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#$Date: 2019-11-23 04:01:45 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232069 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/69/4346931.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_4346931
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 N3 O8 Sm Zn'
_chemical_formula_weight         642.08
_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                   11.3407(14)
_cell_length_b                   11.3407(14)
_cell_length_c                   27.565(7)
_cell_measurement_reflns_used    3473
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.08
_cell_measurement_theta_min      2.20
_cell_volume                     3070.2(9)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0748
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            22443
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.074
_exptl_absorpt_coefficient_mu    4.069
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.084
_exptl_crystal_description       Block
_exptl_crystal_F_000             1878
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 615 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0435P)²+3.5388P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0626
_reflns_Friedel_coverage         0.584
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1734
_reflns_number_total             1913
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02372_si_006.cif
_cod_data_source_block           5
_cod_original_cell_volume        3070.2(11)
_cod_original_sg_symbol_Hall     'P 61 2 (0 0 -1)'
_cod_database_code               4346931
_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   0.641
_shelx_estimated_absorpt_t_max   0.686
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
Sm1 Sm 0.83090(4) 0.0000 0.0000 0.01547(13) Uani 1 2 d S T P
Zn1 Zn 0.53986(12) -0.23007(6) 0.0833 0.0249(3) Uani 1 2 d S T P
O1 O 0.1394(5) -0.7037(5) -0.09522(15) 0.0295(11) Uani 1 1 d . . .
O2 O -0.0188(5) -0.7831(5) -0.03728(16) 0.0299(12) Uani 1 1 d . . .
O3 O 1.0319(5) 0.0553(5) 0.04668(17) 0.0423(15) Uani 1 1 d . . .
O4 O 0.6036(5) -0.1039(5) 0.03148(15) 0.0231(10) Uani 1 1 d . . .
N1 N 0.3926(6) -0.4053(6) 0.04374(18) 0.0293(14) Uani 1 1 d . . .
N2 N 1.5295(12) 0.2648(6) 0.0833 0.074(4) Uani 1 2 d S T P
C1 C 0.4211(8) -0.4126(9) -0.0024(3) 0.047(2) Uani 1 1 d . . .
H1A H 0.5060 -0.3486 -0.0145 0.057 Uiso 1 1 calc R U .
C2 C 0.3293(9) -0.5118(9) -0.0332(3) 0.046(2) Uani 1 1 d . . .
H2A H 0.3550 -0.5150 -0.0650 0.055 Uiso 1 1 calc R U .
C3 C 0.2017(7) -0.6054(6) -0.0182(2) 0.0231(15) Uani 1 1 d . . .
C4 C 0.1717(8) -0.5989(7) 0.0305(2) 0.0272(16) Uani 1 1 d . . .
H4A H 0.0870 -0.6610 0.0433 0.033 Uiso 1 1 calc R U .
C5 C 0.2686(9) -0.5002(7) 0.0590(3) 0.034(2) Uani 1 1 d . . .
H5A H 0.2474 -0.4982 0.0915 0.041 Uiso 1 1 calc R U .
C6 C 0.0993(6) -0.7069(7) -0.0529(2) 0.0216(15) Uani 1 1 d . . .
C7 C 1.0865(9) 0.0432(5) 0.0833 0.027(2) Uani 1 2 d S T P
C8 C 1.2442(9) 0.1221(5) 0.0833 0.029(2) Uani 1 2 d S T P
C9 C 1.3162(8) 0.1854(10) 0.0421(3) 0.045(2) Uani 1 1 d . . .
H9A H 1.2708 0.1795 0.0133 0.054 Uiso 1 1 calc R U .
C10 C 1.4570(10) 0.2580(10) 0.0438(4) 0.058(3) Uani 1 1 d . . .
H10A H 1.5041 0.3047 0.0162 0.069 Uiso 1 1 calc R U .
C11 C 0.5306(9) -0.0354(11) 0.0222(4) 0.063(3) Uani 1 1 d . . .
H11A H 0.4339 -0.1012 0.0221 0.076 Uiso 1 1 calc R U .
H11B H 0.5477 0.0286 0.0483 0.076 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'
Sm Sm -0.1638 3.4418 '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 Sm1 O4 67.9(2) . 8
O4 Sm1 O3 140.64(17) . 8
O4 Sm1 O3 125.37(16) 8 8
O4 Sm1 O3 125.37(16) . .
O4 Sm1 O3 140.64(17) 8 .
O3 Sm1 O3 70.8(3) 8 .
O4 Sm1 O2 133.88(17) . 1_665
O4 Sm1 O2 68.46(16) 8 1_665
O3 Sm1 O2 79.14(17) 8 1_665
O3 Sm1 O2 82.42(17) . 1_665
O4 Sm1 O2 68.46(16) . 8_545
O4 Sm1 O2 133.88(17) 8 8_545
O3 Sm1 O2 82.42(17) 8 8_545
O3 Sm1 O2 79.13(17) . 8_545
O2 Sm1 O2 157.3(2) 1_665 8_545
O4 Sm1 O1 80.49(16) . 10_554
O4 Sm1 O1 74.34(17) 8 10_554
O3 Sm1 O1 70.54(18) 8 10_554
O3 Sm1 O1 139.54(18) . 10_554
O2 Sm1 O1 101.56(15) 1_665 10_554
O2 Sm1 O1 84.42(16) 8_545 10_554
O4 Sm1 O1 74.34(17) . 6
O4 Sm1 O1 80.49(16) 8 6
O3 Sm1 O1 139.53(18) 8 6
O3 Sm1 O1 70.54(18) . 6
O2 Sm1 O1 84.42(16) 1_665 6
O2 Sm1 O1 101.56(15) 8_545 6
O1 Sm1 O1 149.6(2) 10_554 6
O4 Zn1 O4 141.4(3) . 12_545
O4 Zn1 N1 98.2(2) . .
O4 Zn1 N1 107.7(2) 12_545 .
O4 Zn1 N1 107.7(2) . 12_545
O4 Zn1 N1 98.2(2) 12_545 12_545
N1 Zn1 N1 95.3(3) . 12_545
C6 O1 Sm1 127.5(4) . 5_554
C6 O2 Sm1 144.7(5) . 1_445
C7 O3 Sm1 150.9(6) . .
C11 O4 Zn1 116.4(4) . .
C11 O4 Sm1 116.5(4) . .
Zn1 O4 Sm1 123.7(2) . .
C1 N1 C5 116.2(6) . .
C1 N1 Zn1 116.4(5) . .
C5 N1 Zn1 126.9(4) . .
C10 N2 C10 116.0(12) . 12_545
N1 C1 C2 122.2(7) . .
N1 C1 H1A 118.9 . .
C2 C1 H1A 118.9 . .
C3 C2 C1 121.6(7) . .
C3 C2 H2A 119.2 . .
C1 C2 H2A 119.2 . .
C2 C3 C4 116.3(6) . .
C2 C3 C6 121.0(6) . .
C4 C3 C6 122.6(6) . .
C5 C4 C3 118.7(7) . .
C5 C4 H4A 120.6 . .
C3 C4 H4A 120.6 . .
N1 C5 C4 124.8(6) . .
N1 C5 H5A 117.6 . .
C4 C5 H5A 117.6 . .
O1 C6 O2 126.2(6) . .
O1 C6 C3 116.4(6) . .
O2 C6 C3 117.3(6) . .
O3 C7 O3 128.2(10) . 12_545
O3 C7 C8 115.9(5) . .
O3 C7 C8 115.9(5) 12_545 .
C9 C8 C9 118.1(10) . 12_545
C9 C8 C7 121.0(5) . .
C9 C8 C7 121.0(5) 12_545 .
C8 C9 C10 119.3(8) . .
C8 C9 H9A 120.4 . .
C10 C9 H9A 120.4 . .
N2 C10 C9 123.6(9) . .
N2 C10 H10A 118.2 . .
C9 C10 H10A 118.2 . .
C11 C11 O4 113.1(6) 8 .
C11 C11 H11A 109.0 8 .
O4 C11 H11A 109.0 . .
C11 C11 H11B 109.0 8 .
O4 C11 H11B 109.0 . .
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
Sm1 O4 2.398(5) .
Sm1 O4 2.398(5) 8
Sm1 O3 2.411(5) 8
Sm1 O3 2.411(5) .
Sm1 O2 2.412(5) 1_665
Sm1 O2 2.412(5) 8_545
Sm1 O1 2.485(4) 10_554
Sm1 O1 2.485(4) 6
Zn1 O4 1.891(4) .
Zn1 O4 1.891(4) 12_545
Zn1 N1 2.148(6) .
Zn1 N1 2.148(6) 12_545
O1 C6 1.245(8) .
O1 Sm1 2.485(4) 5_554
O2 C6 1.253(8) .
O2 Sm1 2.412(5) 1_445
O3 C7 1.228(6) .
O4 C11 1.413(9) .
N1 C1 1.326(8) .
N1 C5 1.341(10) .
N2 C10 1.343(12) .
N2 C10 1.343(12) 12_545
C1 C2 1.377(10) .
C1 H1A 0.9300 .
C2 C3 1.362(10) .
C2 H2A 0.9300 .
C3 C4 1.396(9) .
C3 C6 1.502(9) .
C4 C5 1.359(10) .
C4 H4A 0.9300 .
C5 H5A 0.9300 .
C7 O3 1.228(6) 12_545
C7 C8 1.549(12) .
C8 C9 1.375(9) .
C8 C9 1.375(9) 12_545
C9 C10 1.384(12) .
C9 H9A 0.9300 .
C10 H10A 0.9300 .
C11 C11 1.410(16) 8
C11 H11A 0.9700 .
C11 H11B 0.9700 .
