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_7034772
_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 H143 N14 O44 Sm6 Zn2, 38(C H4 O), H2 O'
_chemical_formula_sum            'C141 H297 N14 O83 Sm6 Zn2'
_chemical_formula_weight         4549.75
_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     iterative
_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                71.8490(9)
_cell_angle_beta                 88.2919(9)
_cell_angle_gamma                63.4640(9)
_cell_formula_units_Z            2
_cell_length_a                   20.7294(4)
_cell_length_b                   22.2218(4)
_cell_length_c                   25.3356(4)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      2.17
_cell_volume                     9839.2(3)
_computing_cell_refinement       '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, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Bruker SMART APEXII diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.925
_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            214854
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.246
_diffrn_reflns_theta_min         1.107
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.092
_exptl_absorpt_correction_T_max  0.8909
_exptl_absorpt_correction_T_min  0.6581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0741 before and 0.0585 after correction.
The Ratio of minimum to maximum transmission is 0.7387.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             4674
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.144
_platon_squeeze_details          'see _refine_special_details'
_refine_diff_density_max         2.282
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1709
_refine_ls_number_reflns         45021
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0391
_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^+12.6049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30965
_reflns_number_total             45021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01240f2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7034769--7034773.cif.'
_cod_database_code               7034772
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(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
 O103-H10V = O103-H10U
 0.84 with sigma of 0.02
 O44-H44
 0.84 with sigma of 0.02
 H10U-H10V
 1.35 with sigma of 0.04
 N1-H1 \\sim N3-H3 \\sim N5-H5 \\sim N7-H7A \\sim N9-H9
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C105, O105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O109, C109
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C111, O111
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a 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)
5.b 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), C98(H98)
5.c Tetrahedral OH refined with riding coordinates:
 O18(H18), O101(H101), O102(H102), O105(H105), O106(H106), O109(H109),
 O111(H111)
5.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), C105(H10L,H10M,H10N), C106(H10O,
 H10P,H10Q), C109(H10R,H10S,H10T), C111(H11C,H11D,H11E)
5.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O7(H7), O12(H12), O14(H14), O15(H15), O19(H19), O20(H20), O22(H22),
 O23(H23), O26(H26), O28(H28), O100(H100)
;
_shelx_res_checksum              94754
_shelx_fab_checksum              2586
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 8/11/13
_olex2_date_sample_submission    20/10/13
_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-1347
_olex2_submission_special_instructions 'No special instructions were received'