# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1828 ############################################################################## ### CIF submission form for powder structure report (Acta Cryst. C) ### ### (Provisional) Version: 14 March 1997 ### ############################################################################## #============================================================================= data_global #============================================================================== _publ_contact_author ; Dr.Maryjane Tremayne School of Chemistry University of Birmingham Edgbaston Birmingham B15 2TT UK ; _publ_contact_author_phone "44-121-414-3201" _publ_contact_author_fax "44-121-414-3808" _publ_contact_author_email m.tremayne@bham.ac.uk _publ_requested_journal "Chemical Communications" _publ_requested_coeditor_name ? _publ_contact_letter ; This is the powder CIF for the manuscript entitled Direct-space structure solution from laboratory powder diffraction data of an organic cocrystal containing two different molecular components: 1,2,3-trihydroxybenzene-HMTA (1/1). ; #============================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _iucr_compatibility_tag ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== _publ_section_title ; Direct-space structure solution from laboratory powder diffraction data of an organic cocrystal containing two different molecular components: 1,2,3-trihydroxybenzene-HMTA (1/1). ; loop_ _publ_author_name _publ_author_address "Tremayne, Maryjane" ; School of Chemistry University of Birmingham Edgbaston Birmingham B15 2TT UK ; "Glidewell, Christopher" ; Department of Chemistry University of St.Andrews St.Andrews Fife, KY16 9ST UK ; #============================================================================== #_publ_section_synopsis ; ? ; #_publ_section_abstract ; ? ; #_publ_section_comment ; ? ; #_publ_section_experimental ; ? ; #_pd_prep_conditions ; ? ; #_publ_section_references ; ? ; #_publ_section_figure_captions ; ? ; #_publ_section_acknowledgements ; ? ; #============================================================================== data_TIBS _chemical_name_systematic ; 1,2,3-Trihydroxybenzene : hexamethylenetetramine ; _chemical_name_common ? _chemical_formula_moiety "C6 H6 O3 : C6 H12 N4 " _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum "C12 H18 N4 O3" _chemical_formula_weight 266.30 _chemical_melting_point ? _chemical_compound_source "crystallization from methanol" loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 60.0 0.0033 0.0016 "International Tables Vol C Tables 4.2.6.8 and 6.1.1.4" O O 8.0 0.0106 0.0060 "International Tables Vol C Tables 4.2.6.8 and 6.1.1.4" N N 4.0 0.0061 0.0033 "International Tables Vol C Tables 4.2.6.8 and 6.1.1.4" H H 100.0 0.0000 0.0000 "International Tables Vol C Tables 4.2.6.8 and 6.1.1.4" #============================================================================== _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M "P 21/n" _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz "x, y, z" "-x+1/2, y+1/2, -z+1/2" "-x, -y, -z" "x+1/2, -y+1/2, z+1/2" _cell_length_a 10.7691(2) _cell_length_b 7.0107(2) _cell_length_c 16.7519(4) _cell_angle_alpha 90.0 _cell_angle_beta 91.402(2) _cell_angle_gamma 90.0 _cell_volume 1264.38(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273 _cell_special_details ; ? ; _pd_spec_size_axial 30 _pd_spec_size_equat 0.5 _pd_spec_size_thick ? _pd_spec_mounting "disc" _pd_spec_mount_mode transmission _pd_spec_shape plate _pd_char_particle_morphology ? _pd_char_colour "white" _pd_prep_conditions ? _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _exptl_crystal_density_diffrn ? _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================== _exptl_special_details ; ? ; _pd_instr_location ; School of Chemistry, University of St.Andrews, St.Andrews, Fife, Scotland. KY16 9ST. UK. ; _diffrn_ambient_temperature 273 _diffrn_radiation_polarisn_ratio 0.55 _diffrn_radiation_wavelength 1.54056 _diffrn_radiation_type "laboratory" _diffrn_radiation_source "sealed X-ray tube" _diffrn_radiation_monochromator "Ge" _diffrn_measurement_device "position sensitive detector" _diffrn_measurement_method "Debye Scherrer" _computing_data_collection "Win XPOW (STOE & GmbH, 1998)" _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution "OCTOPUS (Tremayne et al. 1997)" _computing_structure_refinement "GSAS (Larson et al. 1994)" _computing_molecular_graphics ? _computing_publication_material ? _pd_meas_2theta_range_min 5.00 _pd_meas_2theta_range_max 74.99 _pd_meas_2theta_range_inc 0.02 _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? #============================================================================== _pd_proc_ls_special_details ; ? ; _pd_proc_ls_profile_function pseudovoigt _pd_proc_ls_pref_orient_corr 0.807 _pd_proc_ls_prof_R_factor 0.0540 _pd_proc_ls_prof_wR_factor 0.0740 _pd_proc_ls_prof_wR_expected ? _refine_ls_R_I_factor ? _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef ? _refine_ls_matrix_type ? _refine_ls_weighting_scheme ? _refine_ls_hydrogen_treatment restr _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 654 _refine_ls_number_parameters 117 _refine_ls_number_restraints 102 _refine_ls_number_constraints ? _refine_ls_goodness_of_fit_all 5.75 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max ? _refine_ls_shift/esd_mean ? _pd_proc_2theta_range_min 8.00 _pd_proc_2theta_range_max 74.99 _pd_proc_2theta_range_inc 0.02 _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? _pd_proc_wavelength 1.54056 #============================================================================== loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity C11 0.156(1) -0.084(2) 0.150(1) 1.0 Uiso 0.024(3) 4 C12 0.217(1) 0.061(2) 0.110(1) 1.0 Uiso 0.024(3) 4 C13 0.347(1) 0.053(2) 0.103(1) 1.0 Uiso 0.024(3) 4 C14 0.411(1) -0.086(2) 0.149(1) 1.0 Uiso 0.024(3) 4 C15 0.348(1) -0.225(2) 0.190(1) 1.0 Uiso 0.024(3) 4 C16 0.220(1) -0.222(2) 0.191(1) 1.0 Uiso 0.024(3) 4 O11 0.0315(7) -0.066(1) 0.1603(6) 1.0 Uiso 0.026(2) 4 O12 0.1508(7) 0.196(2) 0.0648(6) 1.0 Uiso 0.026(2) 4 O13 0.4031(7) 0.176(1) 0.0537(6) 1.0 Uiso 0.026(2) 4 H11 -0.003 0.060 0.153 1.0 Uiso ? 4 H12 0.198 0.273 0.029 1.0 Uiso ? 4 H13 0.488 0.199 0.070 1.0 Uiso ? 4 H14 0.515(2) -0.084(10) 0.150(5) 1.0 Uiso 0.05 4 H15 0.399(3) -0.337(10) 0.222(2) 1.0 Uiso 0.05 4 H16 0.170(3) -0.330(10) 0.225(3) 1.0 Uiso 0.05 4 C21 0.890(1) 0.356(2) 0.0426(7) 1.0 Uiso 0.032(2) 4 N21 0.866(1) 0.244(2) 0.1144(7) 1.0 Uiso 0.033(2) 4 C22 0.665(1) 0.396(2) 0.0205(6) 1.0 Uiso 0.032(2) 4 N22 0.784(1) 0.499(2) 0.0327(7) 1.0 Uiso 0.033(2) 4 C23 0.744(1) 0.145(1) 0.1006(8) 1.0 Uiso 0.032(2) 4 N23 0.638(1) 0.281(2) 0.0900(7) 1.0 Uiso 0.033(2) 4 C24 0.862(1) 0.353(2) 0.1887(6) 1.0 Uiso 0.032(2) 4 N24 0.755(1) 0.490(2) 0.1808(6) 1.0 Uiso 0.033(2) 4 C25 0.777(1) 0.602(1) 0.1097(8) 1.0 Uiso 0.032(2) 4 C26 0.639(1) 0.385(2) 0.1648(7) 1.0 Uiso 0.032(2) 4 H211 0.976(2) 0.435(5) 0.053(3) 1.0 Uiso 0.07 4 H212 0.891(4) 0.274(5) -0.011(1) 1.0 Uiso 0.07 4 H221 0.590(2) 0.504(5) 0.017(3) 1.0 Uiso 0.07 4 H222 0.670(4) 0.321(6) -0.036(1) 1.0 Uiso 0.07 4 H231 0.724(3) 0.062(5) 0.154(2) 1.0 Uiso 0.07 4 H232 0.751(3) 0.061(5) 0.047(2) 1.0 Uiso 0.07 4 H241 0.846(4) 0.268(5) 0.242(1) 1.0 Uiso 0.07 4 H242 0.948(2) 0.431(5) 0.199(3) 1.0 Uiso 0.07 4 H251 0.693(4) 0.699(6) 0.104(2) 1.0 Uiso 0.07 4 H252 0.859(4) 0.693(6) 0.118(2) 1.0 Uiso 0.07 4 H261 0.558(2) 0.483(5) 0.164(3) 1.0 Uiso 0.07 4 H262 0.632(4) 0.287(5) 0.216(1) 1.0 Uiso 0.07 4 #============================================================================== _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 O11 1.361(8) ? ? ? C11 C12 1.395(9) ? ? ? C11 C16 1.363(9) ? ? ? C12 O12 1.391(8) ? ? ? C12 C13 1.410(8) ? ? ? C13 O13 1.347(8) ? ? ? C13 C14 1.414(9) ? ? ? C14 C15 1.384(9) ? ? ? C15 C16 1.376(9) ? ? ? C21 N21 1.466(9) ? ? ? C21 N22 1.523(9) ? ? ? C22 N22 1.477(9) ? ? ? C22 N23 1.456(9) ? ? ? C23 N21 1.492(9) ? ? ? C23 N23 1.498(9) ? ? ? C24 N21 1.464(9) ? ? ? C24 N24 1.505(9) ? ? ? C25 N22 1.481(9) ? ? ? C25 N24 1.454(10) ? ? ? C26 N23 1.456(9) ? ? ? C26 N24 1.463(9) ? ? ? C14 H14 1.11(2) ? ? ? C15 H15 1.09(2) ? ? ? C16 H16 1.10(2) ? ? ? C21 H211 1.09(2) ? ? ? C21 H212 1.08(2) ? ? ? C22 H221 1.11(2) ? ? ? C22 H222 1.09(2) ? ? ? C23 H231 1.10(2) ? ? ? C23 H232 1.08(2) ? ? ? C24 H241 1.09(2) ? ? ? C24 H242 1.09(2) ? ? ? C25 H251 1.14(2) ? ? ? C25 H252 1.09(2) ? ? ? C26 H261 1.10(2) ? ? ? C26 H262 1.11(2) ? ? ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 C11 C12 118(1) ? ? ? ? O11 C11 C16 119(1) ? ? ? ? C12 C11 C16 122(1) ? ? ? ? O12 C12 C11 121(1) ? ? ? ? O12 C12 C13 119(1) ? ? ? ? C11 C12 C13 119(1) ? ? ? ? O13 C13 C12 119(1) ? ? ? ? O13 C13 C14 124(1) ? ? ? ? C12 C13 C14 118(1) ? ? ? ? C13 C14 C15 121(1) ? ? ? ? C14 C15 C16 120(1) ? ? ? ? C11 C16 C15 120(1) ? ? ? ? N21 C21 N22 108(1) ? ? ? ? C21 N21 C23 107(1) ? ? ? ? C21 N21 C24 115(1) ? ? ? ? C23 N21 C24 109(1) ? ? ? ? N22 C22 N23 111(1) ? ? ? ? C21 N22 C22 109(1) ? ? ? ? C21 N22 C25 106(1) ? ? ? ? C22 N22 C25 108(1) ? ? ? ? N21 C23 N23 113(1) ? ? ? ? C22 N23 C23 106(1) ? ? ? ? C22 N23 C26 114(1) ? ? ? ? C23 N23 C26 103(1) ? ? ? ? N21 C24 N24 107(1) ? ? ? ? C24 N24 C25 106(1) ? ? ? ? C24 N24 C26 110(1) ? ? ? ? C25 N24 C26 106(1) ? ? ? ? N22 C25 N24 118(1) ? ? ? ? N23 C26 N24 114(1) ? ? ? ? C13 C14 H14 118(2) ? ? ? ? C15 C14 H14 121(2) ? ? ? ? C14 C15 H15 120(2) ? ? ? ? C16 C15 H15 120(2) ? ? ? ? C11 C16 H16 120(2) ? ? ? ? C15 C16 H16 120(2) ? ? ? ? N21 C21 H211 108(2) ? ? ? ? N21 C21 H212 114(2) ? ? ? ? N22 C21 H211 108(2) ? ? ? ? N22 C21 H212 107(2) ? ? ? ? H211 C21 H212 112(2) ? ? ? ? N22 C22 H221 108(2) ? ? ? ? N23 C22 H221 104(2) ? ? ? ? N22 C22 H222 108(2) ? ? ? ? N23 C22 H222 116(2) ? ? ? ? H221 C22 H222 110(2) ? ? ? ? N21 C23 H231 109(2) ? ? ? ? N21 C23 H232 108(2) ? ? ? ? N23 C23 H231 105(2) ? ? ? ? N23 C23 H232 108(2) ? ? ? ? H231 C23 H232 114(2) ? ? ? ? N21 C24 H241 115(2) ? ? ? ? N24 C24 H241 107(2) ? ? ? ? N21 C24 H242 111(2) ? ? ? ? N24 C24 H242 110(2) ? ? ? ? H241 C24 H242 107(2) ? ? ? ? N22 C25 H251 106(2) ? ? ? ? N22 C25 H252 110(2) ? ? ? ? N24 C25 H252 111(2) ? ? ? ? N24 C25 H251 104(2) ? ? ? ? H251 C25 H252 108(2) ? ? ? ? N23 C26 H261 108(2) ? ? ? ? N23 C26 H262 110(2) ? ? ? ? N24 C26 H261 111(2) ? ? ? ? N24 C26 H262 104(2) ? ? ? ? H261 C26 H262 109(2) ? ? ? ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./