Magnetic and magnetocaloric properties of an unusual family of carbonate-panelled [LnZn] cages.
Sethi, Waqas; Sanz, Sergio; Pedersen, Kasper S.; Sørensen, Mikkel A; Nichol, Gary S.; Lorusso, Giulia; Evangelisti, Marco; Brechin, Euan K.; Piligkos, Stergios; Dalton transactions (Cambridge, England : 2003) 44 (2015) 10315–10320; doi:10.1039/c5dt01240f

data_7034769
_publ_section_title
;
 Magnetic and magnetocaloric properties of an unusual family of
 carbonate-panelled [LnZn] cages.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10315
_journal_page_last               10320
_journal_paper_doi               10.1039/c5dt01240f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C103 H145 Eu6 N14 O44 Zn2, N O3, 30.5(C H4 O), H2 O'
_chemical_formula_sum            'C133.5 H284 Eu6 N15 O78.5 Zn2'
_chemical_formula_weight         4398.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-05-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-07 deposited with the CCDC.
2015-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                71.8158(18)
_cell_angle_beta                 88.3250(15)
_cell_angle_gamma                63.667(2)
_cell_formula_units_Z            2
_cell_length_a                   20.7014(4)
_cell_length_b                   22.2355(5)
_cell_length_c                   25.2949(5)
_cell_measurement_reflns_used    50989
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.7280
_cell_measurement_theta_min      3.0900
_cell_volume                     9832.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_details
;
  1 omega  -91.00  -66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310  169.0000  128.7625 25

  2 omega  -31.00    5.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310   38.0000  120.0000 36

  3 omega  -66.00  -39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310  127.0000  -95.2703 27

  4 omega   22.00   49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310   38.0000  120.0000 27

  5 omega  -18.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310   38.0000  -60.0000 81

  6 omega  -74.00  -28.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310  -38.0000  120.0000 46

  7 omega  -12.00   13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310  -38.0000  120.0000 25

  8 omega  -19.00   30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310  -99.0000  150.0000 49

  9 omega   -1.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -99.0000   60.0000 32

 10 omega   10.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -99.0000 -180.0000 29

 11 omega  -35.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -77.0000 -150.0000 76

 12 omega   -2.00   85.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372   77.0000    0.0000 87

 13 omega  -46.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310   19.0000   90.0000 115

 14 omega  -80.00   17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310  -57.0000  -30.0000 97

 15 omega  -69.00  -27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310  132.0000   -9.6491 42

 16 omega  -20.00   30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310  -99.0000 -120.0000 50

 17 omega  -20.00   20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -99.0000  150.0000 40

 18 omega  -59.00   37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -57.0000  -90.0000 96
;
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0207661000
_diffrn_orient_matrix_UB_12      -0.0375471000
_diffrn_orient_matrix_UB_13      0.0111679000
_diffrn_orient_matrix_UB_21      0.0219421000
_diffrn_orient_matrix_UB_22      0.0037961000
_diffrn_orient_matrix_UB_23      0.0184836000
_diffrn_orient_matrix_UB_31      -0.0239446000
_diffrn_orient_matrix_UB_32      -0.0012721000
_diffrn_orient_matrix_UB_33      0.0204782000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            400774
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.169
_diffrn_reflns_theta_min         2.811
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.211
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.405
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       prism
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          0.5853
_exptl_crystal_size_mid          0.2678
_exptl_crystal_size_min          0.1082
_platon_squeeze_details
'28.5 MeOH per asymmetric unit removed with SQUEEZE'
_refine_diff_density_max         2.306
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1655
_refine_ls_number_reflns         57696
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0292P)^2^+62.5383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                44399
_reflns_number_total             57696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01240f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7034769--7034773.cif.'
_cod_original_formula_sum        'C133.50 H284 Eu6 N15 O78.50 Zn2'
_cod_database_code               7034769
_chemical_oxdiff_formula         'C50 H100 N10 O30 Zn2 Eu6'
_chemical_oxdiff_usercomment     '@ 120 K C-1432'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H44 of O44, H28 of O28, H26 of O26, H22 of O22, H20 of O20,
   H19 of O19, H18 of O18, H12 of O12, H8 of O8, H7 of O7, H4 of O4, H3 of O3,
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H100 of O100, H101 of O101, H14 of O14, All O(H,H) groups
2. Restrained distances
 O44-H44
 0.9 with sigma of 0.01
 N7-H7A = N5-H5 = N1-H1 = N9-H9 = N3-H3A
 0.84 with sigma of 0.02
 O46-N20 \\sim O47-N20 \\sim O45-N20
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O28) \\sim Ueq, Uanis(C98) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 O45, O46, O47, N20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O28, C97, C98
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Free rotating group:
 O102(H10I,H10J)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
  C42(H42A,H42B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B),
 C69(H69A,H69B), C70(H70A,H70B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B),
  C83(H83A,H83B), C84(H84A,H84B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,
 H96B), C97(H97A,H97B), C98(H98A,H98B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3B), C5(H5A), C17(H17), C19(H19A), C31(H31), C33(H33), C45(H45), C47(H47),
  C59(H59), C61(H61), C73(H73), C75(H75), C87(H87), C89(H89)
5.d Tetrahedral OH refined with riding coordinates:
 O19(H19)
5.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C78(H78A,H78B,H78C), C79(H79A,
 H79B,H79C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C100(H10C,H10D,H10E),
 C101(H10F,H10G,H10H)
5.f Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O7(H7), O8(H8), O12(H12), O14(H14), O18(H18), O20(H20),
 O22(H22), O23(H23), O26(H26), O28(H28), O100(H100), O101(H101)
;
_shelx_res_checksum              30368
_shelx_fab_checksum              13237
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 26/11/13
_olex2_date_sample_submission    25/11/13
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'