Regioselective Carbyne Transfer to Ring-Opening Alkyne Metathesis Initiators Gives Access to Telechelic Polymers.
von Kugelgen, Stephen; Sifri, Renee; Bellone, Donatela; Fischer, Felix R.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b02225

data_4126070
_publ_section_title
;
 Regioselective Carbyne Transfer to Ring-Opening Alkyne Metathesis
 Initiators Gives Access to Telechelic Polymers.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b02225
_journal_year                    2017
_chemical_formula_sum            'C23 H23 F18 Mo N O7'
_chemical_formula_weight         863.36
_chemical_name_common            SVK3_32
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.630(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4048(5)
_cell_length_b                   9.2801(5)
_cell_length_c                   17.2135(9)
_cell_measurement_reflns_used    6221
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.33
_cell_volume                     1485.34(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3 v. 2016.1'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-2014
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12658
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.437
_diffrn_reflns_theta_min         1.196
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_description       prism
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 1597 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5057
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0387P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_full    0.875
_reflns_Friedel_fraction_max     0.849
_reflns_number_gt                4262
_reflns_number_total             5057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02225_si_003.cif
_cod_data_source_block           shelx
_cod_database_code               4126070
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              11074
_shelx_hkl_checksum              10873