Expedient synthesis of conjugated triynes via alkyne metathesis
Curbet, Idriss; Colombel-Rouen, Sophie; Manguin, Romane; Clermont, Anthony; Quelhas, Alexandre; Müller, Daniel S.; Roisnel, Thierry; Baslé, Olivier; Trolez, Yann; Mauduit, Marc; Chemical Science 11 (2020) 4934–4938; doi:10.1039/D0SC01124J

data_1557924
_publ_section_title
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 Expedient synthesis of conjugated triynes via alkyne metathesis
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_journal_issue                   19
_journal_name_full               'Chemical Science'
_journal_page_first              4934
_journal_page_last               4938
_journal_paper_doi               10.1039/D0SC01124J
_journal_volume                  11
_journal_year                    2020
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C42 H30 Si2, C H Cl3 '
_chemical_formula_sum            'C43 H31 Cl3 Si2'
_chemical_formula_weight         710.21
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-11-20 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.801(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4193(6)
_cell_length_b                   21.2154(12)
_cell_length_c                   17.2115(8)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.4443
_cell_measurement_theta_min      2.3425
_cell_measurement_wavelength     0.71073
_cell_volume                     3749.1(3)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2019)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (G. Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      0.0335732
_diffrn_orient_matrix_UB_12      -0.0330318
_diffrn_orient_matrix_UB_13      -0.0328280
_diffrn_orient_matrix_UB_21      -0.0900753
_diffrn_orient_matrix_UB_22      -0.0065752
_diffrn_orient_matrix_UB_23      -0.0298436
_diffrn_orient_matrix_UB_31      0.0156696
_diffrn_orient_matrix_UB_32      0.0329760
_diffrn_orient_matrix_UB_33      -0.0388342
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.581
_diffrn_reflns_theta_min         2.137
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0531P)^2^+3.4307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6305
_reflns_number_total             8525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0sc01124j2.cif
_cod_data_source_block           SR540_C6
_cod_depositor_comments
;Adding full bibliography for 1557923--1557928.cif.

 Adding full bibliography for 1557923--1557928.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1557924
_shelx_res_checksum              42476