Zn<sub>2</sub>Ln<sub>2</sub> complexes with carbonate bridges formed by the fixation of carbon dioxide in the atmosphere: single-molecule magnet behaviour and magnetocaloric effect.
Liu, Cai-Ming; Zhang, De-Qing; Hao, Xiang; Zhu, Dao-Ben; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2121–2128; doi:10.1039/c9dt04480a

data_7703291
_publ_section_title
;
 Zn<sub>2</sub>Ln<sub>2</sub> complexes with carbonate bridges formed by
 the fixation of carbon dioxide in the atmosphere: single-molecule magnet
 behaviour and magnetocaloric effect.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2121
_journal_page_last               2128
_journal_paper_doi               10.1039/c9dt04480a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C56 H62 Eu2 F12 N4 O18 Zn2, C H4 O'
_chemical_formula_sum            'C57 H66 Eu2 F12 N4 O19 Zn2'
_chemical_formula_weight         1773.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-09 deposited with the CCDC.	2020-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                76.7550(10)
_cell_angle_beta                 87.4460(10)
_cell_angle_gamma                69.4370(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7920(2)
_cell_length_b                   14.5529(2)
_cell_length_c                   18.1149(2)
_cell_measurement_reflns_used    32310
_cell_measurement_temperature    170.00(11)
_cell_measurement_theta_max      75.4160
_cell_measurement_theta_min      2.5000
_cell_volume                     3311.12(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -34.00  25.00   0.50    0.05    --  -47.20  36.00-101.00  118
  2  \w   -119.00 -74.00   0.50    0.05    --  -47.20 -36.00 101.00   90
  3  \w     63.00 118.00   0.50    0.05    --   47.20  36.00-101.00  110
  4  \w    -26.00  59.00   0.50    0.05    --   47.20 -36.00 101.00  170
  5  \w   -165.00 -90.00   0.50    0.05    --  -99.00 -36.00 101.00  150
  6  \w    -78.00 -52.00   0.50    0.05    --  -99.00  36.00-101.00   52
  7  \w     30.00 116.00   0.50    0.05    --  103.25 -36.00 101.00  172
  8  \w     92.00 162.00   0.50    0.05    --  103.25  36.00-101.00  140
  9  \w    -70.00  -2.00   0.50    0.05    --  -47.20  77.00 -60.00  136
 10  \w    -59.00  25.00   0.50    0.05    --  -47.20  19.00  60.00  168
 11  \w   -110.00 -85.00   0.50    0.05    --  -47.20-125.00-120.00   50
 12  \w     37.00 120.00   0.50    0.05    --   47.20  38.00  90.00  166
 13  \w    -87.00 -28.00   0.50    0.05    --  -99.00  45.00 120.00  118
 14  \w    -60.00 -26.00   0.50    0.05    --  -99.00  77.00-120.00   68
 15  \w   -119.00 -93.00   0.50    0.05    --  -99.00 -15.00 150.00   52
 16  \w    -69.00 -34.00   0.50    0.05    --  -99.00 125.00 -60.00   70
 17  \w    -64.00 -28.00   0.50    0.05    --  -99.00  61.00  30.00   72
 18  \w   -116.00 -41.00   0.50    0.05    --  -99.00 125.00-120.00  150
 19  \w   -115.00 -89.00   0.50    0.05    --  -99.00 125.00 -60.00   52
 20  \w   -115.00 -80.00   0.50    0.05    --  -99.00  61.00  30.00   70
 21  \w   -122.00 -94.00   0.50    0.05    --  -99.00  77.00-120.00   56
 22  \w    -94.00 -25.00   0.50    0.05    --  -99.00  30.00  30.00  138
 23  \w     37.00 107.00   0.50    0.05    --  103.25 -94.00  60.00  140
 24  \w     34.00 110.00   0.50    0.05    --  103.25 -61.00 120.00  152
 25  \w     61.00  87.00   0.50    0.05    --  103.25 -94.00 120.00   52
 26  \w     91.00 148.00   0.50    0.05    --  103.25  45.00-150.00  114
 27  \w     59.00 109.00   0.50    0.05    --  103.25 -94.00-150.00  100
 28  \w     92.00 168.00   0.50    0.05    --  103.25  15.00 150.00  152
 29  \w     34.00 101.00   0.50    0.05    --  103.25 -94.00 -30.00  134
 30  \w     31.00 108.00   0.50    0.05    --  103.25 -94.00  90.00  154
 31  \w     69.00 114.00   0.50    0.05    --  103.25-125.00 -90.00   90
 32  \w     92.00 163.00   0.50    0.05    --  103.25  45.00  30.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0488842000
_diffrn_orient_matrix_UB_12      0.0871623000
_diffrn_orient_matrix_UB_13      0.0402197000
_diffrn_orient_matrix_UB_21      -0.1046839000
_diffrn_orient_matrix_UB_22      -0.0158485000
_diffrn_orient_matrix_UB_23      -0.0003822000
_diffrn_orient_matrix_UB_31      0.0301078000
_diffrn_orient_matrix_UB_32      -0.0750805000
_diffrn_orient_matrix_UB_33      0.0776355000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42470
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.560
_diffrn_reflns_theta_min         2.508
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       cube
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.00049(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         13120
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0365
_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/[\s^2^(Fo^2^)+(0.0596P)^2^+5.8700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12417
_reflns_number_total             13120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04480a2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7703290--7703292.cif.'
_cod_database_code               7703291
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOFZnEu
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C48-F1 \\sim C48-F1A \\sim C48-F2 \\sim C48-F2A \\sim C48-F3 \\sim C48-F3A
 with sigma of 0.01
 C57-F10 \\sim C57-F10A \\sim C57-F11 \\sim C57-F11A \\sim C57-F12 \\sim
C57-F12A
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.02
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F10A-F11A \\sim F11A-F12A \\sim
F12A-F10A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
F10 \\sim F10A \\sim F11 \\sim F11A \\sim F12 \\sim F12A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(F1) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F2A)
\\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F10) \\sim Ueq,
Uanis(F10A) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F12A) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.004
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
5.a Riding coordinates:
 C23(H23A,H23B,H23C), C44(H44A,H44B,H44C)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C31(H31A,H31B),
 C33(H33A,H33B), C34(H34A,H34B), C36(H36A,H36B)
5.c Me refined with riding coordinates:
 C8(H8A,H8B,H8C)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C16(H16), C19(H19), C25(H25), C27(H27), C38(H38), C41(H41),
 C50(H50), C55(H55)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C18(H18A,H18B,
 H18C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C35(H35A,
 H35B,H35C), C40(H40A,H40B,H40C), C47(H47A,H47B,H47C)
5.f Idealised tetrahedral OH refined as rotating group:
 O19(H19A)
;
_shelx_res_checksum              36310
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.897
_oxdiff_exptl_absorpt_empirical_full_min 0.683