Regioselective Termination Reagents for Ring-Opening Alkyne Metathesis Polymerization.
Jeong, Hyangsoo; von Kugelgen, Stephen; Bellone, Donatela; Fischer, Felix R.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b09390

data_4126605
_publ_section_title
;
 Regioselective Termination Reagents for Ring-Opening Alkyne Metathesis
 Polymerization.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b09390
_journal_year                    2017
_chemical_formula_moiety         'C29 H26 F18 Mo N2 O5'
_chemical_formula_sum            'C29 H26 F18 Mo N2 O5'
_chemical_formula_weight         920.46
_chemical_name_common            HJ2035
_chemical_name_systematic        SVK3_36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                77.653(2)
_cell_angle_beta                 80.752(2)
_cell_angle_gamma                84.727(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0185(3)
_cell_length_b                   10.8539(3)
_cell_length_c                   17.1855(5)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.24
_cell_volume                     1798.59(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3 v.2016.5'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.985
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31388
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.393
_diffrn_reflns_theta_min         1.226
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       plate
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         6499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0401P)^2^+1.4501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5518
_reflns_number_total             6499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09390_si_003.cif
_cod_data_source_block           shelx
_cod_database_code               4126605
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.980
_shelx_res_checksum              68097
_shelx_hkl_checksum              35035
_shelx_fab_checksum              88663