Encapsulated Guest-Host Dynamics: Guest Rotational Barriers and Tumbling as a Probe of Host Interior Cavity Space
Jeffrey S. Mugridge; Géza Szigethy; Robert G. Bergman; Kenneth N. Raymond; Journal of the American Chemical Society 132 (2010) 16256–16264; doi:10.1021/ja107656g

data_4103522
_publ_section_title
;
 Encapsulated Guest-Host Dynamics: Guest Rotational Barriers and Tumbling
 as a Probe of Host Interior Cavity Space
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16256
_journal_page_last               16264
_journal_paper_doi               10.1021/ja107656g
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C149.5 H106.5 N13 O88.5 Ga4, 5(C13 H22 P)'
_chemical_formula_sum            'C214.5 H216.5 Ga4 K3 N13 O44.25 P5'
_chemical_formula_weight         4235.54
_chemical_melting_point          ?
_chemical_name_common            'Ga4L6 supramolecular cluster'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.28(3)
_cell_angle_beta                 92.80(3)
_cell_angle_gamma                109.91(3)
_cell_formula_units_Z            2
_cell_length_a                   20.380(4)
_cell_length_b                   20.556(4)
_cell_length_c                   35.192(7)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.225
_cell_measurement_theta_min      3.44
_cell_volume                     13842(5)
_computing_cell_refinement       'Bruker APEX2 v. 2009.1'
_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker APEX2 v. 2009.1'
_computing_molecular_graphics    ORETEP-32
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.336
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w sacans'
_diffrn_radiation_monochromator  'HELIOS multilayer mirrors'
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            99001
_diffrn_reflns_theta_full        54.42
_diffrn_reflns_theta_max         54.42
_diffrn_reflns_theta_min         2.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.611
_exptl_absorpt_correction_T_max  0.8636
_exptl_absorpt_correction_T_min  0.6622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.016
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             4409
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
;
_refine_diff_density_max         1.254
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2453
_refine_ls_number_reflns         33712
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.1038
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2784
_refine_ls_wR_factor_ref         0.3028
_reflns_number_gt                22611
_reflns_number_total             33712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107656g_si_002.cif
_cod_data_source_block           jma7s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        13841(5)
_cod_original_formula_sum        'C214.50 H216.50 Ga4 K3 N13 O44.25 P5'
_cod_database_code               4103522