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_7245917
_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 Gd14 N6 O64), 4(Cl)'
_chemical_formula_sum            'C15 H38 Cl4 Gd7 N3 O32'
_chemical_formula_weight         2015.03
_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             2022-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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                   12.1692(5)
_cell_length_b                   12.1692(5)
_cell_length_c                   18.0220(11)
_cell_measurement_reflns_used    6509
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.442
_cell_measurement_theta_min      2.239
_cell_volume                     2311.31(19)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18930
_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         27.502
_diffrn_reflns_theta_min         2.239
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.220
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.1916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0812 before and 0.0493 after correction. The Ratio of minimum to maximum transmission is 0.7324. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.895
_exptl_crystal_description       block
_exptl_crystal_F_000             1842
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.668
_refine_diff_density_min         -1.958
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1829
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0259P)^2^+41.5045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1561
_reflns_number_total             1829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01350a2.cif
_cod_data_source_block           gd7_0m
_cod_depositor_comments
'Adding full bibliography for 7245917--7245918.cif.'
_cod_original_cell_volume        2311.3(2)
_cod_database_code               7245917
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.495
_shelx_estimated_absorpt_t_min   0.374
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{O1, O1A}
{O2, O2A}
{C1, C1A}
3. Restrained distances
 H6-O6
 0.85 with sigma of 0.02
 O5-H5
 0.85 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Cl3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) = Uanis(O1A)
Uanis(O2) = Uanis(O2A)
Uanis(C1) = Uanis(C1A)
5. Others
 Fixed Sof: O1(0.5) O2(0.5) O3(0.5) O4(0.5) N1(0.5) H1(0.5) C1(0.5) C2(0.5)
 H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5) Cl1(0.16667) Cl2(0.4) Cl3(0.1)
 O1A(0.5) O2A(0.5) C1A(0.5) H1A(0.5)
6.a Riding coordinates:
 O5(H5), O6(H6), O7(H7A,H7B), C3(H3A,H3B)
6.b Ternary CH refined with riding coordinates:
 N1(H1)
6.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
6.d Aromatic/amide H refined with riding coordinates:
 C1A(H1A)
;
_shelx_res_checksum              73413
_shelx_hkl_checksum              60122
_olex2_submission_special_instructions 'No special instructions were received'