#------------------------------------------------------------------------------ #$Date: 2017-08-02 05:23:24 +0300 (Wed, 02 Aug 2017) $ #$Revision: 199448 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/88/7228825.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_7228825 loop_ _publ_author_name 'Bhat, Gulzar A.' 'Kalita, Alok Ch' 'Murugavel, Ramaswamy' _publ_section_title ; Intriguing Structural Chemistry of Neutral and Anionic Layered Monoalkylphosphates: Single-Source Precursors for High-Yield Ceramic Phosphates ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C7CE01066D _journal_year 2017 _chemical_formula_moiety 'C3 H9 O4 P' _chemical_formula_sum 'C3 H9 O4 P' _chemical_formula_weight 140.07 _space_group_crystal_system tetragonal _space_group_IT_number 86 _space_group_name_Hall '-P 4bc' _space_group_name_H-M_alt 'P 42/n' _symmetry_space_group_name_Hall '-P 4bc' _symmetry_space_group_name_H-M 'P 42/n :2' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-03-06 deposited with the CCDC. 2017-08-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.6655(2) _cell_length_b 14.6655(2) _cell_length_c 5.88520(10) _cell_measurement_reflns_used 2077 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 25.00 _cell_measurement_theta_min 2.80 _cell_volume 1265.77(3) _computing_cell_refinement 'CrysAlisPro 1.171.38.41' _computing_data_collection 'CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'Diamond 3.2' _computing_publication_material 'WinGX v2014. 1' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution Sir92 _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_unetI/netI 0.0136 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 9065 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.972 _diffrn_reflns_theta_max 24.972 _diffrn_reflns_theta_min 2.778 _exptl_absorpt_coefficient_mu 0.367 _exptl_absorpt_correction_T_max 0.937 _exptl_absorpt_correction_T_min 0.890 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.470 _exptl_crystal_description block _exptl_crystal_F_000 592 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.363 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.053 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 73 _refine_ls_number_reflns 1110 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0305 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.7472P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.0896 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1076 _reflns_number_total 1110 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce01066d2.cif _cod_data_source_block 7 _cod_original_cell_volume 1265.77(4) _cod_database_code 7228825 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.927 _shelx_estimated_absorpt_t_max 0.971 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL SIR92 run in space group P 42/n CELL 0.71073 14.6655 14.6655 5.8852 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0002 0.0001 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, 1/2 - Y, Z SYMM - Y, 1/2 + X, 1/2 + Z SYMM 1/2 + Y, - X, 1/2 + Z SFAC C H O P UNIT 24 72 32 8 MERG 2 OMIT -3.00 50.00 OMIT 1 1 0 EQIV $1 y, -x+1/2, -z+3/2 HTAB O4 O2_$1 EQIV $2 y, -x+1/2, -z+5/2 HTAB O3 O2_$2 HTAB O4 O2_$1 HTAB O3 O2_$2 FMAP 2 PLAN 25 size 0.08 0.15 0.21 ACTA BOND $H CONF L.S. 10 TEMP -123 WGHT 0.052500 0.747200 FVAR 5.87726 P1 4 0.196563 0.085858 0.974935 11.00000 0.01781 0.01817 = 0.01560 -0.00012 -0.00048 0.00095 O1 3 0.197275 -0.013732 1.066746 11.00000 0.01568 0.02057 = 0.02493 0.00344 -0.00162 -0.00020 O4 3 0.176900 0.076938 0.718034 11.00000 0.02838 0.02098 = 0.01806 -0.00097 -0.00151 0.00198 AFIX 83 H4 2 0.177239 0.128912 0.658058 11.00000 -1.50000 AFIX 0 O3 3 0.113832 0.137883 1.074083 11.00000 0.02325 0.02673 = 0.01893 -0.00345 -0.00234 0.00580 AFIX 83 H3 2 0.117956 0.139491 1.216387 11.00000 -1.50000 AFIX 0 O2 3 0.286429 0.128162 1.030808 11.00000 0.02322 0.02510 = 0.01831 0.00116 -0.00070 -0.00483 C1 1 0.114179 -0.070534 1.055793 11.00000 0.01667 0.02112 = 0.02784 0.00092 -0.00327 -0.00131 AFIX 13 H1 2 0.067598 -0.039641 0.958470 11.00000 -1.20000 AFIX 0 C3 1 0.140772 -0.159583 0.949396 11.00000 0.03684 0.02584 = 0.04936 -0.00970 -0.00387 0.00061 AFIX 33 H3A 2 0.087137 -0.199233 0.939265 11.00000 -1.50000 H3B 2 0.165007 -0.148543 0.796673 11.00000 -1.50000 H3C 2 0.187547 -0.189156 1.042734 11.00000 -1.50000 AFIX 0 C2 1 0.077916 -0.079997 1.293278 11.00000 0.02839 0.04972 = 0.03239 0.00374 0.00552 -0.01055 AFIX 33 H2A 2 0.022601 -0.117480 1.291198 11.00000 -1.50000 H2B 2 0.124017 -0.109181 1.389415 11.00000 -1.50000 H2C 2 0.063466 -0.019507 1.354189 11.00000 -1.50000 AFIX 0 HKLF 4 REM SIR92 run in space group P 42/n REM R1 = 0.0305 for 1076 Fo > 4sig(Fo) and 0.0312 for all 1110 data REM 73 parameters refined using 0 restraints END WGHT 0.0508 0.8140 REM Highest difference peak 0.363, deepest hole -0.403, 1-sigma level 0.053 Q1 1 0.2559 0.1063 0.9998 11.00000 0.05 0.36 Q2 1 0.1810 0.0835 0.8224 11.00000 0.05 0.31 Q3 1 0.1979 0.0298 1.0269 11.00000 0.05 0.30 Q4 1 0.1268 0.1794 1.1961 11.00000 0.05 0.30 Q5 1 0.0978 -0.0752 1.1724 11.00000 0.05 0.23 Q6 1 0.1256 -0.1204 0.9932 11.00000 0.05 0.23 Q7 1 0.1613 -0.0396 1.0566 11.00000 0.05 0.21 Q8 1 0.1399 0.0945 1.0681 11.00000 0.05 0.20 Q9 1 0.1572 0.1470 1.0109 11.00000 0.05 0.19 Q10 1 0.1443 0.1226 0.6558 11.00000 0.05 0.18 Q11 1 0.1923 0.0618 0.6862 11.00000 0.05 0.14 Q12 1 0.1003 -0.0760 1.4053 11.00000 0.05 0.13 Q13 1 0.0650 0.1257 1.0374 11.00000 0.05 0.12 Q14 1 0.0897 -0.1799 0.8397 11.00000 0.05 0.12 Q15 1 0.0891 -0.0410 0.9623 11.00000 0.05 0.11 Q16 1 0.1202 -0.1374 1.3415 11.00000 0.05 0.11 Q17 1 0.2210 -0.0001 1.2186 11.00000 0.05 0.11 Q18 1 0.1664 -0.1969 1.0664 11.00000 0.05 0.09 Q19 1 0.0749 -0.2113 1.0545 11.00000 0.05 0.08 Q20 1 0.1983 -0.1799 0.9407 11.00000 0.05 0.08 Q21 1 0.1646 -0.1522 0.8686 11.00000 0.05 0.08 Q22 1 0.1831 0.0640 0.5061 11.00000 0.05 0.06 Q23 1 0.0597 -0.0112 1.0256 11.00000 0.05 0.06 Q24 1 0.0447 0.0205 1.2261 11.00000 0.05 0.06 Q25 1 0.2462 -0.1192 0.9344 11.00000 0.05 0.06 ; _shelx_res_checksum 6606 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp P1 P 0.19656(3) 0.08586(3) 0.97494(7) 0.01719(19) Uani 1 1 d . . O1 O 0.19728(7) -0.01373(8) 1.0667(2) 0.0204(3) Uani 1 1 d . . O4 O 0.17690(8) 0.07694(8) 0.7180(2) 0.0225(3) Uani 1 1 d . . H4 H 0.1772 0.1289 0.6581 0.034 Uiso 1 1 calc R U O3 O 0.11383(8) 0.13788(8) 1.0741(2) 0.0230(3) Uani 1 1 d . . H3 H 0.1180 0.1395 1.2164 0.034 Uiso 1 1 calc R U O2 O 0.28643(8) 0.12816(8) 1.03081(19) 0.0222(3) Uani 1 1 d . . C1 C 0.11418(11) -0.07053(11) 1.0558(3) 0.0219(4) Uani 1 1 d . . H1 H 0.0676 -0.0396 0.9585 0.026 Uiso 1 1 calc R U C3 C 0.14077(14) -0.15958(14) 0.9494(4) 0.0373(5) Uani 1 1 d . . H3A H 0.0871 -0.1992 0.9393 0.056 Uiso 1 1 calc R U H3B H 0.1650 -0.1485 0.7967 0.056 Uiso 1 1 calc R U H3C H 0.1875 -0.1892 1.0427 0.056 Uiso 1 1 calc R U C2 C 0.07792(13) -0.08000(15) 1.2933(4) 0.0368(5) Uani 1 1 d . . H2A H 0.0226 -0.1175 1.2912 0.055 Uiso 1 1 calc R U H2B H 0.1240 -0.1092 1.3894 0.055 Uiso 1 1 calc R U H2C H 0.0635 -0.0195 1.3542 0.055 Uiso 1 1 calc R U 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 P1 0.0178(3) 0.0182(3) 0.0156(3) -0.00012(15) -0.00048(15) 0.00095(14) O1 0.0157(6) 0.0206(6) 0.0249(6) 0.0034(5) -0.0016(5) -0.0002(4) O4 0.0284(6) 0.0210(6) 0.0181(7) -0.0010(5) -0.0015(5) 0.0020(5) O3 0.0233(6) 0.0267(6) 0.0189(6) -0.0034(5) -0.0023(5) 0.0058(5) O2 0.0232(6) 0.0251(6) 0.0183(6) 0.0012(5) -0.0007(5) -0.0048(5) C1 0.0167(8) 0.0211(8) 0.0278(10) 0.0009(7) -0.0033(7) -0.0013(6) C3 0.0368(11) 0.0258(10) 0.0494(13) -0.0097(9) -0.0039(9) 0.0006(8) C2 0.0284(10) 0.0497(12) 0.0324(11) 0.0037(9) 0.0055(8) -0.0106(8) 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' P P 0.1023 0.0942 '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 O2 P1 O4 114.55(7) O2 P1 O3 113.83(7) O4 P1 O3 105.33(7) O2 P1 O1 107.90(7) O4 P1 O1 105.15(6) O3 P1 O1 109.68(7) C1 O1 P1 120.54(10) P1 O4 H4 109.5 P1 O3 H3 109.5 O1 C1 C3 107.14(14) O1 C1 C2 107.67(14) C3 C1 C2 113.59(16) O1 C1 H1 109.5 C3 C1 H1 109.5 C2 C1 H1 109.5 C1 C3 H3A 109.5 C1 C3 H3B 109.5 H3A C3 H3B 109.5 C1 C3 H3C 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 C1 C2 H2A 109.5 C1 C2 H2B 109.5 H2A C2 H2B 109.5 C1 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 P1 O2 1.4933(12) P1 O4 1.5447(13) P1 O3 1.5475(12) P1 O1 1.5573(12) O1 C1 1.478(2) O4 H4 0.8400 O3 H3 0.8400 C1 C3 1.500(3) C1 C2 1.502(3) C1 H1 1.0000 C3 H3A 0.9800 C3 H3B 0.9800 C3 H3C 0.9800 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 O4 H4 O2 0.84 1.82 2.5828(16) 151.1 7_567 O3 H3 O2 0.84 1.85 2.5852(16) 145.6 7_568 O4 H4 O2 0.84 1.82 2.5828(16) 151.1 7_567 O3 H3 O2 0.84 1.85 2.5852(16) 145.6 7_568 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion O2 P1 O1 C1 174.32(11) O4 P1 O1 C1 -63.01(12) O3 P1 O1 C1 49.81(13) P1 O1 C1 C3 129.52(14) P1 O1 C1 C2 -107.95(15)