Solvent-induced formation of two gadolinium clusters demonstrating strong magnetocaloric effects and ferroelectric properties.
Wang, Yu-Xia; Xu, Qiutong; Ren, Peng; Shi, Wei; Cheng, Peng; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2228–2233; doi:10.1039/c8dt04267e

data_7048732
_publ_section_title
;
 Solvent-induced formation of two gadolinium clusters demonstrating strong
 magnetocaloric effects and ferroelectric properties.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2228
_journal_page_last               2233
_journal_paper_doi               10.1039/c8dt04267e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C20 H43 Gd3 N8 O20, C2 H6 O'
_chemical_formula_sum            'C22 H49 Gd3 N8 O21'
_chemical_formula_weight         1230.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-29
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-20 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.3822(6)
_cell_length_b                   14.9641(3)
_cell_length_c                   9.0770(2)
_cell_measurement_reflns_used    4683
_cell_measurement_temperature    293.00(14)
_cell_measurement_theta_max      29.1449
_cell_measurement_theta_min      2.5419
_cell_volume                     3855.13(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.00(14)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   12.00   59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935  -99.0000  -90.0000 47

  2 omega   56.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   57.0000  -60.0000 30

  3 omega  -80.00  -10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185  -57.0000   30.0000 70
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0031889000
_diffrn_orient_matrix_UB_12      -0.0219946000
_diffrn_orient_matrix_UB_13      0.0684857000
_diffrn_orient_matrix_UB_21      0.0013099000
_diffrn_orient_matrix_UB_22      0.0419944000
_diffrn_orient_matrix_UB_23      0.0360183000
_diffrn_orient_matrix_UB_31      -0.0247543000
_diffrn_orient_matrix_UB_32      -0.0006133000
_diffrn_orient_matrix_UB_33      0.0107294000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9519
_diffrn_reflns_point_group_measured_fraction_full 0.727
_diffrn_reflns_point_group_measured_fraction_max 0.727
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.547
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
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_refine_ls_abs_structure_Flack   -0.037(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         4935
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0026P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.365
_reflns_Friedel_fraction_full    0.418
_reflns_Friedel_fraction_max     0.418
_reflns_number_gt                4367
_reflns_number_total             4935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04267e2.cif
_cod_data_source_block           2-293K
_cod_depositor_comments
'Adding full bibliography for 7048730--7048734.cif.'
_cod_original_cell_volume        3855.15(16)
_cod_database_code               7048732
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C12Sm1
_chemical_oxdiff_usercomment     GD-120K
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.552
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.01
 O6-H6
 0.85 with sigma of 0.01
 O5-H5
 0.85 with sigma of 0.01
 C2AA-C1AA = C3AA-C0AA
 1.54 with sigma of 0.01
 C11-H8
 1.923651 with sigma of 0.02
 C10-H6
 1.899884 with sigma of 0.02
 C4-H5
 1.88822 with sigma of 0.02
 C2AA-C1AA \\sim C1AA-C0AA
 with sigma of 0.01
 C3AA-C0AA \\sim C2AA-C1AA
 with sigma of 0.01
 O3AA-C2AA \\sim O0AA-C3AA
 with sigma of 0.01
 O3AA-C1AA \\sim O0AA-C0AA
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O0AA \\sim C3AA \\sim C0AA \\sim O3AA \\sim C2AA \\sim C1AA: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O0AA) \\sim Ueq, Uanis(O3AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq,
Uanis(C2AA) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(O0AA)=Sof(H0AD)=Sof(C3AA)=
 Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(O3AA)=Sof(H3AA)=Sof(C2AA)=
 Sof(H2AA)=Sof(H2AB)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C2AA(H2AA,
 H2AB), C3AA(H3AB,H3AC)
5.b Idealised Me refined as rotating group:
 C1AA(H1AA,H1AB,H1AC), C0AA(H0AA,H0AB,H0AC)
5.c Idealised tetrahedral OH refined as rotating group:
 O3AA(H3AA), O0AA(H0AD)
;
_olex2_submission_special_instructions 'No special instructions were received'