Wells-Dawson Cages as Molecular Refrigerants
Eufemio Moreno Pineda; Floriana Tuna; Yan-Zhen Zheng; Richard E. P. Winpenny; Eric J. L. McInnes; Inorganic Chemistry 52 (2013) 13702–13707; doi:10.1021/ic402296t

data_4336900
_publ_contact_author_address
;
School of Chemistry and Photon Science Institute, The University of Manchester,
Oxford Road, Manchester M13 9PL, .
UK
;
_publ_contact_author_name        'Richard E. P. Winpenny'
_publ_section_title
;
 Wells-Dawson Cages as Molecular Refrigerants
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13702
_journal_page_last               13707
_journal_paper_doi               10.1021/ic402296t
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C90 H170 Gd6 Ni6 O56 P6, 2(C2 H3 N)'
_chemical_formula_sum            'C94 H176 Gd6 N2 Ni6 O56 P6'
_chemical_formula_weight         3711.94
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-08-30
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_audit_update_record
;
2013-08-30 # Formatted by publCIF

;
_cell_angle_alpha                104.512(3)
_cell_angle_beta                 101.152(3)
_cell_angle_gamma                100.934(3)
_cell_formula_units_Z            1
_cell_length_a                   15.4495(5)
_cell_length_b                   16.0319(5)
_cell_length_c                   16.3513(6)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      26.3470
_cell_measurement_theta_min      3.1210
_cell_volume                     3723.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      104(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.9981
_diffrn_measurement_details
;
  1 omega -105.00   11.00   1.0000   63.5100
omega____ theta____ kappa____ phi______ frames
    -      -21.0746  -63.0000 -102.0000 116

  2 omega   -7.00   23.00   1.0000   63.5100
omega____ theta____ kappa____ phi______ frames
    -      -21.0746  -99.0000 -180.0000 30

  3 omega   -3.00   61.00   1.0000   63.5100
omega____ theta____ kappa____ phi______ frames
    -       22.4808  -99.0000  150.0000 64

  4 omega  -63.00   -8.00   1.0000   63.5100
omega____ theta____ kappa____ phi______ frames
    -       22.4808  -37.0000  120.0000 55

  5 omega   32.00   57.00   1.0000   63.5100
omega____ theta____ kappa____ phi______ frames
    -       22.4808  -37.0000  120.0000 25

  6 omega  -70.00   48.00   1.0000   63.5100
omega____ theta____ kappa____ phi______ frames
    -       22.4808  -77.0000   30.0000 118
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0070460000
_diffrn_orient_matrix_UB_12      0.0381546000
_diffrn_orient_matrix_UB_13      0.0283067000
_diffrn_orient_matrix_UB_21      -0.0259310000
_diffrn_orient_matrix_UB_22      -0.0276282000
_diffrn_orient_matrix_UB_23      0.0190068000
_diffrn_orient_matrix_UB_31      0.0401812000
_diffrn_orient_matrix_UB_32      0.0031000000
_diffrn_orient_matrix_UB_33      0.0313546000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.1115
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25797
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.938
_diffrn_source                   'Enhance (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    3.511
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       block
_exptl_crystal_F_000             1844
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.056
_refine_diff_density_min         -1.823
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         15168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0423P)^2^+15.2647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10992
_reflns_number_total             15168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402296t_si_003.cif
_cod_data_source_block           Ni6Gd6P6_methyl
_cod_original_cell_volume        3723.9(2)
_cod_database_code               4336900