#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:10:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179365 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/62/4326272.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_4326272
loop_
_publ_author_name
'Qiang Gao'
'Xiqu Wang'
'Allan J. Jacobson'
_publ_section_title
;
 Homochiral Frameworks Formed by Reactions of Lanthanide Ions with a
 Chiral Antimony Tartrate Secondary Building Unit
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9073
_journal_page_last               9082
_journal_paper_doi               10.1021/ic201274c
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration rm
_chemical_formula_sum            'C8 H16 Lu N O21 Sb2'
_chemical_formula_weight         880.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.260(3)
_cell_length_b                   11.279(3)
_cell_length_c                   16.619(4)
_cell_measurement_reflns_used    2915
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      2.33
_cell_volume                     1923.2(9)
_computing_cell_refinement       Bruker-ApexII
_computing_data_collection       Bruker-ApexII
_computing_data_reduction        Bruker-ApexII
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0766
_diffrn_reflns_av_sigmaI/netI    0.0968
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12111
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    7.996
_exptl_absorpt_correction_T_max  0.2779
_exptl_absorpt_correction_T_min  0.1963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.042
_exptl_crystal_description       needle
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.190
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.205
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.029(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constrain
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0360
_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)+(0.0076P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0633
_reflns_number_gt                3702
_reflns_number_total             4629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201274c_si_003_14.cif
_cod_data_source_block           1D-Lu
_cod_original_cell_volume        1923.2(8)
_cod_database_code               4326272
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, 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
Lu1 Lu 0.61957(4) 0.33842(3) 0.70963(2) 0.01946(9) Uani 1 1 d .
Sb2 Sb 0.39698(7) 0.50421(5) 0.38290(3) 0.02163(14) Uani 1 1 d .
Sb1 Sb 0.02108(6) 0.61899(6) 0.57514(4) 0.02210(15) Uani 1 1 d .
O1 O 0.4723(7) 0.4123(6) 0.6201(3) 0.0298(17) Uani 1 1 d .
O2 O 0.4868(6) 0.5023(5) 0.5006(3) 0.0245(15) Uani 1 1 d .
O3 O 0.2629(7) 0.4165(5) 0.4476(3) 0.0226(15) Uani 1 1 d .
O4 O 0.1922(7) 0.5400(5) 0.5964(4) 0.0256(16) Uani 1 1 d .
O5 O -0.0215(7) 0.4347(5) 0.5433(4) 0.0271(16) Uani 1 1 d .
O6 O 0.0546(7) 0.2525(6) 0.5601(4) 0.0349(18) Uani 1 1 d .
O7 O 0.2543(7) 0.9014(6) 0.4947(4) 0.0263(16) Uani 1 1 d .
O8 O 0.1488(7) 0.7767(6) 0.5754(4) 0.0281(17) Uani 1 1 d .
O9 O 0.0471(6) 0.6496(6) 0.4585(3) 0.0257(16) Uani 1 1 d .
O10 O 0.0792(6) 0.6730(6) 0.2702(3) 0.0263(16) Uani 1 1 d .
O11 O 0.2261(7) 0.5338(5) 0.3026(4) 0.0249(15) Uani 1 1 d .
O12 O 0.3348(6) 0.6632(6) 0.4170(3) 0.0242(14) Uani 1 1 d .
O13 O 0.8225(8) 0.2280(7) 0.7098(5) 0.051(2) Uani 1 1 d .
O14 O 0.8484(10) 0.4044(7) 0.7419(4) 0.061(3) Uani 1 1 d .
O15 O 1.0142(9) 0.2862(9) 0.7481(4) 0.065(3) Uani 1 1 d .
O16W O 0.7243(6) 0.3807(6) 0.5881(3) 0.0264(16) Uani 1 1 d .
O17W O 0.5549(6) 0.1768(5) 0.6341(3) 0.0242(15) Uani 1 1 d .
O18W O 0.6255(7) 0.5424(5) 0.7262(4) 0.0332(17) Uani 1 1 d .
O19W O 0.6442(7) 0.3725(6) 0.8460(4) 0.0349(18) Uani 1 1 d .
O20W O 0.6198(7) 0.1420(5) 0.7914(4) 0.0348(15) Uani 1 1 d .
O21W O 0.2751(8) 0.1149(7) 0.6217(4) 0.048(2) Uani 1 1 d .
N1 N 0.9005(10) 0.3063(9) 0.7330(5) 0.041(2) Uani 1 1 d .
C1 C 0.4283(9) 0.4344(8) 0.5514(5) 0.021(2) Uani 1 1 d .
C2 C 0.3025(9) 0.3815(8) 0.5261(5) 0.019(2) Uani 1 1 d .
H2 H 0.3122 0.2950 0.5265 0.022 Uiso 1 1 calc R
C3 C 0.1982(10) 0.4146(8) 0.5880(5) 0.024(2) Uani 1 1 d .
H3 H 0.2226 0.3803 0.6400 0.029 Uiso 1 1 calc R
C4 C 0.0701(10) 0.3607(8) 0.5617(5) 0.025(2) Uani 1 1 d .
C5 C 0.1813(9) 0.8155(8) 0.5055(5) 0.020(2) Uani 1 1 d .
C6 C 0.1214(10) 0.7506(7) 0.4342(5) 0.021(2) Uani 1 1 d .
H6 H 0.0624 0.8056 0.4067 0.025 Uiso 1 1 calc R
C7 C 0.2289(9) 0.7169(8) 0.3756(5) 0.022(2) Uani 1 1 d .
H7 H 0.2606 0.7894 0.3496 0.026 Uiso 1 1 calc R
C8 C 0.1713(9) 0.6352(9) 0.3103(5) 0.024(2) 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 0.0033 0.0016 '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'
Lu Lu -0.4720 5.8584 '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'
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
O1 Lu1 O10 73.5(2) . 2_565
O1 Lu1 O17W 75.1(2) . .
O10 Lu1 O17W 86.5(2) 2_565 .
O1 Lu1 O19W 130.7(2) . .
O10 Lu1 O19W 71.0(2) 2_565 .
O17W Lu1 O19W 134.0(2) . .
O1 Lu1 O18W 74.5(2) . .
O10 Lu1 O18W 91.5(3) 2_565 .
O17W Lu1 O18W 148.8(2) . .
O19W Lu1 O18W 73.5(2) . .
O1 Lu1 O16W 70.5(2) . .
O10 Lu1 O16W 143.6(2) 2_565 .
O17W Lu1 O16W 79.8(2) . .
O19W Lu1 O16W 139.7(2) . .
O18W Lu1 O16W 83.6(2) . .
O1 Lu1 O13 139.2(3) . .
O10 Lu1 O13 137.6(2) 2_565 .
O17W Lu1 O13 80.9(3) . .
O19W Lu1 O13 89.4(3) . .
O18W Lu1 O13 119.1(3) . .
O16W Lu1 O13 73.2(3) . .
O1 Lu1 O14 130.4(3) . .
O10 Lu1 O14 139.2(2) 2_565 .
O17W Lu1 O14 128.0(2) . .
O19W Lu1 O14 68.9(2) . .
O18W Lu1 O14 69.9(3) . .
O16W Lu1 O14 72.3(2) . .
O13 Lu1 O14 49.6(3) . .
O1 Lu1 O20W 130.8(2) . .
O10 Lu1 O20W 73.8(2) 2_565 .
O17W Lu1 O20W 67.14(19) . .
O19W Lu1 O20W 68.2(2) . .
O18W Lu1 O20W 141.6(2) . .
O16W Lu1 O20W 128.7(2) . .
O13 Lu1 O20W 64.0(2) . .
O14 Lu1 O20W 98.0(3) . .
O12 Sb2 O3 94.1(2) . .
O12 Sb2 O2 83.5(2) . .
O3 Sb2 O2 78.6(2) . .
O12 Sb2 O11 77.5(2) . .
O3 Sb2 O11 81.7(2) . .
O2 Sb2 O11 151.5(2) . .
O9 Sb1 O4 97.6(3) . .
O9 Sb1 O5 87.5(2) . .
O4 Sb1 O5 78.2(3) . .
O9 Sb1 O8 77.5(2) . .
O4 Sb1 O8 80.6(3) . .
O5 Sb1 O8 152.0(3) . .
C1 O1 Lu1 155.1(6) . .
C1 O2 Sb2 113.6(6) . .
C2 O3 Sb2 115.6(5) . .
C3 O4 Sb1 117.6(6) . .
C4 O5 Sb1 114.2(6) . .
C5 O8 Sb1 115.2(5) . .
C6 O9 Sb1 119.1(5) . .
C8 O10 Lu1 154.9(7) . 2_564
C8 O11 Sb2 114.8(6) . .
C7 O12 Sb2 119.5(5) . .
N1 O13 Lu1 100.8(7) . .
N1 O14 Lu1 96.5(7) . .
O15 N1 O14 123.9(11) . .
O15 N1 O13 123.1(11) . .
O14 N1 O13 113.0(10) . .
O1 C1 O2 123.2(9) . .
O1 C1 C2 119.5(8) . .
O2 C1 C2 117.3(8) . .
O3 C2 C1 113.4(7) . .
O3 C2 C3 110.4(8) . .
C1 C2 C3 108.7(7) . .
O4 C3 C4 113.0(9) . .
O4 C3 C2 109.8(8) . .
C4 C3 C2 108.4(7) . .
O6 C4 O5 122.7(10) . .
O6 C4 C3 121.1(9) . .
O5 C4 C3 116.1(8) . .
O7 C5 O8 123.8(8) . .
O7 C5 C6 120.4(8) . .
O8 C5 C6 115.8(8) . .
O9 C6 C7 111.7(7) . .
O9 C6 C5 112.2(7) . .
C7 C6 C5 109.0(8) . .
O12 C7 C6 110.6(7) . .
O12 C7 C8 112.3(8) . .
C6 C7 C8 108.8(8) . .
O10 C8 O11 126.2(9) . .
O10 C8 C7 117.9(9) . .
O11 C8 C7 115.9(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Lu1 O1 2.279(6) .
Lu1 O10 2.278(6) 2_565
Lu1 O17W 2.311(6) .
Lu1 O19W 2.313(6) .
Lu1 O18W 2.318(6) .
Lu1 O16W 2.336(6) .
Lu1 O13 2.426(8) .
Lu1 O14 2.520(10) .
Lu1 O20W 2.599(6) .
Sb2 O12 1.986(6) .
Sb2 O3 2.007(6) .
Sb2 O2 2.162(6) .
Sb2 O11 2.229(6) .
Sb1 O9 1.987(6) .
Sb1 O4 2.000(7) .
Sb1 O5 2.190(6) .
Sb1 O8 2.209(6) .
O1 C1 1.252(10) .
O2 C1 1.289(10) .
O3 C2 1.423(9) .
O4 C3 1.423(10) .
O5 C4 1.294(11) .
O6 C4 1.231(11) .
O7 C5 1.238(11) .
O8 C5 1.285(10) .
O9 C6 1.429(10) .
O10 C8 1.233(10) .
O10 Lu1 2.278(6) 2_564
O11 C8 1.281(11) .
O12 C7 1.421(11) .
O13 N1 1.253(11) .
O14 N1 1.238(12) .
O15 N1 1.215(13) .
C1 C2 1.483(12) .
C2 C3 1.530(12) .
C3 C4 1.512(14) .
C5 C6 1.524(11) .
C6 C7 1.519(13) .
C7 C8 1.541(12) .
