Liquid-crystalline azines formed by the rare-earth promoted decomposition of hydrazide ?habbe? ligands: structural and thermal properties
Van Deun, Rik; Parac-Vogt, Tatjana N.; Van Hecke, Kristof; Van Meervelt, Luc; Binnemans, Koen; Guillon, Daniel; Donnio, Bertrand; Journal of Materials Chemistry 13 (2003) 1639–; doi:10.1039/b303941m

data_7204656
_publ_section_title
;
 Liquid-crystalline azines formed by the rare-earth promoted
 decomposition of hydrazide ?habbe? ligands: structural and thermal
 properties
;
_journal_issue                   7
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1639
_journal_paper_doi               10.1039/b303941m
_journal_volume                  13
_journal_year                    2003
_chemical_formula_moiety         'C30 H44 N2 O4'
_chemical_formula_sum            'C30 H44 N2 O4'
_chemical_formula_weight         496.67
_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_method           SHELXL-97
_cell_angle_alpha                92.489(8)
_cell_angle_beta                 91.835(6)
_cell_angle_gamma                101.208(7)
_cell_formula_units_Z            1
_cell_length_a                   5.6139(5)
_cell_length_b                   11.0646(12)
_cell_length_c                   11.2402(11)
_cell_measurement_temperature    110(2)
_cell_volume                     683.65(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    PLUTON
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'SMART 6000'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'crossed Goebel mirrors'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1049
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2555
_diffrn_reflns_theta_full        71.12
_diffrn_reflns_theta_max         71.12
_diffrn_reflns_theta_min         3.94
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.9693
_exptl_absorpt_correction_T_min  0.7875
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             270
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.007(2)
_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   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\\s^2^(Fo^2^)+(0.1554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1847
_refine_ls_wR_factor_ref         0.1986
_reflns_number_gt                1978
_reflns_number_total             2555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303941m.txt
_cod_data_source_block           wg15
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204656