#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:36:54 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179669 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/22/4512207.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_4512207
loop_
_publ_author_name
'Sun, Jing-Wen'
'Zhu, Jing'
'Song, Hui-Feng'
'Li, Guang-Ming'
'Yao, Xu'
'Yan, Peng-Fei'
_publ_section_title
;
 Spontaneous Resolution of Racemic Salen-Type Ligand in the Construction
 of 3D Homochiral Lanthanide Frameworks
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5356
_journal_paper_doi               10.1021/cg501211f
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C40 H40 Cl La N6 O10'
_chemical_formula_sum            'C40 H40 Cl La N6 O10'
_chemical_formula_weight         939.14
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 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                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1798(2)
_cell_length_b                   18.1798(2)
_cell_length_c                   16.4174(3)
_cell_measurement_temperature    293(2)
_cell_volume                     5426.03(13)
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11072
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0457
_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)+(0.0656P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                3946
_reflns_number_total             4784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501211f_si_004.cif
_cod_data_source_block           zj33
_cod_depositor_comments
'Adding full bibliography for 4512206--4512208.cif.'
_cod_original_cell_volume        5426.04(16)
_cod_database_code               4512207
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -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
O4A O 0.2626(10) 0.2243(5) 0.7413(6) 0.075(5) Uiso 0.53(3) 1 d P A 1
O4B O 0.2240(11) 0.2267(6) 0.7385(6) 0.069(5) Uiso 0.47(3) 1 d P A 2
C1 C 0.2059(3) 0.4085(3) 1.0452(3) 0.0441(13) Uani 1 1 d . A .
C2 C 0.1573(4) 0.4098(4) 1.1113(4) 0.0611(16) Uani 1 1 d . . .
H2 H 0.1407 0.3655 1.1329 0.073 Uiso 1 1 calc R . .
C3 C 0.1339(4) 0.4729(4) 1.1441(5) 0.076(2) Uani 1 1 d . . .
H3 H 0.1025 0.4708 1.1887 0.091 Uiso 1 1 calc R . .
C4 C 0.1541(5) 0.5400(4) 1.1153(5) 0.092(3) Uani 1 1 d . . .
H4 H 0.1354 0.5827 1.1386 0.110 Uiso 1 1 calc R . .
C5 C 0.2017(4) 0.5439(4) 1.0522(5) 0.073(2) Uani 1 1 d . . .
H5 H 0.2174 0.5896 1.0337 0.088 Uiso 1 1 calc R . .
C6 C 0.2280(3) 0.4794(3) 1.0141(4) 0.0474(14) Uani 1 1 d . . .
C7 C 0.2797(3) 0.4847(3) 0.9500(3) 0.0495(14) Uani 1 1 d . . .
H7 H 0.2921 0.5316 0.9319 0.059 Uiso 1 1 calc R . .
C8 C 0.3702(3) 0.4329(4) 0.8528(4) 0.0527(16) Uani 1 1 d . . .
H8 H 0.3870 0.4840 0.8490 0.063 Uiso 1 1 calc R . .
C9 C 0.4341(4) 0.3859(5) 0.8809(5) 0.074(2) Uani 1 1 d . . .
H9A H 0.4530 0.4059 0.9314 0.089 Uiso 1 1 calc R . .
H9B H 0.4161 0.3367 0.8921 0.089 Uiso 1 1 calc R . .
C10 C 0.4962(5) 0.3808(6) 0.8203(6) 0.100(3) Uani 1 1 d . . .
H10A H 0.5189 0.4287 0.8135 0.120 Uiso 1 1 calc R . .
H10B H 0.5333 0.3469 0.8400 0.120 Uiso 1 1 calc R . .
C11 C 0.4673(5) 0.3553(4) 0.7429(7) 0.104(3) Uani 1 1 d . . .
H11A H 0.4487 0.3056 0.7496 0.124 Uiso 1 1 calc R . .
H11B H 0.5069 0.3537 0.7034 0.124 Uiso 1 1 calc R . .
C12 C 0.4037(4) 0.4056(4) 0.7089(4) 0.0727(18) Uani 1 1 d . . .
H12A H 0.4226 0.4544 0.6976 0.087 Uiso 1 1 calc R . .
H12B H 0.3848 0.3850 0.6586 0.087 Uiso 1 1 calc R . .
C13 C 0.3424(3) 0.4101(3) 0.7721(4) 0.0547(16) Uani 1 1 d . . .
H13 H 0.3205 0.3611 0.7777 0.066 Uiso 1 1 calc R . .
C14 C 0.2236(4) 0.4376(3) 0.7127(4) 0.0635(18) Uani 1 1 d . . .
H14 H 0.2150 0.3873 0.7150 0.076 Uiso 1 1 calc R . .
C15 C 0.1674(4) 0.4810(4) 0.6767(4) 0.0574(17) Uani 1 1 d . . .
C16 C 0.1062(4) 0.4472(4) 0.6425(5) 0.078(2) Uani 1 1 d . . .
H16 H 0.1026 0.3962 0.6452 0.093 Uiso 1 1 calc R . .
C17 C 0.0527(5) 0.4843(6) 0.6062(5) 0.092(3) Uani 1 1 d . . .
H17 H 0.0137 0.4594 0.5821 0.111 Uiso 1 1 calc R . .
C18 C 0.0552(4) 0.5602(5) 0.6045(5) 0.078(2) Uani 1 1 d . . .
H18 H 0.0169 0.5867 0.5811 0.094 Uiso 1 1 calc R . .
C19 C 0.1160(4) 0.5974(4) 0.6380(4) 0.0635(18) Uani 1 1 d . . .
H19 H 0.1180 0.6484 0.6347 0.076 Uiso 1 1 calc R . .
C20 C 0.1728(3) 0.5603(3) 0.6758(3) 0.0498(14) Uani 1 1 d . . .
Cl1 Cl 0.10338(7) 0.10338(7) 1.0000 0.0636(6) Uani 1 2 d S . .
La1 La 0.215199(16) 0.215199(16) 1.0000 0.03951(15) Uani 1 2 d S . .
N1 N 0.3112(3) 0.4292(3) 0.9145(3) 0.0493(12) Uani 1 1 d . . .
N2 N 0.2856(3) 0.4602(2) 0.7426(3) 0.0495(10) Uani 1 1 d . . .
N3 N 0.2342(3) 0.2224(3) 0.8148(3) 0.0705(16) Uani 1 1 d . . .
O1 O 0.2321(2) 0.34906(18) 1.0147(2) 0.0485(9) Uani 1 1 d . . .
O2 O 0.2289(2) 0.5939(2) 0.7094(2) 0.0506(10) Uani 1 1 d . . .
O3 O 0.2397(2) 0.2790(2) 0.8560(2) 0.0621(12) Uani 1 1 d . A .
O5 O 0.2207(3) 0.1625(2) 0.8513(2) 0.0671(12) Uani 1 1 d . A .
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'
N N 0.0061 0.0033 '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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 C1 C2 123.5(5) . .
O1 C1 C6 120.7(5) . .
C2 C1 C6 115.8(5) . .
C3 C2 C1 121.8(7) . .
C3 C2 H2 119.1 . .
C1 C2 H2 119.1 . .
C2 C3 C4 123.0(7) . .
C2 C3 H3 118.5 . .
C4 C3 H3 118.5 . .
C5 C4 C3 119.2(7) . .
C5 C4 H4 120.4 . .
C3 C4 H4 120.4 . .
C4 C5 C6 120.9(7) . .
C4 C5 H5 119.6 . .
C6 C5 H5 119.6 . .
C5 C6 C7 119.9(5) . .
C5 C6 C1 119.4(5) . .
C7 C6 C1 120.6(5) . .
N1 C7 C6 125.0(5) . .
N1 C7 H7 117.5 . .
C6 C7 H7 117.5 . .
N1 C8 C13 110.8(5) . .
N1 C8 C9 108.8(5) . .
C13 C8 C9 112.1(6) . .
N1 C8 H8 108.4 . .
C13 C8 H8 108.4 . .
C9 C8 H8 108.4 . .
C10 C9 C8 114.1(6) . .
C10 C9 H9A 108.7 . .
C8 C9 H9A 108.7 . .
C10 C9 H9B 108.7 . .
C8 C9 H9B 108.7 . .
H9A C9 H9B 107.6 . .
C11 C10 C9 109.0(8) . .
C11 C10 H10A 109.9 . .
C9 C10 H10A 109.9 . .
C11 C10 H10B 109.9 . .
C9 C10 H10B 109.9 . .
H10A C10 H10B 108.3 . .
C10 C11 C12 113.0(7) . .
C10 C11 H11A 109.0 . .
C12 C11 H11A 109.0 . .
C10 C11 H11B 109.0 . .
C12 C11 H11B 109.0 . .
H11A C11 H11B 107.8 . .
C13 C12 C11 109.0(6) . .
C13 C12 H12A 109.9 . .
C11 C12 H12A 109.9 . .
C13 C12 H12B 109.9 . .
C11 C12 H12B 109.9 . .
H12A C12 H12B 108.3 . .
N2 C13 C8 111.3(5) . .
N2 C13 C12 109.0(5) . .
C8 C13 C12 112.1(5) . .
N2 C13 H13 108.1 . .
C8 C13 H13 108.1 . .
C12 C13 H13 108.1 . .
N2 C14 C15 127.4(6) . .
N2 C14 H14 116.3 . .
C15 C14 H14 116.3 . .
C16 C15 C14 119.9(6) . .
C16 C15 C20 119.5(7) . .
C14 C15 C20 120.6(6) . .
C17 C16 C15 122.9(8) . .
C17 C16 H16 118.5 . .
C15 C16 H16 118.5 . .
C16 C17 C18 119.6(8) . .
C16 C17 H17 120.2 . .
C18 C17 H17 120.2 . .
C17 C18 C19 119.9(8) . .
C17 C18 H18 120.1 . .
C19 C18 H18 120.1 . .
C20 C19 C18 121.9(7) . .
C20 C19 H19 119.1 . .
C18 C19 H19 119.1 . .
O2 C20 C19 122.9(6) . .
O2 C20 C15 120.9(6) . .
C19 C20 C15 116.2(6) . .
O1 La1 O1 76.34(17) . 7_557
O1 La1 O2 142.06(13) . 5_546
O1 La1 O2 74.72(12) 7_557 5_546
O1 La1 O2 74.72(12) . 4_455
O1 La1 O2 142.06(13) 7_557 4_455
O2 La1 O2 140.97(17) 5_546 4_455
O1 La1 O5 85.22(14) . 7_557
O1 La1 O5 116.53(12) 7_557 7_557
O2 La1 O5 86.24(14) 5_546 7_557
O2 La1 O5 84.91(14) 4_455 7_557
O1 La1 O5 116.53(12) . .
O1 La1 O5 85.22(14) 7_557 .
O2 La1 O5 84.91(14) 5_546 .
O2 La1 O5 86.24(14) 4_455 .
O5 La1 O5 153.3(2) 7_557 .
O1 La1 O3 72.24(13) . 7_557
O1 La1 O3 68.70(13) 7_557 7_557
O2 La1 O3 74.70(13) 5_546 7_557
O2 La1 O3 123.22(13) 4_455 7_557
O5 La1 O3 47.85(13) 7_557 7_557
O5 La1 O3 150.17(15) . 7_557
O1 La1 O3 68.70(13) . .
O1 La1 O3 72.24(13) 7_557 .
O2 La1 O3 123.22(13) 5_546 .
O2 La1 O3 74.70(13) 4_455 .
O5 La1 O3 150.17(15) 7_557 .
O5 La1 O3 47.85(13) . .
O3 La1 O3 129.69(19) 7_557 .
O1 La1 Cl1 141.83(8) . .
O1 La1 Cl1 141.83(8) 7_557 .
O2 La1 Cl1 70.49(9) 5_546 .
O2 La1 Cl1 70.49(9) 4_455 .
O5 La1 Cl1 76.64(10) 7_557 .
O5 La1 Cl1 76.64(10) . .
O3 La1 Cl1 115.15(10) 7_557 .
O3 La1 Cl1 115.15(10) . .
O1 La1 N3 77.65(15) . 7_557
O1 La1 N3 92.32(14) 7_557 7_557
O2 La1 N3 79.55(15) 5_546 7_557
O2 La1 N3 104.78(15) 4_455 7_557
O5 La1 N3 24.22(12) 7_557 7_557
O5 La1 N3 164.36(15) . 7_557
O3 La1 N3 23.63(13) 7_557 7_557
O3 La1 N3 145.32(16) . 7_557
Cl1 La1 N3 96.33(11) . 7_557
O1 La1 N3 92.32(14) . .
O1 La1 N3 77.65(15) 7_557 .
O2 La1 N3 104.78(15) 5_546 .
O2 La1 N3 79.55(15) 4_455 .
O5 La1 N3 164.36(15) 7_557 .
O5 La1 N3 24.22(12) . .
O3 La1 N3 145.32(16) 7_557 .
O3 La1 N3 23.63(13) . .
Cl1 La1 N3 96.33(11) . .
N3 La1 N3 167.3(2) 7_557 .
C7 N1 C8 126.3(5) . .
C14 N2 C13 122.9(5) . .
O3 N3 O5 118.2(4) . .
O3 N3 O4B 120.1(7) . .
O5 N3 O4B 119.4(7) . .
O3 N3 O4A 116.8(7) . .
O5 N3 O4A 122.2(7) . .
O4B N3 O4A 31.6(5) . .
O3 N3 La1 60.1(3) . .
O5 N3 La1 58.2(2) . .
O4B N3 La1 165.1(9) . .
O4A N3 La1 163.4(8) . .
C1 O1 La1 145.5(3) . .
C20 O2 La1 146.5(4) . 3_554
N3 O3 La1 96.3(3) . .
N3 O5 La1 97.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O4A N3 1.313(12) .
O4B N3 1.269(11) .
C1 O1 1.283(6) .
C1 C2 1.400(8) .
C1 C6 1.443(7) .
C2 C3 1.337(9) .
C2 H2 0.9300 .
C3 C4 1.358(10) .
C3 H3 0.9300 .
C4 C5 1.351(10) .
C4 H4 0.9300 .
C5 C6 1.412(8) .
C5 H5 0.9300 .
C6 C7 1.415(8) .
C7 N1 1.299(7) .
C7 H7 0.9300 .
C8 N1 1.476(8) .
C8 C13 1.477(9) .
C8 C9 1.514(8) .
C8 H8 0.9800 .
C9 C10 1.508(10) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C11 1.451(13) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 C12 1.575(10) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.525(9) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 N2 1.461(7) .
C13 H13 0.9800 .
C14 N2 1.296(8) .
C14 C15 1.419(9) .
C14 H14 0.9300 .
C15 C16 1.391(9) .
C15 C20 1.445(8) .
C16 C17 1.325(12) .
C16 H16 0.9300 .
C17 C18 1.381(12) .
C17 H17 0.9300 .
C18 C19 1.408(10) .
C18 H18 0.9300 .
C19 C20 1.380(9) .
C19 H19 0.9300 .
C20 O2 1.310(7) .
Cl1 La1 2.8747(19) .
La1 O1 2.465(3) .
La1 O1 2.465(3) 7_557
La1 O2 2.518(4) 5_546
La1 O2 2.518(4) 4_455
La1 O5 2.625(4) 7_557
La1 O5 2.625(4) .
La1 O3 2.671(4) 7_557
La1 O3 2.671(4) .
La1 N3 3.062(5) 7_557
La1 N3 3.062(5) .
N3 O3 1.235(6) .
N3 O5 1.267(6) .
O2 La1 2.518(4) 3_554
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.507 0.628 0.084 1782.9 21.0
