#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/46/7204640.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7204640
loop_
_publ_author_name
'Krister Larsson'
'Lars Öhrström'
_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/[σ²(Fo²)+(0.1640P)²+0.6264P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x+1/2, z+1/4'
'y, -x+1/2, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'y+1/2, -x+1, z+3/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr Cr 0.5000 0.5000 0.83326(9) 0.0430(3) Uani 1 2 d S . .
C12 C 0.5609(4) 0.2935(4) 0.7583(4) 0.0573(11) Uani 1 1 d . . .
N12 N 0.4138(3) 0.2689(3) 0.6407(4) 0.0622(11) Uani 1 1 d . . .
N11 N 0.6012(4) 0.3613(3) 0.8157(4) 0.0692(12) Uani 1 1 d . . .
N20 N 0.5969(4) 0.5414(4) 0.9531(4) 0.0687(12) Uani 1 1 d . . .
C13 C 0.4653(4) 0.3196(3) 0.7089(4) 0.0557(10) Uani 1 1 d . . .
C22 C 0.5522(4) 0.5189(4) 1.0336(4) 0.0620(12) Uani 1 1 d . . .
C10 C 0.6894(5) 0.3164(5) 0.8495(5) 0.0805(17) Uani 1 1 d . . .
H10 H 0.7345 0.3466 0.8927 0.097 Uiso 1 1 calc R . .
C11 C 0.7016(5) 0.2206(5) 0.8104(5) 0.0791(17) Uani 1 1 d . . .
H11 H 0.7560 0.1743 0.8212 0.095 Uiso 1 1 calc R . .
C20 C 0.6973(4) 0.5691(5) 0.9787(6) 0.0764(19) Uani 1 1 d . . .
H20 H 0.7487 0.5890 0.9363 0.092 Uiso 1 1 calc R . .
N13 N 0.6183(3) 0.2057(4) 0.7522(4) 0.0650(11) Uani 1 1 d . . .
N10 N 0.4154(3) 0.4074(3) 0.7327(3) 0.0604(10) Uani 1 1 d . . .
C15 C 0.3294(4) 0.4118(4) 0.6770(5) 0.0687(14) Uani 1 1 d . . .
H15 H 0.2792 0.4641 0.6783 0.082 Uiso 1 1 calc R . .
C14 C 0.3286(4) 0.3272(4) 0.6192(5) 0.0708(14) Uani 1 1 d . . .
H14 H 0.2790 0.3122 0.5736 0.085 Uiso 1 1 calc R . .
N21 N 0.6186(3) 0.5319(4) 1.1057(4) 0.0703(13) Uani 1 1 d . . .
C21 C 0.7113(4) 0.5641(5) 1.0682(6) 0.0794(18) Uani 1 1 d . . .
H21 H 0.7723 0.5794 1.1007 0.095 Uiso 1 1 calc R . .
S1 S 0.5000 0.5000 1.35841(17) 0.0678(9) Uani 1 2 d S . .
O101 O 0.5890(3) 0.5245(4) 1.2980(4) 0.0826(13) Uani 1 1 d . . .
O100 O 0.5874(5) 0.0225(5) 0.6665(5) 0.119(3) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0052 0.0029 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0095 0.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3307 1.0133 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1722 0.2093 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0084 0.0063 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N10 Cr N10 96.6(3) . 2_665 ?
N10 Cr N20 160.64(18) . . ?
N10 Cr N20 95.77(18) 2_665 . ?
N10 Cr N20 95.77(18) . 2_665 ?
N10 Cr N20 160.64(18) 2_665 2_665 ?
N20 Cr N20 76.7(3) . 2_665 ?
N10 Cr N11 77.14(17) . . ?
N10 Cr N11 94.12(18) 2_665 . ?
N20 Cr N11 87.14(19) . . ?
N20 Cr N11 103.1(2) 2_665 . ?
N10 Cr N11 94.12(18) . 2_665 ?
N10 Cr N11 77.14(17) 2_665 2_665 ?
N20 Cr N11 103.1(2) . 2_665 ?
N20 Cr N11 87.14(19) 2_665 2_665 ?
N11 Cr N11 167.0(3) . 2_665 ?
N11 C12 N13 112.5(5) . . ?
N11 C12 C13 119.1(5) . . ?
N13 C12 C13 128.5(5) . . ?
C13 N12 C14 107.0(5) . . ?
C12 N11 C10 105.7(5) . . ?
C12 N11 Cr 112.0(3) . . ?
C10 N11 Cr 142.0(4) . . ?
C22 N20 C20 103.5(6) . . ?
C22 N20 Cr 112.5(4) . . ?
C20 N20 Cr 143.1(5) . . ?
N10 C13 N12 110.8(4) . . ?
N10 C13 C12 118.3(5) . . ?
N12 C13 C12 130.8(4) . . ?
N20 C22 N21 111.3(5) . . ?
N20 C22 C22 119.0(3) . 2_665 ?
N21 C22 C22 129.6(3) . 2_665 ?
N11 C10 C11 109.5(5) . . ?
C10 C11 N13 106.6(5) . . ?
C21 C20 N20 112.2(6) . . ?
C12 N13 C11 105.7(5) . . ?
C13 N10 C15 106.0(4) . . ?
C13 N10 Cr 113.0(3) . . ?
C15 N10 Cr 140.7(4) . . ?
N10 C15 C14 109.0(5) . . ?
N12 C14 C15 107.2(5) . . ?
C22 N21 C21 106.8(6) . . ?
C20 C21 N21 106.3(5) . . ?
O100 S1 O100 108.8(7) 8 7_545 ?
O100 S1 O101 109.4(3) 8 2_665 ?
O100 S1 O101 110.7(3) 7_545 2_665 ?
O100 S1 O101 110.7(3) 8 . ?
O100 S1 O101 109.4(3) 7_545 . ?
O101 S1 O101 107.9(4) 2_665 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr N10 2.155(5) . ?
Cr N10 2.155(5) 2_665 ?
Cr N20 2.179(6) . ?
Cr N20 2.179(6) 2_665 ?
Cr N11 2.217(5) . ?
Cr N11 2.217(5) 2_665 ?
C12 N11 1.302(7) . ?
C12 N13 1.348(7) . ?
C12 C13 1.453(7) . ?
N12 C13 1.343(7) . ?
N12 C14 1.360(7) . ?
N11 C10 1.358(8) . ?
N20 C22 1.314(8) . ?
N20 C20 1.385(7) . ?
C13 N10 1.340(6) . ?
C22 N21 1.347(8) . ?
C22 C22 1.423(10) 2_665 ?
C10 C11 1.358(11) . ?
C11 N13 1.367(8) . ?
C20 C21 1.290(11) . ?
N10 C15 1.360(7) . ?
C15 C14 1.363(9) . ?
N21 C21 1.368(8) . ?
S1 O100 1.423(6) 8 ?
S1 O100 1.423(6) 7_545 ?
S1 O101 1.464(5) 2_665 ?
S1 O101 1.464(5) . ?
O100 S1 1.423(6) 3_644 ?
