Lantern-shaped 3d–4f high-nuclearity clusters with magnetocaloric effect
Lin, Qingfang; Li, Jing; Dong, Yayu; Zhou, Guangpeng; Song, You; Xu, Yan; Dalton Transactions 46 (2017) 9745–9749; doi:10.1039/C7DT01978E

data_1546415
_publ_section_title
;
 Lantern-shaped 3d--4f high-nuclearity clusters with magnetocaloric effect
;
_journal_issue                   30
_journal_name_full               'Dalton Transactions'
_journal_page_first              9745
_journal_page_last               9749
_journal_paper_doi               10.1039/C7DT01978E
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C248 H493 Gd52 N54 Ni52 O401.5'
_chemical_formula_weight         21885.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-26 deposited with the CCDC.
2017-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.598(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.737(15)
_cell_length_b                   41.67(2)
_cell_length_c                   29.877(15)
_cell_measurement_reflns_used    9710
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.06
_cell_measurement_theta_min      2.26
_cell_volume                     34103(3)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1167
_diffrn_reflns_av_unetI/netI     0.1391
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            162404
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         0.862
_exptl_absorpt_coefficient_mu    6.466
_exptl_absorpt_correction_T_max  0.511
_exptl_absorpt_correction_T_min  0.424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.131
_exptl_crystal_description       Block
_exptl_crystal_F_000             20710
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_refine_diff_density_max         6.633
_refine_diff_density_min         -3.067
_refine_diff_density_rms         0.503
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1899
_refine_ls_number_reflns         59047
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1361P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2312
_refine_ls_wR_factor_ref         0.2682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32207
_reflns_number_total             59047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01978e2.cif
_cod_data_source_block           a01
_cod_original_cell_volume        34104(30)
_cod_original_formula_sum        'C248 H493 Gd52 N54 Ni52 O401.50'
_cod_database_code               1546415
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.424
_shelx_estimated_absorpt_t_max   0.511
_exptl_absorpt_special_details
;
Rint before and after the absorption correction process are 0.1235 and 0.1186.
;
_shelx_res_checksum              46543