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_7034770
_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 Dy6 N14 O44 Zn2, N O3, 31(C H4 O), H2 O'
_chemical_formula_sum            'C134 H271 Dy6 N15 O79 Zn2'
_chemical_formula_weight         4462.38
_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                71.9837(14)
_cell_angle_beta                 88.2024(10)
_cell_angle_gamma                64.4382(15)
_cell_formula_units_Z            2
_cell_length_a                   20.6705(3)
_cell_length_b                   21.9660(4)
_cell_length_c                   25.1531(3)
_cell_measurement_reflns_used    43831
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.4790
_cell_measurement_theta_min      3.0760
_cell_volume                     9728.1(3)
_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 0.854
_diffrn_measurement_details
;
  1 omega  -80.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -77.0000 -180.0000 104

  2 omega  -56.00   19.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -57.0000    0.0000 75

  3 omega  -94.00  -51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352    0.0000   60.0000 43

  4 omega  -52.00  -21.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  121.0000   -5.6129 31

  5 omega  -20.00   25.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -99.0000 -120.0000 45

  6 omega  -82.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -19.0000  -90.0000 90

  7 omega    4.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -99.0000  -90.0000 27

  8 omega   52.00   79.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  156.0000   84.9304 27

  9 omega   34.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633   19.0000   30.0000 28

 10 omega    5.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633 -114.0000   67.4787 28

 11 omega  -34.00    9.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352   57.0000  -60.0000 43

 12 omega    7.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633 -133.0000 -140.2675 62
;
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0120573000
_diffrn_orient_matrix_UB_12      -0.0373564000
_diffrn_orient_matrix_UB_13      0.0124889000
_diffrn_orient_matrix_UB_21      -0.0252758000
_diffrn_orient_matrix_UB_22      0.0061745000
_diffrn_orient_matrix_UB_23      0.0197773000
_diffrn_orient_matrix_UB_31      -0.0261421000
_diffrn_orient_matrix_UB_32      0.0014404000
_diffrn_orient_matrix_UB_33      -0.0185697000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            159016
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.974
_diffrn_reflns_theta_min         2.751
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.605
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.334
_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    1.523
_exptl_crystal_description       plate
_exptl_crystal_F_000             4536
_exptl_crystal_size_max          0.4576
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.0328
_platon_squeeze_details          '27 MeOH removed with SQUEEZE.'
_refine_diff_density_max         1.913
_refine_diff_density_min         -1.443
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1703
_refine_ls_number_reflns         44027
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0464P)^2^+64.1551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30393
_reflns_number_total             44027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01240f2.cif
_cod_data_source_block           eb3254
_cod_depositor_comments
'Adding full bibliography for 7034769--7034773.cif.'
_cod_database_code               7034770
_chemical_oxdiff_formula         'C80 H200 N10 O20 Dy6 Zn2'
_chemical_oxdiff_usercomment     '@ 120 K C-1373.1'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H104 of O104, H44 of O44, H28' of O28', H28 of O28, H26 of
  O26, H22 of O22, H20 of O20, H19 of O19, H18 of O18, H15 of O15, H12 of O12,
  H11 of O11, H7 of O7, H4 of O4, H101 of O101, H102 of O102, All C(H,H) groups,
   All N(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H14 of O14, H100 of O100
2. Shared sites
{C97, C97'}
3. Restrained distances
 O28-C98 = O28'-C98'
 1.43 with sigma of 0.01
 H10P-H10O
 1.35 with sigma of 0.02
 O47-N20 \\sim O45-N20 \\sim O46-N20
 with sigma of 0.02
 O46-O47 \\sim O47-O45 \\sim O45-O46
 with sigma of 0.02
 N14-C97' \\sim N14-C97
 with sigma of 0.02
 C98-C97 \\sim C98'-C97'
 with sigma of 0.02
 O28-C98 \\sim O28'-C98'
 with sigma of 0.02
 N1-H1 \\sim N3-H3 \\sim N5-H5 \\sim N7-H7A \\sim N9-H9
 with sigma of 0.02
4. Restrained planarity
 O45, O46, O47, N20
 with sigma of 0.1
5. Rigid bond restraints
 O38, O39, O40, C203
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O30, C200
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O32, C201
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O35, O36, C202
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O38, O39, O40, C203
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O42, O43, C204
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C98, C98
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O28', C98'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
O38 \\sim O39 \\sim O40 \\sim C203: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
O32 \\sim C201: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O35 \\sim O36 \\sim C202: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O38 \\sim O39 \\sim O40 \\sim C203: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
O42 \\sim O43 \\sim C204: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C97 \\sim C98: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O28' \\sim C98': within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C97) = Uanis(C97')
7. 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, C98
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O28, O28', C97, C97', C98, C98'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O101, C101
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O102, C102
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O102, C102
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
8. Others
 Sof(O28')=Sof(H28')=Sof(C97')=Sof(H97C)=Sof(H97D)=Sof(C98')=Sof(H98C)=
 Sof(H98D)=1-FVAR(1)
 Sof(O28)=Sof(H28)=Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(C98)=Sof(H98A)=Sof(H98B)=
 FVAR(1)
9.a Free rotating group:
 O103(H10O,H10P)
9.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), C97'(H97C,H97D), C98(H98A,H98B), C98'(H98C,H98D)
9.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), 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)
9.d Tetrahedral OH refined with riding coordinates:
 O15(H15), O18(H18), O28(H28), O28'(H28'), O100(H100), O101(H101), O102(H102),
 O104(H104)
9.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), C102(H10I,H10J,H10K), C104(H10L,H10M,H10N)
9.f Idealised tetrahedral OH refined as rotating group:
 O4(H4), O7(H7), O11(H11), O12(H12), O14(H14), O19(H19), O20(H20), O22(H22),
 O23(H23), O26(H26)
;
_shelx_res_checksum              78913
_shelx_fab_checksum              69641
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 14/11/13
_olex2_date_sample_submission    4/11/13
_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_original_sample_id C-1373.1
_olex2_submission_special_instructions 'No special instructions were received'