Catalytic alkene cyclohydroamination via an imido mechanism.
Gott, Andrew L; Clarke, Adam J; Clarkson, Guy J; Scott, Peter; Chemical communications (Cambridge, England)  (2008) 1422–1424; doi:10.1039/b718373a

data_7102989
_publ_section_title
;
 Catalytic alkene cyclohydroamination via an imido mechanism.
;
_journal_issue                   12
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1422
_journal_page_last               1424
_journal_paper_doi               10.1039/b718373a
_journal_year                    2008
_chemical_absolute_configuration rm
_chemical_formula_sum            'C70 H118 N6 O4 Zr2'
_chemical_formula_weight         1290.14
_chemical_name_common            in_paper_2
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.098(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9465(7)
_cell_length_b                   9.9106(7)
_cell_length_c                   36.050(3)
_cell_measurement_reflns_used    4776
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.90
_cell_volume                     3539.6(4)
_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      293(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_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  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            21778
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.28
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  0.9864
_exptl_absorpt_correction_T_min  0.8011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.437
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 3715 Friedel pairs'
_refine_ls_abs_structure_Flack   0.20(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         9976
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0804
_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^)+(0.0000P)^2^+25.4311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1819
_reflns_number_gt                8304
_reflns_number_total             9976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718373a.txt
_cod_data_source_block           ag10
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7102989