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_1557923
_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         'C44 H30'
_chemical_formula_sum            'C44 H30'
_chemical_formula_weight         558.68
_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_update_record
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2019-04-04 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
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_cell_angle_alpha                93.791(3)
_cell_angle_beta                 94.905(3)
_cell_angle_gamma                98.931(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9378(9)
_cell_length_b                   9.9882(8)
_cell_length_c                   17.7699(15)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.48
_cell_measurement_wavelength     0.71073
_cell_volume                     1730.4(3)
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2017)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41529
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.914
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.000
_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    1.072
_exptl_crystal_description       prism
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+0.8492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6557
_reflns_number_total             7909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0sc01124j2.cif
_cod_data_source_block           RMA82
_cod_depositor_comments
;Adding full bibliography for 1557923--1557928.cif.

 Adding full bibliography for 1557923--1557928.cif.
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_cod_database_code               1557923
_shelx_res_checksum              66050
_shelx_fab_checksum              32917