Structural characterization of M(s-cis-η4-C4H6)(Me4C5SiMe2NR) (M = Ti or Zr, R = CMe3 or CHCMe(1-C10H7))
Dahlmann, Marc; Schottek, Jörg; Fröhlich, Roland; Kunz, Doris; Nissinen, Maija; Erker, Gerhard; Fink, Gerhard; Kleinschmidt, Ralph; Journal of the Chemical Society, Dalton Transactions  (2000) 1881–; doi:10.1039/b000570n

data_7009387
_publ_section_title
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 Structural characterization of M(s-cis-\h4-C4H6)(Me4C5SiMe2NR)
 (M&#x2005;=&#x2005;Ti or Zr, R&#x2005;=&#x2005;CMe3 or CHCMe(1-C10H7))
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1881
_journal_paper_doi               10.1039/b000570n
_journal_year                    2000
_chemical_formula_sum            'C19 H33 N Si Zr'
_chemical_formula_weight         394.77
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.338(2)
_cell_length_b                   12.819(2)
_cell_length_c                   15.032(5)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      20.67
_cell_measurement_theta_min      8.47
_cell_volume                     1992.1(8)
_computing_cell_refinement       'Express (Nonius B.V., 1994)'
_computing_data_collection       'Express (Nonius B.V., 1994)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'SCHAKAL (Keller, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4218
_diffrn_reflns_theta_full        26.29
_diffrn_reflns_theta_max         26.29
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.9701
_exptl_absorpt_correction_T_min  0.8877
_exptl_absorpt_correction_type   'empirical via \y scan data'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    'refined as riding atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2112
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0506P)^2^+2.3981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                1300
_reflns_number_total             2112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b000570n.txt
_cod_data_source_block           erk_672
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7009387