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_1512382
_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         'C52 H90 Si2'
_chemical_formula_sum            'C52 H90 Si2'
_chemical_formula_weight         771.42
_chemical_melting_point          403.8(8)
_chemical_name_common            C14satNpcage
_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                93.875(3)
_cell_angle_beta                 102.751(2)
_cell_angle_gamma                110.568(2)
_cell_formula_units_Z            4
_cell_length_a                   13.327(3)
_cell_length_b                   17.391(4)
_cell_length_c                   23.422(5)
_cell_measurement_reflns_used    6798
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.59
_cell_measurement_theta_min      2.37
_cell_volume                     4894.1(19)
_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 8.31
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.897
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43207
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_correction_T_min  0.8273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         17014
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.0781
_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^)+(0.0962P)^2^+6.4124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1899
_refine_ls_wR_factor_ref         0.2273
_reflns_number_gt                10102
_reflns_number_total             17014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol402464d_si_002.cif
_cod_data_source_block           NpC14cage
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '129.8-131.4 deg. C' was changed to
'403.8(8)' - 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        4894.2(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512382