Carbon‒fluorine bond cleavage in fluoroarenes via a niobium(iii) imido complex: from stoichiometric to catalytic hydrodefluorination
Gianetti, Thomas L.; Bergman, Robert G.; Arnold, John; Chemical Science 5 (2014) 2517–; doi:10.1039/c4sc00006d

data_1516532
_publ_section_title
;
 Carbon--fluorine bond cleavage in fluoroarenes via a niobium(iii) imido
 complex: from stoichiometric to catalytic hydrodefluorination
;
_journal_issue                   6
_journal_name_full               'Chemical Science'
_journal_page_first              2517
_journal_paper_doi               10.1039/c4sc00006d
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C39 H54 F2 N3 Nb'
_chemical_formula_sum            'C39 H54 F2 N3 Nb'
_chemical_formula_weight         695.76
_chemical_name_common            'Complex 2d'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                79.714(2)
_cell_angle_beta                 87.243(2)
_cell_angle_gamma                88.804(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9151(4)
_cell_length_b                   12.3010(4)
_cell_length_c                   13.7072(5)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      2.35
_cell_volume                     1808.60(11)
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42043
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.9708
_exptl_absorpt_correction_T_min  0.9427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rode
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+1.2845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                5860
_reflns_number_total             6684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc00006d2.cif
_cod_data_source_block           (3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1516532