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#$Date: 2019-11-23 04:02:01 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232070 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/69/4346932.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_4346932
loop_
_publ_author_name
'He, Xingxiang'
'Liu, Ying'
'Lv, Yun'
'Dong, Yayu'
'Hu, Gonghao'
'Zhou, Shuai'
'Xu, Yan'
_publ_section_title
;
 L- and D-[LnZn(IN)3(C2H4O2)]n (Ln = Eu, Sm, and Gd): Chiral
 Enantiomerically 3D 3d-4f Coordination Polymers Constructed by
 Interesting Butterfly-like Building Units and -[Ln-O-Zn]n- Helices.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2048
_journal_page_last               2054
_journal_paper_doi               10.1021/acs.inorgchem.5b02372
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C20 H16 Gd N3 O8 Zn'
_chemical_formula_weight         648.98
_space_group_crystal_system      hexagonal
_space_group_IT_number           178
_space_group_name_Hall           'P 61 2 (0 0 5)'
_space_group_name_H-M_alt        'P 61 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.3308(8)
_cell_length_b                   11.3308(8)
_cell_length_c                   27.468(4)
_cell_measurement_reflns_used    3462
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.21
_cell_volume                     3054.1(5)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            22159
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.485
_diffrn_reflns_theta_min         2.075
_exptl_absorpt_coefficient_mu    4.470
_exptl_absorpt_correction_T_max  0.6161
_exptl_absorpt_correction_T_min  0.5734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_description       Block
_exptl_crystal_F_000             1890
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 668 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0309P)²+5.1523P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0537
_reflns_Friedel_coverage         0.585
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1824
_reflns_number_total             1901
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02372_si_007.cif
_cod_data_source_block           6
_cod_original_cell_volume        3054.1(6)
_cod_original_sg_symbol_Hall     'P 61 2 (0 0 -1)'
_cod_database_code               4346932
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.573
_shelx_estimated_absorpt_t_max   0.616
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
'y, x, -z+1/3'
'x-y, -y, -z'
'-x, -x+y, -z+2/3'
'-y, -x, -z+5/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/6'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Gd1 Gd 0.83039(3) 0.0000 0.0000 0.01546(11) Uani 1 2 d S T P
Zn1 Zn 0.54052(10) -0.22974(5) 0.0833 0.0247(2) Uani 1 2 d S T P
O1 O 0.1373(4) -0.7056(4) -0.09557(14) 0.0286(9) Uani 1 1 d . . .
O2 O -0.0202(4) -0.7857(4) -0.03683(14) 0.0293(10) Uani 1 1 d . . .
O3 O 1.0311(5) 0.0552(5) 0.04651(16) 0.0430(13) Uani 1 1 d . . .
O4 O 0.6052(4) -0.1045(4) 0.03116(14) 0.0244(8) Uani 1 1 d . . .
N1 N 0.3931(5) -0.4060(5) 0.04382(16) 0.0292(12) Uani 1 1 d . . .
N2 N 1.5282(10) 0.2641(5) 0.0833 0.064(3) Uani 1 2 d S T P
C1 C 0.4197(7) -0.4141(8) -0.0023(2) 0.049(2) Uani 1 1 d . . .
H1A H 0.5045 -0.3499 -0.0144 0.058 Uiso 1 1 calc R U .
C2 C 0.3278(8) -0.5132(8) -0.0337(2) 0.050(2) Uani 1 1 d . . .
H2A H 0.3530 -0.5160 -0.0657 0.060 Uiso 1 1 calc R U .
C3 C 0.2012(6) -0.6064(6) -0.01792(19) 0.0240(13) Uani 1 1 d . . .
C4 C 0.1707(7) -0.6004(7) 0.0309(2) 0.0303(14) Uani 1 1 d . . .
H4A H 0.0862 -0.6626 0.0438 0.036 Uiso 1 1 calc R U .
C5 C 0.2687(8) -0.5007(6) 0.0590(2) 0.0358(17) Uani 1 1 d . . .
H5A H 0.2477 -0.4980 0.0916 0.043 Uiso 1 1 calc R U .
C6 C 0.0979(6) -0.7089(6) -0.0530(2) 0.0203(12) Uani 1 1 d . . .
C7 C 1.0850(8) 0.0425(4) 0.0833 0.0251(19) Uani 1 2 d S T P
C8 C 1.2412(9) 0.1206(4) 0.0833 0.0283(19) Uani 1 2 d S T P
C9 C 1.3149(7) 0.1849(8) 0.0417(3) 0.0407(18) Uani 1 1 d . . .
H9A H 1.2701 0.1793 0.0127 0.049 Uiso 1 1 calc R U .
C10 C 1.4558(8) 0.2573(9) 0.0438(3) 0.057(2) Uani 1 1 d . . .
H10A H 1.5032 0.3043 0.0161 0.068 Uiso 1 1 calc R U .
C11 C 0.5322(9) -0.0352(10) 0.0224(3) 0.066(3) Uani 1 1 d . . .
H11A H 0.4354 -0.1006 0.0226 0.079 Uiso 1 1 calc R U .
H11B H 0.5506 0.0293 0.0486 0.079 Uiso 1 1 calc R U .
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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
O4 Gd1 O4 68.5(2) 8 .
O4 Gd1 O2 68.35(15) 8 1_665
O4 Gd1 O2 134.49(15) . 1_665
O4 Gd1 O2 134.49(15) 8 8_545
O4 Gd1 O2 68.35(15) . 8_545
O2 Gd1 O2 156.8(2) 1_665 8_545
O4 Gd1 O3 125.46(15) 8 8
O4 Gd1 O3 140.27(16) . 8
O2 Gd1 O3 79.01(16) 1_665 8
O2 Gd1 O3 82.12(15) 8_545 8
O4 Gd1 O3 140.27(16) 8 .
O4 Gd1 O3 125.46(15) . .
O2 Gd1 O3 82.12(15) 1_665 .
O2 Gd1 O3 79.01(16) 8_545 .
O3 Gd1 O3 70.6(2) 8 .
O4 Gd1 O1 80.56(14) 8 6
O4 Gd1 O1 74.69(15) . 6
O2 Gd1 O1 84.59(14) 1_665 6
O2 Gd1 O1 101.44(13) 8_545 6
O3 Gd1 O1 139.29(16) 8 6
O3 Gd1 O1 70.42(16) . 6
O4 Gd1 O1 74.69(15) 8 10_554
O4 Gd1 O1 80.56(14) . 10_554
O2 Gd1 O1 101.44(13) 1_665 10_554
O2 Gd1 O1 84.59(14) 8_545 10_554
O3 Gd1 O1 70.42(16) 8 10_554
O3 Gd1 O1 139.29(16) . 10_554
O1 Gd1 O1 150.0(2) 6 10_554
O4 Zn1 O4 140.7(3) 12_545 .
O4 Zn1 N1 98.31(18) 12_545 12_545
O4 Zn1 N1 107.93(19) . 12_545
O4 Zn1 N1 107.93(19) 12_545 .
O4 Zn1 N1 98.30(18) . .
N1 Zn1 N1 95.4(3) 12_545 .
C6 O1 Gd1 128.0(4) . 5_554
C6 O2 Gd1 145.4(4) . 1_445
C7 O3 Gd1 150.5(5) . .
C11 O4 Zn1 115.5(4) . .
C11 O4 Gd1 116.3(4) . .
Zn1 O4 Gd1 124.4(2) . .
C1 N1 C5 115.4(5) . .
C1 N1 Zn1 116.9(4) . .
C5 N1 Zn1 127.1(4) . .
C10 N2 C10 115.9(10) . 12_545
N1 C1 C2 123.4(6) . .
N1 C1 H1A 118.3 . .
C2 C1 H1A 118.3 . .
C3 C2 C1 120.4(6) . .
C3 C2 H2A 119.8 . .
C1 C2 H2A 119.8 . .
C2 C3 C4 117.3(6) . .
C2 C3 C6 120.4(5) . .
C4 C3 C6 122.2(5) . .
C5 C4 C3 117.9(6) . .
C5 C4 H4A 121.1 . .
C3 C4 H4A 121.1 . .
N1 C5 C4 125.6(6) . .
N1 C5 H5A 117.2 . .
C4 C5 H5A 117.2 . .
O1 C6 O2 126.3(5) . .
O1 C6 C3 116.5(5) . .
O2 C6 C3 117.1(5) . .
O3 C7 O3 128.9(8) 12_545 .
O3 C7 C8 115.6(4) 12_545 .
O3 C7 C8 115.6(4) . .
C9 C8 C9 117.2(9) . 12_545
C9 C8 C7 121.4(4) . .
C9 C8 C7 121.4(4) 12_545 .
C10 C9 C8 119.3(7) . .
C10 C9 H9A 120.4 . .
C8 C9 H9A 120.4 . .
N2 C10 C9 124.1(8) . .
N2 C10 H10A 118.0 . .
C9 C10 H10A 118.0 . .
C11 C11 O4 112.5(6) 8 .
C11 C11 H11A 109.1 8 .
O4 C11 H11A 109.1 . .
C11 C11 H11B 109.1 8 .
O4 C11 H11B 109.1 . .
H11A C11 H11B 107.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 O4 2.372(4) 8
Gd1 O4 2.372(4) .
Gd1 O2 2.382(4) 1_665
Gd1 O2 2.382(4) 8_545
Gd1 O3 2.402(4) 8
Gd1 O3 2.402(4) .
Gd1 O1 2.456(4) 6
Gd1 O1 2.456(4) 10_554
Zn1 O4 1.888(4) 12_545
Zn1 O4 1.888(4) .
Zn1 N1 2.149(5) 12_545
Zn1 N1 2.149(5) .
O1 C6 1.247(7) .
O1 Gd1 2.456(4) 5_554
O2 C6 1.257(7) .
O2 Gd1 2.382(4) 1_445
O3 C7 1.227(5) .
O4 C11 1.416(8) .
N1 C1 1.315(8) .
N1 C5 1.342(9) .
N2 C10 1.339(10) .
N2 C10 1.339(10) 12_545
C1 C2 1.386(9) .
C1 H1A 0.9300 .
C2 C3 1.358(9) .
C2 H2A 0.9300 .
C3 C4 1.394(8) .
C3 C6 1.512(8) .
C4 C5 1.362(9) .
C4 H4A 0.9300 .
C5 H5A 0.9300 .
C7 O3 1.227(5) 12_545
C7 C8 1.532(11) .
C8 C9 1.389(8) .
C8 C9 1.389(8) 12_545
C9 C10 1.384(10) .
C9 H9A 0.9300 .
C10 H10A 0.9300 .
C11 C11 1.412(15) 8
C11 H11A 0.9700 .
C11 H11B 0.9700 .
