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_4110043
_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 beta'
_chemical_name_systematic
; 
Ethynylbenzene, polymorph beta at 0.4 GPa
;
_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                71.03(3)
_cell_angle_beta                 82.30(3)
_cell_angle_gamma                78.49(3)
_cell_formula_units_Z            6
_cell_length_a                   5.8187(12)
_cell_length_b                   9.1892(18)
_cell_length_c                   18.204(4)
_cell_measurement_reflns_used    1944
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.31
_cell_volume                     899.5(4)
_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 0.138
_diffrn_measured_fraction_theta_max 0.138
_diffrn_measurement_device_type  'Kuma KM4CCD \k geometry'
_diffrn_measurement_method       '\w scans'
_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  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4054
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Katrusiak, A. (2003). REDSHABS - Program for correcting
reflections intensities for DAC absorption, gasket shadowing
and sample crystal absorption. Adam Mickiewicz University, Pozna\'n.
Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.050
_refine_diff_density_min         -0.059
_refine_diff_density_rms         0.012
_refine_ls_extinction_coef       0.018(6)
_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   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0412P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                417
_reflns_number_total             616
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ja074885rsi20070703_084723.cif
_cod_data_source_block           1pha
_cod_original_cell_volume        899.5(3)
_cod_database_code               4110043