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_4113201
_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            'C28 H41 Cl N O3 Pd0.5'
_chemical_formula_weight         528.27
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2004-03-12T10:27:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.205(2)
_cell_length_b                   10.282(2)
_cell_length_c                   34.245(8)
_cell_measurement_temperature    296(2)
_cell_volume                     2884.8(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 0.546
_diffrn_measured_fraction_theta_max 0.546
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_unetI/netI     0.0882
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            2535
_diffrn_reflns_theta_full        24.19
_diffrn_reflns_theta_max         24.19
_diffrn_reflns_theta_min         6.12
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       needle
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.023(4)
_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   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         2535
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.1049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+20.5919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2046
_refine_ls_wR_factor_ref         0.2216
_reflns_number_gt                1916
_reflns_number_total             2535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0471673rom20040520_065758.cif
_cod_data_source_block           H.Allouchi_345C5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C28 H41 Cl N O3 Pd0.50'
_cod_database_code               4113201