CH Bond Activation of Unsaturated Hydrocarbons by a Niobium Methyl Cyclopropyl Precursor. Cyclopropyl Ring Opening and Alkyne Coupling Reaction
Oulié, Pascal; Dinoi, Chiara; Li, Chen; Sournia-Saquet, Alix; Jacob, Kane; Vendier, Laure; Etienne, Michel; Organometallics 36 (2017) 53–; doi:10.1021/acs.organomet.6b00506

data_4086864
_publ_section_title
;
 CH Bond Activation of Unsaturated Hydrocarbons by a Niobium Methyl
 Cyclopropyl Precursor. Cyclopropyl Ring Opening and Alkyne Coupling
 Reaction
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              53
_journal_paper_doi               10.1021/acs.organomet.6b00506
_journal_volume                  36
_journal_year                    2017
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H36 B N6 Nb O, 0.5(C6 H6)'
_chemical_formula_sum            'C29 H39 B N6 Nb O'
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_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2yn'
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_atom_sites_solution_primary     direct
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_cell_angle_alpha                90
_cell_angle_beta                 93.803(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7378(5)
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_cell_volume                     2933.15(16)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
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_diffrn_ambient_temperature      180
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0362695
_diffrn_orient_matrix_UB_12      -0.0219685
_diffrn_orient_matrix_UB_13      -0.0238638
_diffrn_orient_matrix_UB_21      -0.0018817
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_diffrn_orient_matrix_UB_23      0.0172189
_diffrn_orient_matrix_UB_31      -0.0368369
_diffrn_orient_matrix_UB_32      0.0247421
_diffrn_orient_matrix_UB_33      0.0193295
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22799
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_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
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_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         6002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                3884
_reflns_number_total             6002
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om6b00506_si_002.cif
_cod_data_source_block           op035
_cod_depositor_comments
'Adding full bibliography for 4086864--4086868.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4086864