#------------------------------------------------------------------------------
#$Date: 2019-11-23 07:47:30 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232471 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/77/4347729.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_4347729
loop_
_publ_author_name
'Wu, Jianfeng'
'Zhao, Lang'
'Zhang, Li'
'Li, Xiao-Lei'
'Guo, Mei'
'Tang, Jinkui'
_publ_section_title
;
 Metallosupramolecular Coordination Complexes: The Design of
 Heterometallic 3d-4f Gridlike Structures.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5514
_journal_page_last               5519
_journal_paper_doi               10.1021/acs.inorgchem.6b00529
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C88 H92 Dy4 N32 O32 S4 Zn4'
_chemical_formula_sum            'C88 H92 Dy4 N32 O32 S4 Zn4'
_chemical_formula_weight         3149.65
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0282(16)
_cell_length_b                   24.0282(16)
_cell_length_c                   34.364(2)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.84
_cell_measurement_theta_min      2.40
_cell_volume                     19840(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.812
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0917
_diffrn_reflns_av_unetI/netI     0.1153
_diffrn_reflns_Laue_measured_fraction_full 0.812
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            47083
_diffrn_reflns_point_group_measured_fraction_full 0.812
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.070
_diffrn_reflns_theta_min         1.034
_exptl_absorpt_coefficient_mu    2.054
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_description       block
_exptl_crystal_F_000             6192
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.994
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         8114
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1412
_refine_ls_R_factor_gt           0.0911
_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)+(0.1823P)²+42.8804P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2816
_refine_ls_wR_factor_ref         0.3122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4796
_reflns_number_total             8114
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b00529_si_002.cif
_cod_data_source_block           Dy4Zn4
_cod_original_cell_volume        19840(3)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4347729
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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
O5 O 0.6882(4) 0.6233(4) 0.4398(3) 0.050(2) Uani 1 1 d . .
H5D H 0.6552 0.6146 0.4387 0.060 Uiso 1 1 d R U
C1 C 0.6405(7) 0.5032(8) 0.4504(4) 0.062(5) Uani 1 1 d . .
H1A H 0.6219 0.5322 0.4651 0.074 Uiso 1 1 calc R U
H1B H 0.6158 0.4714 0.4488 0.074 Uiso 1 1 calc R U
C2 C 0.6909(7) 0.4875(6) 0.4699(4) 0.048(4) Uani 1 1 d . .
C3 C 0.6881(7) 0.4574(9) 0.5035(4) 0.063(5) Uani 1 1 d . .
H3 H 0.6541 0.4462 0.5137 0.076 Uiso 1 1 calc R U
C4 C 0.7404(9) 0.4434(8) 0.5228(5) 0.072(6) Uani 1 1 d . .
H4 H 0.7397 0.4259 0.5469 0.086 Uiso 1 1 calc R U
C5 C 0.7902(7) 0.4559(6) 0.5058(4) 0.048(3) Uani 1 1 d . .
H5 H 0.8240 0.4459 0.5170 0.057 Uiso 1 1 calc R U
C6 C 0.7875(6) 0.4849(6) 0.4701(4) 0.045(3) Uani 1 1 d . .
C7 C 0.8386(6) 0.4993(6) 0.4493(4) 0.041(3) Uani 1 1 d . .
H7 H 0.8737 0.4901 0.4587 0.049 Uiso 1 1 calc R U
C8 C 0.8667(6) 0.5646(6) 0.3630(4) 0.042(3) Uani 1 1 d . .
C9 C 0.9150(6) 0.5778(6) 0.3387(4) 0.042(3) Uani 1 1 d . .
C10 C 0.9111(6) 0.6128(6) 0.3061(4) 0.045(3) Uani 1 1 d . .
H10 H 0.8772 0.6274 0.2979 0.054 Uiso 1 1 calc R U
C11 C 0.9600(7) 0.6245(7) 0.2870(4) 0.060(4) Uani 1 1 d . .
H11 H 0.9591 0.6477 0.2653 0.072 Uiso 1 1 calc R U
C12 C 1.0113(6) 0.6024(7) 0.2992(5) 0.057(4) Uani 1 1 d . .
H12 H 1.0442 0.6113 0.2864 0.069 Uiso 1 1 calc R U
C13 C 1.0110(6) 0.5668(6) 0.3312(4) 0.043(3) Uani 1 1 d . .
C14 C 1.0593(6) 0.5377(6) 0.3459(3) 0.039(3) Uani 1 1 d . .
C15 C 0.7010(5) 0.6575(6) 0.3289(3) 0.036(3) Uani 1 1 d . .
H15 H 0.6937 0.6916 0.3172 0.043 Uiso 1 1 calc R U
C16 C 0.6802(5) 0.6033(6) 0.3128(3) 0.037(3) Uani 1 1 d . .
C17 C 0.6541(6) 0.6008(7) 0.2759(4) 0.047(3) Uani 1 1 d . .
H17 H 0.6487 0.6330 0.2613 0.056 Uiso 1 1 calc R U
C18 C 0.6379(6) 0.5524(6) 0.2627(4) 0.046(3) Uani 1 1 d . .
H18 H 0.6169 0.5501 0.2400 0.055 Uiso 1 1 calc R U
C19 C 0.6531(7) 0.5023(7) 0.2839(4) 0.053(4) Uani 1 1 d . .
H19 H 0.6442 0.4673 0.2741 0.064 Uiso 1 1 calc R U
C20 C 0.6803(6) 0.5075(7) 0.3179(4) 0.052(4) Uani 1 1 d . .
C21 C 0.7002(7) 0.4600(7) 0.3399(5) 0.053(4) Uani 1 1 d . .
H21A H 0.6694 0.4439 0.3542 0.063 Uiso 1 1 calc R U
H21B H 0.7141 0.4321 0.3220 0.063 Uiso 1 1 calc R U
C22 C 1.0063(7) 0.5613(7) 0.4744(4) 0.051(4) Uani 1 1 d . .
O6 O 0.9468(6) 0.4274(5) 0.3914(4) 0.071(3) Uani 1 1 d . .
H6D H 0.9507 0.3926 0.3916 0.085 Uiso 1 1 d R U
Dy1 Dy 0.74264(3) 0.56563(3) 0.39599(2) 0.0345(3) Uani 1 1 d . .
N1 N 0.7392(5) 0.5022(5) 0.4543(3) 0.040(3) Uani 1 1 d . .
N2 N 0.8315(5) 0.5258(5) 0.4168(3) 0.039(2) Uani 1 1 d . .
N3 N 0.8797(5) 0.5374(5) 0.3952(3) 0.040(3) Uani 1 1 d . .
N4 N 0.9628(4) 0.5557(4) 0.3503(2) 0.030(2) Uani 1 1 d . .
N5 N 1.0488(4) 0.5048(4) 0.3757(3) 0.034(2) Uani 1 1 d . .
N6 N 0.7291(4) 0.6529(5) 0.3594(3) 0.035(2) Uani 1 1 d . .
N7 N 0.6929(5) 0.5592(5) 0.3328(3) 0.037(2) Uani 1 1 d . .
N8 N 0.9857(5) 0.5392(5) 0.4491(3) 0.047(3) Uani 1 1 d . .
O1 O 0.6535(4) 0.5241(5) 0.4099(3) 0.054(3) Uani 1 1 d . .
H1D H 0.6309 0.5111 0.3945 0.080 Uiso 1 1 calc R U
O2 O 0.8167(4) 0.5763(4) 0.3524(2) 0.040(2) Uani 1 1 d . .
O3 O 1.1076(4) 0.5468(4) 0.3314(2) 0.0353(19) Uani 1 1 d . .
O4 O 0.7428(5) 0.4746(4) 0.3662(3) 0.051(2) Uani 1 1 d . .
H4D H 0.7414 0.4542 0.3853 0.061 Uiso 1 1 calc R U
S1 S 1.03724(19) 0.59427(19) 0.51053(11) 0.0601(11) Uani 1 1 d . .
Zn1 Zn 0.96433(6) 0.50625(6) 0.39880(4) 0.0345(4) Uani 1 1 d . .
O7 O 0.7149(7) 0.7217(7) 0.4791(5) 0.109(5) Uani 1 1 d . .
H7D H 0.6948 0.7089 0.4965 0.131 Uiso 1 1 d R U
H7E H 0.6995 0.7519 0.4709 0.131 Uiso 1 1 d R U
O8 O 0.5602(8) 0.5341(11) 0.3659(5) 0.140(7) Uani 1 1 d . U
H8D H 0.5606 0.4995 0.3683 0.168 Uiso 1 1 d R U
H8E H 0.5809 0.5430 0.3477 0.168 Uiso 1 1 d 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'
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'
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'
S S 0.1246 0.1234 '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
C2 C1 O1 110.1(13) . .
N1 C2 C3 121.8(15) . .
N1 C2 C1 118.6(13) . .
C3 C2 C1 119.6(14) . .
C2 C3 C4 117.8(15) . .
C5 C4 C3 120.5(14) . .
C4 C5 C6 116.1(15) . .
N1 C6 C5 122.8(14) . .
N1 C6 C7 117.0(12) . .
C5 C6 C7 120.1(14) . .
N2 C7 C6 115.2(13) . .
O2 C8 N3 124.4(14) . .
O2 C8 C9 122.0(12) . .
N3 C8 C9 113.5(12) . .
N4 C9 C10 122.4(13) . .
N4 C9 C8 115.3(12) . .
C10 C9 C8 122.3(12) . .
C11 C10 C9 116.6(13) . .
C10 C11 C12 121.9(13) . .
C13 C12 C11 117.7(14) . .
N4 C13 C12 120.3(13) . .
N4 C13 C14 114.9(11) . .
C12 C13 C14 124.8(13) . .
O3 C14 N5 125.2(12) . .
O3 C14 C13 120.5(12) . .
N5 C14 C13 114.1(12) . .
N6 C15 C16 114.3(11) . .
N7 C16 C17 122.9(13) . .
N7 C16 C15 115.8(10) . .
C17 C16 C15 120.9(12) . .
C18 C17 C16 118.7(14) . .
C17 C18 C19 119.2(12) . .
C20 C19 C18 118.7(14) . .
C19 C20 N7 121.0(15) . .
C19 C20 C21 122.6(15) . .
N7 C20 C21 116.3(13) . .
O4 C21 C20 112.2(12) . .
N8 C22 S1 178.7(15) . .
O2 Dy1 O3 73.1(3) . 11_676
O2 Dy1 O1 148.0(3) . .
O3 Dy1 O1 137.7(3) 11_676 .
O2 Dy1 O4 80.0(4) . .
O3 Dy1 O4 146.8(3) 11_676 .
O1 Dy1 O4 73.2(4) . .
O2 Dy1 O5 138.0(4) . .
O3 Dy1 O5 69.6(3) 11_676 .
O1 Dy1 O5 68.6(4) . .
O4 Dy1 O5 141.3(4) . .
O2 Dy1 N2 64.3(3) . .
O3 Dy1 N2 74.4(3) 11_676 .
O1 Dy1 N2 123.7(4) . .
O4 Dy1 N2 76.6(4) . .
O5 Dy1 N2 120.8(3) . .
O2 Dy1 N6 71.4(3) . .
O3 Dy1 N6 65.2(3) 11_676 .
O1 Dy1 N6 109.6(4) . .
O4 Dy1 N6 123.7(3) . .
O5 Dy1 N6 76.0(3) . .
N2 Dy1 N6 126.6(4) . .
O2 Dy1 N7 79.2(3) . .
O3 Dy1 N7 126.5(3) 11_676 .
O1 Dy1 N7 73.8(3) . .
O4 Dy1 N7 64.8(3) . .
O5 Dy1 N7 108.6(3) . .
N2 Dy1 N7 130.6(4) . .
N6 Dy1 N7 62.9(3) . .
O2 Dy1 N1 126.9(4) . .
O3 Dy1 N1 103.1(3) 11_676 .
O1 Dy1 N1 64.1(4) . .
O4 Dy1 N1 77.8(3) . .
O5 Dy1 N1 80.5(4) . .
N2 Dy1 N1 63.9(4) . .
N6 Dy1 N1 156.2(4) . .
N7 Dy1 N1 130.0(4) . .
C2 N1 C6 120.5(12) . .
C2 N1 Dy1 120.8(10) . .
C6 N1 Dy1 118.6(9) . .
C7 N2 N3 116.4(11) . .
C7 N2 Dy1 124.0(10) . .
N3 N2 Dy1 119.2(7) . .
C8 N3 N2 110.3(11) . .
C8 N3 Zn1 116.1(10) . .
N2 N3 Zn1 132.3(8) . .
C9 N4 C13 121.1(11) . .
C9 N4 Zn1 119.5(9) . .
C13 N4 Zn1 119.4(8) . .
C14 N5 N6 112.8(10) . 16_756
C14 N5 Zn1 116.8(9) . .
N6 N5 Zn1 129.9(7) 16_756 .
C15 N6 N5 117.8(11) . 11_676
C15 N6 Dy1 124.9(9) . .
N5 N6 Dy1 117.2(7) 11_676 .
C16 N7 C20 119.2(11) . .
C16 N7 Dy1 121.6(8) . .
C20 N7 Dy1 119.2(9) . .
C22 N8 Zn1 167.4(12) . .
C1 O1 Dy1 120.2(8) . .
C8 O2 Dy1 120.3(8) . .
C14 O3 Dy1 118.7(8) . 16_756
C21 O4 Dy1 119.7(9) . .
O6 Zn1 N8 124.0(5) . .
O6 Zn1 N4 116.8(5) . .
N8 Zn1 N4 119.1(5) . .
O6 Zn1 N3 97.1(5) . .
N8 Zn1 N3 99.0(5) . .
N4 Zn1 N3 74.7(4) . .
O6 Zn1 N5 97.9(5) . .
N8 Zn1 N5 94.8(5) . .
N4 Zn1 N5 74.3(4) . .
N3 Zn1 N5 149.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O5 Dy1 2.427(10) .
C1 C2 1.43(2) .
C1 O1 1.512(17) .
C2 N1 1.327(19) .
C2 C3 1.36(2) .
C3 C4 1.46(3) .
C4 C5 1.37(3) .
C5 C6 1.411(18) .
C6 N1 1.347(19) .
C6 C7 1.46(2) .
C7 N2 1.297(16) .
C8 O2 1.287(17) .
C8 N3 1.319(16) .
C8 C9 1.46(2) .
C9 N4 1.327(17) .
C9 C10 1.404(19) .
C10 C11 1.37(2) .
C11 C12 1.41(2) .
C12 C13 1.394(19) .
C13 N4 1.358(17) .
C13 C14 1.445(19) .
C14 O3 1.283(16) .
C14 N5 1.318(16) .
C15 N6 1.252(15) .
C15 C16 1.502(18) .
C16 N7 1.299(17) .
C16 C17 1.416(17) .
C17 C18 1.31(2) .
C18 C19 1.45(2) .
C19 C20 1.34(2) .
C20 N7 1.375(19) .
C20 C21 1.45(2) .
C21 O4 1.411(17) .
C22 N8 1.132(18) .
C22 S1 1.650(16) .
O6 Zn1 1.957(13) .
Dy1 O2 2.340(9) .
Dy1 O3 2.387(9) 11_676
Dy1 O1 2.411(10) .
Dy1 O4 2.414(11) .
Dy1 N2 2.446(11) .
Dy1 N6 2.467(11) .
Dy1 N7 2.484(10) .
Dy1 N1 2.519(10) .
N2 N3 1.404(16) .
N3 Zn1 2.171(12) .
N4 Zn1 2.048(9) .
N5 N6 1.410(15) 16_756
N5 Zn1 2.179(11) .
N6 N5 1.409(15) 11_676
N8 Zn1 1.970(12) .
O3 Dy1 2.387(9) 16_756
