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_7034771
_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 H144 Gd6 N14 O44 Zn2, N O3, 31(C H4 O), H2 O'
_chemical_formula_sum            'C134 H270 Gd6 N43 O79 Zn2'
_chemical_formula_weight         4822.15
_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
_atom_sites_solution_primary     direct
_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                71.9252(14)
_cell_angle_beta                 88.2848(12)
_cell_angle_gamma                63.8427(17)
_cell_formula_units_Z            2
_cell_length_a                   20.6864(3)
_cell_length_b                   22.1669(4)
_cell_length_c                   25.2175(4)
_cell_measurement_reflns_used    130966
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.0420
_cell_measurement_theta_min      3.0800
_cell_volume                     9789.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_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    9.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633 -133.0000   20.6584 60

  2 omega  -23.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633   77.0000  -30.0000 76

  3 omega    7.00   79.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633   57.0000   90.0000 72

  4 omega  -14.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633   38.0000 -150.0000 95

  5 omega  -55.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -38.0000   30.0000 86

  6 omega  -19.00   48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -99.0000  -90.0000 67

  7 omega  -65.00   40.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -77.0000 -180.0000 105

  8 omega   17.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633 -153.0000  142.7422 66

  9 omega  -53.00  -20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  -57.0000    0.0000 33

 10 omega   30.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912   57.0000  150.0000 55

 11 omega  -15.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912   77.0000   60.0000 103

 12 omega   12.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912   38.0000  -90.0000 43

 13 omega   -9.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912   73.0000  -76.0000 94

 14 omega  -84.00  -36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0850  149.0000 -136.3878 48

 15 omega  -20.00   36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  -99.0000  150.0000 56

 16 omega  -81.00  -34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0850  145.0000   57.2570 47

 17 omega  -11.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912 -110.0000   65.9331 72

 18 omega  -59.00   46.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  -77.0000 -180.0000 105

 19 omega  -20.00   38.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  -99.0000  -90.0000 58

 20 omega   34.00  100.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912 -178.0000  -60.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0061076000
_diffrn_orient_matrix_UB_12      0.0338646000
_diffrn_orient_matrix_UB_13      -0.0187791000
_diffrn_orient_matrix_UB_21      0.0275600000
_diffrn_orient_matrix_UB_22      -0.0167465000
_diffrn_orient_matrix_UB_23      -0.0153939000
_diffrn_orient_matrix_UB_31      -0.0261852000
_diffrn_orient_matrix_UB_32      -0.0002947000
_diffrn_orient_matrix_UB_33      -0.0173126000
_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     0.0517
_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            400725
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.220
_diffrn_reflns_theta_min         2.809
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.342
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1120 before and 0.0691 after correction.
The Ratio of minimum to maximum transmission is 0.6929.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       block
_exptl_crystal_F_000             4902
_exptl_crystal_size_max          0.578
_exptl_crystal_size_mid          0.3932
_exptl_crystal_size_min          0.1282
_platon_squeeze_details          ' see _refine_special_details'
_refine_diff_density_max         2.355
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1683
_refine_ls_number_reflns         57700
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0294P)^2^+64.1611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                44403
_reflns_number_total             57700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01240f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7034769--7034773.cif.'
_cod_database_code               7034771
_chemical_oxdiff_formula         'C100 H200 N10 O40 Gd10 Zn10'
_chemical_oxdiff_usercomment     '@ 120 K C-1281'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H4 of O4, H7 of O7, H8 of O8, H12 of O12, H18 of O18, H19
  of O19, H20 of O20, H22 of O22, H26 of O26, H28 of O28, H44 of O44, All C(H,
  H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H14 of O14, H100 of O100, H101 of O101, H102 of O102
2. Restrained distances
 O46-N20 \\sim O47-N20 \\sim O45-N20
 with sigma of 0.02
 N1-H1 \\sim N3-H3A \\sim N7-H7A \\sim N5-H5 \\sim N9-H9
 with sigma of 0.02
3. Rigid bond restraints
 O38, O39, O40, C114
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O30, C111
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O32, C112
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O35, O36, C113
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O42, O43, C115
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O38 \\sim O39 \\sim O40 \\sim C114: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
O32 \\sim C112: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O35 \\sim O36 \\sim C113: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O42 \\sim O43 \\sim C115: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(O28) \\sim Ueq, Uanis(C98) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
5. 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
6.a Free rotating group:
 O103(H10L,H10M)
6.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), 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)
6.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), C68(H68), C73(H73), C75(H75), C87(H87), C89(H89)
6.d 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)
6.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O7(H7), O8(H8), O12(H12), O14(H14), O18(H18), O19(H19), O20(H20),
 O22(H22), O23(H23), O26(H26), O28(H28), O100(H100), O101(H101), O102(H102)
;
_shelx_res_checksum              56674
_shelx_fab_checksum              29556
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 9/10/13
_olex2_date_sample_submission    8/10/13
_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-1281
_olex2_submission_special_instructions 'No special instructions were received'