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#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/28/8102867.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_8102867
loop_
_publ_author_name
'Xiaoli Ma'
'Zhi Yang'
'Carola Schulzke'
_publ_section_title
;
 Crystal structure of bis(1,3-diisopropyl-4,5-dimethylimidazolium)
 hexamolybdate, [C11H21N2]2[Mo6O19]
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              775
_journal_volume                  225
_journal_year                    2010
_chemical_formula_sum            'C22 H42 Mo6 N4 O19'
_chemical_formula_weight         1242.24
_chemical_name_systematic
; 
1,3-diisopropyl-4,5-dimethylimidazol-2-ylidene hexamolybdate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.941(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0840(5)
_cell_length_b                   12.7449(8)
_cell_length_c                   13.0142(6)
_cell_measurement_temperature    133(2)
_cell_volume                     1828.57(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe IPDS2'
_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  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26164
_diffrn_reflns_theta_full        24.73
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    2.075
_exptl_absorpt_correction_T_max  0.6816
_exptl_absorpt_correction_T_min  0.5748
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0172
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0235P)²+2.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0437
_reflns_number_gt                2880
_reflns_number_total             3106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3217.cff
_cod_data_source_block           12673217
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               8102867
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Mo1 Mo 0.051648(18) 0.539829(16) 0.172785(15) 0.01588(6) Uani 1 1 d . . .
Mo2 Mo -0.199076(17) 0.475153(16) 0.033054(16) 0.01663(7) Uani 1 1 d . . .
Mo3 Mo -0.040343(18) 0.676646(15) -0.034459(16) 0.01592(7) Uani 1 1 d . . .
O1 O 0.08940(17) 0.56077(15) 0.29956(14) 0.0275(4) Uani 1 1 d . . .
O2 O 0.08297(15) 0.38488(13) 0.16111(13) 0.0202(4) Uani 1 1 d . . .
O3 O 0.20330(14) 0.55221(13) 0.11373(13) 0.0195(4) Uani 1 1 d . . .
O4 O 0.0000 0.5000 0.0000 0.0121(4) Uani 1 2 d S . .
O5 O 0.00324(15) 0.66903(13) 0.11955(13) 0.0196(4) Uani 1 1 d . . .
O6 O -0.11565(15) 0.49532(13) 0.16817(13) 0.0194(4) Uani 1 1 d . . .
O7 O -0.12440(15) 0.33112(13) 0.04530(13) 0.0205(4) Uani 1 1 d . . .
O8 O -0.34269(16) 0.44976(15) 0.05576(15) 0.0285(4) Uani 1 1 d . . .
O9 O -0.19529(14) 0.61733(13) 0.00781(13) 0.0195(4) Uani 1 1 d . . .
O10 O -0.07594(17) 0.80440(14) -0.05085(15) 0.0277(4) Uani 1 1 d . . .
N1 N 0.53533(17) 0.52193(15) 0.27521(15) 0.0156(4) Uani 1 1 d . . .
N2 N 0.54917(17) 0.67541(15) 0.20626(15) 0.0162(4) Uani 1 1 d . . .
C1 C 0.4771(2) 0.59312(18) 0.21440(18) 0.0167(5) Uani 1 1 d . . .
H1 H 0.3967 0.5864 0.1819 0.020 Uiso 1 1 calc R . .
C2 C 0.6499(2) 0.55996(19) 0.30836(18) 0.0167(5) Uani 1 1 d . . .
C3 C 0.6596(2) 0.65574(19) 0.26481(18) 0.0165(5) Uani 1 1 d . . .
C4 C 0.7415(2) 0.5005(2) 0.3776(2) 0.0215(5) Uani 1 1 d . . .
H4A H 0.8083 0.5474 0.4024 0.032 Uiso 1 1 calc R . .
H4B H 0.7731 0.4422 0.3391 0.032 Uiso 1 1 calc R . .
H4C H 0.7033 0.4729 0.4366 0.032 Uiso 1 1 calc R . .
C5 C 0.7643(2) 0.7296(2) 0.2717(2) 0.0217(5) Uani 1 1 d . . .
H5A H 0.8214 0.7114 0.3317 0.033 Uiso 1 1 calc R . .
H5B H 0.7352 0.8015 0.2792 0.033 Uiso 1 1 calc R . .
H5C H 0.8054 0.7244 0.2087 0.033 Uiso 1 1 calc R . .
C11 C 0.4826(2) 0.41962(18) 0.30333(19) 0.0173(5) Uani 1 1 d . . .
H11A H 0.5493 0.3761 0.3391 0.021 Uiso 1 1 calc R . .
C12 C 0.3886(2) 0.4376(2) 0.3782(2) 0.0255(6) Uani 1 1 d . . .
H12A H 0.4243 0.4795 0.4368 0.038 Uiso 1 1 calc R . .
H12B H 0.3617 0.3698 0.4032 0.038 Uiso 1 1 calc R . .
H12C H 0.3190 0.4751 0.3430 0.038 Uiso 1 1 calc R . .
C13 C 0.4322(2) 0.3618(2) 0.2064(2) 0.0249(6) Uani 1 1 d . . .
H13A H 0.4940 0.3592 0.1577 0.037 Uiso 1 1 calc R . .
H13B H 0.3603 0.3987 0.1744 0.037 Uiso 1 1 calc R . .
H13C H 0.4099 0.2902 0.2244 0.037 Uiso 1 1 calc R . .
C21 C 0.5190(2) 0.77141(18) 0.14394(18) 0.0169(5) Uani 1 1 d . . .
H21A H 0.5508 0.8336 0.1851 0.020 Uiso 1 1 calc R . .
C22 C 0.3825(2) 0.7836(2) 0.1211(2) 0.0218(5) Uani 1 1 d . . .
H22A H 0.3444 0.7771 0.1855 0.033 Uiso 1 1 calc R . .
H22B H 0.3511 0.7289 0.0727 0.033 Uiso 1 1 calc R . .
H22C H 0.3640 0.8528 0.0906 0.033 Uiso 1 1 calc R . .
C23 C 0.5810(2) 0.7676(2) 0.0456(2) 0.0266(6) Uani 1 1 d . . .
H23A H 0.6687 0.7601 0.0631 0.040 Uiso 1 1 calc R . .
H23B H 0.5642 0.8326 0.0065 0.040 Uiso 1 1 calc R . .
H23C H 0.5502 0.7077 0.0037 0.040 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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
O1 Mo1 O5 105.08(8) . . ?
O1 Mo1 O3 103.88(8) . . ?
O5 Mo1 O3 90.51(7) . . ?
O1 Mo1 O6 102.57(8) . . ?
O5 Mo1 O6 90.55(7) . . ?
O3 Mo1 O6 152.28(7) . . ?
O1 Mo1 O2 101.68(8) . . ?
O5 Mo1 O2 153.24(7) . . ?
O3 Mo1 O2 83.44(7) . . ?
O6 Mo1 O2 83.23(7) . . ?
O1 Mo1 O4 176.49(7) . . ?
O5 Mo1 O4 78.35(5) . . ?
O3 Mo1 O4 76.64(5) . . ?
O6 Mo1 O4 76.47(5) . . ?
O2 Mo1 O4 74.89(5) . . ?
O8 Mo2 O9 105.08(8) . . ?
O8 Mo2 O6 103.90(8) . . ?
O9 Mo2 O6 90.80(7) . . ?
O8 Mo2 O3 102.24(8) . 3_565 ?
O9 Mo2 O3 89.99(7) . 3_565 ?
O6 Mo2 O3 152.67(7) . 3_565 ?
O8 Mo2 O7 101.52(8) . . ?
O9 Mo2 O7 153.37(7) . . ?
O6 Mo2 O7 83.93(7) . . ?
O3 Mo2 O7 83.21(7) 3_565 . ?
O8 Mo2 O4 176.73(7) . . ?
O9 Mo2 O4 78.02(5) . . ?
O6 Mo2 O4 76.90(5) . . ?
O3 Mo2 O4 76.55(5) 3_565 . ?
O7 Mo2 O4 75.36(5) . . ?
O10 Mo3 O2 105.26(8) . 3_565 ?
O10 Mo3 O7 105.22(8) . 3_565 ?
O2 Mo3 O7 94.17(7) 3_565 3_565 ?
O10 Mo3 O9 101.73(8) . . ?
O2 Mo3 O9 86.41(7) 3_565 . ?
O7 Mo3 O9 151.86(7) 3_565 . ?
O10 Mo3 O5 101.63(8) . . ?
O2 Mo3 O5 151.94(7) 3_565 . ?
O7 Mo3 O5 86.35(7) 3_565 . ?
O9 Mo3 O5 80.38(7) . . ?
O10 Mo3 O4 175.31(7) . . ?
O2 Mo3 O4 77.72(5) 3_565 . ?
O7 Mo3 O4 77.97(5) 3_565 . ?
O9 Mo3 O4 74.67(5) . . ?
O5 Mo3 O4 74.96(5) . . ?
Mo3 O2 Mo1 117.05(8) 3_565 . ?
Mo1 O3 Mo2 116.47(8) . 3_565 ?
Mo2 O4 Mo2 180.0 3_565 . ?
Mo2 O4 Mo1 89.665(8) 3_565 3_565 ?
Mo2 O4 Mo1 90.336(8) . 3_565 ?
Mo2 O4 Mo1 90.336(8) 3_565 . ?
Mo2 O4 Mo1 89.664(8) . . ?
Mo1 O4 Mo1 180.000(10) 3_565 . ?
Mo2 O4 Mo3 89.983(7) 3_565 . ?
Mo2 O4 Mo3 90.018(7) . . ?
Mo1 O4 Mo3 90.096(7) 3_565 . ?
Mo1 O4 Mo3 89.904(7) . . ?
Mo2 O4 Mo3 90.018(7) 3_565 3_565 ?
Mo2 O4 Mo3 89.981(7) . 3_565 ?
Mo1 O4 Mo3 89.904(7) 3_565 3_565 ?
Mo1 O4 Mo3 90.096(7) . 3_565 ?
Mo3 O4 Mo3 180.0 . 3_565 ?
Mo1 O5 Mo3 116.56(8) . . ?
Mo2 O6 Mo1 115.95(8) . . ?
Mo3 O7 Mo2 116.36(8) 3_565 . ?
Mo2 O9 Mo3 117.11(8) . . ?
C1 N1 C2 108.69(19) . . ?
C1 N1 C11 124.45(19) . . ?
C2 N1 C11 126.86(19) . . ?
C1 N2 C3 108.4(2) . . ?
C1 N2 C21 126.11(19) . . ?
C3 N2 C21 125.50(19) . . ?
N1 C1 N2 109.1(2) . . ?
C3 C2 N1 107.1(2) . . ?
C3 C2 C4 129.1(2) . . ?
N1 C2 C4 123.7(2) . . ?
C2 C3 N2 106.7(2) . . ?
C2 C3 C5 129.7(2) . . ?
N2 C3 C5 123.6(2) . . ?
N1 C11 C12 109.81(19) . . ?
N1 C11 C13 109.91(19) . . ?
C12 C11 C13 113.0(2) . . ?
N2 C21 C23 109.77(19) . . ?
N2 C21 C22 110.76(19) . . ?
C23 C21 C22 111.6(2) . . ?
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
Mo1 O1 1.6810(17) . ?
Mo1 O5 1.8445(16) . ?
Mo1 O3 1.9257(17) . ?
Mo1 O6 1.9341(16) . ?
Mo1 O2 2.0136(17) . ?
Mo1 O4 2.3185(2) . ?
Mo2 O8 1.6802(18) . ?
Mo2 O9 1.8428(17) . ?
Mo2 O6 1.9174(17) . ?
Mo2 O3 1.9376(17) 3_565 ?
Mo2 O7 2.0132(17) . ?
Mo2 O4 2.3132(2) . ?
Mo3 O10 1.6837(17) . ?
Mo3 O2 1.8422(17) 3_565 ?
Mo3 O7 1.8486(17) 3_565 ?
Mo3 O9 2.0048(16) . ?
Mo3 O5 2.0148(17) . ?
Mo3 O4 2.3298(2) . ?
O2 Mo3 1.8421(17) 3_565 ?
O3 Mo2 1.9376(17) 3_565 ?
O4 Mo2 2.3132(2) 3_565 ?
O4 Mo1 2.3185(2) 3_565 ?
O4 Mo3 2.3298(2) 3_565 ?
O7 Mo3 1.8486(17) 3_565 ?
N1 C1 1.327(3) . ?
N1 C2 1.386(3) . ?
N1 C11 1.490(3) . ?
N2 C1 1.330(3) . ?
N2 C3 1.396(3) . ?
N2 C21 1.487(3) . ?
C2 C3 1.355(4) . ?
C2 C4 1.492(3) . ?
C3 C5 1.490(3) . ?
C11 C12 1.515(3) . ?
C11 C13 1.517(3) . ?
C21 C23 1.515(3) . ?
C21 C22 1.519(3) . ?
