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_7160089
_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         'C64 H132 Si4'
_chemical_formula_sum            'C64 H132 Si4'
_chemical_formula_weight         1014.05
_chemical_melting_point          324.0(10)
_chemical_name_common            2a
_chemical_name_systematic        tricycloalkane
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                114.915(6)
_cell_angle_beta                 92.110(5)
_cell_angle_gamma                92.923(5)
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_cell_length_b                   13.7449(13)
_cell_length_c                   13.8357(13)
_cell_measurement_reflns_used    4601
_cell_measurement_temperature    250(2)
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_cell_volume                     1722.4(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
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_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      250(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.956
_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  0.0579
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.956
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_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -16
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_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32186
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.085
_diffrn_reflns_theta_min         3.802
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  0.95
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_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    0.978
_exptl_crystal_description       prism
_exptl_crystal_F_000             572
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.658
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_refine_ls_extinction_method     none
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+1.1586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1837
_refine_ls_wR_factor_ref         0.2109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4906
_reflns_number_total             6601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01143k2.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '323-325 K' was changed to
'324.0(10)' -- 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               7160089
_shelx_estimated_absorpt_t_min   0.790
_shelx_estimated_absorpt_t_max   0.886
_shelx_res_checksum              55819