Two heptanuclear cluster-based 3D metal–organic frameworks with a good magnetocaloric effect
Cao, Shouying; Fan, Chenpeng; Lu, Mengwen; Li, Meng; Zhou, Yuhang; Wang, Hongxia; Lin, Qingfang; Liang, Lili; CrystEngComm 25 (2023) 309–313; doi:10.1039/D2CE01350A

data_7245918
_publ_section_title
;
 Two heptanuclear cluster-based 3D metal--organic frameworks with a good
 magnetocaloric effect
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              309
_journal_page_last               313
_journal_paper_doi               10.1039/D2CE01350A
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         '0.5(C30 H76 Dy14 N6 O64), 4(Cl)'
_chemical_formula_sum            'C15 H38 Cl4 Dy7 N3 O32'
_chemical_formula_weight         2051.74
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-10-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-03 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   12.0761(3)
_cell_length_b                   12.0761(3)
_cell_length_c                   17.8609(5)
_cell_measurement_reflns_used    12573
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.5050
_cell_measurement_theta_min      1.9510
_cell_volume                     2255.73(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.984
_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    -62.00 -37.00   0.50    1.37    --  -11.30 119.00  82.00   50
  2  \w    -10.00  16.00   0.50    1.37    --   10.52  60.00 -37.00   52
  3  \w     27.00  85.00   0.50    1.37    --   10.52  60.00 -37.00  116
  4  \w    -43.00  70.00   0.50    1.37    --  -11.30  35.00  37.00  226
  5  \w      0.00  33.00   0.50    1.37    --  -11.30 -99.00 120.00   66
  6  \w     -6.00  22.00   0.50    1.37    --  -11.30 -99.00  60.00   56
  7  \w     24.00  50.00   0.50    1.37    --   10.52 -99.00 -90.00   52
  8  \w    -10.00  33.00   0.50    1.37    --  -11.30 -99.00-180.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0517458000
_diffrn_orient_matrix_UB_12      0.0141415000
_diffrn_orient_matrix_UB_13      0.0244268000
_diffrn_orient_matrix_UB_21      0.0429744000
_diffrn_orient_matrix_UB_22      0.0460905000
_diffrn_orient_matrix_UB_23      -0.0258140000
_diffrn_orient_matrix_UB_31      -0.0086556000
_diffrn_orient_matrix_UB_32      0.0476922000
_diffrn_orient_matrix_UB_33      0.0177369000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18339
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.495
_diffrn_reflns_theta_min         1.947
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.775
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.64a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.021
_exptl_crystal_description       block
_exptl_crystal_F_000             1870
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.927
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1592
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0373
_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/[\s^2^(Fo^2^)+(0.0308P)^2^+61.7569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1441
_reflns_number_total             1592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01350a2.cif
_cod_data_source_block           dy7
_cod_depositor_comments
'Adding full bibliography for 7245917--7245918.cif.'
_cod_original_cell_volume        2255.73(13)
_cod_database_code               7245918
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.386
_shelx_estimated_absorpt_t_min   0.386
_diffrn_oxdiff_digest_frames
;
015e1e20f3e32e6737faa49c487116d287007049e70
;
_diffrn_oxdiff_digest_hkl
;
01bf9311f117225989357a328ca7a3c90cef4d
;
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Shared sites
{C1, C1A}
{O3, O3A}
{O4, O4A}
2. Restrained distances
 O6-C4
 1.25 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl3: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
Uanis(Cl3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl3) = Uanis(Cl2)
Uanis(C1) = Uanis(C1A)
Uanis(O3) = Uanis(O3A)
Uanis(O4) = Uanis(O4A)
4. Others
 Sof(Cl3)=0.5*(1-FVAR(2))
 Sof(Cl2)=0.5*FVAR(2)
 Fixed Sof: O3(0.5) O4(0.5) O5(0.5) O6(0.5) N1(0.5) H1A(0.5) C1(0.5) C2(0.5)
 H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5) Cl1(0.166667) O3A(0.5) O4A(0.5)
 C1A(0.5) H1AA(0.5)
5.a Riding coordinates:
 N1(H1A)
5.b Rotating group:
 O1W(H1WA,H1WB)
5.c Ternary CH refined with riding coordinates:
 O1(H1), O2(H2)
5.d Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
5.e Aromatic/amide H refined with riding coordinates:
 C1A(H1AA)
;
_shelx_res_checksum              87000
_shelx_hkl_checksum              42836
_shelx_fab_checksum              22194
_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 1.331
_oxdiff_exptl_absorpt_empirical_full_min 0.597