Regioselective [2+2] and [4+2] cycloaddition reactivity in an asymmetric niobium(bisimido) moiety towards unsaturated organic molecules.
Obenhuber, A. H.; Gianetti, T. L.; Bergman, R. G.; Arnold, J.; Chemical communications (Cambridge, England) 51 (2014) 1278–1281; doi:10.1039/c4cc07851a

data_7116196
_publ_section_title
;
 Regioselective [2+2] and [4+2] cycloaddition reactivity in an asymmetric
 niobium(bisimido) moiety towards unsaturated organic molecules.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1278
_journal_page_last               1281
_journal_paper_doi               10.1039/c4cc07851a
_journal_volume                  51
_journal_year                    2014
_chemical_formula_moiety         'C47 H60 N3 Nb'
_chemical_formula_sum            'C47 H60 N3 Nb'
_chemical_formula_weight         759.89
_chemical_name_common            'Complex 4'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_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
_audit_update_record
;
2014-09-28 deposited with the CCDC.
2014-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                86.853(10)
_cell_angle_beta                 76.422(9)
_cell_angle_gamma                65.449(8)
_cell_formula_units_Z            2
_cell_length_a                   10.7140(19)
_cell_length_b                   11.714(2)
_cell_length_c                   18.976(3)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      2.21
_cell_volume                     2103.3(6)
_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
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0379
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45285
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_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.9810
_exptl_absorpt_correction_T_min  0.9387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rode
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.858
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+1.5412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                6831
_reflns_number_total             7757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc07851a2.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/rss-feeds/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 2935 2014-11-11 08:27:57Z andrius 
;
_cod_original_cell_volume        2103.3(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7116196