A (10,3)-b net by sulfate hydrogen-bonded biimidazolate complexes
Krister Larsson; Lars Öhrström; CrystEngComm 5 (2003) 222–225; doi:10.1039/b303107a

data_7204640
_publ_section_title
;
 A (10,3)-b net by sulfate hydrogen-bonded biimidazolate complexes
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              222
_journal_page_last               225
_journal_paper_doi               10.1039/b303107a
_journal_volume                  5
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H15 Cr1 N12'
_chemical_formula_sum            'C18 H15 Cr N12 O4 S'
_chemical_formula_weight         547.48
_space_group_IT_number           80
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      80
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2002-10-25T13:01:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8274(7)
_cell_length_b                   12.8274(7)
_cell_length_c                   14.2567(7)
_cell_measurement_reflns_used    5528
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36.99
_cell_measurement_theta_min      2.75
_cell_measurement_wavelength     0.924
_cell_volume                     2345.8(2)
_computing_cell_refinement       'Twinsolve (Rigaku, 1998-2002)'
_computing_data_reduction        'Twinsolve (Rigaku, 1998-2002)'
_computing_molecular_graphics
;
Ortep-3 for Windows (Farrugia, 1997)
DIAMOND - Visual Crystal Structure Information System
    CRYSTAL IMPACT, Postfach 1251, D-53002 Bonn
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9044
_diffrn_measured_fraction_theta_max 0.8746
_diffrn_radiation_monochromator  'Si (111) single crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.9240
_diffrn_reflns_av_R_equivalents  0.120
_diffrn_reflns_av_sigmaI/netI    0.009
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6527
_diffrn_reflns_theta_full        36.6
_diffrn_reflns_theta_max         36.6
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    1.251
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2811
_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:  4/m
Friedel opposites are equivalent.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.55
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1966
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0692
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.1640P)^2^+0.6264P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1969
_refine_ls_wR_factor_ref         0.2001
_reflns_number_gt                1870
_reflns_number_total             1966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303107a.txt
_cod_data_source_block           crbiim2
_cod_database_code               7204640