Synthesis, structures, and alkene hydrosilation activities of neutral tripodal amidozirconium alkyls
Jia, Li; Zhao, Jiquan; Ding, Errun; Brennessel, William W.; Journal of the Chemical Society, Dalton Transactions  (2002) 2608–; doi:10.1039/b200789d

data_7011518
_publ_section_title
;
 Synthesis, structures, and alkene hydrosilation activities of neutral
 tripodal amidozirconium alkyls
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2608
_journal_paper_doi               10.1039/b200789d
_journal_year                    2002
_chemical_formula_moiety         'C32 H49 N3 Si3 Zr'
_chemical_formula_sum            'C32 H49 N3 Si3 Zr'
_chemical_formula_weight         651.23
_chemical_name_common            3a
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 108.717(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.402(3)
_cell_length_b                   9.9224(7)
_cell_length_c                   17.614(1)
_cell_measurement_reflns_used    3495
_cell_measurement_temperature    173(2)
_cell_volume                     7018.8(8)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20413
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.886961
_exptl_absorpt_correction_type   multiscans
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6196
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+2.1935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                5016
_reflns_number_total             6196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200789d.txt
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7011518