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_4349793
_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         'C59 H73 Er4 N13 O23, C H4 O, H2 O'
_chemical_formula_sum            'C60 H79 Er4 N13 O25'
_chemical_formula_weight         2051.40
_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'
_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                 127.7200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.452(2)
_cell_length_b                   32.301(2)
_cell_length_c                   19.9402(15)
_cell_measurement_reflns_used    20324
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     15005.2(18)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_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_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.979
_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  0.0455
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            76320
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.686
_diffrn_reflns_theta_min         3.013
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.511
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   REQAB(Rigaku,1998)
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             8016
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.630
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     948
_refine_ls_number_reflns         17204
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0235P)^2^+66.8638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15020
_reflns_number_total             17204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00658f2.cif
_cod_data_source_block           m20161021h1_sq
_cod_original_cell_volume        15005.5(19)
_cod_database_code               4349793
_shelx_shelxl_version_number     2014/8
_shelx_estimated_absorpt_t_max   0.614
_shelx_estimated_absorpt_t_min   0.437
_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
 O21-H21
 0.87 with sigma of 0.01
 C58-H21
 1.912983 with sigma of 0.02
 Er4-H21
 3.091569 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O24) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Free rotating group:
 O27(H27A,H27B)
4.b Rotating group:
 O22(H22A,H22B), O23(H23A,H23B)
4.c 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), C55(H55)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C22(H22C,H22D,
 H22E), 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), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C)
4.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6), O9(H9), O12(H12), O24(H24A)
;
_shelx_res_checksum              85619
_shelx_hkl_checksum              32508
_shelx_fab_checksum              15529
_olex2_submission_special_instructions 'No special instructions were received'