Ring-closing metathesis of dialkenylcycloalkanes for the synthesis of fused bicycloalkanes and tricycloalkanes.
Tu, Yuyang; Inagaki, Yusuke; Ohara, Kazuaki; Yamaguchi, Kentaro; Setaka, Wataru; Organic & biomolecular chemistry 22 (2024) 6950–6954; doi:10.1039/d4ob01143k

data_7160091
_publ_section_title
;
 Ring-closing metathesis of dialkenylcycloalkanes for the synthesis of
 fused bicycloalkanes and tricycloalkanes.
;
_journal_issue                   34
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6950
_journal_page_last               6954
_journal_paper_doi               10.1039/d4ob01143k
_journal_volume                  22
_journal_year                    2024
_chemical_compound_source        no
_chemical_formula_moiety         'C80 H164 Si4'
_chemical_formula_sum            'C80 H164 Si4'
_chemical_formula_weight         1238.46
_chemical_melting_point          338.5(5)
_chemical_name_common            2b
_chemical_name_systematic        tricycloalkane
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-08-05 deposited with the CCDC.	2024-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9494(4)
_cell_length_b                   8.4932(2)
_cell_length_c                   66.5433(18)
_cell_measurement_reflns_used    6552
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      59.2622
_cell_measurement_theta_min      3.2409
_cell_volume                     8448.9(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2020)'
_computing_publication_material  'WinGX (Farrugia, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Sir-2019 (IUCr, 2019)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1447
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       82
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            121616
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.028
_diffrn_reflns_theta_min         2.656
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.974
_exptl_crystal_description       plate
_exptl_crystal_F_000             2800
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.00056(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+1.9372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5943
_reflns_number_total             8371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01143k2.cif
_cod_data_source_block           2b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '338-339 K' was changed to
'338.5(5)' -- the average value was taken and precision was
estimated.

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7160089--7160091.cif.
;
_cod_database_code               7160091
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.868
_shelx_estimated_absorpt_t_max   0.948
_shelx_res_checksum              41664