Metal Complexes of Cinchonine as Chiral Building Blocks: A Strategy for the Construction of Nanotubular Architectures and Helical Coordination Polymers
Tomasz Kaczorowski; Iwona Justyniak; Teodozja Lipińska; Janusz Lipkowski; Janusz Lewiński; Journal of the American Chemical Society 131 (2009) 5393–5395; doi:10.1021/ja8098867

data_4104216
_publ_contact_author
;
   Prof. Janusz Lewi\'nski,
   Department of Chemistry
   Warsaw University of Technology
   Noakowskiego 3,
   PL-00-664 Warszawa
   Poland
;
_publ_contact_author_email       lewin@ch.pw.edu.pl
_publ_contact_author_fax         '048 22 2347279'
_publ_contact_author_phone       '048 22 2347315'
_publ_section_title
;
 Metal Complexes of Cinchonine as Chiral Building Blocks: A Strategy for
 the Construction of Nanotubular Architectures and Helical Coordination
 Polymers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5393
_journal_page_last               5395
_journal_paper_doi               10.1021/ja8098867
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_sum            'C83 H92 Al2 Cl2 N8 O4'
_chemical_formula_weight         1390.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   18.9541(2)
_cell_length_b                   18.9541(2)
_cell_length_c                   22.4362(4)
_cell_measurement_reflns_used    10696
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     6980.50(16)
_computing_cell_refinement       'Denzo & Scalepak (Otwinowski, Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction        'Denzo & Scalepak (Otwinowski, Minor, 1997)'
_computing_molecular_graphics
;
DIAMOND v2.1 (Brandenburg, 1999)
Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565,
ORTEP III (Burnett, Johnson, 1996)
;
_computing_publication_material
;
SHELXL-97 (Sheldrick, 1997),
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  71 frames, \w rotation 1.6\% per frame (190s per frame)
  65 frames, \w rotation 1.6\% per frame (190s per frame) 
  60 frames, \w rotation 1.6\% per frame (190s per frame) 
  71 frames, \w rotation 1.6\% per frame (190s per frame)
  68 frames, \w rotation 1.6\% per frame (190s per frame)
  65 frames, \w rotation 1.6\% per frame (190s per frame)
;
_diffrn_measurement_device       '\k-geometry diffractometr'
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'area detector \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  0.0650
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14422
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepak (Otwinowski, Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.992
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2214
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         8515
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1442P)^2^+2.4081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.2079
_reflns_number_gt                6565
_reflns_number_total             8515
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja8098867_si_006.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        6980.36(16)
_cod_database_code               4104216