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_4086865
_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         'C27 H40 B N6 Nb'
_chemical_formula_sum            'C27 H40 B N6 Nb'
_chemical_formula_weight         552.37
_chemical_name_systematic
;
 ?
;
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_symmetry_Int_Tables_number      14
_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     direct
_atom_sites_solution_secondary   difmap
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_audit_creation_method           'WinGX routine CIF_UPDATE'
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_cell_angle_beta                 109.051(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_measurement_temperature    180(2)
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_cell_measurement_wavelength     0.71073
_cell_volume                     2812.41(8)
_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
;
        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
;
        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)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.017505
_diffrn_orient_matrix_UB_12      -0.0343646
_diffrn_orient_matrix_UB_13      -0.0205373
_diffrn_orient_matrix_UB_21      0.0562708
_diffrn_orient_matrix_UB_22      0.017373
_diffrn_orient_matrix_UB_23      0.008611
_diffrn_orient_matrix_UB_31      0.0198598
_diffrn_orient_matrix_UB_32      -0.0189729
_diffrn_orient_matrix_UB_33      0.0450838
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.014
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
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_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29260
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.906
_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    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+1.9866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                4958
_reflns_number_total             5744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00506_si_002.cif
_cod_data_source_block           op040610
_cod_depositor_comments
'Adding full bibliography for 4086864--4086868.cif.'
_cod_original_cell_volume        2812.41(7)
_cod_database_code               4086865