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_7703292
_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 F12 Gd2 N4 O18 Zn2, C H4 O'
_chemical_formula_sum            'C57 H66 F12 Gd2 N4 O19 Zn2'
_chemical_formula_weight         1784.37
_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   geom
_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                76.8600(10)
_cell_angle_beta                 87.5650(10)
_cell_angle_gamma                69.4190(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7623(2)
_cell_length_b                   14.5407(2)
_cell_length_c                   18.0644(2)
_cell_measurement_reflns_used    36631
_cell_measurement_temperature    170.01(10)
_cell_measurement_theta_max      30.7900
_cell_measurement_theta_min      1.5630
_cell_volume                     3292.83(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (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      170.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -67.00 -41.00   0.50    0.50    --    5.00  45.00 174.38   52
  2  \w   -104.00 -79.00   0.50    0.50    --  -14.80  45.00 170.56   50
  3  \w   -103.00  74.00   0.50    0.50    --  -14.80  45.00  60.00  354
  4  \w    -17.00  74.00   0.50    0.50    --  -14.80  45.00 -19.90  182
  5  \w   -104.00  74.00   0.50    0.50    --  -14.80  45.00 120.00  356
  6  \w     49.00  74.00   0.50    0.50    --  -14.80  45.00 179.28   50
  7  \w    -62.00 -36.00   0.50    0.50    --  -14.80  45.00   0.00   52
  8  \w    -29.00  24.00   0.50    0.50    --  -14.80  45.00   0.00  106
  9  \w    -23.00  22.00   0.50    0.50    --  -14.80  45.00 179.28   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0405793000
_diffrn_orient_matrix_UB_12      0.0251557000
_diffrn_orient_matrix_UB_13      -0.0283280000
_diffrn_orient_matrix_UB_21      0.0368065000
_diffrn_orient_matrix_UB_22      -0.0078433000
_diffrn_orient_matrix_UB_23      -0.0287406000
_diffrn_orient_matrix_UB_31      -0.0058761000
_diffrn_orient_matrix_UB_32      -0.0465652000
_diffrn_orient_matrix_UB_33      0.0000669000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46745
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         1.582
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.814
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         12944
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+3.8151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11953
_reflns_number_total             12944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04480a2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7703290--7703292.cif.'
_cod_database_code               7703292
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOFZnGd
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 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.b 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.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C40(H40A,H40B,H40C), C44(H44A,
 H44B,H44C), C47(H47A,H47B,H47C)
5.d Idealised tetrahedral OH refined as rotating group:
 O19(H19A)
;
_shelx_res_checksum              41530
_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 1.242
_oxdiff_exptl_absorpt_empirical_full_min 0.759