#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:10:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179365 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/62/4326266.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_4326266
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 N O21 Sb2 Tb'
_chemical_formula_weight         864.64
_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                   10.2675(3)
_cell_length_b                   11.2978(4)
_cell_length_c                   16.8401(6)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      2.32
_cell_volume                     1953.45(11)
_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 0.998
_diffrn_measured_fraction_theta_max 0.876
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12465
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.82
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    6.439
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.940
_exptl_crystal_description       plate
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.173
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.165
_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       0.0063(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constrain
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0211
_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)+(0.0330P)²+2.4565P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0563
_reflns_number_gt                4761
_reflns_number_total             4767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201274c_si_003_08.cif
_cod_data_source_block           1D-Tb
_cod_database_code               4326266
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
Tb1 Tb 0.622780(17) 0.337176(16) 0.710521(11) 0.01504(6) Uani 1 1 d .
Sb2 Sb 0.40097(2) 0.50375(2) 0.383622(15) 0.01704(7) Uani 1 1 d .
Sb1 Sb 0.02675(3) 0.62000(2) 0.573782(16) 0.01748(7) Uani 1 1 d .
O1 O 0.4772(3) 0.4189(3) 0.6182(2) 0.0274(7) Uani 1 1 d .
O2 O 0.4916(3) 0.5044(3) 0.50020(19) 0.0222(6) Uani 1 1 d .
O3 O 0.2694(3) 0.4172(3) 0.44824(17) 0.0191(6) Uani 1 1 d .
O4 O 0.1975(3) 0.5416(3) 0.5952(2) 0.0219(6) Uani 1 1 d .
O5 O -0.0152(3) 0.4373(3) 0.5425(2) 0.0245(6) Uani 1 1 d .
O6 O 0.0608(4) 0.2540(3) 0.5620(2) 0.0320(8) Uani 1 1 d .
O7 O 0.2591(3) 0.8995(3) 0.4924(2) 0.0242(6) Uani 1 1 d .
O8 O 0.1519(3) 0.7774(3) 0.57255(19) 0.0237(6) Uani 1 1 d .
O9 O 0.0537(3) 0.6479(3) 0.45809(18) 0.0210(6) Uani 1 1 d .
O10 O 0.0865(3) 0.6700(3) 0.27035(18) 0.0236(6) Uani 1 1 d .
O11 O 0.2302(3) 0.5319(3) 0.30556(18) 0.0214(6) Uani 1 1 d .
O12 O 0.3394(3) 0.6622(3) 0.41645(17) 0.0191(6) Uani 1 1 d .
O13 O 0.8334(4) 0.2224(4) 0.7068(3) 0.0442(10) Uani 1 1 d .
O14 O 0.8510(4) 0.4008(4) 0.7459(3) 0.0441(10) Uani 1 1 d .
O15 O 1.0222(4) 0.2865(6) 0.7475(3) 0.0615(15) Uani 1 1 d .
O16W O 0.7318(3) 0.3811(3) 0.5881(2) 0.0278(7) Uani 1 1 d .
O17W O 0.5547(3) 0.1724(3) 0.6316(2) 0.0276(7) Uani 1 1 d .
O18W O 0.6307(4) 0.5467(3) 0.7279(2) 0.0280(7) Uani 1 1 d .
O19W O 0.6415(3) 0.3740(3) 0.84866(18) 0.0257(7) Uani 1 1 d .
O20W O 0.6214(3) 0.1416(3) 0.7892(2) 0.0259(6) Uani 1 1 d .
O21W O 0.2777(4) 0.1168(4) 0.6197(3) 0.0418(9) Uani 1 1 d .
N1 N 0.9068(4) 0.3026(5) 0.7335(3) 0.0328(10) Uani 1 1 d .
C1 C 0.4356(4) 0.4385(4) 0.5505(3) 0.0170(7) Uani 1 1 d .
C2 C 0.3081(4) 0.3828(4) 0.5255(2) 0.0171(7) Uani 1 1 d .
H2 H 0.3186 0.2965 0.5263 0.020 Uiso 1 1 calc R
C3 C 0.2053(4) 0.4166(4) 0.5875(2) 0.0181(8) Uani 1 1 d .
H3 H 0.2305 0.3827 0.6388 0.022 Uiso 1 1 calc R
C4 C 0.0751(4) 0.3630(4) 0.5622(2) 0.0199(8) Uani 1 1 d .
C5 C 0.1854(4) 0.8157(4) 0.5031(3) 0.0181(7) Uani 1 1 d .
C6 C 0.1246(4) 0.7489(4) 0.4337(2) 0.0172(7) Uani 1 1 d .
H6 H 0.0650 0.8025 0.4059 0.021 Uiso 1 1 calc R
C7 C 0.2354(4) 0.7147(4) 0.3762(2) 0.0164(7) Uani 1 1 d .
H7 H 0.2671 0.7871 0.3507 0.020 Uiso 1 1 calc R
C8 C 0.1780(4) 0.6348(4) 0.3122(2) 0.0170(7) 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'
Tb Tb -0.1723 4.1537 '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 Tb1 O19W 129.28(12) . .
O1 Tb1 O10 73.63(12) . 2_565
O19W Tb1 O10 70.31(11) . 2_565
O1 Tb1 O18W 73.31(13) . .
O19W Tb1 O18W 72.73(13) . .
O10 Tb1 O18W 90.73(13) 2_565 .
O1 Tb1 O17W 75.63(13) . .
O19W Tb1 O17W 134.84(13) . .
O10 Tb1 O17W 86.83(12) 2_565 .
O18W Tb1 O17W 148.24(13) . .
O1 Tb1 O16W 69.28(12) . .
O19W Tb1 O16W 140.30(12) . .
O10 Tb1 O16W 142.60(11) 2_565 .
O18W Tb1 O16W 83.35(13) . .
O17W Tb1 O16W 79.63(13) . .
O1 Tb1 O14 129.52(15) . .
O19W Tb1 O14 69.09(14) . .
O10 Tb1 O14 138.61(13) 2_565 .
O18W Tb1 O14 69.93(14) . .
O17W Tb1 O14 128.64(13) . .
O16W Tb1 O14 73.16(14) . .
O1 Tb1 O13 137.05(15) . .
O19W Tb1 O13 92.57(15) . .
O10 Tb1 O13 140.25(14) 2_565 .
O18W Tb1 O13 118.91(13) . .
O17W Tb1 O13 80.60(14) . .
O16W Tb1 O13 71.62(14) . .
O14 Tb1 O13 49.88(15) . .
O1 Tb1 O20W 132.45(12) . .
O19W Tb1 O20W 69.27(12) . .
O10 Tb1 O20W 75.38(11) 2_565 .
O18W Tb1 O20W 141.97(11) . .
O17W Tb1 O20W 67.45(11) . .
O16W Tb1 O20W 128.48(12) . .
O14 Tb1 O20W 97.34(14) . .
O13 Tb1 O20W 64.95(13) . .
O12 Sb2 O3 94.30(13) . .
O12 Sb2 O2 83.16(12) . .
O3 Sb2 O2 78.38(11) . .
O12 Sb2 O11 77.45(11) . .
O3 Sb2 O11 81.81(12) . .
O2 Sb2 O11 151.03(11) . .
O9 Sb1 O4 97.17(13) . .
O9 Sb1 O5 86.63(13) . .
O4 Sb1 O5 78.24(12) . .
O9 Sb1 O8 77.36(12) . .
O4 Sb1 O8 81.22(13) . .
O5 Sb1 O8 152.09(13) . .
C1 O1 Tb1 154.3(3) . .
C1 O2 Sb2 114.1(3) . .
C2 O3 Sb2 116.5(2) . .
C3 O4 Sb1 118.3(3) . .
C4 O5 Sb1 114.3(3) . .
C5 O8 Sb1 115.8(3) . .
C6 O9 Sb1 118.9(2) . .
C8 O10 Tb1 156.3(3) . 2_564
C8 O11 Sb2 114.1(3) . .
C7 O12 Sb2 119.5(2) . .
N1 O13 Tb1 97.7(3) . .
N1 O14 Tb1 97.6(3) . .
O15 N1 O13 122.8(6) . .
O15 N1 O14 122.5(6) . .
O13 N1 O14 114.7(4) . .
O1 C1 O2 124.4(4) . .
O1 C1 C2 118.7(4) . .
O2 C1 C2 116.9(4) . .
O3 C2 C1 112.6(3) . .
O3 C2 C3 111.3(3) . .
C1 C2 C3 107.7(3) . .
O4 C3 C4 111.7(3) . .
O4 C3 C2 110.4(3) . .
C4 C3 C2 108.3(3) . .
O6 C4 O5 124.0(4) . .
O6 C4 C3 119.9(4) . .
O5 C4 C3 116.2(4) . .
O7 C5 O8 123.7(4) . .
O7 C5 C6 121.5(4) . .
O8 C5 C6 114.8(3) . .
O9 C6 C5 112.8(3) . .
O9 C6 C7 111.1(3) . .
C5 C6 C7 107.6(3) . .
O12 C7 C8 112.8(3) . .
O12 C7 C6 111.4(3) . .
C8 C7 C6 107.9(3) . .
O10 C8 O11 123.8(4) . .
O10 C8 C7 120.3(4) . .
O11 C8 C7 115.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O1 2.346(3) .
Tb1 O19W 2.371(3) .
Tb1 O10 2.375(3) 2_565
Tb1 O18W 2.387(3) .
Tb1 O17W 2.392(3) .
Tb1 O16W 2.398(3) .
Tb1 O14 2.522(4) .
Tb1 O13 2.522(4) .
Tb1 O20W 2.577(3) .
Sb2 O12 1.978(3) .
Sb2 O3 1.992(3) .
Sb2 O2 2.172(3) .
Sb2 O11 2.215(3) .
Sb1 O9 1.993(3) .
Sb1 O4 1.997(3) .
Sb1 O5 2.174(3) .
Sb1 O8 2.195(3) .
O1 C1 1.237(5) .
O2 C1 1.266(5) .
O3 C2 1.416(5) .
O4 C3 1.420(5) .
O5 C4 1.294(5) .
O6 C4 1.240(6) .
O7 C5 1.226(5) .
O8 C5 1.294(6) .
O9 C6 1.414(5) .
O10 C8 1.240(5) .
O10 Tb1 2.375(3) 2_564
O11 C8 1.285(5) .
O12 C7 1.397(5) .
O13 N1 1.261(7) .
O14 N1 1.266(7) .
O15 N1 1.223(6) .
C1 C2 1.512(5) .
C2 C3 1.532(6) .
C3 C4 1.528(6) .
C5 C6 1.524(5) .
C6 C7 1.543(6) .
C7 C8 1.524(6) .
