#------------------------------------------------------------------------------ #$Date: 2015-08-08 03:49:42 +0300 (Sat, 08 Aug 2015) $ #$Revision: 153073 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/52/02/1520226.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_1520226 loop_ _publ_author_name 'Xu, Jun' 'Yu, Hongde' 'Yang, Liulin' 'Wu, Guanglu' 'Wang, Zhiqiang' 'Wang, Dong' 'Zhang, Xi' _publ_section_title ; Self-assembling 1D core/shell microrods by the introduction of additives: a one-pot and shell-tunable method ; _journal_issue 8 _journal_name_full 'Chem. Sci.' _journal_page_first 4907 _journal_paper_doi 10.1039/C5SC01631B _journal_volume 6 _journal_year 2015 _chemical_formula_moiety 'C5 H11 N6, Cl' _chemical_formula_sum 'C5 H11 Cl N6' _chemical_formula_weight 190.65 _chemical_name_common 'dimethyl melamine hydrochloride' _chemical_name_systematic Mela-DM?HCl _space_group_IT_number 53 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2' _symmetry_space_group_name_H-M 'P m n a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _audit_update_record ; 2015-05-05 deposited with the CCDC. 2015-06-03 downloaded from the CCDC. ; _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.4782(13) _cell_length_b 9.5193(19) _cell_length_c 14.311(3) _cell_measurement_reflns_used 2947 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 29.2 _cell_measurement_theta_min 2.5 _cell_volume 882.5(3) _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 153(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Rigaku Saturn724+' _diffrn_measurement_method dtprofit.ref _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 7576 _diffrn_reflns_theta_full 29.12 _diffrn_reflns_theta_max 29.12 _diffrn_reflns_theta_min 2.14 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.390 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 400 _exptl_crystal_size_max 0.125 _exptl_crystal_size_mid 0.085 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.329 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.093 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 85 _refine_ls_number_reflns 1283 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0355 _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^)+(0.0600P)^2^+0.7000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.1214 _reflns_number_gt 1053 _reflns_number_total 1283 _reflns_threshold_expression I>2sigma(I) _iucr_refine_instructions_details ; TITL bo2923 in Pmna CELL 0.71073 6.4782 9.5193 14.3112 90.000 90.000 90.000 ZERR 4.00 0.0013 0.0019 0.0029 0.000 0.000 0.000 LATT 1 SYMM 0.5+X, Y, 0.5-Z SYMM 0.5+X, -Y, 0.5+Z SYMM X, -Y, -Z SFAC C H N Cl UNIT 20 44 24 4 EQIV $1 X, 1+Y, Z EQIV $2 1-X, 1-Y, 1-z HTAB N3 CL1_$1 HTAB N4 CL1 HTAB N5 CL1_$1 HTAB N6 N1_$2 HTAB N6 CL1_$2 L.S. 4 ACTA BOND $H FMAP 2 PLAN 10 WGHT 0.060000 0.700000 FVAR 0.76824 CL1 4 0.500000 0.084728 0.640662 10.50000 0.08305 0.01382 = 0.02491 0.00127 0.00000 0.00000 N1 3 0.500000 0.525887 0.635971 10.50000 0.02690 0.01410 = 0.01644 -0.00044 0.00000 0.00000 N2 3 0.500000 0.615123 0.794591 10.50000 0.02330 0.01533 = 0.01760 -0.00066 0.00000 0.00000 N3 3 0.500000 0.768410 0.665763 10.50000 0.03281 0.01274 = 0.01613 0.00012 0.00000 0.00000 H3 2 0.500000 0.868390 0.643920 10.50000 -1.20000 N4 3 0.500000 0.378992 0.761877 10.50000 0.03102 0.01455 = 0.01846 0.00101 0.00000 0.00000 H4D 2 0.500000 0.309368 0.721080 10.50000 -1.20000 N5 3 0.500000 0.857180 0.814065 10.50000 0.03873 0.01518 = 0.01786 -0.00288 0.00000 0.00000 H5D 2 0.500000 0.941088 0.786875 10.50000 -1.20000 N6 3 0.500000 0.686553 0.515144 10.50000 0.05002 0.01601 = 0.01564 -0.00114 0.00000 0.00000 H6A 2 0.500000 0.624560 0.475288 10.50000 -1.20000 H6B 2 0.500000 0.783500 0.494676 10.50000 -1.20000 C1 1 0.500000 0.657495 0.605664 10.50000 0.02444 0.01548 = 0.01788 -0.00198 0.00000 0.00000 C2 1 0.500000 0.509898 0.730652 10.50000 0.01733 0.01686 = 0.01721 -0.00020 0.00000 0.00000 C3 1 0.500000 0.744223 0.759971 10.50000 0.02097 0.01677 = 0.01678 -0.00203 0.00000 0.00000 C4 1 0.500000 0.339972 0.860111 10.50000 0.03794 0.02176 = 0.02151 0.00627 0.00000 0.00000 AFIX 137 H4A 2 0.566886 0.250678 0.867546 10.50000 -1.50000 H4B 2 0.360327 0.333627 0.882124 10.50000 -1.50000 H4C 2 0.572787 0.409851 0.895519 10.50000 -1.50000 AFIX 0 C5 1 0.500000 0.852342 0.915593 10.50000 0.04512 0.02709 = 0.01821 -0.00714 0.00000 0.00000 AFIX 137 H5A 2 0.367446 0.881309 0.938575 10.50000 -1.50000 H5B 2 0.604514 0.914344 0.939271 10.50000 -1.50000 H5C 2 0.528040 0.758179 0.935979 10.50000 -1.50000 HKLF 4 REM bo2923 in Pmna REM R1 = 0.0355 for 1053 Fo > 4sig(Fo) and 0.0476 for all 1283 data REM 85 parameters refined using 0 restraints END ; _cod_data_source_file c5sc01631b3.cif _cod_data_source_block bo2923 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius Adding full bibliography for 1520226.cif. ; _cod_cif_authors_sg_H-M Pmna _cod_database_code 1520226 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' 'x, -y, -z' '-x, -y, -z' '-x-1/2, -y, z-1/2' '-x-1/2, y, -z-1/2' '-x, y, 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 Cl1 Cl 0.5000 0.08473(6) 0.64066(5) 0.0406(3) Uani 1 2 d S N1 N 0.5000 0.5259(2) 0.63597(13) 0.0191(4) Uani 1 2 d S N2 N 0.5000 0.6151(2) 0.79459(13) 0.0187(4) Uani 1 2 d S N3 N 0.5000 0.7684(2) 0.66576(13) 0.0206(4) Uani 1 2 d S H3 H 0.5000 0.868(3) 0.644(2) 0.025 Uiso 1 2 d S N4 N 0.5000 0.3790(2) 0.76188(14) 0.0213(4) Uani 1 2 d S H4D H 0.5000 0.309(3) 0.721(2) 0.026 Uiso 1 2 d S N5 N 0.5000 0.8572(2) 0.81406(14) 0.0239(5) Uani 1 2 d S H5D H 0.5000 0.941(3) 0.787(2) 0.029 Uiso 1 2 d S N6 N 0.5000 0.6866(2) 0.51514(15) 0.0272(5) Uani 1 2 d S H6A H 0.5000 0.625(4) 0.475(2) 0.033 Uiso 1 2 d S H6B H 0.5000 0.783(3) 0.495(2) 0.033 Uiso 1 2 d S C1 C 0.5000 0.6575(2) 0.60566(16) 0.0193(5) Uani 1 2 d S C2 C 0.5000 0.5099(2) 0.73065(15) 0.0171(4) Uani 1 2 d S C3 C 0.5000 0.7442(2) 0.75997(15) 0.0182(4) Uani 1 2 d S C4 C 0.5000 0.3400(3) 0.86011(17) 0.0271(5) Uani 1 2 d S H4A H 0.5669 0.2507 0.8675 0.041 Uiso 0.50 1 calc PR H4B H 0.3603 0.3336 0.8821 0.041 Uiso 0.50 1 calc PR H4C H 0.5728 0.4099 0.8955 0.041 Uiso 0.50 1 calc PR C5 C 0.5000 0.8523(3) 0.91559(17) 0.0301(6) Uani 1 2 d S H5A H 0.3674 0.8813 0.9386 0.045 Uiso 0.50 1 calc PR H5B H 0.6045 0.9143 0.9393 0.045 Uiso 0.50 1 calc PR H5C H 0.5280 0.7582 0.9360 0.045 Uiso 0.50 1 calc PR 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 Cl1 0.0831(6) 0.0138(3) 0.0249(3) 0.0013(2) 0.000 0.000 N1 0.0269(10) 0.0141(8) 0.0164(8) -0.0004(7) 0.000 0.000 N2 0.0233(10) 0.0153(9) 0.0176(8) -0.0007(7) 0.000 0.000 N3 0.0328(11) 0.0127(9) 0.0161(8) 0.0001(7) 0.000 0.000 N4 0.0310(11) 0.0146(8) 0.0185(9) 0.0010(7) 0.000 0.000 N5 0.0387(13) 0.0152(9) 0.0179(9) -0.0029(7) 0.000 0.000 N6 0.0500(14) 0.0160(9) 0.0156(9) -0.0011(7) 0.000 0.000 C1 0.0244(12) 0.0155(10) 0.0179(10) -0.0020(8) 0.000 0.000 C2 0.0173(10) 0.0169(10) 0.0172(10) -0.0002(7) 0.000 0.000 C3 0.0210(11) 0.0168(10) 0.0168(10) -0.0020(8) 0.000 0.000 C4 0.0379(15) 0.0218(11) 0.0215(11) 0.0063(9) 0.000 0.000 C5 0.0451(17) 0.0271(12) 0.0182(11) -0.0071(9) 0.000 0.000 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 C1 N1 C2 115.51(19) C3 N2 C2 115.63(19) C1 N3 C3 119.48(19) C1 N3 H3 122.7(17) C3 N3 H3 117.9(17) C2 N4 C4 124.5(2) C2 N4 H4D 118.9(19) C4 N4 H4D 116.6(19) C3 N5 C5 123.9(2) C3 N5 H5D 118(2) C5 N5 H5D 118(2) C1 N6 H6A 122(2) C1 N6 H6B 119.7(19) H6A N6 H6B 118(3) N6 C1 N1 121.1(2) N6 C1 N3 117.1(2) N1 C1 N3 121.7(2) N4 C2 N2 117.9(2) N4 C2 N1 116.1(2) N2 C2 N1 126.0(2) N5 C3 N2 122.3(2) N5 C3 N3 116.1(2) N2 C3 N3 121.6(2) N4 C4 H4A 109.5 N4 C4 H4B 109.5 H4A C4 H4B 109.5 N4 C4 H4C 109.5 H4A C4 H4C 109.5 H4B C4 H4C 109.5 N5 C5 H5A 109.5 N5 C5 H5B 109.5 H5A C5 H5B 109.5 N5 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C1 1.326(3) N1 C2 1.364(3) N2 C3 1.325(3) N2 C2 1.357(3) N3 C1 1.362(3) N3 C3 1.368(3) N3 H3 1.00(3) N4 C2 1.324(3) N4 C4 1.454(3) N4 H4D 0.88(3) N5 C3 1.325(3) N5 C5 1.454(3) N5 H5D 0.89(3) N6 C1 1.325(3) N6 H6A 0.82(3) N6 H6B 0.97(3) C4 H4A 0.9600 C4 H4B 0.9600 C4 H4C 0.9600 C5 H5A 0.9600 C5 H5B 0.9600 C5 H5C 0.9600 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 N3 H3 Cl1 1.00(3) 2.06(3) 3.032(2) 163(2) 1_565 N4 H4D Cl1 0.88(3) 2.43(3) 3.295(2) 167(3) . N5 H5D Cl1 0.89(3) 2.50(3) 3.294(2) 149(3) 1_565 N6 H6A N1 0.82(3) 2.14(4) 2.961(3) 176(3) 5_666 N6 H6B Cl1 0.97(3) 2.31(3) 3.116(2) 141(3) 5_666