Enhancement of Magnetocaloric Effect through Fixation of Carbon Dioxide: Molecular Assembly from Ln<sub>4</sub> to Ln<sub>4</sub> Cluster Pairs.
Wu, Jianfeng; Li, Xiao-Lei; Zhao, Lang; Guo, Mei; Tang, Jinkui; Inorganic chemistry 56 (2017) 4104–4111; doi:10.1021/acs.inorgchem.7b00094

data_4349396
_publ_section_title
;
 Enhancement of Magnetocaloric Effect through Fixation of Carbon Dioxide:
 Molecular Assembly from Ln<sub>4</sub> to Ln<sub>4</sub> Cluster Pairs.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4104
_journal_page_last               4111
_journal_paper_doi               10.1021/acs.inorgchem.7b00094
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C134 H120 N8 O42 Tb8, 2(C2 H3 N)'
_chemical_formula_sum            'C138 H130 N10 O42 Tb8'
_chemical_formula_weight         3871.87
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-18
_audit_creation_method
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Olex2 1.2-beta
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
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_cell_angle_alpha                90
_cell_angle_beta                 114.844(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5040(11)
_cell_length_b                   32.684(2)
_cell_length_c                   18.1251(10)
_cell_measurement_reflns_used    8914
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.39
_cell_volume                     7797.0(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1110
_diffrn_reflns_av_unetI/netI     0.1239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47530
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.18
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    3.653
_exptl_absorpt_correction_T_max  0.464
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.649
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_exptl_crystal_F_000             3768
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
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_refine_diff_density_min         -1.644
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         15491
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_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+47.3222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9446
_reflns_number_total             15491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00094_si_002.cif
_cod_data_source_block           Tb8
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'multi_scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4349396
_shelx_shelxl_version_number     2014/7
_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
2. Restrained distances
 C9-C10 = C9-C11 = C30-C29 = C29-C28
 1.52 with sigma of 0.02
 C61-C62 = C68-C69
 1.52 with sigma of 0.01
 C10-C11
 2.48 with sigma of 0.02
3. Rigid bond restraints
 C4, C5, C9, C10, N2, C11, C9, C11, N1, C9, C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(C31) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(N5) \\sim Ueq,
Uanis(C68) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C9(H9), C29(H29)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C28(H28A,H28B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C14(H14), C15(H15), C16(H16),
 C22(H22), C23(H23), C24(H24), C27(H27), C31(H31), C33(H33), C34(H34), C35(H35),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C49(H49), C50(H50),
 C51(H51), C52(H52), C53(H53), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
  C63(H63), C64(H64), C65(H65), C66(H66), C67(H67)
5.d Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C13(C14,C15,C16,C17,C18), C21(C22,C23,C24,C25,C26),
 C32(C33,C34,C35,C36,C37), C41(C42,C43,C44,C45,C46), C48(C49,C50,C51,C52,C53),
 C55(C56,C57,C58,C59,C60), C62(C63,C64,C65,C66,C67)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C30(H30A,H30B,
 H30C), C38(H38A,H38B,H38C), C10(H10A,H10B,H10C), C69(H69A,H69B,H69C)
;
_olex2_submission_special_instructions 'No special instructions were received'