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_1557927
_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         'C14 H14'
_chemical_formula_sum            'C14 H14'
_chemical_formula_weight         182.25
_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
;
2019-04-04 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.902(5)
_cell_angle_beta                 91.564(5)
_cell_angle_gamma                91.339(4)
_cell_formula_units_Z            4
_cell_length_a                   7.5855(9)
_cell_length_b                   8.3989(11)
_cell_length_c                   17.377(2)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5963
_cell_measurement_theta_min      2.4260
_cell_measurement_wavelength     0.71073
_cell_volume                     1106.2(2)
_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, 2018)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.982
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21175
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         3.347
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.897
_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    1.094
_exptl_crystal_description       prism
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.270
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+0.4906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4166
_reflns_number_total             4978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0sc01124j2.cif
_cod_data_source_block           ANC42
_cod_depositor_comments
;Adding full bibliography for 1557923--1557928.cif.

 Adding full bibliography for 1557923--1557928.cif.
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_cod_database_code               1557927
_shelx_res_checksum              60754