#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003443.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_2003443 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 933 _journal_page_last 935 _publ_section_title ; p-Anisidinium Dihydrog\'enophosphate ; _chemical_formula_moiety 'C7 H12 N1 O5 P1' _chemical_formula_sum 'C7 H12 N1 O5 P1' _chemical_formula_structural '(1-4,CH~3~O-C~6~H~4~-NH~3~)H~2~PO~4~' _chemical_formula_weight 221.15 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _[local]_cod_cif_authors_sg_H-M 'P 21/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 9.3781(5) _cell_length_b 8.2216(6) _cell_length_c 13.5971(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.903(4) _cell_angle_gamma 90.00 _cell_volume 1013.11(10) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14 _cell_measurement_theta_max 16 _exptl_absorpt_coefficient_mu 0.269 _cell_measurement_temperature 293(2) _exptl_crystal_description prisme _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_colour incolore _chemical_compound_source ? _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 1852 _reflns_number_total 1774 _reflns_number_observed 1603 _reflns_observed_criterion 'I>2\s(I)' _diffrn_reflns_av_R_equivalents 0.0110 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1.6 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0394 _refine_ls_wR_factor_obs 0.1033 _refine_ls_wR_factor_all 0.1060 _refine_ls_goodness_of_fit_obs 1.164 _refine_ls_goodness_of_fit_all 1.130 _refine_ls_number_reflns 1774 _refine_ls_number_parameters 176 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme 'calc w=1/[\s^2^(F~o~^2^)+(0.0591P)^2^+0.3749P]' _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.351 _refine_diff_density_min -0.360 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1994)' _refine_ls_extinction_coef 0.0525(45) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'P' 'P' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1023 0.094 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv P 1 0.41440(5) 0.22869(6) 0.42869(4) 0.0292(2) O1 1 0.4796(2) 0.1971(2) 0.5408(1) 0.0349(4) O2 1 0.2678(1) 0.3132(2) 0.4043(1) 0.0413(4) O3 1 0.3975(2) 0.0647(2) 0.3692(1) 0.0494(5) O4 1 0.5194(2) 0.3386(2) 0.3851(1) 0.0431(4) O5 1 0.4281(2) 0.2623(3) 1.0530(1) 0.0686(6) N 1 0.2457(2) 0.1396(2) 0.6355(1) 0.0344(4) C1 1 0.2913(2) 0.1703(3) 0.7452(1) 0.0332(5) C2 1 0.2561(3) 0.0614(3) 0.8105(2) 0.0540(7) C3 1 0.2998(4) 0.0878(3) 0.9148(2) 0.0585(7) C4 1 0.3787(3) 0.2243(3) 0.9520(2) 0.0472(6) C5 1 0.4129(3) 0.3345(4) 0.8848(2) 0.0636(8) C6 1 0.3692(3) 0.3076(3) 0.7815(2) 0.0550(7) C7 1 0.3873(6) 0.1583(5) 1.1245(2) 0.0817(11) HO3 1 0.438(3) -0.010(4) 0.400(2) 0.067(9) HO4 1 0.588(4) 0.300(4) 0.386(3) 0.074(11) H1N 1 0.232(2) 0.027(3) 0.622(2) 0.045(6) H2N 1 0.311(3) 0.175(3) 0.606(2) 0.046(7) H3N 1 0.161(3) 0.189(3) 0.605(2) 0.040(6) HC2 1 0.207(3) -0.029(4) 0.788(2) 0.071(9) HC3 1 0.277(3) 0.013(4) 0.956(2) 0.072(9) HC5 1 0.469(4) 0.429(4) 0.912(2) 0.085(10) HC6 1 0.393(3) 0.379(4) 0.734(2) 0.076(9) H1C7 1 0.407(4) 0.049(5) 1.119(2) 0.082(11) H2C7 1 0.435(3) 0.202(4) 1.187(3) 0.082(10) H3C7 1 0.274(4) 0.170(4) 1.114(2) 0.091(12) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 P 0.0257(3) 0.0020(2) 0.0064(2) 0.0290(3) 0.0047(2) 0.0323(3) O1 0.0389(8) 0.0013(6) 0.0070(6) 0.0317(7) 0.0012(6) 0.0328(8) O2 0.0260(7) 0.0035(6) 0.0102(6) 0.0399(8) 0.0095(7) 0.0577(10) O3 0.0681(11) 0.0078(8) -0.0046(7) 0.0353(9) -0.0003(7) 0.0349(8) O4 0.0319(8) 0.0066(7) 0.0175(7) 0.0453(9) 0.0176(7) 0.0555(10) O5 0.0915(15) -0.0038(11) 0.0071(9) 0.0755(13) -0.0116(9) 0.0338(9) N 0.0332(10) -0.0003(8) 0.0079(8) 0.0365(10) -0.0009(8) 0.0330(9) C1 0.032(1) 0.0010(8) 0.0063(8) 0.036(1) -0.0023(8) 0.031(1) C2 0.075(2) -0.022(1) 0.013(1) 0.047(1) -0.003(1) 0.039(1) C3 0.088(2) -0.012(1) 0.021(1) 0.051(1) 0.003(1) 0.038(1) C4 0.0536(1) 0.004(1) 0.007(1) 0.053(1) -0.007(1) 0.033(1) C5 0.082(2) -0.030(2) 0.011(1) 0.060(2) -0.015(1) 0.046(1) C6 0.076(2) -0.022(1) 0.016(1) 0.048(1) -0.002(1) 0.042(1) C7 0.126(3) 0.020(2) 0.022(2) 0.083(2) -0.001(2) 0.037(1)