Three different product types from reactions of lithiated cyclic aminals with trivalent organometal chlorides.
Hellmann, Benjamin J.; Kamps, Ina; Mix, Andreas; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Chemical communications (Cambridge, England) 46 (2010) 6536–6538; doi:10.1039/c0cc01830a

data_7112798
_publ_section_title
;
 Three different product types from reactions of lithiated cyclic aminals
 with trivalent organometal chlorides.
;
_journal_issue                   35
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6536
_journal_page_last               6538
_journal_paper_doi               10.1039/c0cc01830a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C18 H29 N4 Y, 0.5 (C7 H8)'
_chemical_formula_sum            'C21.5 H33 N4 Y'
_chemical_formula_weight         436.43
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 129.264(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.8849(19)
_cell_length_b                   12.5835(9)
_cell_length_c                   17.2346(13)
_cell_measurement_reflns_used    352
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      40.1903
_cell_measurement_theta_min      6.2816
_cell_volume                     4346.3(6)
_computing_cell_refinement       'APEX2 v2009.11-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2009, 11, 1, 0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      225(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker AXS X8 Prospector Ultra with APEX II'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'Quazar Montel multilayer optic Montel200'
_diffrn_radiation_source         'I\mS Incoatec Microfocus'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27268
_diffrn_reflns_theta_full        72.19
_diffrn_reflns_theta_max         72.19
_diffrn_reflns_theta_min         5.14
_exptl_absorpt_coefficient_mu    3.855
_exptl_absorpt_correction_T_max  0.7741
_exptl_absorpt_correction_T_min  0.2818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
;
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+2.8608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                4117
_reflns_number_total             4337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc01830a.txt
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C21.50 H33 N4 Y'
_cod_database_code               7112798