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_4336905
_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         'C132 H252 Ni6 O56 P6 Y6'
_chemical_formula_sum            'C132 H252 Ni6 O56 P6 Y6'
_chemical_formula_weight         3806.86
_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
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2013-09-01 # Formatted by publCIF

;
_cell_angle_alpha                81.023(6)
_cell_angle_beta                 70.241(5)
_cell_angle_gamma                69.087(7)
_cell_formula_units_Z            1
_cell_length_a                   16.2833(9)
_cell_length_b                   17.5109(15)
_cell_length_c                   18.3682(9)
_cell_measurement_reflns_used    5486
_cell_measurement_temperature    150.03(18)
_cell_measurement_theta_max      23.4480
_cell_measurement_theta_min      3.3110
_cell_volume                     4600.6(6)
_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      150.03(18)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.9974
_diffrn_measurement_details
;
  1 omega   66.00   93.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673 -178.0000  -30.0000 27

  2 omega   -8.00   64.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  -99.0000   30.0000 72

  3 omega   21.00   80.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673 -123.0000 -172.0000 59

  4 omega  -76.00  -36.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  123.0000  -92.0000 40

  5 omega  -17.00   32.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   57.0000  -60.0000 49

  6 omega  -83.00  -37.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798 -178.0000  -30.0000 46

  7 omega  -92.00  -54.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -57.0000  120.0000 38

  8 omega  -97.00   45.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -19.0000  120.0000 142
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0009755000
_diffrn_orient_matrix_UB_12      0.0347871000
_diffrn_orient_matrix_UB_13      -0.0257375000
_diffrn_orient_matrix_UB_21      0.0253007000
_diffrn_orient_matrix_UB_22      -0.0259466000
_diffrn_orient_matrix_UB_23      -0.0317618000
_diffrn_orient_matrix_UB_31      -0.0419305000
_diffrn_orient_matrix_UB_32      0.0001240000
_diffrn_orient_matrix_UB_33      -0.0038853000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0988
_diffrn_reflns_av_unetI/netI     0.1966
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37268
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.993
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    2.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57650
_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    1.374
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.983
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         18760
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.2103
_refine_ls_R_factor_gt           0.0931
_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^)+(0.1289P)^2^+0.7513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2279
_refine_ls_wR_factor_ref         0.2952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8259
_reflns_number_total             18760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402296t_si_008.cif
_cod_data_source_block           Ni6Y6P6_octyl
_cod_database_code               4336905