Cocrystallization with Acetylene: Molecular Complex with Methanol
Kirchner, Michael T.; Das, Dinabandhu; Boese, Roland; Crystal Growth & Design 8 (2008) 763–; doi:10.1021/cg0701877

data_4503068
_publ_section_title
;
 Cocrystallization with Acetylene: Molecular Complex with Methanol
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              763
_journal_paper_doi               10.1021/cg0701877
_journal_volume                  8
_journal_year                    2008
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C H4 O, C2 H2'
_chemical_formula_sum            'C3 H6 O'
_chemical_formula_weight         58.08
_chemical_melting_point          161
_chemical_name_common            'ethine methanol cocrystal'
_chemical_name_systematic        'ethine methanol cocrystal'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.565(3)
_cell_length_b                   7.314(5)
_cell_length_c                   13.165(8)
_cell_measurement_reflns_used    553
_cell_measurement_temperature    155(2)
_cell_measurement_theta_max      19.459
_cell_measurement_theta_min      3.945
_cell_volume                     439.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      155(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART  CCD area detector'
_diffrn_measurement_method
;
one run in omega at 0.3\% scan width
with 740 frames, phi = 0\%, chi = 0\% 
;
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1843
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2150
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_correction_T_min  0.7384
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
Empirical absobtion correction by TWINABS 1.05.  TWINABS is run with 0.003 as
restraint to the scale factor esd and 1/4 as orders of spherical harmonics on
data of 1.1 A resolution of components one and two for parameter refinement.
R(int) drops from 7.36% to 4.94%. The scale factor is around 1.0. In the best
error model factor g was 0.2088 and was not refinded. The first two components
are better in Rint than the last two components.  The transmission ratio is
0.752782 and a spherical absorbtion correction is not applied. Theoretical
values for minimum and maximum transmission based on the size of the crystal
are 0.9809 and 0.9809.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       oligocrystaline
_exptl_crystal_F_000             128
_exptl_crystal_recrystallization_method
;
The crystallization was performed in a sealed and pressurized capillary on the
diffractometer at a temperature of 161 K with a miniature zone melting
procedure using focused infrared-laser-radiation according to: R. Boese,
M.Nussbaumer, "In Situ crystallisation Techniques", in: "Organic  Crystal
Chemistry", Ed. D.W. Jones, Oxford University Press, Oxford, England, (1994)
20-37
;
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.722
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         2152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.722
_refine_ls_R_factor_all          0.1974
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0641P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1427
_reflns_number_gt                631
_reflns_number_total             2152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0701877-file003.cif
_cod_data_source_block           3
_cod_original_cell_volume        439.5(4)
_cod_database_code               4503068