Chiral Alkoxide-Functionalized Guanidinates from Ring-Opening Rearrangement of Aminooxazolinate Complexes
Gott, Andrew L.; Coles, Stuart R.; Clarke, Adam J.; Clarkson, Guy J.; Scott, Peter; Organometallics 26 (2007) 136–; doi:10.1021/om0607649

data_4072539
_publ_section_title
;
 Chiral Alkoxide-Functionalized Guanidinates from Ring-Opening
 Rearrangement of Aminooxazolinate Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              136
_journal_paper_doi               10.1021/om0607649
_journal_volume                  26
_journal_year                    2007
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C29 H40 Hf N4 O'
_chemical_formula_weight         639.14
_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                   9.0546(11)
_cell_length_b                   15.272(2)
_cell_length_c                   20.203(3)
_cell_measurement_reflns_used    7528
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      70.12
_cell_measurement_theta_min      3.12
_cell_volume                     2793.7(6)
_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 0.938
_diffrn_measured_fraction_theta_max 0.939
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15518
_diffrn_reflns_theta_full        70.65
_diffrn_reflns_theta_max         70.65
_diffrn_reflns_theta_min         3.63
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    7.106
_exptl_absorpt_correction_T_max  0.5368
_exptl_absorpt_correction_T_min  0.3100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4885
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0275P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                4647
_reflns_number_total             4885
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0607649si20060822_033624.cif
_cod_data_source_block           ag4
_cod_original_cell_volume        2793.8(7)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4072539