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_4336903
_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         '2(C60 H115 Ni3 O28 P3 Y3)'
_chemical_formula_sum            'C120 H230 Ni6 O56 P6 Y6'
_chemical_formula_weight         3640.57
_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     iterative
_audit_creation_date             2013-08-30
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;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_audit_update_record
;
2013-09-01 # Formatted by publCIF

;
_cell_angle_alpha                84.0060(18)
_cell_angle_beta                 88.9737(18)
_cell_angle_gamma                89.5098(16)
_cell_formula_units_Z            2
_cell_length_a                   16.6447(4)
_cell_length_b                   20.5345(4)
_cell_length_c                   25.1562(6)
_cell_measurement_reflns_used    17821
_cell_measurement_temperature    128.40(10)
_cell_measurement_theta_max      26.2670
_cell_measurement_theta_min      3.2250
_cell_volume                     8549.6(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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      128.40(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.9979
_diffrn_measured_fraction_theta_max 0.9979
_diffrn_measurement_details
;
  1 omega  -42.00   -1.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  -57.0000 -120.0000 41

  2 omega   10.00   49.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673   57.0000   60.0000 39

  3 omega  -51.00    0.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  -77.0000    0.0000 51

  4 omega  -11.00   66.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  -99.0000  -60.0000 77

  5 omega   35.00   95.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  178.0000  -60.0000 60

  6 omega  -89.00   -1.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000   30.0000 88

  7 omega  -61.00  -36.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798 -178.0000  150.0000 25

  8 omega  -93.00   11.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000  120.0000 104
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0189063000
_diffrn_orient_matrix_UB_12      0.0022174000
_diffrn_orient_matrix_UB_13      0.0247866000
_diffrn_orient_matrix_UB_21      -0.0169872000
_diffrn_orient_matrix_UB_22      0.0316258000
_diffrn_orient_matrix_UB_23      0.0011690000
_diffrn_orient_matrix_UB_31      -0.0342142000
_diffrn_orient_matrix_UB_32      -0.0141859000
_diffrn_orient_matrix_UB_33      0.0137208000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            71957
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.981
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    2.784
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.414
_exptl_crystal_description       plate
_exptl_crystal_F_000             3780
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.743
_refine_diff_density_min         -1.572
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1549
_refine_ls_number_reflns         34886
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0919P)^2^+39.3827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.2015
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22742
_reflns_number_total             34886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402296t_si_006.cif
_cod_data_source_block           Ni6Y6P6_hexyl
_cod_database_code               4336903