#------------------------------------------------------------------------------
#$Date: 2015-12-04 14:46:28 +0100 (vie 04 de dic de 2015) $
#$Revision: 170729 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/81/7118123.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_7118123
loop_
_publ_author_name
'Jianfeng Wu'
'Lang Zhao'
'Mei Guo'
'Jinkui Tang'
_publ_section_title
;
 Constructing supramolecular grids: from 4f square to 3d-4f grid
;
_journal_name_full               Chem.Commun.
_journal_page_first              17317
_journal_paper_doi               10.1039/C5cc06960B
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C76 H76 Cl12 Dy4 N28 O16'
_chemical_formula_weight         2713.04
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n'
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-07-28 deposited with the CCDC.
2015-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.9388(14)
_cell_length_b                   21.9388(14)
_cell_length_c                   16.3350(11)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.34
_cell_measurement_theta_min      2.42
_cell_volume                     7862.2(9)
_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      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0795
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49144
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.148
_diffrn_reflns_theta_min         1.554
_exptl_absorpt_coefficient_mu    2.130
_exptl_absorpt_correction_T_max  0.639
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.229
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         7803
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.0817
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1854P)²+24.3332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2662
_refine_ls_wR_factor_ref         0.3436
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                3872
_reflns_number_total             7803
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5cc06960b2_a.cif
_cod_data_source_block           Dy4L4Cl
_cod_original_cell_volume        7862.2(11)
_cod_database_code               7118123
_audit_block_doi                 10.5517/cc1jhxlj
_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+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6545(7) 0.3671(7) 0.0478(11) 0.114(5) Uani 1 1 d . U . . .
H1 H 0.6785 0.3928 0.0798 0.137 Uiso 1 1 calc R U . . .
C2 C 0.6579(8) 0.3714(8) -0.0363(11) 0.116(5) Uani 1 1 d . U . . .
H2 H 0.6854 0.3978 -0.0610 0.139 Uiso 1 1 calc R U . . .
C3 C 0.6237(10) 0.3394(10) -0.0779(15) 0.143(7) Uani 1 1 d . U . . .
H3 H 0.6245 0.3455 -0.1342 0.172 Uiso 1 1 calc R U . . .
C4 C 0.5827(7) 0.2935(8) -0.0475(10) 0.113(5) Uani 1 1 d . U . . .
H4 H 0.5589 0.2683 -0.0804 0.136 Uiso 1 1 calc R U . . .
C5 C 0.5832(7) 0.2916(7) 0.0389(9) 0.090(4) Uani 1 1 d . U . . .
C6 C 0.5461(6) 0.2461(6) 0.0788(8) 0.089(4) Uani 1 1 d . . . . .
H6 H 0.5236 0.2176 0.0495 0.107 Uiso 1 1 calc R U . . .
C7 C 0.5086(5) 0.2155(5) 0.2790(7) 0.062(3) Uani 1 1 d . . . . .
C8 C 0.4717(5) 0.1714(6) 0.3270(7) 0.072(3) Uani 1 1 d . . . . .
C9 C 0.4604(7) 0.1829(7) 0.4063(9) 0.102(4) Uani 1 1 d . U . . .
H9 H 0.4771 0.2170 0.4314 0.123 Uiso 1 1 calc R U . . .
C10 C 0.4244(8) 0.1444(8) 0.4494(11) 0.125(5) Uani 1 1 d . U . . .
H10 H 0.4145 0.1526 0.5037 0.151 Uiso 1 1 calc R U . . .
C11 C 0.4026(8) 0.0924(8) 0.4110(10) 0.122(5) Uani 1 1 d . U . . .
H11 H 0.3788 0.0641 0.4386 0.146 Uiso 1 1 calc R U . . .
C12 C 0.4179(6) 0.0848(6) 0.3300(7) 0.082(3) Uani 1 1 d . . . . .
C13 C 0.6752(7) 0.3123(6) 0.4272(9) 0.092(4) Uani 1 1 d . U . . .
H13 H 0.7051 0.2965 0.3929 0.111 Uiso 1 1 calc R U . . .
C14 C 0.6843(8) 0.3105(8) 0.5098(12) 0.118(5) Uani 1 1 d . U . . .
H14 H 0.7187 0.2912 0.5308 0.141 Uiso 1 1 calc R U . . .
C15 C 0.6447(8) 0.3361(7) 0.5602(10) 0.106(5) Uani 1 1 d . U . . .
H15 H 0.6515 0.3368 0.6164 0.127 Uiso 1 1 calc R U . . .
C16 C 0.5905(7) 0.3630(7) 0.5256(11) 0.109(5) Uani 1 1 d . U . . .
H16 H 0.5613 0.3804 0.5594 0.130 Uiso 1 1 calc R U . . .
C17 C 0.5829(6) 0.3625(6) 0.4455(9) 0.085(3) Uani 1 1 d . U . . .
C18 C 0.5305(6) 0.3876(6) 0.4054(9) 0.092(4) Uani 1 1 d . . . . .
H18 H 0.5010 0.4077 0.4361 0.111 Uiso 1 1 calc R U . . .
C19 C 0.4717(6) 0.3951(6) 0.2118(9) 0.081(3) Uani 1 1 d . . . . .
Cl1 Cl 0.66646(15) 0.22209(15) 0.25160(18) 0.0791(9) Uani 1 1 d . . . . .
Cl2 Cl 0.4767(3) 0.1027(2) 0.0763(3) 0.145(2) Uani 1 1 d . U . . .
Dy1 Dy 0.60167(3) 0.32697(3) 0.24120(4) 0.0723(3) Uani 1 1 d . . . . .
N1 N 0.6174(5) 0.3268(5) 0.0846(8) 0.088(3) Uani 1 1 d . U . . .
N2 N 0.5461(4) 0.2475(4) 0.1574(6) 0.071(2) Uani 1 1 d . . . . .
N3 N 0.5123(4) 0.2059(4) 0.1983(6) 0.070(2) Uani 1 1 d . . . . .
H3A H 0.4947 0.1758 0.1744 0.084 Uiso 1 1 calc R U . . .
N4 N 0.4509(4) 0.1233(5) 0.2880(6) 0.073(2) Uani 1 1 d . . . . .
N5 N 0.6251(5) 0.3358(4) 0.3941(7) 0.082(3) Uani 1 1 d . . . . .
N6 N 0.5240(5) 0.3830(4) 0.3307(7) 0.078(3) Uani 1 1 d . . . . .
N7 N 0.4751(5) 0.4062(5) 0.2925(7) 0.078(3) Uani 1 1 d . . . . .
H7 H 0.4477 0.4268 0.3181 0.094 Uiso 1 1 calc R U . . .
O1 O 0.5338(4) 0.2591(4) 0.3138(5) 0.078(2) Uani 1 1 d . . . . .
O2 O 0.5112(4) 0.3663(4) 0.1754(5) 0.089(2) Uani 1 1 d . U . . .
O3 O 0.6174(5) 0.4344(5) 0.2283(7) 0.128(4) Uani 1 1 d . U . . .
H3B H 0.6015 0.4365 0.1816 0.193 Uiso 1 1 d R U . . .
H3C H 0.6141 0.4706 0.2465 0.193 Uiso 1 1 d R U . . .
O4 O 0.7080(4) 0.3497(5) 0.2366(6) 0.105(3) Uani 1 1 d . U . . .
H4A H 0.7047 0.3464 0.1848 0.157 Uiso 1 1 d R U . . .
H4B H 0.7102 0.3882 0.2414 0.157 Uiso 1 1 d R U . . .
Cl3 Cl 0.7564(6) 0.4728(5) 0.2288(7) 0.300(6) Uani 1 1 d . 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'
Dy Dy -0.1892 4.4098 '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
N1 C1 C2 121.5(18) . .
C3 C2 C1 118.6(19) . .
C2 C3 C4 126(2) . .
C5 C4 C3 111.1(18) . .
N1 C5 C4 123.9(15) . .
N1 C5 C6 118.2(13) . .
C4 C5 C6 117.8(16) . .
N2 C6 C5 115.7(14) . .
O1 C7 N3 122.9(10) . .
O1 C7 C8 120.3(10) . .
N3 C7 C8 116.8(10) . .
N4 C8 C9 123.6(12) . .
N4 C8 C7 117.2(10) . .
C9 C8 C7 119.2(11) . .
C8 C9 C10 119.5(15) . .
C9 C10 C11 118.6(16) . .
C12 C11 C10 116.8(15) . .
N4 C12 C11 124.2(13) . .
N4 C12 C19 118.7(11) . 7_566
C11 C12 C19 117.1(12) . 7_566
N5 C13 C14 122.3(16) . .
C15 C14 C13 120.5(17) . .
C14 C15 C16 118.1(16) . .
C17 C16 C15 119.4(16) . .
C16 C17 N5 121.4(14) . .
C16 C17 C18 123.5(15) . .
N5 C17 C18 115.0(13) . .
N6 C18 C17 120.9(13) . .
O2 C19 N7 121.9(12) . .
O2 C19 C12 122.4(13) . 8_656
N7 C19 C12 115.6(10) . 8_656
O4 Dy1 O3 69.5(4) . .
O4 Dy1 O1 138.3(3) . .
O3 Dy1 O1 137.7(3) . .
O4 Dy1 O2 135.6(3) . .
O3 Dy1 O2 74.2(4) . .
O1 Dy1 O2 86.1(3) . .
O4 Dy1 N2 126.7(3) . .
O3 Dy1 N2 134.5(4) . .
O1 Dy1 N2 62.8(3) . .
O2 Dy1 N2 67.0(3) . .
O4 Dy1 N5 79.5(4) . .
O3 Dy1 N5 89.0(4) . .
O1 Dy1 N5 72.0(3) . .
O2 Dy1 N5 124.9(3) . .
N2 Dy1 N5 132.6(3) . .
O4 Dy1 N6 124.6(3) . .
O3 Dy1 N6 70.9(4) . .
O1 Dy1 N6 66.8(3) . .
O2 Dy1 N6 62.3(3) . .
N2 Dy1 N6 108.6(3) . .
N5 Dy1 N6 62.6(3) . .
O4 Dy1 N1 80.7(4) . .
O3 Dy1 N1 84.0(4) . .
O1 Dy1 N1 124.6(3) . .
O2 Dy1 N1 70.7(3) . .
N2 Dy1 N1 61.8(4) . .
N5 Dy1 N1 160.3(4) . .
N6 Dy1 N1 131.0(3) . .
O4 Dy1 Cl1 70.5(3) . .
O3 Dy1 Cl1 140.0(3) . .
O1 Dy1 Cl1 76.6(2) . .
O2 Dy1 Cl1 139.6(2) . .
N2 Dy1 Cl1 72.6(2) . .
N5 Dy1 Cl1 84.1(2) . .
N6 Dy1 Cl1 136.2(3) . .
N1 Dy1 Cl1 89.5(2) . .
C5 N1 C1 118.7(14) . .
C5 N1 Dy1 119.3(9) . .
C1 N1 Dy1 121.5(12) . .
C6 N2 N3 118.5(11) . .
C6 N2 Dy1 123.9(9) . .
N3 N2 Dy1 117.5(7) . .
C7 N3 N2 114.5(9) . .
C12 N4 C8 117.2(11) . .
C13 N5 C17 118.2(13) . .
C13 N5 Dy1 122.3(10) . .
C17 N5 Dy1 119.4(8) . .
C18 N6 N7 121.4(12) . .
C18 N6 Dy1 121.9(9) . .
N7 N6 Dy1 116.7(8) . .
N6 N7 C19 115.6(10) . .
C7 O1 Dy1 121.7(7) . .
C19 O2 Dy1 123.3(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.346(18) .
C1 C2 1.38(2) .
C2 C3 1.23(2) .
C3 C4 1.44(3) .
C4 C5 1.41(2) .
C5 N1 1.310(19) .
C5 C6 1.445(18) .
C6 N2 1.285(15) .
C7 O1 1.243(13) .
C7 N3 1.337(14) .
C7 C8 1.484(16) .
C8 N4 1.315(14) .
C8 C9 1.343(17) .
C9 C10 1.35(2) .
C10 C11 1.39(2) .
C11 C12 1.375(19) .
C12 N4 1.307(14) .
C12 C19 1.501(18) 7_566
C13 N5 1.328(16) .
C13 C14 1.36(2) .
C14 C15 1.32(2) .
C15 C16 1.44(2) .
C16 C17 1.32(2) .
C17 N5 1.380(18) .
C17 C18 1.433(17) .
C18 N6 1.232(16) .
C19 O2 1.226(14) .
C19 N7 1.343(17) .
C19 C12 1.501(18) 8_656
Cl1 Dy1 2.710(3) .
Dy1 O4 2.387(9) .
Dy1 O3 2.392(11) .
Dy1 O1 2.416(8) .
Dy1 O2 2.416(9) .
Dy1 N2 2.530(10) .
Dy1 N5 2.558(12) .
Dy1 N6 2.559(11) .
Dy1 N1 2.581(12) .
N2 N3 1.352(12) .
N6 N7 1.341(13) .
