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_4086866
_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         'C30 H38 B N6 Nb'
_chemical_formula_sum            'C30 H38 B N6 Nb'
_chemical_formula_weight         586.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_date             2015-07-24T16:20:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.684(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0651(5)
_cell_length_b                   14.9952(7)
_cell_length_c                   17.7145(9)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.92
_cell_measurement_theta_min      2.51
_cell_measurement_wavelength     0.71073
_cell_volume                     2933.2(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       \w-\f
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49107
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.44
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         5980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+6.8731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1186
_reflns_number_gt                4543
_reflns_number_total             5980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00506_si_002.cif
_cod_data_source_block           po051010
_cod_depositor_comments
'Adding full bibliography for 4086864--4086868.cif.'
_cod_database_code               4086866