Luminescence and magnetocaloric effect of Ln4 clusters (Ln = Eu, Gd, Tb, Er) bridged by CO32− deriving from the spontaneous fixation of carbon dioxide in the atmosphere
Chen, Hong-Man; Wang, Wen-Min; Li, Xiao-Qin; Chu, Xiao-Ya; Nie, Yao-Yao; Liu, Zhen; Huang, Shao-Xia; Shen, Hai-Yun; Cui, Jian-Zhong; Gao, Hong-Ling; Inorganic Chemistry Frontiers 5 (2018) 394–; doi:10.1039/C7QI00658F

data_4349791
_publ_section_title
;
 Luminescence and magnetocaloric effect of Ln4 clusters (Ln = Eu, Gd, Tb,
 Er) bridged by CO32&#x2212; deriving from the spontaneous fixation of
 carbon dioxide in the atmosphere
;
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              394
_journal_paper_doi               10.1039/C7QI00658F
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C57 H70 Eu4 N12 O23, 2(C H4 O), 5(H2 O)'
_chemical_formula_sum            'C59 H88 Eu4 N12 O30'
_chemical_formula_weight         2053.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-10-05 deposited with the CCDC.
2017-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.346(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1944(13)
_cell_length_b                   22.2882(17)
_cell_length_c                   21.5409(18)
_cell_measurement_reflns_used    20763
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     7565.1(11)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b42'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Xtalab P200'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            75835
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_min         3.031
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.360
_exptl_absorpt_correction_T_max  0.6883
_exptl_absorpt_correction_T_min  0.5527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4072
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.493
_refine_diff_density_min         -1.379
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         17191
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      2.478
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+8.9601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0606
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14453
_reflns_number_total             17191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00658f2.cif
_cod_data_source_block           shelx
_cod_database_code               4349791
_shelx_shelxl_version_number     2014/8
_shelx_estimated_absorpt_t_max   0.689
_shelx_estimated_absorpt_t_min   0.525
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O27-O31
 0.85 with sigma of 0.01
 O22-H22
 0.87 with sigma of 0.01
 O23-H23
 0.87 with sigma of 0.01
 C55-H22
 1.884264 with sigma of 0.02
 Eu1-H22
 3.127226 with sigma of 0.02
 C56-H23
 1.900045 with sigma of 0.02
 Eu3-H23
 3.110053 with sigma of 0.02
3.a Riding coordinates:
 O30(H30D,H30E), O31(H31A,H31B)
3.b Free rotating group:
 O26(H26A,H26B), O27(H27A,H27B), O28(H28A,H28B)
3.c Rotating group:
 O20(H20A,H20B), O21(H21A,H21B)
3.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C5(H5), C7(H7), C13(H13), C14(H14), C16(H16), C18(H18),
 C24(H24), C25(H25), C27(H27), C29(H29), C35(H35), C36(H36), C38(H38), C40(H40),
  C47(H47), C52(H52)
3.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C22(H22A,H22B,
 H22C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C41(H41A,H41B,H41C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C59(H59A,H59B,
 H59C), C62(H62A,H62B,H62C)
3.f Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6), O9(H9), O12(H12), O24(H24A), O29(H29A)
;
_shelx_res_checksum              2061
_shelx_hkl_checksum              13153
_olex2_submission_special_instructions 'No special instructions were received'