Synthesis, optical properties, crystal structures and phase behaviour of symmetric, conjugated ethynylarene-based rigid rods with terminal carboxylate groups
Tolulope M. Fasina; Jonathan C. Collings; Jacqueline M. Burke; Andrei S. Batsanov; Richard M. Ward; David Albesa-Jové; Laurent Porrès; Andrew Beeby; Judith A. K. Howard; Andrew J. Scott; William Clegg; Stephen W. Watt; Christopher Viney; Todd B. Marder; Journal of Materials Chemistry 15 (2005) 690–; doi:10.1039/b413514h

data_7203686
_publ_section_title
;
 Synthesis, optical properties, crystal structures and phase behaviour
 of symmetric, conjugated ethynylarene-based rigid rods with terminal
 carboxylate groups
;
_journal_issue                   6
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              690
_journal_paper_doi               10.1039/b413514h
_journal_volume                  15
_journal_year                    2005
_chemical_formula_moiety         'C20 H14 O4'
_chemical_formula_sum            'C20 H14 O4'
_chemical_formula_weight         318.31
_chemical_melting_point          463.5(5)
_chemical_name_common            1,4-Bis(4-carbomethoxyphenyl)butadiyne
_chemical_name_systematic
;
1,4-Bis(4-carbomethoxyphenyl)butadiyne
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.204(3)
_cell_angle_beta                 72.585(3)
_cell_angle_gamma                75.457(3)
_cell_formula_units_Z            2
_cell_length_a                   7.0249(5)
_cell_length_b                   10.4613(8)
_cell_length_c                   11.7016(8)
_cell_measurement_reflns_used    884
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      60.873
_cell_measurement_theta_min      6.190
_cell_volume                     778.97(10)
_computing_cell_refinement       'SMART V5.625 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.02a (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V5.1 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'ProteumM APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
'60W microfocus Bede Microsource with glass polycapillary optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6778
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0663P)^2^+0.1963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1406
_reflns_number_gt                3456
_reflns_number_total             4305
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b413514h.txt
_cod_data_source_block           (6)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '463--464' was changed to '463.5(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        779.0(1)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203686