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_4349394
_publ_section_title
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 Enhancement of Magnetocaloric Effect through Fixation of Carbon Dioxide:
 Molecular Assembly from Ln<sub>4</sub> to Ln<sub>4</sub> Cluster Pairs.
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_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 Dy8 N8 O42, 4(C H4 O), 2(O)'
_chemical_formula_sum            'C138 H144 Dy8 N8 O48'
_chemical_formula_weight         3982.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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
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_cell_angle_gamma                90
_cell_formula_units_Z            2
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_cell_length_b                   18.3023(15)
_cell_length_c                   26.224(2)
_cell_measurement_reflns_used    5614
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.59
_cell_measurement_theta_min      2.23
_cell_volume                     6983.3(10)
_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      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.1490
_diffrn_reflns_av_unetI/netI     0.1708
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            44323
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         0.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.313
_exptl_absorpt_correction_T_max  0.404
_exptl_absorpt_correction_T_min  0.386
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
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_exptl_crystal_description       block
_exptl_crystal_F_000             3880
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_refine_diff_density_min         -1.522
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
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_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
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_reflns_Friedel_coverage         0.000
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_reflns_number_total             13783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00094_si_002.cif
_cod_data_source_block           Dy8
_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               4349394
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
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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
 O23-C69
 1.45 with sigma of 0.02
 C29-C30 = C9-C10 = C10-C11 = C28-C29 = N4-C30
 1.5 with sigma of 0.02
 C9-C11 = C11-N2 = C30-C28 = C28-N3
 2.49 with sigma of 0.02
3. Rigid bond restraints
 O8, C38, N2, C10, N4, C30, C9, C10, C23, C24, N2, C10, N2, C12, C12, C13, C43,
  C44, N3, C29
 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(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O22) \\sim Ueq,
Uanis(O23) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(O24)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C10(H10), C29(H29)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C30(H30A,H30B)
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),
  C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C48(H48), C49(H49),
 C50(H50), C51(H51), C52(H52), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
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), C40(C41,C42,C43,C44,C45), C47(C48,C49,C50,C51,C52),
 C54(C55,C56,C57,C58,C59), C61(C62,C63,C64,C65,C66)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C68(H68A,H68B,H68C), C69(H69A,
 H69B,H69C)
5.f Idealised tetrahedral OH refined as rotating group:
 O22(H22A), O23(H23A)
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_olex2_submission_special_instructions 'No special instructions were received'