Reaction of [σ:η5-(C9H6)C2B9H10]Zr(NMe2)(DME) with Guanidines: Metallacarborane-Mediated C-N Bond Cleavage and 1,5-Sigmatropic Rearrangement
Hao Shen; Hoi-Shan Chan; Zuowei Xie; Journal of the American Chemical Society 129 (2007) 12934–12935; doi:10.1021/ja0754498

data_4110109
_publ_section_title
;
 Reaction of [\s:\h5-(C9H6)C2B9H10]Zr(NMe2)(DME) with Guanidines:
 Metallacarborane-Mediated C-N Bond Cleavage and 1,5-Sigmatropic
 Rearrangement
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12934
_journal_page_last               12935
_journal_paper_doi               10.1021/ja0754498
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C34 H58 B9 N5 Zr'
_chemical_formula_weight         725.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.426(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9845(18)
_cell_length_b                   11.8691(14)
_cell_length_c                   21.506(3)
_cell_measurement_reflns_used    972
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.94
_cell_measurement_theta_min      2.22
_cell_volume                     4072.9(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER SMART CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.2374
_diffrn_reflns_av_sigmaI/netI    0.1601
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21678
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9154
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_meas      0
_exptl_crystal_description       prism
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7165
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1981
_reflns_number_gt                4052
_reflns_number_total             7165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0754498si20070721_070318_3.cif
_cod_data_source_block           5a
_cod_original_cell_volume        4072.9(8)
_cod_database_code               4110109