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_4086867
_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         'C32 H42 B Fe N6 Nb'
_chemical_formula_sum            'C32 H42 B Fe N6 Nb'
_chemical_formula_weight         670.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-24T16:42:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 105.849(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4037(10)
_cell_length_b                   15.8380(13)
_cell_length_c                   19.2775(16)
_cell_measurement_reflns_used    3914
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.28
_cell_measurement_theta_min      2.28
_cell_measurement_wavelength     0.71073
_cell_volume                     3349.4(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0892
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_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            38066
_diffrn_reflns_theta_full        24.48
_diffrn_reflns_theta_max         24.48
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.9743
_exptl_absorpt_correction_T_min  0.8975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.124
_reflns_number_gt                3936
_reflns_number_total             5529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00506_si_002.cif
_cod_data_source_block           CL1051
_cod_depositor_comments
'Adding full bibliography for 4086864--4086868.cif.'
_cod_database_code               4086867