Syntheses and Structures of Cationic and Neutral, Homo- and Heteroleptic tert-Butoxides of the Group 4 Metals
Edmond Y. Njua; Alexander Steiner; Lothar Stahl; Inorganic Chemistry 49 (2010) 2163–2172; doi:10.1021/ic9019537

data_4314962
_publ_contact_author_address
;Department of Chemistry
University of North Dakota
Grand Forks, ND 58202
USA
;
_publ_contact_author_email       lstahl@chem.und.edu
_publ_contact_author_fax         701-777-2331
_publ_contact_author_name        'Lothar Stahl'
_publ_contact_author_phone       701-777-2242
_publ_section_title
;
 Syntheses and Structures of Cationic and Neutral, Homo- and Heteroleptic
 tert-Butoxides of the Group 4 Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2163
_journal_page_last               2172
_journal_paper_doi               10.1021/ic9019537
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C24 H54 O6 Sn Zr'
_chemical_formula_weight         648.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           156
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2"'
_symmetry_space_group_name_H-M   'P 3 m 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   17.1304(12)
_cell_length_b                   17.1304(12)
_cell_length_c                   9.4890(14)
_cell_measurement_temperature    173(2)
_cell_volume                     2411.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20647
_diffrn_reflns_theta_full        28.19
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    1.130
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.409
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.61(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         4162
_refine_ls_number_restraints     820
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+4.9417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                3616
_reflns_number_total             4162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9019537_si_001_8.cif
_cod_data_source_block           7
_cod_database_code               4314962