Reactions of (-)-sparteine with alkali metal HMDS complexes: conventional meets the unconventional.
Clark, Natalie M; García-Alvarez, Pablo; Kennedy, Alan R; O'Hara, Charles T; Robertson, Gemma M; Chemical communications (Cambridge, England)  (2009) 5835–5837; doi:10.1039/b908722b

data_7104912
_publ_section_title
;
 Reactions of (-)-sparteine with alkali metal HMDS complexes:
 conventional meets the unconventional.
;
_journal_issue                   39
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5835
_journal_page_last               5837
_journal_paper_doi               10.1039/b908722b
_journal_year                    2009
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C60 H143 N9 Na6 O Si10'
_chemical_formula_weight         1425.67
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 90.450(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.2491(4)
_cell_length_b                   16.2717(3)
_cell_length_c                   14.9831(3)
_cell_measurement_reflns_used    7094
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      72.8966
_cell_measurement_theta_min      4.6630
_cell_volume                     4449.00(16)
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13781
_diffrn_reflns_theta_full        69.00
_diffrn_reflns_theta_max         73.19
_diffrn_reflns_theta_min         6.93
_exptl_absorpt_coefficient_mu    1.973
_exptl_absorpt_correction_T_max  0.9200
_exptl_absorpt_correction_T_min  0.4830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.17 (release 11-02-2008 CrysAlis171 .NET)
(compiled Feb 11 2008,09:33:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6757
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0669P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                5176
_reflns_number_total             6757
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b908722B.txt
_cod_data_source_block           pgagem7
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7104912