A new family of decanuclear Ln7Cr3 clusters exhibiting a magnetocaloric effect
Yin, Jia-Jia; Lu, Tian-Qi; Chen, Cheng; Shi, Hai-Yan; Zhuang, Gui-Lin; Zheng, Jun; Fang, Xiaolong; Zheng, Xiu-Ying; RSC Advances 11 (2021) 17346–17351; doi:10.1039/D1RA02734D

data_7242827
_publ_section_title
;
 A new family of decanuclear Ln7Cr3 clusters exhibiting a magnetocaloric
 effect
;
_journal_issue                   28
_journal_name_full               'RSC Advances'
_journal_page_first              17346
_journal_page_last               17351
_journal_paper_doi               10.1039/D1RA02734D
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C22 H44.31 Cr2 Gd5 O40.83, 2(Cl O3.96)'
_chemical_formula_sum            'C22 H138 Cl7 Cr2 Gd5 O102'
_chemical_formula_weight         3173.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc23y8fs
_audit_creation_date             2019-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-06 deposited with the CCDC.	2021-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.483(0)
_cell_length_b                   23.488(0)
_cell_length_c                   18.895(0)
_cell_measurement_reflns_used    23172
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.07
_cell_measurement_theta_min      2.95
_cell_volume                     8646.668
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
 698 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32300
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.820
_diffrn_reflns_theta_min         3.763
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    29.807
_exptl_absorpt_correction_T_max  0.2330
_exptl_absorpt_correction_T_min  0.0107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6292
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.3
_platon_squeeze_details
;
;
_refine_diff_density_max         1.717
_refine_diff_density_min         -1.366
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         8036
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0709
_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^)+(0.1108P)^2^+44.7856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.1984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5463
_reflns_number_total             8036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra02734d2.cif
_cod_data_source_block           Gd5Cr2
_cod_original_cell_volume        8647.1
_cod_database_code               7242827
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H10 of O10, H12 of O12, H13 of O13, H11 of O11
 At 1.5 times of:
  All C(H,H,H) groups, H9 of O9, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O8W) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O16)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Rotating group:
 O8W(H8WA,H8WB)
3.b Ternary CH refined with riding coordinates:
 O11(H11), O12(H12), O13(H13)
3.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B)
3.d Aromatic/amide H refined with riding coordinates:
 O10(H10)
3.e Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              66240
_shelx_fab_checksum              12828
_platon_gd5cr2_details
;
Because of disorder, 7 ClO4- and 33 water molecules were omited. 
This valueis calculated based upon elemental analysis data,
and TGA data.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'