#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:10:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179365 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/62/4326267.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_4326267
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 Dy N O21 Sb2'
_chemical_formula_weight         868.22
_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                   10.2594(4)
_cell_length_b                   11.2855(4)
_cell_length_c                   16.7969(7)
_cell_measurement_reflns_used    9730
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.33
_cell_volume                     1944.79(13)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14439
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    6.673
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.965
_exptl_crystal_description       plate
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.005
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(7)
_refine_ls_extinction_coef       0.0112(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constrain
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0215
_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)+(0.0311P)²+1.8067P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0559
_reflns_number_gt                4604
_reflns_number_total             4656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201274c_si_003_09.cif
_cod_data_source_block           1D-Dy
_cod_database_code               4326267
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
Dy1 Dy 0.622439(17) 0.337423(17) 0.710534(11) 0.01404(7) Uani 1 1 d .
Sb2 Sb 0.40056(3) 0.50367(3) 0.383484(16) 0.01581(8) Uani 1 1 d .
Sb1 Sb 0.02588(3) 0.61987(3) 0.574031(17) 0.01625(8) Uani 1 1 d .
O1 O 0.4771(3) 0.4187(3) 0.6188(2) 0.0255(7) Uani 1 1 d .
O2 O 0.4914(3) 0.5038(3) 0.50053(19) 0.0204(6) Uani 1 1 d .
O3 O 0.2690(3) 0.4163(3) 0.44828(18) 0.0184(6) Uani 1 1 d .
O4 O 0.1963(3) 0.5410(3) 0.5952(2) 0.0197(7) Uani 1 1 d .
O5 O -0.0161(3) 0.4370(3) 0.5428(2) 0.0229(7) Uani 1 1 d .
O6 O 0.0595(4) 0.2539(3) 0.5622(2) 0.0311(8) Uani 1 1 d .
O7 O 0.2585(3) 0.8998(3) 0.4926(2) 0.0228(7) Uani 1 1 d .
O8 O 0.1520(3) 0.7775(3) 0.5727(2) 0.0219(7) Uani 1 1 d .
O9 O 0.0528(3) 0.6479(3) 0.45778(18) 0.0192(6) Uani 1 1 d .
O10 O 0.0859(3) 0.6703(3) 0.27026(19) 0.0227(7) Uani 1 1 d .
O11 O 0.2295(3) 0.5323(3) 0.30533(19) 0.0207(7) Uani 1 1 d .
O12 O 0.3392(3) 0.6630(3) 0.41659(18) 0.0190(6) Uani 1 1 d .
O13 O 0.8317(4) 0.2234(4) 0.7068(3) 0.0421(10) Uani 1 1 d .
O14 O 0.8503(4) 0.4012(4) 0.7456(3) 0.0417(10) Uani 1 1 d .
O15 O 1.0205(4) 0.2859(6) 0.7474(3) 0.0566(14) Uani 1 1 d .
O16W O 0.7309(3) 0.3811(3) 0.5882(2) 0.0254(8) Uani 1 1 d .
O17W O 0.5552(3) 0.1735(3) 0.6321(2) 0.0246(7) Uani 1 1 d .
O18W O 0.6295(4) 0.5458(3) 0.7268(2) 0.0271(7) Uani 1 1 d .
O19W O 0.6418(3) 0.3739(3) 0.84815(19) 0.0241(7) Uani 1 1 d .
O20W O 0.6210(3) 0.1419(3) 0.7892(2) 0.0243(7) Uani 1 1 d .
O21W O 0.2773(4) 0.1173(4) 0.6197(3) 0.0402(10) Uani 1 1 d .
N1 N 0.9061(4) 0.3036(5) 0.7333(3) 0.0297(10) Uani 1 1 d .
C1 C 0.4343(4) 0.4380(4) 0.5509(3) 0.0162(8) Uani 1 1 d .
C2 C 0.3066(4) 0.3829(4) 0.5258(2) 0.0156(8) Uani 1 1 d .
H2 H 0.3168 0.2966 0.5268 0.019 Uiso 1 1 calc R
C3 C 0.2056(4) 0.4168(4) 0.5876(3) 0.0171(8) Uani 1 1 d .
H3 H 0.2314 0.3833 0.6390 0.020 Uiso 1 1 calc R
C4 C 0.0747(4) 0.3621(4) 0.5626(3) 0.0185(9) Uani 1 1 d .
C5 C 0.1847(4) 0.8156(4) 0.5035(3) 0.0175(8) Uani 1 1 d .
C6 C 0.1245(4) 0.7490(4) 0.4338(2) 0.0155(8) Uani 1 1 d .
H6 H 0.0650 0.8030 0.4060 0.019 Uiso 1 1 calc R
C7 C 0.2344(4) 0.7143(4) 0.3756(3) 0.0166(8) Uani 1 1 d .
H7 H 0.2659 0.7868 0.3499 0.020 Uiso 1 1 calc R
C8 C 0.1773(4) 0.6347(4) 0.3117(3) 0.0163(8) 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'
Dy Dy -0.1892 4.4098 '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 Dy1 O19W 129.32(12) . .
O1 Dy1 O10 73.55(12) . 2_565
O19W Dy1 O10 70.50(12) . 2_565
O1 Dy1 O18W 72.88(13) . .
O19W Dy1 O18W 73.19(13) . .
O10 Dy1 O18W 90.89(13) 2_565 .
O1 Dy1 O17W 75.74(13) . .
O19W Dy1 O17W 134.85(13) . .
O10 Dy1 O17W 86.79(12) 2_565 .
O18W Dy1 O17W 147.86(13) . .
O1 Dy1 O16W 69.39(12) . .
O19W Dy1 O16W 140.24(13) . .
O10 Dy1 O16W 142.60(12) 2_565 .
O18W Dy1 O16W 83.10(13) . .
O17W Dy1 O16W 79.56(13) . .
O1 Dy1 O13 137.19(15) . .
O19W Dy1 O13 92.41(15) . .
O10 Dy1 O13 140.12(14) 2_565 .
O18W Dy1 O13 119.12(14) . .
O17W Dy1 O13 80.50(14) . .
O16W Dy1 O13 71.64(14) . .
O1 Dy1 O14 129.52(15) . .
O19W Dy1 O14 69.02(14) . .
O10 Dy1 O14 138.73(13) 2_565 .
O18W Dy1 O14 70.14(14) . .
O17W Dy1 O14 128.55(13) . .
O16W Dy1 O14 73.11(14) . .
O13 Dy1 O14 49.92(15) . .
O1 Dy1 O20W 132.32(13) . .
O19W Dy1 O20W 69.27(12) . .
O10 Dy1 O20W 75.23(11) 2_565 .
O18W Dy1 O20W 142.41(12) . .
O17W Dy1 O20W 67.38(12) . .
O16W Dy1 O20W 128.47(12) . .
O13 Dy1 O20W 64.97(13) . .
O14 Dy1 O20W 97.49(14) . .
O12 Sb2 O3 94.59(13) . .
O12 Sb2 O2 83.22(13) . .
O3 Sb2 O2 78.31(12) . .
O12 Sb2 O11 77.45(12) . .
O3 Sb2 O11 81.90(13) . .
O2 Sb2 O11 151.01(12) . .
O4 Sb1 O9 97.12(14) . .
O4 Sb1 O5 78.04(13) . .
O9 Sb1 O5 86.66(13) . .
O4 Sb1 O8 81.20(14) . .
O9 Sb1 O8 77.34(12) . .
O5 Sb1 O8 151.93(13) . .
C1 O1 Dy1 154.5(3) . .
C1 O2 Sb2 113.8(3) . .
C2 O3 Sb2 116.8(3) . .
C3 O4 Sb1 119.1(3) . .
C4 O5 Sb1 114.4(3) . .
C5 O8 Sb1 115.7(3) . .
C6 O9 Sb1 118.5(2) . .
C8 O10 Dy1 156.1(3) . 2_564
C8 O11 Sb2 114.5(3) . .
C7 O12 Sb2 118.7(3) . .
N1 O13 Dy1 98.1(3) . .
N1 O14 Dy1 97.7(3) . .
O15 N1 O14 123.5(6) . .
O15 N1 O13 122.3(6) . .
O14 N1 O13 114.2(4) . .
O1 C1 O2 123.5(4) . .
O1 C1 C2 119.4(4) . .
O2 C1 C2 117.1(4) . .
O3 C2 C1 112.7(4) . .
O3 C2 C3 112.2(3) . .
C1 C2 C3 107.3(4) . .
O4 C3 C2 111.1(4) . .
O4 C3 C4 111.4(4) . .
C2 C3 C4 108.0(4) . .
O6 C4 O5 123.5(4) . .
O6 C4 C3 120.7(4) . .
O5 C4 C3 115.8(4) . .
O7 C5 O8 123.6(4) . .
O7 C5 C6 121.2(4) . .
O8 C5 C6 115.2(4) . .
O9 C6 C5 112.9(3) . .
O9 C6 C7 110.8(3) . .
C5 C6 C7 108.4(3) . .
O12 C7 C8 113.5(4) . .
O12 C7 C6 110.8(3) . .
C8 C7 C6 108.4(3) . .
O10 C8 O11 124.4(4) . .
O10 C8 C7 119.9(4) . .
O11 C8 C7 115.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.332(3) .
Dy1 O19W 2.356(3) .
Dy1 O10 2.363(3) 2_565
Dy1 O18W 2.368(3) .
Dy1 O17W 2.373(3) .
Dy1 O16W 2.388(3) .
Dy1 O13 2.503(4) .
Dy1 O14 2.516(4) .
Dy1 O20W 2.572(3) .
Sb2 O12 1.984(3) .
Sb2 O3 1.995(3) .
Sb2 O2 2.176(3) .
Sb2 O11 2.215(3) .
Sb1 O4 1.994(3) .
Sb1 O9 1.997(3) .
Sb1 O5 2.173(4) .
Sb1 O8 2.199(3) .
O1 C1 1.242(6) .
O2 C1 1.269(6) .
O3 C2 1.409(5) .
O4 C3 1.411(6) .
O5 C4 1.301(6) .
O6 C4 1.231(6) .
O7 C5 1.229(6) .
O8 C5 1.285(6) .
O9 C6 1.417(5) .
O10 C8 1.235(6) .
O10 Dy1 2.363(3) 2_564
O11 C8 1.278(5) .
O12 C7 1.402(5) .
O13 N1 1.264(7) .
O14 N1 1.259(7) .
O15 N1 1.214(6) .
C1 C2 1.510(6) .
C2 C3 1.516(6) .
C3 C4 1.537(6) .
C5 C6 1.522(6) .
C6 C7 1.542(6) .
C7 C8 1.518(6) .
