
_chemical_name_systematic
; 
 trisbiimdazolecobalt(III) oxalate chloride hydrate 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 106.979(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.0103(8)
_cell_length_b                   20.9727(10)
_cell_length_c                   21.3754(11)
_cell_measurement_reflns_used    7213
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.23
_cell_measurement_theta_min      2.27
_cell_volume                     6007.0(6)
_computing_cell_refinement       'TWINSOLVE (Svensson, 2005)'
_computing_data_reduction        TWINSOLVE
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'MARCCD, MARDTB Phi-Axis Goniometer'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_monochromator  Si(220)
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.90703
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9194
_diffrn_reflns_theta_full        33.48
_diffrn_reflns_theta_max         33.48
_diffrn_reflns_theta_min         4.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;  
 Shape and scale corrections using equivalent reflections.
 Shape function based on spherical harmonics.
 Highest even and odd order for spherical harmonics:  4  and  1
 Laue group:  2/m (b)
 Friedel opposites are equivalent.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         4960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1114P)^2^+35.0235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1946
_refine_ls_wR_factor_ref         0.2061
_reflns_number_gt                4332
_reflns_number_total             4960
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cg900075jsup1.cif
_cod_data_source_block           4
_cod_original_cell_volume        6007.1(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C20 H29 Cl Co N12 O9.50'
_cod_database_code               4509454