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_4349397
_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         'C80 H70 Dy4 N4 O21, 2(C H4 O), H2 O'
_chemical_formula_sum            'C82 H80 Dy4 N4 O24'
_chemical_formula_weight         2155.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-17
_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                101.9800(10)
_cell_angle_beta                 106.2790(10)
_cell_angle_gamma                90.9140(10)
_cell_formula_units_Z            2
_cell_length_a                   14.8351(7)
_cell_length_b                   15.0820(7)
_cell_length_c                   20.5183(10)
_cell_measurement_reflns_used    8147
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      2.39
_cell_volume                     4297.3(4)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0774
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22145
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.167
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    3.512
_exptl_absorpt_correction_T_max  0.478
_exptl_absorpt_correction_T_min  0.464
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
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_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.395
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_R_factor_gt           0.0472
_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^)+(0.0664P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10955
_reflns_number_total             15169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00094_si_002.cif
_cod_data_source_block           Dy4
_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               4349397
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H25-H82A = H25-H82B
 2.15 with sigma of 0.02
3. Rigid bond restraints
 O22, C83
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C68, C73, C69, C70, C70, C71, C71, C72, C72, C73
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73)
\\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5.a Riding coordinates:
 O23(H23A,H23B)
5.b Ternary CH refined with riding coordinates:
 C10(H10), C29(H29)
5.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C28(H28A,H28B)
5.d 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), C69(H69), C70(H70),
 C71(H71), C72(H72), C73(H73), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80)
5.e Fitted hexagon refined as free rotating group:
 C68(C69,C70,C71,C72,C73)
5.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C30(H30A,H30B,H30C), C38(H38A,H38B,H38C), C82(H82A,H82B,H82C), C83(H83A,
 H83B,H83C)
5.g Idealised tetrahedral OH refined as rotating group:
 O25(H25), O22(H22A)
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_olex2_submission_special_instructions 'No special instructions were received'