Constrained geometry aminooxazolinate ligands giving chiral zirconium guanidinates; catalytic cyclohydroamination
Gott, Andrew L.; Clarkson, Guy J.; Deeth, Robert J.; Hammond, Max. L.; Morton, Colin; Scott, Peter; Dalton Transactions  (2008) 2983–2990; doi:10.1039/b803831g

data_7004180
_publ_section_title
;
 Constrained geometry aminooxazolinate ligands giving chiral zirconium
 guanidinates; catalytic cyclohydroamination
;
_journal_issue                   22
_journal_name_full               'Dalton Transactions'
_journal_page_first              2983
_journal_page_last               2990
_journal_paper_doi               10.1039/b803831g
_journal_year                    2008
_chemical_formula_sum            'C20 H34 N4 Si Zr'
_chemical_formula_weight         449.82
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.5630(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0781(4)
_cell_length_b                   17.2011(7)
_cell_length_c                   12.9809(5)
_cell_measurement_reflns_used    4756
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.4
_cell_volume                     2248.05(15)
_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      220(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1004
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11491
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.8927
_exptl_absorpt_correction_T_min  0.7980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         4.613
_refine_diff_density_min         -2.509
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1403
_refine_ls_R_factor_gt           0.1124
_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^)+(0.1935P)^2^+16.2059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2914
_refine_ls_wR_factor_ref         0.3184
_reflns_number_gt                2923
_reflns_number_total             3944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b803831g.txt
_cod_data_source_block           cr1m
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7004180