Cage Size Effects on the Rotation of Molecular Gyrotops with 1,4-Naphthalenediyl Rotor in Solution.
Setaka, Wataru; Koyama, Akiko; Yamaguchi, Kentaro; Organic letters 15 (2013) 5092–5095; doi:10.1021/ol402464d

data_1512383
_publ_section_title
;
 Cage Size Effects on the Rotation of Molecular Gyrotops with
 1,4-Naphthalenediyl Rotor in Solution.
;
_journal_issue                   19
_journal_name_full               'Organic letters'
_journal_page_first              5092
_journal_page_last               5095
_journal_paper_doi               10.1021/ol402464d
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         '2(C58 H102 Si2), 1.5(C4 H8 O)'
_chemical_formula_sum            'C122 H216 O1.5 Si4'
_chemical_formula_weight         1819.31
_chemical_melting_point          388.0(7)
_chemical_name_common            C16satNpcage
_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                85.1370(10)
_cell_angle_beta                 80.2820(10)
_cell_angle_gamma                75.0800(10)
_cell_formula_units_Z            2
_cell_length_a                   14.1947(12)
_cell_length_b                   15.1832(13)
_cell_length_c                   28.719(2)
_cell_measurement_reflns_used    4170
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22.95
_cell_measurement_theta_min      2.34
_cell_volume                     5889.5(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.1060
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28812
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9820
_exptl_absorpt_correction_T_min  0.9010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1247
_refine_ls_number_reflns         22315
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1435
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+0.9175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1625
_reflns_number_gt                11608
_reflns_number_total             22315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol402464d_si_003.cif
_cod_data_source_block           NpC16cage
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '114.2-115.6 deg. C' was changed to
'388.0(7)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Triclinic' changed to
'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        5889.5(9)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_original_formula_sum        'C122 H216 O1.50 Si4'
_cod_database_code               1512383