#------------------------------------------------------------------------------ #$Date: 2016-03-24 02:12:01 +0200 (Thu, 24 Mar 2016) $ #$Revision: 179561 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/50/30/4503066.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4503066 loop_ _publ_author_name 'Kirchner, Michael T.' 'Das, Dinabandhu' 'Boese, Roland' _publ_section_title ; Cocrystallization with Acetylene: Molecular Complex with Methanol ; _journal_issue 3 _journal_name_full 'Crystal Growth & 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_name_common Methanol _chemical_name_systematic ; Methanol ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _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 4.6469(9) _cell_length_b 4.9285(10) _cell_length_c 9.0403(18) _cell_measurement_reflns_used 421 _cell_measurement_temperature 122(2) _cell_measurement_theta_max 25.287 _cell_measurement_theta_min 4.502 _cell_volume 207.04(7) _computing_cell_refinement 'Bruker SMART' _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 122(2) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 0.745 _diffrn_measured_fraction_theta_max 0.745 _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method ; one run in omega at 0.3\% scan width with 760 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 0.0133 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 811 _diffrn_reflns_theta_full 28.28 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 4.51 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_T_max 0.9736 _exptl_absorpt_correction_T_min 0.8286 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; Empirical absobtion correction by SADABS 2.10. SADABS is run with 0.005 as restraint to the scale factor esd and 3/6 as orders of spherical harmonics on data of 0.1 A resolution. R(int) drops from 3.70% to 1.18%. In the best error model factor g was 0.0331 and was not refinded. The transmission ratio is 0.851099 and a spherical absorbtion correction is not applied. Theoretical values for minimum and maximum transmission based on the size of the capillary are 0.9736 and 0.9736. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cylindrical _exptl_crystal_F_000 72 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.208 _refine_diff_density_min -0.096 _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 1.107 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 21 _refine_ls_number_reflns 243 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.107 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0338 _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^)+(0.0541P)^2^+0.0249P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.0959 _reflns_number_gt 210 _reflns_number_total 243 _reflns_threshold_expression >2sigma(I) _cod_data_source_file cg0701877-file001.cif _cod_data_source_block 1 _cod_original_sg_symbol_H-M P212121 _cod_database_code 4503066 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags O1 O 0.2254(3) 0.3025(2) 0.93036(12) 0.0360(5) Uani 1 1 d . H1 H 0.3754 0.2722 0.9795 0.054 Uiso 1 1 calc R C2 C 0.2535(5) 0.5526(3) 0.85490(17) 0.0397(7) Uani 1 1 d . H2A H 0.2754 0.6997 0.9270 0.060 Uiso 1 1 calc R H2B H 0.0813 0.5849 0.7948 0.060 Uiso 1 1 calc R H2C H 0.4232 0.5465 0.7906 0.060 Uiso 1 1 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0239(12) 0.0416(7) 0.0426(6) 0.0138(5) -0.0039(6) -0.0028(7) C2 0.047(2) 0.0317(8) 0.0406(8) 0.0065(6) -0.0008(12) 0.0030(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 O1 H1 109.5 O1 C2 H2A 109.5 O1 C2 H2B 109.5 H2A C2 H2B 109.5 O1 C2 H2C 109.5 H2A C2 H2C 109.5 H2B C2 H2C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C2 1.4148(19) O1 H1 0.8400 C2 H2A 0.9800 C2 H2B 0.9800 C2 H2C 0.9800 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O1 0.84 1.86 2.6929(11) 174.1 4_557