#------------------------------------------------------------------------------
#$Date: 2017-04-13 04:57:16 +0300 (Thu, 13 Apr 2017) $
#$Revision: 195397 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/80/7228062.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_7228062
loop_
_publ_author_name
'Li, Zhongyi'
'Zhang, Chi'
'Zhai, Bin'
'Han, Jing-Cheng'
'Pei, Meng-Chun'
'Zhang, Jian-Jun'
'Zhang, Fuli'
'Li, Suzhi'
'Cao, Guangxiu'
_publ_section_title
;
 Linking heterometallic Cu-Ln chain unit with 2-methylenesuccinate bridge
 to form 2D network exhibiting large magnetocaloric effect
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00356K
_journal_year                    2017
_chemical_formula_sum            'C20 H32 Cu O24 Tb2'
_chemical_formula_weight         1037.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-02-14 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                109.296(2)
_cell_angle_beta                 99.958(2)
_cell_angle_gamma                98.927(2)
_cell_formula_units_Z            1
_cell_length_a                   6.9630(4)
_cell_length_b                   10.5852(5)
_cell_length_c                   11.4644(6)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      3.05
_cell_volume                     764.74(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26211
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.051
_exptl_absorpt_coefficient_mu    5.363
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.254
_exptl_crystal_description       block
_exptl_crystal_F_000             503
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.264
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2689
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0229
_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)+(0.0355P)²+3.5799P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2607
_reflns_number_total             2689
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce00356k2.cif
_cod_data_source_block           1_a
_cod_database_code               7228062
_shelx_shelxl_version_number     2016/6
_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, -y, -z'
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
Tb1 Tb 0.64102(3) 0.70710(2) 0.09937(2) 0.01415(9) Uani 1 1 d . . .
Cu1 Cu 1.000000 1.000000 0.500000 0.01979(17) Uani 1 2 d S . P
O1 O 0.7313(5) 0.7455(4) 0.3197(3) 0.0276(7) Uani 1 1 d . . .
O2 O 0.7808(5) 0.8799(4) 0.5205(3) 0.0285(7) Uani 1 1 d . . .
O3 O 0.2351(6) 0.8082(4) 0.3730(3) 0.0343(8) Uani 1 1 d . . .
O4 O 0.1885(5) 0.9043(4) 0.5662(3) 0.0271(7) Uani 1 1 d . . .
O5 O 0.6138(4) 0.4746(3) 0.0939(3) 0.0199(6) Uani 1 1 d . . .
O6 O 0.6402(5) 0.2626(3) 0.0554(3) 0.0237(7) Uani 1 1 d . . .
O7 O 1.1359(5) 0.3989(3) 0.0336(3) 0.0262(7) Uani 1 1 d . . .
O8 O 1.2312(5) 0.2222(3) 0.0625(3) 0.0253(7) Uani 1 1 d . . .
O9 O 0.9712(5) 0.8553(4) 0.1976(3) 0.0273(7) Uani 1 1 d D . .
H9B H 1.044(7) 0.888(6) 0.157(5) 0.033 Uiso 1 1 d D U .
H9A H 1.054(7) 0.845(6) 0.255(4) 0.033 Uiso 1 1 d D U .
O10 O 0.6009(6) 0.9340(4) 0.1851(4) 0.0373(9) Uani 1 1 d D . .
H10D H 0.495(6) 0.960(6) 0.166(5) 0.045 Uiso 1 1 d D U .
H10C H 0.657(8) 0.979(6) 0.263(2) 0.045 Uiso 1 1 d D U .
O11 O 0.3326(5) 0.6671(3) 0.1571(3) 0.0258(7) Uani 1 1 d D . .
H11A H 0.303(8) 0.708(5) 0.226(3) 0.031 Uiso 1 1 d D U .
H11B H 0.246(7) 0.593(4) 0.125(5) 0.031 Uiso 1 1 d D U .
O12 O 0.2387(5) 0.9711(4) 0.0833(4) 0.0321(8) Uani 1 1 d D . .
H12B H 0.251(9) 0.926(6) 0.009(3) 0.038 Uiso 1 1 d D U .
H12A H 0.228(9) 1.038(4) 0.060(6) 0.038 Uiso 1 1 d D U .
C1 C 0.6884(6) 0.7751(5) 0.4251(4) 0.0180(8) Uani 1 1 d . . .
C2 C 0.5247(7) 0.6796(5) 0.4466(4) 0.0245(10) Uani 1 1 d . . .
H2A H 0.431144 0.625508 0.365408 0.029 Uiso 1 1 calc R U .
H2B H 0.583933 0.616605 0.478267 0.029 Uiso 1 1 calc R U .
C3 C 0.4099(7) 0.7514(5) 0.5387(5) 0.0256(10) Uani 1 1 d . . .
C4 C 0.2687(6) 0.8262(5) 0.4877(4) 0.0216(9) Uani 1 1 d . . .
C5 C 0.4170(12) 0.7371(9) 0.6480(8) 0.066(2) Uani 1 1 d . . .
H5A H 0.494518 0.681323 0.671363 0.080 Uiso 1 1 calc R U .
H5B H 0.344536 0.782741 0.702639 0.080 Uiso 1 1 calc R U .
C6 C 0.7094(6) 0.3874(4) 0.1156(4) 0.0161(8) Uani 1 1 d . . .
C7 C 0.9049(7) 0.4384(5) 0.2161(4) 0.0257(10) Uani 1 1 d . . .
H7A H 0.977978 0.522718 0.213258 0.031 Uiso 1 1 calc R U .
H7B H 0.876257 0.459507 0.299425 0.031 Uiso 1 1 calc R U .
C8 C 1.0346(7) 0.3355(5) 0.1988(4) 0.0264(10) Uani 1 1 d . . .
C9 C 1.1388(6) 0.3166(4) 0.0920(4) 0.0185(8) Uani 1 1 d . . .
C10 C 1.0616(9) 0.2659(8) 0.2729(6) 0.0507(17) Uani 1 1 d . . .
H10A H 1.145264 0.204657 0.259633 0.061 Uiso 1 1 calc R U .
H10B H 0.997172 0.277470 0.339092 0.061 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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
O10 Tb1 O11 79.45(14) . .
O10 Tb1 O1 80.28(13) . .
O11 Tb1 O1 74.99(11) . .
O10 Tb1 O9 72.58(13) . .
O11 Tb1 O9 137.35(11) . .
O1 Tb1 O9 69.12(11) . .
O10 Tb1 O5 153.00(13) . .
O11 Tb1 O5 78.91(11) . .
O1 Tb1 O5 78.67(11) . .
O9 Tb1 O5 114.61(11) . .
O10 Tb1 O8 85.89(13) . 2_765
O11 Tb1 O8 138.25(11) . 2_765
O1 Tb1 O8 140.51(11) . 2_765
O9 Tb1 O8 71.46(11) . 2_765
O5 Tb1 O8 121.09(10) . 2_765
O10 Tb1 O7 133.08(13) . 2_765
O11 Tb1 O7 145.11(11) . 2_765
O1 Tb1 O7 117.03(11) . 2_765
O9 Tb1 O7 74.33(12) . 2_765
O5 Tb1 O7 72.38(10) . 2_765
O8 Tb1 O7 52.23(10) 2_765 2_765
O10 Tb1 O6 71.81(11) . 2_665
O11 Tb1 O6 69.40(11) . 2_665
O1 Tb1 O6 137.84(11) . 2_665
O9 Tb1 O6 127.65(11) . 2_665
O5 Tb1 O6 114.66(10) . 2_665
O8 Tb1 O6 68.90(10) 2_765 2_665
O7 Tb1 O6 105.10(11) 2_765 2_665
O10 Tb1 O5 121.50(11) . 2_665
O11 Tb1 O5 71.80(10) . 2_665
O1 Tb1 O5 134.87(10) . 2_665
O9 Tb1 O5 150.79(11) . 2_665
O5 Tb1 O5 65.73(11) . 2_665
O8 Tb1 O5 83.55(10) 2_765 2_665
O7 Tb1 O5 78.49(10) 2_765 2_665
O6 Tb1 O5 50.74(9) 2_665 2_665
O10 Tb1 C9 110.10(14) . 2_765
O11 Tb1 C9 150.04(11) . 2_765
O1 Tb1 C9 133.69(11) . 2_765
O9 Tb1 C9 71.56(12) . 2_765
O5 Tb1 C9 96.68(11) . 2_765
O8 Tb1 C9 26.03(11) 2_765 2_765
O7 Tb1 C9 26.21(12) 2_765 2_765
O6 Tb1 C9 86.28(11) 2_665 2_765
O5 Tb1 C9 79.34(11) 2_665 2_765
O10 Tb1 C6 95.83(12) . 2_665
O11 Tb1 C6 66.43(11) . 2_665
O1 Tb1 C6 141.23(11) . 2_665
O9 Tb1 C6 146.59(11) . 2_665
O5 Tb1 C6 90.13(11) . 2_665
O8 Tb1 C6 76.61(11) 2_765 2_665
O7 Tb1 C6 93.86(11) 2_765 2_665
O6 Tb1 C6 24.98(11) 2_665 2_665
O5 Tb1 C6 25.91(11) 2_665 2_665
C9 Tb1 C6 84.09(11) 2_765 2_665
O2 Cu1 O2 180.0 2_776 .
O2 Cu1 O4 89.62(14) 2_776 2_676
O2 Cu1 O4 90.38(14) . 2_676
O2 Cu1 O4 90.38(14) 2_776 1_655
O2 Cu1 O4 89.62(14) . 1_655
O4 Cu1 O4 180.0 2_676 1_655
C1 O1 Tb1 149.8(3) . .
C1 O2 Cu1 117.3(3) . .
C4 O4 Cu1 117.9(3) . 1_455
C6 O5 Tb1 145.6(3) . .
C6 O5 Tb1 93.5(2) . 2_665
Tb1 O5 Tb1 114.27(11) . 2_665
C6 O6 Tb1 95.2(2) . 2_665
C9 O7 Tb1 93.0(3) . 2_765
C9 O8 Tb1 94.5(2) . 2_765
Tb1 O9 H9B 124(4) . .
Tb1 O9 H9A 123(4) . .
H9B O9 H9A 104(6) . .
Tb1 O10 H10D 125(4) . .
Tb1 O10 H10C 117(4) . .
H10D O10 H10C 109(3) . .
Tb1 O11 H11A 129(4) . .
Tb1 O11 H11B 125(4) . .
H11A O11 H11B 103(6) . .
H12B O12 H12A 89(6) . .
O1 C1 O2 123.5(4) . .
O1 C1 C2 120.6(4) . .
O2 C1 C2 115.8(4) . .
C3 C2 C1 114.5(4) . .
C3 C2 H2A 108.6 . .
C1 C2 H2A 108.6 . .
C3 C2 H2B 108.6 . .
C1 C2 H2B 108.6 . .
H2A C2 H2B 107.6 . .
C5 C3 C2 122.1(5) . .
C5 C3 C4 122.8(5) . .
C2 C3 C4 114.7(4) . .
O3 C4 O4 123.4(4) . .
O3 C4 C3 119.0(4) . .
O4 C4 C3 117.6(4) . .
C3 C5 H5A 120.0 . .
C3 C5 H5B 120.0 . .
H5A C5 H5B 120.0 . .
O6 C6 O5 119.9(4) . .
O6 C6 C7 120.7(4) . .
O5 C6 C7 119.3(4) . .
O6 C6 Tb1 59.9(2) . 2_665
O5 C6 Tb1 60.6(2) . 2_665
C7 C6 Tb1 173.3(3) . 2_665
C8 C7 C6 112.8(4) . .
C8 C7 H7A 109.0 . .
C6 C7 H7A 109.0 . .
C8 C7 H7B 109.0 . .
C6 C7 H7B 109.0 . .
H7A C7 H7B 107.8 . .
C10 C8 C9 119.9(5) . .
C10 C8 C7 123.0(5) . .
C9 C8 C7 117.1(4) . .
O8 C9 O7 120.2(4) . .
O8 C9 C8 120.7(4) . .
O7 C9 C8 119.0(4) . .
O8 C9 Tb1 59.5(2) . 2_765
O7 C9 Tb1 60.8(2) . 2_765
C8 C9 Tb1 176.3(3) . 2_765
C8 C10 H10A 120.0 . .
C8 C10 H10B 120.0 . .
H10A C10 H10B 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O10 2.357(3) .
Tb1 O11 2.372(3) .
Tb1 O1 2.373(3) .
Tb1 O9 2.415(3) .
Tb1 O5 2.418(3) .
Tb1 O8 2.466(3) 2_765
Tb1 O7 2.495(3) 2_765
Tb1 O6 2.541(3) 2_665
Tb1 O5 2.554(3) 2_665
Tb1 C9 2.854(4) 2_765
Tb1 C6 2.926(4) 2_665
Cu1 O2 1.929(3) 2_776
Cu1 O2 1.929(3) .
Cu1 O4 1.975(3) 2_676
Cu1 O4 1.975(3) 1_655
O1 C1 1.246(5) .
O2 C1 1.255(6) .
O3 C4 1.238(6) .
O4 C4 1.277(6) .
O5 C6 1.281(5) .
O6 C6 1.241(5) .
O7 C9 1.263(5) .
O8 C9 1.257(5) .
O9 H9B 0.85(2) .
O9 H9A 0.84(2) .
O10 H10D 0.847(19) .
O10 H10C 0.85(2) .
O11 H11A 0.84(2) .
O11 H11B 0.84(2) .
O12 H12B 0.86(2) .
O12 H12A 0.85(2) .
C1 C2 1.511(6) .
C2 C3 1.510(7) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C5 1.305(9) .
C3 C4 1.512(6) .
C5 H5A 0.9300 .
C5 H5B 0.9300 .
C6 C7 1.513(6) .
C7 C8 1.506(7) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C10 1.305(8) .
C8 C9 1.501(6) .
C10 H10A 0.9300 .
C10 H10B 0.9300 .
