Structures, fluorescence properties and magnetic properties of a series of rhombus-shaped LnIII4 clusters: magnetocaloric effect and single-molecule-magnet behavior
Wang, Wen-Min; Zhang, Li; Li, Xian-Zhen; He, Li-Yuan; Wang, Xin-Xin; Shi, Ying; Wang, Jie; Dong, Jie; Wu, Zhi-Lei; New Journal of Chemistry 43 (2019) 12941–; doi:10.1039/C9NJ02872B

data_7058612
_publ_section_title
;
 Structures, fluorescence properties and magnetic properties of a series
 of rhombus-shaped LnIII4 clusters: magnetocaloric effect and
 single-molecule-magnet behavior
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12941
_journal_paper_doi               10.1039/C9NJ02872B
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C128 H120 Er4 N12 O16, 2(C2 H3 N)'
_chemical_formula_sum            'C132 H126 Er4 N14 O16'
_chemical_formula_weight         2833.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-01 deposited with the CCDC.    2019-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                99.075(2)
_cell_angle_beta                 93.174(4)
_cell_angle_gamma                111.225(4)
_cell_formula_units_Z            1
_cell_length_a                   12.890(3)
_cell_length_b                   15.336(3)
_cell_length_c                   16.618(3)
_cell_measurement_reflns_used    8980
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3001.2(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38475
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.608
_diffrn_reflns_theta_min         3.012
_exptl_absorpt_coefficient_mu    2.839
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.171
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         13537
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0431P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11372
_reflns_number_total             13537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02872b2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7058609--7058615.cif.'
_cod_database_code               7058612
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.601
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C13 \\sim C14: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 O8(H8)
3.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C35(H35A,H35B), C53(H53A,H53B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C28(H28),
  C30(H30), C31(H31), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39),
 C42(H42), C43(H43), C46(H46), C48(H48), C49(H49), C51(H51), C52(H52), C57(H57),
  C62(H62)
3.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C36(H36A,H36B,H36C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C65(H65A,
 H65B,H65C)
;
_shelx_res_checksum              39515
_olex2_submission_special_instructions 'No special instructions were received'