#------------------------------------------------------------------------------
#$Date: 2017-04-13 04:57:16 +0300 (Thu, 13 Apr 2017) $
#$Revision: 195397 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/80/7228060.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_7228060
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 La2 O24'
_chemical_formula_weight         997.81
_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                108.747(2)
_cell_angle_beta                 100.358(2)
_cell_angle_gamma                99.018(2)
_cell_formula_units_Z            1
_cell_length_a                   7.0117(5)
_cell_length_b                   10.8073(9)
_cell_length_c                   11.6598(9)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.04
_cell_volume                     800.92(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0226
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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            17757
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.035
_exptl_absorpt_coefficient_mu    3.372
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_description       block
_exptl_crystal_F_000             487
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.088
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2825
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0346P)²+0.9261P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2700
_reflns_number_total             2825
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce00356k2.cif
_cod_data_source_block           1_a
_cod_database_code               7228060
_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
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.35318(2) 0.29090(2) 0.89576(2) 0.01627(7) Uani 1 1 d . . . . .
Cu1 Cu 0.000000 0.000000 0.500000 0.02199(12) Uani 1 2 d S . P . .
O1 O 0.3751(3) 0.5296(2) 0.90421(19) 0.0239(4) Uani 1 1 d . . . . .
C1 C 0.2860(4) 0.6182(3) 0.8856(3) 0.0182(6) Uani 1 1 d . . . . .
O2 O 0.3548(3) 0.7394(2) 0.9484(2) 0.0278(5) Uani 1 1 d . . . . .
C2 C 0.0964(4) 0.5733(3) 0.7825(3) 0.0278(7) Uani 1 1 d . . . . .
H2A H 0.130980 0.558739 0.702994 0.033 Uiso 1 1 calc R U . . .
H2B H 0.020927 0.488351 0.779095 0.033 Uiso 1 1 calc R U . . .
C3 C -0.0325(4) 0.6741(3) 0.8009(3) 0.0262(7) Uani 1 1 d . . . . .
O3 O -0.1235(4) 0.6082(2) 0.9633(2) 0.0322(5) Uani 1 1 d . . . . .
O4 O -0.2248(3) 0.7807(2) 0.9366(2) 0.0311(5) Uani 1 1 d . . . . .
C4 C -0.1314(4) 0.6892(3) 0.9065(3) 0.0217(6) Uani 1 1 d . . . . .
C5 C -0.0607(7) 0.7425(5) 0.7292(4) 0.0583(12) Uani 1 1 d . . . . .
H5A H -0.143525 0.802289 0.742795 0.070 Uiso 1 1 calc R U . . .
H5B H 0.001924 0.731969 0.663907 0.070 Uiso 1 1 calc R U . . .
O5 O 0.2636(3) 0.2501(2) 0.66951(19) 0.0316(5) Uani 1 1 d . . . . .
C6 C 0.3080(4) 0.2180(3) 0.5659(3) 0.0204(6) Uani 1 1 d . . . . .
O6 O 0.2185(3) 0.1131(2) 0.4748(2) 0.0301(5) Uani 1 1 d . . . . .
C7 C 0.4727(4) 0.3098(3) 0.5450(3) 0.0272(7) Uani 1 1 d . . . . .
O7 O 0.7619(4) 0.1894(3) 0.6241(2) 0.0381(6) Uani 1 1 d . . . . .
O8 O 0.8136(3) 0.0957(2) 0.43646(19) 0.0284(5) Uani 1 1 d . . . . .
C8 C 0.5887(5) 0.2417(3) 0.4569(3) 0.0285(7) Uani 1 1 d . . . . .
C9 C 0.7304(4) 0.1703(3) 0.5109(3) 0.0243(6) Uani 1 1 d . . . . .
O9 O 0.0126(3) 0.1339(2) 0.7951(2) 0.0320(5) Uani 1 1 d D . . . .
H9B H -0.066(5) 0.147(4) 0.740(3) 0.038 Uiso 1 1 d D U . . .
H9A H -0.057(5) 0.103(4) 0.836(3) 0.038 Uiso 1 1 d D U . . .
O10 O 0.3980(4) 0.0580(3) 0.8086(3) 0.0498(8) Uani 1 1 d D . . . .
H10D H 0.328(5) 0.008(4) 0.738(2) 0.060 Uiso 1 1 d D U . . .
H10C H 0.499(4) 0.030(4) 0.831(4) 0.060 Uiso 1 1 d D U . . .
C10B C 0.5265(12) 0.4295(8) 0.6090(8) 0.042(2) Uani 0.517(10) 1 d . . P A 1
H10F H 0.621(13) 0.488(9) 0.599(8) 0.050 Uiso 0.517(10) 1 d . U P A 1
H10E H 0.443(12) 0.465(8) 0.667(8) 0.050 Uiso 0.517(10) 1 d . U P A 1
C10A C 0.5855(10) 0.2556(7) 0.3492(6) 0.028(2) Uani 0.483(10) 1 d . . P A 2
H10A H 0.508991 0.309521 0.324159 0.034 Uiso 0.483(10) 1 calc R U P A 2
H10B H 0.659772 0.211439 0.297754 0.034 Uiso 0.483(10) 1 calc R U P A 2
O11 O 0.6794(3) 0.3393(2) 0.8385(2) 0.0331(5) Uani 1 1 d D . . . .
H11A H 0.772(5) 0.408(3) 0.875(3) 0.040 Uiso 1 1 d D U . . .
H11B H 0.708(6) 0.303(4) 0.772(2) 0.040 Uiso 1 1 d D U . . .
O12 O 0.7557(4) 0.0242(2) 0.9148(2) 0.0355(5) Uani 1 1 d D . . . .
H12A H 0.740(6) 0.074(4) 0.983(2) 0.043 Uiso 1 1 d D U . . .
H12B H 0.758(6) -0.052(3) 0.920(4) 0.043 Uiso 1 1 d 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'
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'
La La -0.2871 2.4523 '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
O5 La1 O10 79.47(9) . .
O5 La1 O11 74.52(7) . .
O10 La1 O11 80.41(10) . .
O5 La1 O1 80.29(7) . .
O10 La1 O1 154.29(10) . .
O11 La1 O1 79.04(8) . .
O5 La1 O9 69.97(7) . .
O10 La1 O9 71.66(9) . .
O11 La1 O9 137.92(8) . .
O1 La1 O9 115.46(7) . .
O5 La1 O4 141.42(8) . 2_567
O10 La1 O4 86.27(10) . 2_567
O11 La1 O4 138.10(8) . 2_567
O1 La1 O4 119.41(7) . 2_567
O9 La1 O4 71.53(8) . 2_567
O5 La1 O3 119.96(7) . 2_567
O10 La1 O3 131.54(10) . 2_567
O11 La1 O3 144.79(8) . 2_567
O1 La1 O3 72.95(7) . 2_567
O9 La1 O3 74.92(8) . 2_567
O4 La1 O3 49.90(7) 2_567 2_567
O5 La1 O2 136.14(7) . 2_667
O10 La1 O2 71.37(7) . 2_667
O11 La1 O2 68.95(8) . 2_667
O1 La1 O2 114.58(7) . 2_667
O9 La1 O2 126.77(7) . 2_667
O4 La1 O2 69.14(7) 2_567 2_667
O3 La1 O2 103.90(7) 2_567 2_667
O5 La1 O1 135.71(7) . 2_667
O10 La1 O1 119.32(7) . 2_667
O11 La1 O1 70.46(7) . 2_667
O1 La1 O1 67.27(7) . 2_667
O9 La1 O1 151.26(7) . 2_667
O4 La1 O1 82.36(7) 2_567 2_667
O3 La1 O1 79.19(7) 2_567 2_667
O2 La1 O1 48.88(6) 2_667 2_667
O5 La1 C4 135.55(8) . 2_567
O10 La1 C4 109.55(10) . 2_567
O11 La1 C4 148.75(8) . 2_567
O1 La1 C4 96.00(7) . 2_567
O9 La1 C4 72.13(8) . 2_567
O4 La1 C4 24.98(8) 2_567 2_567
O3 La1 C4 24.94(8) 2_567 2_567
O2 La1 C4 85.86(7) 2_667 2_567
O1 La1 C4 79.13(7) 2_667 2_567
O5 La1 C1 140.72(7) . 2_667
O10 La1 C1 94.71(8) . 2_667
O11 La1 C1 66.21(7) . 2_667
O1 La1 C1 90.99(7) . 2_667
O9 La1 C1 145.01(7) . 2_667
O4 La1 C1 75.64(7) 2_567 2_667
O3 La1 C1 93.05(7) 2_567 2_667
O2 La1 C1 24.07(7) 2_667 2_667
O1 La1 C1 24.88(7) 2_667 2_667
C4 La1 C1 83.19(7) 2_567 2_667
O6 Cu1 O6 180.0 . 2_556
O6 Cu1 O8 90.10(9) . 2_656
O6 Cu1 O8 89.90(9) 2_556 2_656
O6 Cu1 O8 89.90(9) . 1_455
O6 Cu1 O8 90.10(9) 2_556 1_455
O8 Cu1 O8 180.00(12) 2_656 1_455
C1 O1 La1 148.47(19) . .
C1 O1 La1 93.04(16) . 2_667
La1 O1 La1 112.73(7) . 2_667
O2 C1 O1 121.1(3) . .
O2 C1 C2 120.2(3) . .
O1 C1 C2 118.7(3) . .
O2 C1 La1 59.27(15) . 2_667
O1 C1 La1 62.08(14) . 2_667
C2 C1 La1 176.06(19) . 2_667
C1 O2 La1 96.66(17) . 2_667
C3 C2 C1 112.7(3) . .
C3 C2 H2A 109.1 . .
C1 C2 H2A 109.1 . .
C3 C2 H2B 109.1 . .
C1 C2 H2B 109.1 . .
H2A C2 H2B 107.8 . .
C5 C3 C4 121.1(3) . .
C5 C3 C2 122.8(3) . .
C4 C3 C2 116.2(3) . .
C4 O3 La1 93.85(18) . 2_567
C4 O4 La1 95.66(18) . 2_567
O3 C4 O4 120.5(3) . .
O3 C4 C3 119.3(3) . .
O4 C4 C3 120.2(3) . .
O3 C4 La1 61.21(15) . 2_567
O4 C4 La1 59.37(15) . 2_567
C3 C4 La1 176.2(2) . 2_567
C3 C5 H5A 120.0 . .
C3 C5 H5B 120.0 . .
H5A C5 H5B 120.0 . .
C6 O5 La1 149.6(2) . .
O6 C6 O5 123.4(3) . .
O6 C6 C7 116.6(3) . .
O5 C6 C7 120.0(3) . .
C6 O6 Cu1 116.31(19) . .
C10B C7 C8 121.8(5) . .
C10B C7 C6 121.7(4) . .
C8 C7 C6 115.8(3) . .
C9 O8 Cu1 119.61(19) . 1_655
C10A C8 C7 123.0(4) . .
C10A C8 C9 122.6(4) . .
C7 C8 C9 114.0(3) . .
O7 C9 O8 123.8(3) . .
O7 C9 C8 118.9(3) . .
O8 C9 C8 117.3(3) . .
La1 O9 H9B 120(3) . .
La1 O9 H9A 123(3) . .
H9B O9 H9A 107(4) . .
La1 O10 H10D 118(3) . .
La1 O10 H10C 126(3) . .
H10D O10 H10C 113(3) . .
C7 C10B H10F 125(5) . .
C7 C10B H10E 116(5) . .
H10F C10B H10E 119(7) . .
C8 C10A H10A 120.0 . .
C8 C10A H10B 120.0 . .
H10A C10A H10B 120.0 . .
La1 O11 H11A 126(3) . .
La1 O11 H11B 128(3) . .
H11A O11 H11B 104(4) . .
H12A O12 H12B 107(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 O5 2.473(2) .
La1 O10 2.487(2) .
La1 O11 2.520(2) .
La1 O1 2.529(2) .
La1 O9 2.530(2) .
La1 O4 2.573(2) 2_567
La1 O3 2.614(2) 2_567
La1 O2 2.619(2) 2_667
La1 O1 2.677(2) 2_667
La1 C4 2.976(3) 2_567
La1 C1 3.026(3) 2_667
Cu1 O6 1.932(2) .
Cu1 O6 1.932(2) 2_556
Cu1 O8 1.974(2) 2_656
Cu1 O8 1.974(2) 1_455
O1 C1 1.275(3) .
C1 O2 1.243(4) .
C1 C2 1.516(4) .
C2 C3 1.510(4) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C5 1.292(5) .
C3 C4 1.495(4) .
O3 C4 1.258(4) .
O4 C4 1.263(4) .
C5 H5A 0.9300 .
C5 H5B 0.9300 .
O5 C6 1.256(4) .
C6 O6 1.254(4) .
C6 C7 1.508(4) .
C7 C10B 1.224(8) .
C7 C8 1.503(4) .
O7 C9 1.240(4) .
O8 C9 1.274(4) .
C8 C10A 1.308(7) .
C8 C9 1.519(4) .
O9 H9B 0.836(19) .
O9 H9A 0.841(19) .
O10 H10D 0.829(18) .
O10 H10C 0.840(18) .
C10B H10F 0.89(9) .
C10B H10E 1.00(9) .
C10A H10A 0.9300 .
C10A H10B 0.9300 .
O11 H11A 0.839(19) .
O11 H11B 0.826(19) .
O12 H12A 0.840(19) .
O12 H12B 0.846(19) .
