A series of [2 × 2] square grid LnIII4 clusters: a large magnetocaloric effect and single-molecule-magnet behavior
Wang, Wen-Min; Li, Xian-Zhen; Zhang, Li; Chen, Jia-Li; Wang, Jun-Hua; Wu, Zhi-Lei; Cui, Jian-Zhong; New Journal of Chemistry 43 (2019) 7419–; doi:10.1039/C8NJ04454F

data_7058285
_publ_section_title
;
 A series of [2 \\times 2] square grid LnIII4 clusters: a large
 magnetocaloric effect and single-molecule-magnet behavior
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7419
_journal_paper_doi               10.1039/C8NJ04454F
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C60 H56 Gd4 N12 O16, 4(C H4 O)'
_chemical_formula_sum            'C64 H72 Gd4 N12 O20'
_chemical_formula_weight         1958.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-08 deposited with the CCDC.    2019-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.0660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.4296(10)
_cell_length_b                   8.4017(3)
_cell_length_c                   30.5551(10)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.54
_cell_volume                     6855.3(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.0
_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  0.0605
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            40689
_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         26.021
_diffrn_reflns_theta_min         2.414
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.902
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0851 before and 0.0609 after correction.
The Ratio of minimum to maximum transmission is 0.6924.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_description       block
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.154
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         6748
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+51.5849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5300
_reflns_number_total             6748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04454f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7058283--7058286.cif.'
_cod_database_code               7058285
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.631
_shelx_estimated_absorpt_t_min   0.368
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O4-H4
 0.87 with sigma of 0.01
 O1-H1
 0.85 with sigma of 0.02
 C15-H4
 1.895697 with sigma of 0.02
 Gd1-H4
 3.07824 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O10 \\sim C32: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C10(H10), C12(H12), C13(H13), C26(H26), C22(H22), C5(H5),
 C19(H19), C8(H8), C27(H27), C4(H4A), C17(H17), C3(H3), C11(H11), C18(H18)
4.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C32(H32A,H32B,
 H32C)
4.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O10(H10A)
;
_shelx_res_checksum              8865
_olex2_submission_special_instructions 'No special instructions were received'