#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:40:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179454 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/51/4335109.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_4335109
loop_
_publ_author_name
'Qiang Gao'
'Xiqu Wang'
'Joshua Tapp'
'Angela Moeller'
'Allan J. Jacobson'
_publ_section_title
;
 Antimony Tartrate Transition-Metal-Oxo Chiral Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6610
_journal_page_last               6616
_journal_paper_doi               10.1021/ic4006345
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_formula_sum            'C24 H51 Cr Ni3 O66 Sb12'
_chemical_formula_weight         3084.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           182
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c 2c'
_symmetry_space_group_name_H-M   'P 63 2 2'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   13.3451(2)
_cell_length_b                   13.3451(2)
_cell_length_c                   23.8732(6)
_cell_measurement_reflns_used    7665
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.2837
_cell_measurement_theta_min      2.4529
_cell_volume                     3682.01(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  Bruker-ApexII
_diffrn_measurement_method       'narrow frame'
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23797
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    5.333
_exptl_absorpt_correction_T_max  0.596
_exptl_absorpt_correction_T_min  0.457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.782
_exptl_crystal_description       block
_exptl_crystal_F_000             2886
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.771
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0192
_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/[σ²(Fo²)+(0.0383P)²+0.1872P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0559
_reflns_number_gt                2964
_reflns_number_total             3054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4006345_si_004.cif
_cod_data_source_block           211131
_cod_database_code               4335109
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -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
Sb1 Sb 0.230177(18) 0.242282(18) 0.209130(10) 0.02216(7) Uani 1 1 d .
Sb2 Sb 0.18257(2) 0.10151(2) 0.076248(9) 0.02697(7) Uani 1 1 d .
Ni1 Ni 0.0000 0.0000 0.30555(3) 0.01829(15) Uani 0.50 3 d SP
Ni2 Ni 0.6667 0.3333 0.06533(3) 0.02102(15) Uani 1 3 d S
Cr1 Cr 0.0000 0.0000 0.30555(3) 0.01829(15) Uani 0.50 3 d SP
O1 O 0.3184(2) 0.3348(2) 0.13142(10) 0.0317(6) Uani 1 1 d .
O2 O 0.3187(3) 0.4574(3) 0.06821(13) 0.0452(8) Uani 1 1 d .
O3 O 0.1459(2) 0.3236(2) 0.18855(10) 0.0271(5) Uani 1 1 d .
O4 O -0.1307(2) 0.2180(2) 0.11712(13) 0.0351(7) Uani 1 1 d .
O5 O -0.0352(3) 0.4013(3) 0.14648(18) 0.0537(10) Uani 1 1 d .
O6 O 0.0566(2) 0.2213(2) 0.07863(11) 0.0317(5) Uani 1 1 d .
O7 O 0.6516(2) 0.2037(2) 0.11619(12) 0.0349(6) Uani 1 1 d .
O8 O 0.5290(3) 0.2200(2) 0.01666(11) 0.0371(6) Uani 1 1 d .
O9 O 0.0000 0.0000 0.06786(17) 0.0287(9) Uani 1 3 d S
O10 O 0.1471(2) 0.1068(2) 0.15607(10) 0.0234(5) Uani 1 1 d .
O11 O 0.06829(14) 0.1366(3) 0.2500 0.0196(6) Uani 1 2 d S
O12 O 0.0000 0.4976(3) 0.0000 0.0361(8) Uani 1 2 d S
O13 O 0.0812(13) 0.5406(7) 0.2500 0.198(5) Uiso 1 2 d S
C1 C 0.2792(3) 0.3974(3) 0.11003(17) 0.0298(8) Uani 1 1 d .
C2 C 0.1726(3) 0.3867(3) 0.13801(16) 0.0281(8) Uani 1 1 d .
H2 H 0.1868 0.4646 0.1463 0.034 Uiso 1 1 calc R
C3 C 0.0701(3) 0.3284(3) 0.09738(16) 0.0305(8) Uani 1 1 d .
H3 H 0.0891 0.3789 0.0646 0.037 Uiso 1 1 calc R
C4 C -0.0389(3) 0.3165(3) 0.12288(17) 0.0325(8) Uani 1 1 d .
O14 O 0.3333 0.6667 0.2500 0.145(7) Uiso 1 6 d S
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'
Ni Ni 0.3393 1.1124 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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'
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
O3 Sb1 O10 97.29(10) . .
O3 Sb1 O11 79.10(9) . .
O10 Sb1 O11 76.96(9) . .
O3 Sb1 O1 77.00(10) . .
O10 Sb1 O1 82.81(10) . .
O11 Sb1 O1 146.25(7) . .
O10 Sb2 O6 96.09(10) . 5
O10 Sb2 O9 83.94(13) . .
O6 Sb2 O9 80.60(8) 5 .
O10 Sb2 O4 79.06(11) . 5
O6 Sb2 O4 76.10(11) 5 5
O9 Sb2 O4 149.34(11) . 5
O10 Ni1 O10 100.33(9) 12 10
O10 Ni1 O10 100.33(9) 12 11
O10 Ni1 O10 100.33(9) 10 11
O10 Ni1 O11 162.61(8) 12 3
O10 Ni1 O11 79.66(8) 10 3
O10 Ni1 O11 96.75(8) 11 3
O10 Ni1 O11 79.66(8) 12 5
O10 Ni1 O11 96.75(8) 10 5
O10 Ni1 O11 162.61(8) 11 5
O11 Ni1 O11 83.07(9) 3 5
O10 Ni1 O11 96.75(8) 12 .
O10 Ni1 O11 162.61(8) 10 .
O10 Ni1 O11 79.66(8) 11 .
O11 Ni1 O11 83.07(9) 3 .
O11 Ni1 O11 83.07(9) 5 .
O10 Ni1 Cr1 117.54(7) 12 10
O10 Ni1 Cr1 117.54(7) 10 10
O10 Ni1 Cr1 117.54(7) 11 10
O11 Ni1 Cr1 49.96(6) 3 10
O11 Ni1 Cr1 49.96(6) 5 10
O11 Ni1 Cr1 49.96(6) . 10
O10 Ni1 Ni1 117.54(7) 12 10
O10 Ni1 Ni1 117.54(7) 10 10
O10 Ni1 Ni1 117.54(7) 11 10
O11 Ni1 Ni1 49.96(6) 3 10
O11 Ni1 Ni1 49.96(6) 5 10
O11 Ni1 Ni1 49.96(6) . 10
Cr1 Ni1 Ni1 0.0 10 10
O7 Ni2 O7 88.20(12) . 3_655
O7 Ni2 O7 88.20(12) . 5_665
O7 Ni2 O7 88.20(12) 3_655 5_665
O7 Ni2 O8 88.31(12) . 3_655
O7 Ni2 O8 92.27(11) 3_655 3_655
O7 Ni2 O8 176.46(12) 5_665 3_655
O7 Ni2 O8 92.27(11) . .
O7 Ni2 O8 176.46(12) 3_655 .
O7 Ni2 O8 88.31(12) 5_665 .
O8 Ni2 O8 91.25(12) 3_655 .
O7 Ni2 O8 176.46(12) . 5_665
O7 Ni2 O8 88.31(12) 3_655 5_665
O7 Ni2 O8 92.27(11) 5_665 5_665
O8 Ni2 O8 91.25(12) 3_655 5_665
O8 Ni2 O8 91.25(12) . 5_665
C1 O1 Sb1 114.7(2) . .
C2 O3 Sb1 119.8(2) . .
C4 O4 Sb2 114.3(2) . 3
C3 O6 Sb2 119.6(2) . 3
Sb2 O9 Sb2 119.12(3) . 5
Sb2 O9 Sb2 119.12(3) . 3
Sb2 O9 Sb2 119.12(3) 5 3
Sb2 O10 Cr1 126.16(12) . 10
Sb2 O10 Ni1 126.16(12) . 10
Cr1 O10 Ni1 0.00(4) 10 10
Sb2 O10 Sb1 127.01(12) . .
Cr1 O10 Sb1 104.86(11) 10 .
Ni1 O10 Sb1 104.86(11) 10 .
Cr1 O11 Ni1 0.00(3) 10 10
Cr1 O11 Ni1 80.07(12) 10 .
Ni1 O11 Ni1 80.07(12) 10 .
Cr1 O11 Sb1 98.28(2) 10 .
Ni1 O11 Sb1 98.28(2) 10 .
Ni1 O11 Sb1 137.04(4) . .
Cr1 O11 Sb1 137.04(4) 10 11
Ni1 O11 Sb1 137.04(4) 10 11
Ni1 O11 Sb1 98.28(2) . 11
Sb1 O11 Sb1 110.22(14) . 11
O2 C1 O1 124.4(4) . .
O2 C1 C2 120.0(3) . .
O1 C1 C2 115.4(3) . .
O3 C2 C1 112.3(3) . .
O3 C2 C3 110.1(3) . .
C1 C2 C3 109.1(3) . .
O3 C2 H2 108.4 . .
C1 C2 H2 108.4 . .
C3 C2 H2 108.4 . .
O6 C3 C4 112.9(3) . .
O6 C3 C2 110.0(3) . .
C4 C3 C2 111.5(3) . .
O6 C3 H3 107.4 . .
C4 C3 H3 107.4 . .
C2 C3 H3 107.4 . .
O5 C4 O4 124.4(4) . .
O5 C4 C3 119.3(4) . .
O4 C4 C3 116.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 O3 1.976(2) .
Sb1 O10 2.024(2) .
Sb1 O11 2.1358(18) .
Sb1 O1 2.213(2) .
Sb2 O10 1.973(2) .
Sb2 O6 2.002(3) 5
Sb2 O9 2.1239(4) .
Sb2 O4 2.271(3) 5
Ni1 O10 1.981(2) 12
Ni1 O10 1.981(2) 10
Ni1 O10 1.981(2) 11
Ni1 O11 2.062(2) 3
Ni1 O11 2.062(2) 5
Ni1 O11 2.062(2) .
Ni1 Cr1 2.6524(14) 10
Ni1 Ni1 2.6524(14) 10
Ni2 O7 2.040(3) .
Ni2 O7 2.040(3) 3_655
Ni2 O7 2.040(3) 5_665
Ni2 O8 2.058(3) 3_655
Ni2 O8 2.058(3) .
Ni2 O8 2.058(3) 5_665
O1 C1 1.291(4) .
O2 C1 1.222(5) .
O3 C2 1.411(4) .
O4 C4 1.279(5) .
O4 Sb2 2.271(3) 3
O5 C4 1.243(5) .
O6 C3 1.420(5) .
O6 Sb2 2.002(3) 3
O9 Sb2 2.1239(4) 5
O9 Sb2 2.1239(4) 3
O10 Cr1 1.981(2) 10
O10 Ni1 1.981(2) 10
O11 Cr1 2.062(2) 10
O11 Ni1 2.062(2) 10
O11 Sb1 2.1358(18) 11
C1 C2 1.512(5) .
C2 C3 1.534(5) .
C2 H2 0.9800 .
C3 C4 1.510(5) .
C3 H3 0.9800 .
