Ring-closing metathesis for the synthesis of a molecular gyrotop.
Setaka, Wataru; Higa, Sayaka; Yamaguchi, Kentaro; Organic & biomolecular chemistry 12 (2014) 3354–3357; doi:10.1039/c4ob00470a

data_7153752
_publ_section_title
;
 Ring-closing metathesis for the synthesis of a molecular gyrotop.
;
_journal_issue                   21
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3354
_journal_page_last               3357
_journal_paper_doi               10.1039/c4ob00470a
_journal_volume                  12
_journal_year                    2014
_chemical_formula_moiety         'C60 H112 Si2'
_chemical_formula_sum            'C60 H112 Si2'
_chemical_formula_weight         889.68
_chemical_melting_point          355.6(5)
_chemical_name_common            MolGyroIsomer
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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                95.313(2)
_cell_angle_beta                 90.751(3)
_cell_angle_gamma                92.942(2)
_cell_formula_units_Z            4
_cell_length_a                   14.530(3)
_cell_length_b                   18.768(3)
_cell_length_c                   21.753(4)
_cell_measurement_reflns_used    2047
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      1.40
_cell_volume                     5897.8(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 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.1861
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28912
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.18
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9926
_exptl_absorpt_correction_T_min  0.9761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         22201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.2370
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1068P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1959
_refine_ls_wR_factor_ref         0.2645
_reflns_number_gt                8026
_reflns_number_total             22201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ob00470a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '82-83 deg.C' was changed to
'355.6(5)' - 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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7153751--7153752.cif.
;
_cod_original_cell_volume        5897.9(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7153752