Magnetocaloric effect in 1D-polymers bearing 15-metallacrown-5 {GdCu<sub>5</sub>}<sup>3+</sup> units and anionic oxalate complexes.
Pavlishchuk, Anna V.; Kolotilov, Sergey V.; Zeller, Matthias; Pavlishchuk, Vitaly V.; Pointillart, Fabrice; Addison, Anthony W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15713–15724; doi:10.1039/d4dt02413c

data_7716981
_publ_section_title
;
 Magnetocaloric effect in 1D-polymers bearing 15-metallacrown-5
 {GdCu<sub>5</sub>}<sup>3+</sup> units and anionic oxalate complexes.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15713
_journal_page_last               15724
_journal_paper_doi               10.1039/d4dt02413c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H64.63 Cu13 Gd2 N20 O56.32, 11.48(H2 O)'
_chemical_formula_sum            'C32 H87.6 Cu13 Gd2 N20 O67.8'
_chemical_formula_weight         2978.24
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-07-02 deposited with the CCDC.	2024-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                97.361(2)
_cell_angle_beta                 100.370(2)
_cell_angle_gamma                99.751(2)
_cell_formula_units_Z            1
_cell_length_a                   9.2930(13)
_cell_length_b                   14.602(2)
_cell_length_c                   16.484(2)
_cell_measurement_reflns_used    9132
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.84
_cell_measurement_theta_min      2.83
_cell_volume                     2139.3(5)
_computing_cell_refinement       'Apex2 v2008.2-4'
_computing_data_collection       'Apex2 v2008.2-4 (Bruker, 2008)'
_computing_data_reduction        'Apex2 v2008.2-4'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015a, 2018), 
SHELXLE Rev1385 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45021
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.825
_diffrn_reflns_theta_min         2.068
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.813
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.3945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2008.2-4 (Bruker, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.312
_exptl_crystal_description       plate
_exptl_crystal_F_000             1467
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.440
_refine_diff_density_min         -1.738
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         13190
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0295P)^2^+4.9138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11220
_reflns_number_total             13190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02413c2.cif
_cod_data_source_block           09mz399_0m
_cod_depositor_comments
'Adding full bibliography for 7716981--7716983.cif.'
_cod_original_formula_sum        'C32 H87.60 Cu13 Gd2 N20 O67.80'
_cod_database_code               7716981
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.201
_shelx_estimated_absorpt_t_max   0.645
_shelx_res_checksum              7382
_shelx_hkl_checksum              78840