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_4503067
_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'
_chemical_formula_sum            'C H4 O'
_chemical_formula_weight         32.04
_chemical_melting_point          175.37
_chemical_name_common            Methanol
_chemical_name_systematic        Methanol
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      36
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 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                   6.401(2)
_cell_length_b                   7.220(3)
_cell_length_c                   4.6470(10)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      8.5
_cell_volume                     214.76(12)
_computing_cell_refinement
;
Siemens P3-PC diffractometer program V.4.24
;
_computing_data_collection
;
Siemens P3-PC diffractometer program V.4.24
;
_computing_data_reduction        'Siemens XDISK V.4.20.2 1991 PC'
_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      160(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Nicolet R3m/V four circle diffractometer
;
_diffrn_measurement_method       'Wyckoff scan mode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0117
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1551
_diffrn_reflns_theta_full        39.99
_diffrn_reflns_theta_max         39.99
_diffrn_reflns_theta_min         4.25
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9745
_exptl_absorpt_correction_T_min  0.9745
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylindrical
_exptl_crystal_F_000             72
_exptl_crystal_recrystallization_method
;
The crystallization was performed in a sealed capillary on the
diffractometer at a temperature of 150 K with a miniature zone melting
procedure using focused infrared-radiation according to
D. Brodalla, D. Mootz, R. Boese, W. O\&swald, 
J. Appl. Cryst. 1985, 18, 316.
;
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.101
_refine_diff_density_rms         0.030
_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   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         387
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0736P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                275
_reflns_number_total             387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0701877-file002.cif
_cod_data_source_block           2
_cod_database_code               4503067