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_4336901
_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        'Eufemio Moreno Pineda'
_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 H254 Gd6 Ni6 O56 P6, 4(C2 H3 N)'
_chemical_formula_sum            'C140 H266 Gd6 N4 Ni6 O56 P6'
_chemical_formula_weight         4383.13
_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             2013-08-26
_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                79.888(2)
_cell_angle_beta                 70.274(2)
_cell_angle_gamma                68.785(2)
_cell_formula_units_Z            1
_cell_length_a                   16.4562(4)
_cell_length_b                   17.6336(4)
_cell_length_c                   18.5683(4)
_cell_measurement_reflns_used    17298
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      26.3750
_cell_measurement_theta_min      1.8080
_cell_volume                     4719.5(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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
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      100.15
_diffrn_measured_fraction_theta_full 0.9848
_diffrn_measured_fraction_theta_max 0.9848
_diffrn_measurement_details
;
  1 omega    2.20  182.15   0.2999    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000   73.8966  -25.8022 600

  2 omega    2.20  182.15   0.2999    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000   73.8966   94.1986 600

  3 omega    2.20  182.15   0.2999    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000   73.8966  214.1966 600
;
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0420920000
_diffrn_orient_matrix_UB_12      -0.0220695000
_diffrn_orient_matrix_UB_13      -0.0254520000
_diffrn_orient_matrix_UB_21      0.0234322000
_diffrn_orient_matrix_UB_22      0.0175982000
_diffrn_orient_matrix_UB_23      0.0144764000
_diffrn_orient_matrix_UB_31      0.0051087000
_diffrn_orient_matrix_UB_32      -0.0327407000
_diffrn_orient_matrix_UB_33      0.0282059000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37205
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.651
_diffrn_source                   'Enhance (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    2.783
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84399
_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    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.517
_refine_diff_density_min         -1.644
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         19008
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+46.4142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15932
_reflns_number_total             19008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402296t_si_004.cif
_cod_data_source_block           Ni6Gd6P6_octyl
_cod_database_code               4336901