A Discrete Ortho-Lithiated Acetophenone Imine Derivative: Isolation, Characterization, and Synthesis of Group IV Metal Complexes
Baiz, Tamam I.; Schmidt, Joseph A. R.; Organometallics 26 (2007) 4094–; doi:10.1021/om700530z

data_4073679
_publ_section_title
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 A Discrete Ortho-Lithiated Acetophenone Imine Derivative:&#x00A0;
 Isolation, Characterization, and Synthesis of Group IV Metal Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4094
_journal_paper_doi               10.1021/om700530z
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C46 H62 N2 O4 Si2 Zr, 0.25(C4H10O)'
_chemical_formula_sum            'C47 H64.5 N2 O4.25 Si2 Zr'
_chemical_formula_weight         872.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_creation_method           SHELXL-97
_cell_angle_alpha                81.983(1)
_cell_angle_beta                 77.081(1)
_cell_angle_gamma                65.461(1)
_cell_formula_units_Z            2
_cell_length_a                   11.4685(6)
_cell_length_b                   12.6056(6)
_cell_length_c                   18.3425(9)
_cell_measurement_reflns_used    5204
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      23.6
_cell_measurement_theta_min      1.5
_cell_volume                     2347.9(2)
_computing_cell_refinement       'Bruker SAINT v6.22'
_computing_data_collection       'Bruker SMART v5.625'
_computing_data_reduction        'Bruker SAINT v6.22'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      135(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       \w-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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0932
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37986
_diffrn_reflns_theta_full        34.51
_diffrn_reflns_theta_max         34.51
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             925
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.421
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         18213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0997P)^2^+0.9296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.2098
_reflns_number_gt                10839
_reflns_number_total             18213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700530z-file002.cif
_cod_data_source_block           (PIPARet')2Zr(CH2SiMe3)2_1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C47 H64.50 N2 O4.25 Si2 Zr'
_cod_database_code               4073679