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_1557926
_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         'C34 H26'
_chemical_formula_sum            'C34 H26'
_chemical_formula_weight         434.55
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-06-04 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                94.453(3)
_cell_angle_beta                 104.612(3)
_cell_angle_gamma                98.456(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5611(8)
_cell_length_b                   10.3957(10)
_cell_length_c                   14.5334(13)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.5185
_cell_measurement_theta_min      2.4961
_cell_measurement_wavelength     0.71073
_cell_volume                     1229.1(2)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.914
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.874
_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    1.174
_exptl_crystal_description       plate
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.6251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4477
_reflns_number_total             5570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0sc01124j2.cif
_cod_data_source_block           IC726F2
_cod_depositor_comments
;Adding full bibliography for 1557923--1557928.cif.

 Adding full bibliography for 1557923--1557928.cif.
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_cod_database_code               1557926
_shelx_res_checksum              82664