Calcium amido-bisoxazoline complexes in asymmetric hydroamination/cyclisation catalysis
Tracy D. Nixon; Benjamin D. Ward; Chem.Commun. 48 (2012) 11790–; doi:10.1039/c2cc37021b

data_7108641
_publ_section_title
;
 Calcium amido-bisoxazoline complexes in asymmetric
 hydroamination/cyclisation catalysis
;
_journal_name_full               Chem.Commun.
_journal_page_first              11790
_journal_paper_doi               10.1039/c2cc37021b
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_sum            'C64 H56 Ca N6 O4'
_chemical_formula_weight         1013.23
_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                 108.383(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.685(2)
_cell_length_b                   20.844(4)
_cell_length_c                   13.606(2)
_cell_measurement_reflns_used    3746
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.5
_cell_measurement_theta_min      21.5
_cell_volume                     2606.5(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  'rotating anode'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40544
_diffrn_reflns_theta_full        68.87
_diffrn_reflns_theta_max         68.87
_diffrn_reflns_theta_min         4.03
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_T_max  0.8420
_exptl_absorpt_correction_T_min  0.5882
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.071(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         8997
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                8592
_reflns_number_total             8997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37021b.txt
_cod_data_source_block           tdn2
_cod_original_cell_volume        2606.5(9)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7108641