A Generalized Model for the Molecular Arrangement in the Columnar Mesophases of Polycatenar Mesogens. Crystal and Molecular Structure of Two Hexacatenar Mesogens
Bertrand Donnio; Benoît Heinrich; Hassan Allouchi; Jens Kain; Siegmar Diele; Daniel Guillon; Duncan W. Bruce; Journal of the American Chemical Society 126 (2004) 15258–15268; doi:10.1021/ja0471673

data_4113202
_publ_contact_author             'Hassan Allouchi'
_publ_contact_author_email       hassan.allouchi@univ-tours.fr
_publ_section_title
;
 A Generalized Model for the Molecular Arrangement in the Columnar
 Mesophases of Polycatenar Mesogens. Crystal and Molecular Structure of
 Two Hexacatenar Mesogens
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15258
_journal_page_last               15268
_journal_paper_doi               10.1021/ja0471673
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C37 H59 Cl N O3 Pd0.5'
_chemical_formula_weight         654.5
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2004-03-11T18:34:59-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                85.9580(10)
_cell_angle_beta                 89.6730(10)
_cell_angle_gamma                85.248(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9605(3)
_cell_length_b                   9.0629(3)
_cell_length_c                   23.4280(8)
_cell_measurement_temperature    296(2)
_cell_volume                     1891.29(11)
_computing_data_collection       'KappaCCD (Nonius, 1998)'
_computing_data_reduction        'Denzo(Otwinowski & Miror, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.95
_diffrn_measured_fraction_theta_max 0.95
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7929
_diffrn_reflns_theta_full        27.08
_diffrn_reflns_theta_max         27.08
_diffrn_reflns_theta_min         4.02
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       needle
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.0015(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7929
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.5741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                5243
_reflns_number_total             7929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0471673rom20040520_065845.cif
_cod_data_source_block           H.Allouchi_234C8
_cod_original_formula_sum        'C37 H59 Cl N O3 Pd0.50'
_cod_database_code               4113202