Single Diastereomer Half-Sandwich Salicyloxazoline Complexes of Titanium and Zirconium
Gott, Andrew L.; Clarke, Adam J.; Clarkson, Guy J.; Munslow, Ian J.; Wade, Andrew R.; Scott, Peter; Organometallics 27 (2008) 2706–; doi:10.1021/om8002027

data_4071507
_publ_section_title
;
 Single Diastereomer Half-Sandwich Salicyloxazoline Complexes of Titanium
 and Zirconium
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2706
_journal_paper_doi               10.1021/om8002027
_journal_volume                  27
_journal_year                    2008
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C37 H53 Cl2 N O2 Zr'
_chemical_formula_weight         705.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   9.861(3)
_cell_length_b                   16.787(5)
_cell_length_c                   22.046(6)
_cell_measurement_reflns_used    5810
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      2.27
_cell_volume                     3649.4(18)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Siemens SMART diffractometer'
_diffrn_measurement_method       '\w 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  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23794
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.9360
_exptl_absorpt_correction_T_min  0.7003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.221
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 3892 Friedel pairs'
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         9072
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0671P)^2^+2.6026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1425
_reflns_number_gt                7375
_reflns_number_total             9072
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8002027-file001.cif
_cod_data_source_block           aw3
_cod_original_cell_volume        3649.3(18)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4071507