#------------------------------------------------------------------------------
#$Date: 2017-04-13 03:57:16 +0200 (Thu, 13 Apr 2017) $
#$Revision: 195397 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/7/22/80/7228059.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_7228059
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 Dy2 O24'
_chemical_formula_weight         1044.99
_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                109.409(4)
_cell_angle_beta                 99.928(4)
_cell_angle_gamma                98.943(4)
_cell_formula_units_Z            1
_cell_length_a                   6.9551(8)
_cell_length_b                   10.5490(11)
_cell_length_c                   11.4502(12)
_cell_measurement_reflns_used    9725
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      3.05
_cell_volume                     759.75(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      299(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  0.0283
_diffrn_reflns_av_unetI/netI     0.0156
_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            21325
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.055
_exptl_absorpt_coefficient_mu    5.661
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.284
_exptl_crystal_description       block
_exptl_crystal_F_000             505
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.000
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2667
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0211
_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)+(0.0316P)²+2.8483P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2547
_reflns_number_total             2667
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce00356k2.cif
_cod_data_source_block           1_a
_cod_original_cell_volume        759.75(14)
_cod_database_code               7228059
_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
Dy1 Dy 0.64039(3) 0.70704(2) 0.09877(2) 0.01472(8) Uani 1 1 d . . .
Cu1 Cu 1.000000 1.000000 0.500000 0.02034(17) Uani 1 2 d S . P
O1 O 0.7306(5) 0.7452(3) 0.3182(3) 0.0281(7) Uani 1 1 d . . .
C1 C 0.6882(6) 0.7742(5) 0.4243(4) 0.0189(9) Uani 1 1 d . . .
O2 O 0.7810(5) 0.8792(3) 0.5200(3) 0.0283(7) Uani 1 1 d . . .
C2 C 0.5235(7) 0.6779(5) 0.4449(4) 0.0263(10) Uani 1 1 d . . .
H2A H 0.429757 0.624194 0.363448 0.032 Uiso 1 1 calc R U .
H2B H 0.582266 0.614143 0.475989 0.032 Uiso 1 1 calc R U .
O3 O 0.2346(5) 0.8080(4) 0.3724(3) 0.0345(8) Uani 1 1 d . . .
C3 C 0.4099(7) 0.7498(5) 0.5372(4) 0.0251(10) Uani 1 1 d . . .
O4 O 0.1890(5) 0.9041(3) 0.5664(3) 0.0268(7) Uani 1 1 d . . .
C4 C 0.2693(6) 0.8262(5) 0.4875(4) 0.0226(9) Uani 1 1 d . . .
O5 O 0.6393(5) 0.2626(3) 0.0559(3) 0.0243(7) Uani 1 1 d . . .
C5 C 0.4169(11) 0.7362(8) 0.6471(7) 0.0645(19) Uani 1 1 d . . .
H5A H 0.494331 0.680294 0.670679 0.077 Uiso 1 1 calc R U .
H5B H 0.344420 0.782341 0.701712 0.077 Uiso 1 1 calc R U .
O6 O 0.6130(4) 0.4753(3) 0.0940(3) 0.0201(6) Uani 1 1 d . . .
C6 C 0.7088(6) 0.3882(4) 0.1159(4) 0.0164(8) Uani 1 1 d . . .
O7 O 1.1374(5) 0.3994(3) 0.0331(3) 0.0264(7) Uani 1 1 d . . .
C7 C 0.9053(7) 0.4400(5) 0.2159(4) 0.0253(10) Uani 1 1 d . . .
H7A H 0.978209 0.524284 0.212237 0.030 Uiso 1 1 calc R U .
H7B H 0.877549 0.462156 0.299673 0.030 Uiso 1 1 calc R U .
O8 O 1.2320(5) 0.2225(3) 0.0625(3) 0.0253(7) Uani 1 1 d . . .
C8 C 1.0352(6) 0.3362(5) 0.1985(4) 0.0252(10) Uani 1 1 d . . .
O9 O 0.9688(5) 0.8544(4) 0.1965(3) 0.0283(7) Uani 1 1 d D . .
C9 C 1.1396(6) 0.3176(4) 0.0920(4) 0.0185(9) Uani 1 1 d . . .
H9A H 1.043(6) 0.887(5) 0.158(4) 0.022 Uiso 1 1 d D U .
H9B H 1.049(6) 0.845(5) 0.255(4) 0.022 Uiso 1 1 d D U .
O10 O 0.6011(5) 0.9334(4) 0.1844(3) 0.0362(9) Uani 1 1 d D . .
C10 C 1.0609(9) 0.2670(7) 0.2728(6) 0.0513(17) Uani 1 1 d . . .
H10A H 1.144457 0.205458 0.260018 0.062 Uiso 1 1 calc R U .
H10B H 0.995649 0.279105 0.338805 0.062 Uiso 1 1 calc R U .
H10C H 0.498(7) 0.963(7) 0.165(7) 0.062 Uiso 1 1 d D U .
H10D H 0.667(9) 0.985(6) 0.259(3) 0.062 Uiso 1 1 d D U .
O11 O 0.3331(5) 0.6683(3) 0.1563(3) 0.0264(7) Uani 1 1 d D . .
H11A H 0.247(6) 0.594(3) 0.127(5) 0.032 Uiso 1 1 d D U .
H11B H 0.308(8) 0.705(5) 0.227(3) 0.032 Uiso 1 1 d D U .
O12 O 0.2385(5) 0.9706(4) 0.0832(3) 0.0317(8) Uani 1 1 d D . .
H12A H 0.235(9) 1.042(4) 0.066(5) 0.038 Uiso 1 1 d D U .
H12B H 0.250(9) 0.923(5) 0.009(3) 0.038 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'
Dy Dy -0.1892 4.4098 '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 Dy1 O11 79.22(13) . .
O10 Dy1 O1 80.38(13) . .
O11 Dy1 O1 75.10(11) . .
O10 Dy1 O9 72.63(12) . .
O11 Dy1 O9 137.29(11) . .
O1 Dy1 O9 69.10(11) . .
O10 Dy1 O6 152.77(13) . .
O11 Dy1 O6 79.05(11) . .
O1 Dy1 O6 78.33(11) . .
O9 Dy1 O6 114.46(11) . .
O10 Dy1 O8 85.91(13) . 2_765
O11 Dy1 O8 138.12(11) . 2_765
O1 Dy1 O8 140.50(11) . 2_765
O9 Dy1 O8 71.46(11) . 2_765
O6 Dy1 O8 121.30(10) . 2_765
O10 Dy1 O7 133.23(13) . 2_765
O11 Dy1 O7 145.25(11) . 2_765
O1 Dy1 O7 116.70(11) . 2_765
O9 Dy1 O7 74.25(11) . 2_765
O6 Dy1 O7 72.37(10) . 2_765
O8 Dy1 O7 52.44(10) 2_765 2_765
O10 Dy1 O5 71.88(11) . 2_665
O11 Dy1 O5 69.42(11) . 2_665
O1 Dy1 O5 138.10(11) . 2_665
O9 Dy1 O5 127.62(11) . 2_665
O6 Dy1 O5 114.84(10) . 2_665
O8 Dy1 O5 68.77(10) 2_765 2_665
O7 Dy1 O5 105.16(11) 2_765 2_665
O10 Dy1 O6 121.75(10) . 2_665
O11 Dy1 O6 71.98(10) . 2_665
O1 Dy1 O6 134.75(10) . 2_665
O9 Dy1 O6 150.68(11) . 2_665
O6 Dy1 O6 65.72(11) . 2_665
O8 Dy1 O6 83.61(10) 2_765 2_665
O7 Dy1 O6 78.42(10) 2_765 2_665
O5 Dy1 O6 50.95(9) 2_665 2_665
O10 Dy1 C9 110.25(14) . 2_765
O11 Dy1 C9 150.10(11) . 2_765
O1 Dy1 C9 133.51(11) . 2_765
O9 Dy1 C9 71.52(11) . 2_765
O6 Dy1 C9 96.73(11) . 2_765
O8 Dy1 C9 26.18(11) 2_765 2_765
O7 Dy1 C9 26.27(11) 2_765 2_765
O5 Dy1 C9 86.26(11) 2_665 2_765
O6 Dy1 C9 79.29(10) 2_665 2_765
O10 Dy1 C6 96.00(12) . 2_665
O11 Dy1 C6 66.41(11) . 2_665
O1 Dy1 C6 141.28(11) . 2_665
O9 Dy1 C6 146.69(11) . 2_665
O6 Dy1 C6 90.16(11) . 2_665
O8 Dy1 C6 76.66(11) 2_765 2_665
O7 Dy1 C6 93.93(11) 2_765 2_665
O5 Dy1 C6 25.12(11) 2_665 2_665
O6 Dy1 C6 25.99(10) 2_665 2_665
C9 Dy1 C6 84.14(11) 2_765 2_665
O2 Cu1 O2 180.0 . 2_776
O2 Cu1 O4 90.43(14) . 2_676
O2 Cu1 O4 89.57(14) 2_776 2_676
O2 Cu1 O4 89.57(14) . 1_655
O2 Cu1 O4 90.43(14) 2_776 1_655
O4 Cu1 O4 180.0 2_676 1_655
C1 O1 Dy1 150.1(3) . .
O1 C1 O2 123.4(4) . .
O1 C1 C2 120.5(4) . .
O2 C1 C2 116.0(4) . .
C1 O2 Cu1 117.4(3) . .
C3 C2 C1 114.2(4) . .
C3 C2 H2A 108.7 . .
C1 C2 H2A 108.7 . .
C3 C2 H2B 108.7 . .
C1 C2 H2B 108.7 . .
H2A C2 H2B 107.6 . .
C5 C3 C2 122.5(5) . .
C5 C3 C4 122.3(5) . .
C2 C3 C4 114.9(4) . .
C4 O4 Cu1 117.6(3) . 1_455
O3 C4 O4 123.4(4) . .
O3 C4 C3 118.8(4) . .
O4 C4 C3 117.8(4) . .
C6 O5 Dy1 95.0(2) . 2_665
C3 C5 H5A 120.0 . .
C3 C5 H5B 120.0 . .
H5A C5 H5B 120.0 . .
C6 O6 Dy1 145.4(3) . .
C6 O6 Dy1 93.5(2) . 2_665
Dy1 O6 Dy1 114.28(11) . 2_665
O5 C6 O6 119.9(4) . .
O5 C6 C7 120.8(4) . .
O6 C6 C7 119.3(4) . .
O5 C6 Dy1 59.9(2) . 2_665
O6 C6 Dy1 60.5(2) . 2_665
C7 C6 Dy1 172.9(3) . 2_665
C9 O7 Dy1 93.2(2) . 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 . .
C9 O8 Dy1 94.4(2) . 2_765
C10 C8 C9 120.4(5) . .
C10 C8 C7 122.7(5) . .
C9 C8 C7 116.9(4) . .
Dy1 O9 H9A 125(3) . .
Dy1 O9 H9B 123(3) . .
H9A O9 H9B 104(5) . .
O8 C9 O7 119.9(4) . .
O8 C9 C8 120.5(4) . .
O7 C9 C8 119.5(4) . .
O8 C9 Dy1 59.4(2) . 2_765
O7 C9 Dy1 60.6(2) . 2_765
C8 C9 Dy1 176.4(3) . 2_765
Dy1 O10 H10C 127(5) . .
Dy1 O10 H10D 119(5) . .
H10C O10 H10D 109(7) . .
C8 C10 H10A 120.0 . .
C8 C10 H10B 120.0 . .
H10A C10 H10B 120.0 . .
Dy1 O11 H11A 126(4) . .
Dy1 O11 H11B 128(4) . .
H11A O11 H11B 101(5) . .
H12A O12 H12B 94(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O10 2.340(3) .
Dy1 O11 2.358(3) .
Dy1 O1 2.361(3) .
Dy1 O9 2.397(3) .
Dy1 O6 2.404(3) .
Dy1 O8 2.454(3) 2_765
Dy1 O7 2.480(3) 2_765
Dy1 O5 2.531(3) 2_665
Dy1 O6 2.542(3) 2_665
Dy1 C9 2.843(4) 2_765
Dy1 C6 2.914(4) 2_665
Cu1 O2 1.925(3) .
Cu1 O2 1.925(3) 2_776
Cu1 O4 1.977(3) 2_676
Cu1 O4 1.977(3) 1_655
O1 C1 1.249(5) .
C1 O2 1.254(6) .
C1 C2 1.513(6) .
C2 C3 1.503(6) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
O3 C4 1.240(5) .
C3 C5 1.307(8) .
C3 C4 1.513(6) .
O4 C4 1.276(5) .
O5 C6 1.242(5) .
C5 H5A 0.9300 .
C5 H5B 0.9300 .
O6 C6 1.279(5) .
C6 C7 1.513(6) .
O7 C9 1.260(5) .
C7 C8 1.510(6) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
O8 C9 1.258(5) .
C8 C10 1.300(7) .
C8 C9 1.498(6) .
O9 H9A 0.84(2) .
O9 H9B 0.84(2) .
O10 H10C 0.85(2) .
O10 H10D 0.84(2) .
C10 H10A 0.9300 .
C10 H10B 0.9300 .
O11 H11A 0.83(2) .
O11 H11B 0.83(2) .
O12 H12A 0.84(2) .
O12 H12B 0.86(2) .
