Direct Synthesis of Dialkylaryl-vinylsilane Derivatives: Metathesis of Dialkylaryl-iso-propenylsilane and Its Application to Tetracyclic Silacycle Dye Synthesis
YOSHIOKA, Shohei; Takehara, Tsunayoshi; MATSUZAKI, Tsuyoshi; Suzuki, Takeyuki; Tsujino, Hirofumi; Uno, Tadayuki; Tsutumi, Y.; Murai, Kenichi; Fujioka, Hiromichi; Arisawa, Mitsuhiro; Chemical Communications  (2019) –; doi:10.1039/C9CC06777A

data_7124406
_publ_section_title
;
 Direct Synthesis of Dialkylaryl-vinylsilane Derivatives: Metathesis of
 Dialkylaryl-iso-propenylsilane and Its Application to Tetracyclic
 Silacycle Dye Synthesis
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06777A
_journal_year                    2019
_chemical_formula_moiety         'C40 H59 Cl2 N2 P Ru'
_chemical_formula_sum            'C40 H59 Cl2 N2 P Ru'
_chemical_formula_weight         770.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc232007
_audit_update_record
;
2019-07-04 deposited with the CCDC.    2019-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 104.1210(17)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.2448(2)
_cell_length_b                   18.3117(2)
_cell_length_c                   17.9788(3)
_cell_measurement_reflns_used    17583
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.33
_cell_measurement_theta_min      2.54
_cell_volume                     3909.45(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            63555
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.513
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1624.00
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     421
_refine_ls_number_reflns         8970
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0361P)^2^+2.6507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7522
_reflns_number_total             8970
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9cc06777a2.cif
_cod_data_source_block           xcalibur
_cod_database_code               7124406
_shelx_res_checksum              35173