#------------------------------------------------------------------------------ #$Date: 2014-10-25 18:23:10 +0100 (Sat, 25 Oct 2014) $ #$Revision: 125873 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/49/2104981.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2104981 loop_ _publ_author_name 'Mermer, Adrian' 'Starynowicz, Przemys\/law' _publ_section_title ; Charge-density distribution in hydrogen methylphosphonates of calcium and lithium ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 399 _journal_page_last 408 _journal_volume 67 _journal_year 2011 _chemical_formula_sum 'C H4 Li O3 P' _chemical_formula_weight 101.95 _chemical_name_common 'lithium hydrogen methylphosphonate' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_creation_date '15-Jul-07 T14:53:42-00:00' _audit_creation_method 'XD routine XDCIF' _cell_angle_alpha 90 _cell_angle_beta 96.12(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.267(5) _cell_length_b 4.604(2) _cell_length_c 9.384(3) _cell_measurement_reflns_used 20862 _cell_measurement_temperature 85(2) _cell_measurement_theta_max 75.7572 _cell_measurement_theta_min 4.9262 _cell_volume 398.1(3) _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_molecular_graphics 'Volkov et al, (2006)' _computing_publication_material 'Volkov et al, (2006)' _computing_structure_refinement 'Volkov et al, (2006)' _diffrn_ambient_temperature 85(2) _diffrn_detector_area_resol_mean 8.1956 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measurement_device_type 'Xcalibur, Onyx' _diffrn_measurement_method '\w and \p scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 30520 _diffrn_reflns_theta_full 54.82 _diffrn_reflns_theta_max 75.7572 _diffrn_reflns_theta_min 4.9262 _exptl_absorpt_coefficient_mu 0.530 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_correction_T_min 0.832 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 208 _exptl_crystal_size_max 0.4594 _exptl_crystal_size_mid 0.3363 _exptl_crystal_size_min 0.0557 _refine_diff_density_max 0.346 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.045 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.47 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 169 _refine_ls_number_reflns 4610 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.031 _refine_ls_R_factor_gt 0.015 _refine_ls_shift/su_max 0.03694 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; calc w1 = 1/[s^2^(Fo)] ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.015 _reflns_number_gt 6325 _reflns_number_total 8219 _reflns_threshold_expression >3sigma(I) _[local]_cod_data_source_file so5049.cif _[local]_cod_data_source_block mpli _cod_database_code 2104981 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z loop_ _atom_local_axes_atom_label _atom_local_axes_atom0 _atom_local_axes_ax1 _atom_local_axes_atom1 _atom_local_axes_atom2 _atom_local_axes_ax2 P O(2) Z P O(3) Y O(1) H(1) Z O(1) P Y O(3) P Z O(3) O(1) Y O(2) P Z O(2) LI Y C H(4) Z C H(2) Y LI O(2) Z LI P Y H(2) C Z H(2) H(4) Y H(3) C Z H(3) H(2) Y H(4) C Z H(4) H(2) Y H(1) O(1) Z H(1) P Y loop_ _atom_rho_multipole_atom_label _atom_rho_multipole_coeff_Pv _atom_rho_multipole_coeff_P00 _atom_rho_multipole_coeff_P11 _atom_rho_multipole_coeff_P1-1 _atom_rho_multipole_coeff_P10 _atom_rho_multipole_coeff_P20 _atom_rho_multipole_coeff_P21 _atom_rho_multipole_coeff_P2-1 _atom_rho_multipole_coeff_P22 _atom_rho_multipole_coeff_P2-2 _atom_rho_multipole_coeff_P30 _atom_rho_multipole_coeff_P31 _atom_rho_multipole_coeff_P3-1 _atom_rho_multipole_coeff_P32 _atom_rho_multipole_coeff_P3-2 _atom_rho_multipole_coeff_P33 _atom_rho_multipole_coeff_P3-3 _atom_rho_multipole_coeff_P40 _atom_rho_multipole_coeff_P41 _atom_rho_multipole_coeff_P4-1 _atom_rho_multipole_coeff_P42 _atom_rho_multipole_coeff_P4-2 _atom_rho_multipole_coeff_P43 _atom_rho_multipole_coeff_P4-3 _atom_rho_multipole_coeff_P44 _atom_rho_multipole_coeff_P4-4 _atom_rho_multipole_kappa _atom_rho_multipole_kappa_prime0 _atom_rho_multipole_kappa_prime1 _atom_rho_multipole_kappa_prime2 _atom_rho_multipole_kappa_prime3 _atom_rho_multipole_kappa_prime4 _atom_rho_multipole_radial_slater_n0 _atom_rho_multipole_radial_slater_zeta0 _atom_rho_multipole_radial_slater_n1 _atom_rho_multipole_radial_slater_zeta1 _atom_rho_multipole_radial_slater_n2 _atom_rho_multipole_radial_slater_zeta2 _atom_rho_multipole_radial_slater_n3 _atom_rho_multipole_radial_slater_zeta3 _atom_rho_multipole_radial_slater_n4 _atom_rho_multipole_radial_slater_zeta4 P 5.20(10) 0 0.07(2) 0.07(2) 0.11(2) 0.09(2) 0.036(17) -0.13(2) -0.090(17) -0.044(19) 0.55(3) -0.031(15) 0.034(16) 0.093(15) -0.018(16) -0.036(14) -0.41(2) 0 0 0 0 0 0 0 0 0 0.963(5) 0.765(10) 0.764773 0.764773 0.764773 0.764773 4 3.459 6 5.1885 6 5.1885 6 5.1885 6 5.1885 O(1) 6.21(4) 0 -0.012(8) -0.026(8) -0.034(8) -0.009(7) 0.018(8) 0.016(7) 0.036(7) 0.005(8) 0.059(8) 0.004(7) -0.048(7) 0.002(7) -0.016(7) -0.002(7) -0.005(7) 0 0 0 0 0 0 0 0 0 0.992(3) 1.01(6) 1.009537 1.009537 1.009537 1.009537 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 O(3) 6.32(3) 0 0.000(10) 0.025(10) -0.081(13) -0.041(10) 0.014(10) -0.019(9) 0.005(9) -0.001(9) 0.054(11) 0.013(11) 0.004(10) -0.032(10) -0.004(10) -0.003(9) 0.031(10) 0 0 0 0 0 0 0 0 0 0.9856(18) 0.73 0.73 0.73 0.73 0.73 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 O(2) 6.32(3) 0 -0.006(10) 0.010(10) -0.108(13) -0.027(10) 0.016(10) 0.012(10) -0.004(9) -0.001(8) 0.067(11) -0.029(11) 0.031(10) 0.030(10) 0.013(10) 0.010(10) -0.021(9) 0 0 0 0 0 0 0 0 0 0.9856(18) 0.73 0.73 0.73 0.73 0.73 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 C 4.48(10) 0 -0.003(18) -0.02(2) -0.01(2) -0.030(18) 0.019(14) 0.005(15) -0.008(16) 0.016(14) 0.28(3) -0.046(18) -0.041(19) -0.026(18) -0.029(16) -0.009(17) -0.29(3) 0 0 0 0 0 0 0 0 0 0.975(6) 0.84(3) 0.84209 0.84209 0.84209 0.84209 2 3.1762 2 3.1762 2 3.1762 3 3.1762 4 3.1762 LI 0.34(12) 0 0.20(7) 0.10(5) -0.03(6) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 2 1.2792 2 1.2792 2 1.2792 3 1.2792 4 1.2792 H(2) 0.83(3) 0 -0.029(15) -0.054(14) 0.15(2) 0.02(2) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.2 1.2 1.2 1.2 1.2 1.2 0 2 1 2 2 2 3 2 4 2 H(3) 0.75(3) 0 -0.070(13) -0.008(14) 0.109(18) 0.053(19) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.2 1.2 1.2 1.2 1.2 1.2 0 2 1 2 2 2 3 2 4 2 H(4) 0.89(3) 0 0.031(13) 0.031(15) 0.141(19) 0.10(2) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.2 1.2 1.2 1.2 1.2 1.2 0 2 1 2 2 2 3 2 4 2 H(1) 0.664(16) 0 -0.104(11) -0.182(11) 0.197(14) 0.12(2) -0.026(17) -0.105(15) 0.011(15) 0.019(14) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.2 1.2 1.2 1.2 1.2 1.2 0 2 1 2 2 2 3 2 4 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_occupancy _atom_site_symmetry_multiplicity _atom_site_adp_type P P 0.702565(6) 0.100820(11) 0.925332(5) 0.006 1 4 Uani O(1) O 0.75694(3) -0.11478(5) 1.05052(2) 0.011 1 4 Uani O(3) O 0.640403(19) 0.36966(3) 0.990615(18) 0.009 1 4 Uani O(2) O 0.596249(19) -0.05190(4) 0.817823(18) 0.009 1 4 Uani C C 0.86195(3) 0.20363(6) 0.84614(3) 0.014 1 4 Uani LI Li 0.50745(6) 0.10053(10) 0.64061(5) 0.011 1 4 Uani H(2) H 0.908304 0.016652 0.796195 0.04 1 4 Uani H(3) H 0.827395 0.364978 0.764563 0.036 1 4 Uani H(4) H 0.942114 0.282895 0.930629 0.037 1 4 Uani H(1) H 0.723309 -0.3097 1.010264 0.024 1 4 Uani 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 P 0.007178(17) 0.005580(16) 0.006224(16) 0.000142(12) -0.000020(11) 0.000047(11) O(1) 0.01440(7) 0.00730(5) 0.00980(6) 0.00160(5) -0.00388(5) -0.00054(5) O(3) 0.01101(5) 0.00643(4) 0.00896(5) -0.00068(4) 0.00099(4) 0.00075(4) O(2) 0.01048(5) 0.00781(4) 0.00739(4) 0.00004(4) -0.00151(4) -0.00103(4) C 0.00988(7) 0.01817(9) 0.01472(8) 0.00179(7) 0.00338(6) -0.00118(6) LI 0.01262(17) 0.01022(16) 0.00910(15) 0.00009(12) -0.00011(13) 0.00056(13) H(2) 0.034295 0.038506 0.05078 -0.01019 0.020632 0.005678 H(3) 0.031855 0.043255 0.034146 0.019282 0.006529 -0.000435 H(4) 0.022728 0.053814 0.033546 -0.002958 -0.00312 -0.012673 H(1) 0.033559 0.012588 0.024381 0.000199 -0.006757 -0.001819 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 ; E. Clementi and C. Roetti. Atomic Data and Nuclear Data Tables. 14 177-478 (1974) ; H H 0.0000 0.0000 ; E. Clementi and C. Roetti. Atomic Data and Nuclear Data Tables. 14 177-478 (1974) ; Li Li -0.0003 0.0001 ; E. Clementi and C. Roetti. Atomic Data and Nuclear Data Tables. 14 177-478 (1974) ; O O 0.0106 0.0060 ; E. Clementi and C. Roetti. Atomic Data and Nuclear Data Tables. 14 177-478 (1974) ; P P 0.1023 0.0942 ; E. Clementi and C. Roetti. Atomic Data and Nuclear Data Tables. 14 177-478 (1974) ; 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 O(1) P O(3) 108.443(11) 1_555 1_555 1_555 yes O(1) P O(2) 109.804(11) 1_555 1_555 1_555 yes O(1) P C 105.286(13) 1_555 1_555 1_555 yes O(3) P O(2) 113.615(10) 1_555 1_555 1_555 yes O(3) P C 108.499(12) 1_555 1_555 1_555 yes O(2) P C 110.831(12) 1_555 1_555 1_555 yes P O(1) H(1) 102.652 1_555 1_555 1_555 yes P C H(2) 110.535 1_555 1_555 1_555 yes P C H(3) 106.180 1_555 1_555 1_555 yes P C H(4) 108.401 1_555 1_555 1_555 yes H(2) C H(3) 109.64 1_555 1_555 1_555 yes H(2) C H(4) 107.93 1_555 1_555 1_555 yes H(3) C H(4) 114.15 1_555 1_555 1_555 yes 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 P O(1) 1.5789(2) 1_555 1_555 yes P O(3) 1.52131(17) 1_555 1_555 yes P O(2) 1.50695(17) 1_555 1_555 yes P C 1.7866(2) 1_555 1_555 yes O(1) H(1) 1.0100 1_555 1_555 yes C H(2) 1.0900 1_555 1_555 yes C H(3) 1.0900 1_555 1_555 yes C H(4) 1.0900 1_555 1_555 yes 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(3) P O(1) H(1) 138.129 1_555 1_555 1_555 1_555 yes O(2) P O(1) H(1) 13.455 1_555 1_555 1_555 1_555 yes O(1) P C H(2) 65.25 1_555 1_555 1_555 1_555 yes O(1) P C H(3) -175.91 1_555 1_555 1_555 1_555 yes O(1) P C H(4) -52.860 1_555 1_555 1_555 1_555 yes C P O(1) H(1) -105.902 1_555 1_555 1_555 1_555 yes O(3) P C H(2) -178.82 1_555 1_555 1_555 1_555 yes O(3) P C H(3) -59.983 1_555 1_555 1_555 1_555 yes O(3) P C H(4) 63.071 1_555 1_555 1_555 1_555 yes O(2) P C H(2) -53.421 1_555 1_555 1_555 1_555 yes O(2) P C H(3) 65.416 1_555 1_555 1_555 1_555 yes O(2) P C H(4) -171.53 1_555 1_555 1_555 1_555 yes _cod_database_fobs_code 2104981 _journal_paper_doi 10.1107/S0108768111030515