Activation of olefin metathesis complexes containing unsymmetrical unsaturated N-heterocyclic carbenes by copper and gold transmetalation
Kamal, Fadwa; Colombel-Rouen, Sophie; DUMAS, Adrien; Guegan, Jean Paul; Roisnel, Thierry; Dorcet, Vincent; Basle, Olivier; Rouen, Mathieu; Mauduit, Marc; Chemical Communications  (2019) –; doi:10.1039/C9CC05776E

data_7124103
_publ_section_title
;
 Activation of olefin metathesis complexes containing unsymmetrical
 unsaturated N-heterocyclic carbenes by copper and gold transmetalation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05776E
_journal_year                    2019
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C31 H34 B F5 N2'
_chemical_formula_sum            'C31 H34 B F5 N2'
_chemical_formula_weight         540.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-07-05 deposited with the CCDC.    2019-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.302(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3875(17)
_cell_length_b                   19.402(3)
_cell_length_c                   15.257(4)
_cell_measurement_reflns_used    8874
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.5613
_cell_measurement_theta_min      2.4035
_cell_measurement_wavelength     0.71073
_cell_volume                     2749.7(10)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'PLATON, A.L.Spek, Acta Cryst. 2009, D65, 148-155'
_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 0.976
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      0.0929090
_diffrn_orient_matrix_UB_12      0.0071128
_diffrn_orient_matrix_UB_13      -0.0236333
_diffrn_orient_matrix_UB_21      -0.0109511
_diffrn_orient_matrix_UB_22      -0.0461196
_diffrn_orient_matrix_UB_23      -0.0294633
_diffrn_orient_matrix_UB_31      -0.0531951
_diffrn_orient_matrix_UB_32      0.0219174
_diffrn_orient_matrix_UB_33      -0.0543284
_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  0.0909
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21188
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_min         2.431
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.506
_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    1.305
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.670
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0893
_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^)+(0.1857P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2275
_refine_ls_wR_factor_ref         0.2646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4164
_reflns_number_total             6168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9cc05776e2.cif
_cod_data_source_block           FK480_2
_cod_database_code               7124103
_shelx_res_checksum              11109