Nearly Isostructural Polymorphs of Ethynylbenzene: Resolution of \τbCH...π(arene) and Cooperative \τbCH...π(C\τbC) Interactions by Pressure Freezing
Kamil Dziubek; Marcin Podsiadło; Andrzej Katrusiak; Journal of the American Chemical Society 129 (2007) 12620–12621; doi:10.1021/ja074885r

data_4110048
_publ_contact_author_fax         +48(61)8658008
_publ_contact_author_phone       +48(61)8291443
_publ_section_title
;
 Nearly Isostructural Polymorphs of Ethynylbenzene: Resolution of
 \\tbCH...\p(arene) and Cooperative \\tbCH...\p(C\\tbC) Interactions by
 Pressure Freezing
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12620
_journal_page_last               12621
_journal_paper_doi               10.1021/ja074885r
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C8 H6'
_chemical_formula_sum            'C8 H6'
_chemical_formula_weight         102.13
_chemical_melting_point          228
_chemical_name_common            'phenylacetylene, polymorph alpha at 100K'
_chemical_name_systematic
; 
Ethynylbenzene, polymorph alpha at 100K
;
_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                77.59(3)
_cell_angle_beta                 81.62(3)
_cell_angle_gamma                80.75(3)
_cell_formula_units_Z            5
_cell_length_a                   5.7585(12)
_cell_length_b                   9.1743(18)
_cell_length_c                   15.417(3)
_cell_measurement_reflns_used    1142
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.38
_cell_measurement_theta_min      2.43
_cell_volume                     779.9(3)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction, 2004)'
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2004)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2004)'
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.710
_diffrn_measured_fraction_theta_max 0.710
_diffrn_measurement_device_type  'Kuma KM-4-CCD'
_diffrn_measurement_method       \w
_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  0.1049
_diffrn_reflns_av_sigmaI/netI    0.2175
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8569
_diffrn_reflns_theta_full        29.38
_diffrn_reflns_theta_max         29.38
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             270
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.032(17)
_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   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         3047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.2622
_refine_ls_R_factor_gt           0.1087
_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^)+(0.1532P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3042
_refine_ls_wR_factor_ref         0.3882
_reflns_number_gt                996
_reflns_number_total             3047
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ja074885rsi20070703_084857.cif
_cod_data_source_block           2pha_nis
_cod_database_code               4110048