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_1512384
_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         'C64 H114 Si2'
_chemical_formula_sum            'C64 H114 Si2'
_chemical_formula_weight         939.73
_chemical_melting_point          406.8(8)
_chemical_name_common            C18cageNp
_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                66.601(2)
_cell_angle_beta                 82.719(2)
_cell_angle_gamma                68.828(2)
_cell_formula_units_Z            2
_cell_length_a                   14.5354(18)
_cell_length_b                   14.7161(18)
_cell_length_c                   16.738(2)
_cell_measurement_reflns_used    11731
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      1.50
_cell_volume                     3063.5(6)
_computing_cell_refinement       'APEX 2 Bruker'
_computing_data_collection       'APEX 2 Bruker'
_computing_data_reduction        'APEX 2 Bruker'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15302
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.24
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9907
_exptl_absorpt_correction_T_min  0.9816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS(Bruker)
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.019
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         11731
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+1.1247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                7753
_reflns_number_total             11731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol402464d_si_004.cif
_cod_data_source_block           NpC18cage
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '132.9-134.5 deg. C' was changed to
'406.8(8)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3063.4(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512384