Cleavage and Reorganization of Zr-C/Si-C Bonds Leading to Zr/Si-N Organometallic and Heterocyclic Compounds
Shaoguang Zhang; Wen-Xiong Zhang; Jing Zhao; Zhenfeng Xi; Journal of the American Chemical Society 132 (2010) 14042–14045; doi:10.1021/ja1074932

data_4103254
_publ_contact_author_address
;
Beijing National Laboratory for Molecular Sciences (BNLMS),
Key Laboratory of Bioorganic Chemistry and Molecular Engineering of Ministry 
of Education, College of Chemistry, Peking University,
Beijing 100871, China,
;
_publ_contact_author_email       zfxi@pku.edu.cn
_publ_contact_author_name        'Zhenfeng Xi'
_publ_section_title
;
 Cleavage and Reorganization of Zr-C/Si-C Bonds Leading to Zr/Si-N
 Organometallic and Heterocyclic Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14042
_journal_page_last               14045
_journal_paper_doi               10.1021/ja1074932
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C42 H44 N2 Si Zr'
_chemical_formula_weight         696.10
_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                 94.65(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.934(3)
_cell_length_b                   15.239(3)
_cell_length_c                   15.016(3)
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      1.28
_cell_volume                     3634.2(12)
_computing_cell_refinement       Rapid-AUTO
_computing_data_collection       'Rapid-AUTO (Rigaku,2000)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC,2000)'
_computing_molecular_graphics    'Siemens SHELXTL V4.2,(Sheldrick,1990)'
_computing_publication_material  SHELXL-97,(Sheldrick,1997)
_computing_structure_refinement  SHELXL-97,(Sheldrick,1997)
_computing_structure_solution    SHELXS-97,(Sheldrick,1997)
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       \W
_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  0.0804
_diffrn_reflns_av_sigmaI/netI    0.8027
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8306
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.9643
_exptl_absorpt_correction_T_min  0.9303
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
                                  HIGASHI, T. (1995). Abscor-empirical 
                                  Absorption Correction based on Fourier 
                                  Series Approximation. 
                                  Rigaku Corporation,Tokyo,Japan. 
;
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.0077(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.759
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         8306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.759
_refine_ls_R_factor_all          0.3024
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.2400
_reflns_number_gt                1526
_reflns_number_total             8306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1074932_si_009.cif
_cod_data_source_block           zsg29b
_cod_original_cell_volume        3634.1(13)
_cod_database_code               4103254