#------------------------------------------------------------------------------
#$Date: 2017-04-13 04:57:16 +0300 (Thu, 13 Apr 2017) $
#$Revision: 195397 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/80/7228061.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_7228061
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 Gd2 O24'
_chemical_formula_weight         1034.49
_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                109.198(3)
_cell_angle_beta                 100.025(3)
_cell_angle_gamma                98.983(3)
_cell_formula_units_Z            1
_cell_length_a                   6.9675(8)
_cell_length_b                   10.6078(12)
_cell_length_c                   11.4879(13)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      3.05
_cell_volume                     768.54(15)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.995
_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  0.0235
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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            9686
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.050
_exptl_absorpt_coefficient_mu    5.050
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.235
_exptl_crystal_description       block
_exptl_crystal_F_000             501
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.060
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         2699
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0228
_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)+(0.0332P)²+3.0116P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2634
_reflns_number_total             2699
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce00356k2.cif
_cod_data_source_block           1_a
_cod_database_code               7228061
_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
Gd1 Gd 0.64118(3) 0.70737(2) 0.09979(2) 0.01398(9) Uani 1 1 d . . .
Cu1 Cu 1.000000 1.000000 0.500000 0.02071(17) Uani 1 2 d S . P
O1 O 0.7315(5) 0.7457(4) 0.3209(3) 0.0289(7) Uani 1 1 d . . .
C1 C 0.6887(6) 0.7757(4) 0.4261(4) 0.0190(9) Uani 1 1 d . . .
O2 O 0.7808(5) 0.8809(3) 0.5213(3) 0.0278(7) Uani 1 1 d . . .
C2 C 0.5241(7) 0.6804(5) 0.4474(4) 0.0262(10) Uani 1 1 d . . .
H2A H 0.430559 0.626660 0.366342 0.031 Uiso 1 1 calc R U .
H2B H 0.582985 0.617342 0.478969 0.031 Uiso 1 1 calc R U .
O3 O 0.2357(5) 0.8085(4) 0.3733(3) 0.0347(8) Uani 1 1 d . . .
C3 C 0.4101(7) 0.7516(5) 0.5388(4) 0.0268(10) Uani 1 1 d . U .
O4 O 0.1884(5) 0.9040(3) 0.5660(3) 0.0274(7) Uani 1 1 d . . .
C4 C 0.2694(6) 0.8265(5) 0.4877(4) 0.0219(9) Uani 1 1 d . . .
O5 O 0.6151(4) 0.4742(3) 0.0942(3) 0.0204(6) Uani 1 1 d . . .
C5 C 0.4166(12) 0.7380(9) 0.6484(8) 0.067(2) Uani 1 1 d . U .
H5A H 0.493781 0.682474 0.672286 0.080 Uiso 1 1 calc R U .
H5B H 0.343913 0.783699 0.702412 0.080 Uiso 1 1 calc R U .
O6 O 0.6405(5) 0.2623(3) 0.0547(3) 0.0245(7) Uani 1 1 d . . .
C6 C 0.7098(6) 0.3871(4) 0.1155(4) 0.0168(8) Uani 1 1 d . . .
O7 O 1.1345(5) 0.3977(3) 0.0336(3) 0.0265(7) Uani 1 1 d . . .
C7 C 0.9050(7) 0.4373(5) 0.2162(4) 0.0266(10) Uani 1 1 d . . .
H7A H 0.978666 0.521603 0.213938 0.032 Uiso 1 1 calc R U .
H7B H 0.875983 0.457782 0.299158 0.032 Uiso 1 1 calc R U .
C8 C 1.0347(6) 0.3339(5) 0.1986(4) 0.0261(10) Uani 1 1 d . . .
O8 O 1.2305(5) 0.2215(3) 0.0626(3) 0.0260(7) Uani 1 1 d . . .
C9 C 1.1379(6) 0.3162(4) 0.0923(4) 0.0200(9) Uani 1 1 d . . .
H9B H 1.050(7) 0.887(6) 0.160(5) 0.041(17) Uiso 1 1 d D . .
H9A H 1.055(6) 0.848(5) 0.258(4) 0.028(14) Uiso 1 1 d D . .
O9 O 0.9720(5) 0.8564(4) 0.1986(3) 0.0282(7) Uani 1 1 d D . .
C10 C 1.0613(10) 0.2647(8) 0.2728(6) 0.0540(17) Uani 1 1 d . . .
H10A H 1.145058 0.203799 0.259865 0.065 Uiso 1 1 calc R U .
H10B H 0.996680 0.276315 0.338587 0.065 Uiso 1 1 calc R U .
H10C H 0.493(7) 0.960(7) 0.165(6) 0.08(3) Uiso 1 1 d D . .
H10D H 0.660(8) 0.986(5) 0.262(3) 0.045(17) Uiso 1 1 d D . .
O10 O 0.6006(6) 0.9349(3) 0.1859(4) 0.0385(9) Uani 1 1 d D . .
O11 O 0.3305(5) 0.6663(3) 0.1576(3) 0.0273(7) Uani 1 1 d D . .
H11A H 0.238(8) 0.596(4) 0.124(6) 0.06(2) Uiso 1 1 d D . .
H11B H 0.312(9) 0.707(6) 0.229(3) 0.041(17) Uiso 1 1 d D . .
O12 O 1.2394(5) -0.0283(4) 0.0836(4) 0.0324(8) Uani 1 1 d D . .
H12B H 1.220(10) 0.039(5) 0.063(6) 0.05(2) Uiso 1 1 d D . .
H12A H 1.242(11) -0.074(7) 0.007(3) 0.06(2) Uiso 1 1 d D . .
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'
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
O10 Gd1 O1 80.18(13) . .
O10 Gd1 O11 79.50(13) . .
O1 Gd1 O11 74.89(11) . .
O10 Gd1 O9 72.46(13) . .
O1 Gd1 O9 69.13(11) . .
O11 Gd1 O9 137.27(11) . .
O10 Gd1 O5 153.08(13) . .
O1 Gd1 O5 78.72(11) . .
O11 Gd1 O5 78.99(11) . .
O9 Gd1 O5 114.56(11) . .
O10 Gd1 O8 86.01(13) . 2_765
O1 Gd1 O8 140.60(11) . 2_765
O11 Gd1 O8 138.32(11) . 2_765
O9 Gd1 O8 71.54(11) . 2_765
O5 Gd1 O8 120.90(10) . 2_765
O10 Gd1 O7 132.95(13) . 2_765
O1 Gd1 O7 117.22(11) . 2_765
O11 Gd1 O7 145.17(11) . 2_765
O9 Gd1 O7 74.39(12) . 2_765
O5 Gd1 O7 72.40(10) . 2_765
O8 Gd1 O7 51.99(10) 2_765 2_765
O10 Gd1 O6 71.80(11) . 2_665
O1 Gd1 O6 137.70(11) . 2_665
O11 Gd1 O6 69.41(11) . 2_665
O9 Gd1 O6 127.61(11) . 2_665
O5 Gd1 O6 114.77(10) . 2_665
O8 Gd1 O6 68.96(10) 2_765 2_665
O7 Gd1 O6 105.05(11) 2_765 2_665
O10 Gd1 O5 121.38(11) . 2_665
O1 Gd1 O5 134.93(10) . 2_665
O11 Gd1 O5 71.76(10) . 2_665
O9 Gd1 O5 150.90(11) . 2_665
O5 Gd1 O5 65.93(11) . 2_665
O8 Gd1 O5 83.44(10) 2_765 2_665
O7 Gd1 O5 78.59(10) 2_765 2_665
O6 Gd1 O5 50.62(9) 2_665 2_665
O10 Gd1 C9 110.23(14) . 2_765
O1 Gd1 C9 133.83(11) . 2_765
O11 Gd1 C9 149.96(11) . 2_765
O9 Gd1 C9 71.74(12) . 2_765
O5 Gd1 C9 96.46(11) . 2_765
O8 Gd1 C9 26.03(11) 2_765 2_765
O7 Gd1 C9 25.98(11) 2_765 2_765
O6 Gd1 C9 86.31(11) 2_665 2_765
O5 Gd1 C9 79.24(10) 2_665 2_765
O10 Gd1 C6 95.85(12) . 2_665
O1 Gd1 C6 141.20(11) . 2_665
O11 Gd1 C6 66.49(11) . 2_665
O9 Gd1 C6 146.55(11) . 2_665
O5 Gd1 C6 90.25(11) . 2_665
O8 Gd1 C6 76.55(11) 2_765 2_665
O7 Gd1 C6 93.80(11) 2_765 2_665
O6 Gd1 C6 24.98(11) 2_665 2_665
O5 Gd1 C6 25.78(10) 2_665 2_665
C9 Gd1 C6 83.98(11) 2_765 2_665
O2 Cu1 O2 180.0 . 2_776
O2 Cu1 O4 90.41(14) . 2_676
O2 Cu1 O4 89.59(14) 2_776 2_676
O2 Cu1 O4 89.59(14) . 1_655
O2 Cu1 O4 90.41(14) 2_776 1_655
O4 Cu1 O4 180.0 2_676 1_655
C1 O1 Gd1 149.8(3) . .
O1 C1 O2 123.7(4) . .
O1 C1 C2 120.4(4) . .
O2 C1 C2 115.8(4) . .
C1 O2 Cu1 117.0(3) . .
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 122.5(5) . .
C5 C3 C4 122.5(5) . .
C2 C3 C4 114.6(4) . .
C4 O4 Cu1 118.0(3) . 1_455
O3 C4 O4 123.5(4) . .
O3 C4 C3 119.0(4) . .
O4 C4 C3 117.5(4) . .
C6 O5 Gd1 146.0(3) . .
C6 O5 Gd1 93.4(2) . 2_665
Gd1 O5 Gd1 114.06(11) . 2_665
C3 C5 H5A 120.0 . .
C3 C5 H5B 120.0 . .
H5A C5 H5B 120.0 . .
C6 O6 Gd1 95.3(2) . 2_665
O6 C6 O5 120.0(4) . .
O6 C6 C7 120.6(4) . .
O5 C6 C7 119.3(4) . .
O6 C6 Gd1 59.7(2) . 2_665
O5 C6 Gd1 60.8(2) . 2_665
C7 C6 Gd1 173.5(3) . 2_665
C9 O7 Gd1 93.3(3) . 2_765
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 120.5(5) . .
C10 C8 C7 122.8(5) . .
C9 C8 C7 116.7(4) . .
C9 O8 Gd1 94.6(3) . 2_765
O7 C9 O8 120.0(4) . .
O7 C9 C8 119.6(4) . .
O8 C9 C8 120.3(4) . .
O7 C9 Gd1 60.7(2) . 2_765
O8 C9 Gd1 59.4(2) . 2_765
C8 C9 Gd1 176.4(3) . 2_765
Gd1 O9 H9B 125(4) . .
Gd1 O9 H9A 124(4) . .
H9B O9 H9A 101(5) . .
C8 C10 H10A 120.0 . .
C8 C10 H10B 120.0 . .
H10A C10 H10B 120.0 . .
Gd1 O10 H10C 124(4) . .
Gd1 O10 H10D 120(4) . .
H10C O10 H10D 109(3) . .
Gd1 O11 H11A 128(5) . .
Gd1 O11 H11B 124(4) . .
H11A O11 H11B 105(6) . .
H12B O12 H12A 90(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 O10 2.372(3) .
Gd1 O1 2.387(3) .
Gd1 O11 2.390(3) .
Gd1 O9 2.423(3) .
Gd1 O5 2.431(3) .
Gd1 O8 2.479(3) 2_765
Gd1 O7 2.508(3) 2_765
Gd1 O6 2.543(3) 2_665
Gd1 O5 2.566(3) 2_665
Gd1 C9 2.871(4) 2_765
Gd1 C6 2.933(4) 2_665
Cu1 O2 1.929(3) .
Cu1 O2 1.929(3) 2_776
Cu1 O4 1.978(3) 2_676
Cu1 O4 1.978(3) 1_655
O1 C1 1.246(5) .
C1 O2 1.258(5) .
C1 C2 1.515(6) .
C2 C3 1.503(7) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
O3 C4 1.238(6) .
C3 C5 1.308(9) .
C3 C4 1.512(6) .
O4 C4 1.281(5) .
O5 C6 1.278(5) .
C5 H5A 0.9300 .
C5 H5B 0.9300 .
O6 C6 1.244(5) .
C6 C7 1.514(6) .
O7 C9 1.260(6) .
C7 C8 1.512(7) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C10 1.303(8) .
C8 C9 1.497(6) .
O8 C9 1.264(5) .
O9 H9B 0.85(2) .
O9 H9A 0.85(2) .
C10 H10A 0.9300 .
C10 H10B 0.9300 .
O10 H10C 0.85(2) .
O10 H10D 0.85(2) .
O11 H11A 0.84(2) .
O11 H11B 0.83(2) .
O12 H12B 0.84(2) .
O12 H12A 0.86(2) .
