# cm990578b.cif data_CRYSTALS_cif _audit_creation_date 99-08-28 _audit_creation_method CRYSTALS [NH3CH2CH2NH3][Ga(H2PO4)(P2O7)] #**************************************************************************** # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission to accompany manuscript number CM990578B ; _publ_contact_author_name 'Ann M. Chippindale' _publ_contact_author_address ; Chemical Crystallography Laboratory 9 Parks Road OXFORD OX1 3PD ; _publ_contact_author_phone ' 01865 270 824 ' _publ_contact_author_fax ' 01865 272 699 ' _publ_contact_author_email 'ann.chippindale@chem.ox.ac.uk ' #========================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Amine-templated Unidimensional Phosphate-Pyrophosphates of Gallium and Vanadium, [NH3CH2CH2NH3][M(H2PO4)(P2O7)] ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Chippindale, Ann M.' ; to whom correspondence should be addressed ; ; Chemical Crystallography Laboratory 9 Parks Road Oxford OX1 3PD ; #============================================================================== # 4. TEXT _publ_section_exptl_refinement ; H atoms of organic amine placed geometrically after each cycle. H atoms of inorganic framework located in difference Fourier maps ; ## -----------------REFERENCES ----------------------## _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699. Larsen, A. C. (1967), Acta Cryst. 23, 440-449. North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), Acta Cryst, A24, 351-359. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-Nonius CAD4 ' _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction ; RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994) ; _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; Cameron ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic ; ethyldiammonium gallium dihydrogen phosphate diphosphate ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary Direct_Methods _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment ; mixed ; #**************************************************************************** _cell_length_a 8.6139(4) _cell_angle_alpha 90 _cell_length_b 14.929(1) _cell_angle_beta 106.541(4) _cell_length_c 9.3109(4) _cell_angle_gamma 90 _cell_volume 1147.82 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,y+1/2,z' 'x,-y,z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Ga ' -1.3540 0.7770 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135 1.7189 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.2830 0.4340 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0470 0.0320 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0170 0.0090 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0290 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C2 H12 Ga1 P3 O11 N2 ' _chemical_formula_moiety ' C2 H12 Ga1 P3 O11 N2 ' _chemical_compound_source ; solvothermal synthesis ; _chemical_formula_weight 402.76 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16 _cell_measurement_theta_max 34 _cell_measurement_temperature 293 _cell_formula_units_Z 4.00 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' clear ' _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.16 _exptl_crystal_density_diffrn 2.33 _exptl_crystal_density_meas ? _exptl_crystal_F_000 808.23 _exptl_absorpt_coefficient_mu 7.96 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_process_details '\y scan' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 3 _diffrn_standards_decay_% 7.82 _diffrn_ambient_temperature 293 _diffrn_reflns_number 2861 _reflns_number_total 2116 _diffrn_reflns_av_R_equivalents 0.03 _reflns_number_observed 2049 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 70.00 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -11 _reflns_limit_l_max 11 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -2.10 _refine_diff_density_max 1.63 _refine_ls_number_reflns 2049 _refine_ls_number_parameters 179 _refine_ls_R_factor_obs 0.0439 _refine_ls_wR_factor_obs 0.0503 _refine_ls_goodness_of_fit_obs 1.1104 _refine_ls_shift/esd_max 0.021976 _refine_ls_abs_structure_details ' from Flack enantiopole 0.000' _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method 2\q/\w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type GA1 0.1832(1) 0.49051(4) 0.3041(1) 0.0103 1.0000 Uani P1 0.4448(2) 0.43635(9) 0.6265(2) 0.0107 1.0000 Uani P2 -0.0700(2) 0.53315(9) -0.0130(2) 0.0126 1.0000 Uani P3 0.0909(2) 0.36694(8) 0.0198(2) 0.0108 1.0000 Uani O1 0.3310(4) 0.4218(2) 0.4733(4) 0.0147 1.0000 Uani O2 0.3754(4) 0.5259(3) 0.2447(4) 0.0148 1.0000 Uani O3 -0.4121(5) 0.5026(3) 0.1198(5) 0.0192 1.0000 Uani O4 0.5173(5) 0.3417(3) 0.6851(5) 0.0223 1.0000 Uani O5 0.0425(5) 0.5570(3) 0.1403(4) 0.0166 1.0000 Uani O6 -0.0009(5) 0.4359(2) 0.3637(4) 0.0138 1.0000 Uani O7 -0.2413(5) 0.5632(3) -0.0358(4) 0.0190 1.0000 Uani O8 -0.0737(4) 0.4251(3) -0.0192(5) 0.0183 1.0000 Uani O9 0.1751(4) 0.3780(2) 0.1888(4) 0.0119 1.0000 Uani O10 0.1959(5) 0.5969(2) 0.4285(4) 0.0138 1.0000 Uani O11 0.0362(5) 0.2714(2) -0.0167(4) 0.0148 1.0000 Uani N1 -0.4793(6) 0.3390(4) 0.2491(6) 0.0232 1.0000 Uani N2 0.1820(7) 0.7474(4) -0.0547(6) 0.0242 1.0000 Uani C1 -0.4871(8) 0.2974(5) 0.1003(8) 0.0320 1.0000 Uani C2 -0.3173(8) 0.2765(5) 0.1006(7) 0.0330 1.0000 Uani H3 -0.34(1) 0.532(6) 0.07(1) 0.0500 1.0000 Uiso H4 -0.47(1) 0.703(5) 0.111(8) 0.0500 1.0000 Uiso H111 -0.5914 0.3538 0.2527 0.0258 1.0000 Uiso H112 -0.4130 0.3949 0.2623 0.0258 1.0000 Uiso H113 -0.4286 0.2958 0.3312 0.0258 1.0000 Uiso H121 0.2951 0.7332 -0.0559 0.0286 1.0000 Uiso H122 0.1378 0.7968 -0.1273 0.0286 1.0000 Uiso H123 0.1126 0.6929 -0.0839 0.0286 1.0000 Uiso H11 -0.5372 0.3402 0.0175 0.0259 1.0000 Uiso H12 -0.5528 0.2411 0.0863 0.0259 1.0000 Uiso H21 -0.2482 0.3310 0.1300 0.0288 1.0000 Uiso H22 -0.2733 0.2271 0.1735 0.0288 1.0000 Uiso 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 GA1 0.0154(3) 0.0080(3) 0.0113(3) -0.0007(3) 0.0070(2) 0.0003(3) P1 0.0147(6) 0.0094(6) 0.0112(6) -0.0010(5) 0.0063(4) 0.0013(5) P2 0.0142(6) 0.0125(6) 0.0141(7) 0.0017(5) 0.0072(5) 0.0013(5) P3 0.0165(6) 0.0068(6) 0.0124(6) -0.0004(5) 0.0057(4) -0.0011(4) O1 0.023(2) 0.011(2) 0.014(2) -0.002(1) 0.006(1) 0.001(1) O2 0.020(2) 0.016(2) 0.016(2) 0.003(2) 0.010(1) -0.003(1) O3 0.021(2) 0.030(2) 0.028(2) 0.013(2) 0.018(2) 0.009(2) O4 0.036(2) 0.017(2) 0.021(2) 0.002(2) 0.007(2) 0.010(2) O5 0.025(2) 0.011(2) 0.019(2) -0.003(1) 0.005(2) 0.003(1) O6 0.022(2) 0.013(2) 0.018(2) -0.006(2) 0.013(1) -0.004(1) O7 0.019(2) 0.029(2) 0.021(2) 0.008(2) 0.012(2) 0.006(2) O8 0.014(2) 0.018(2) 0.026(2) 0.004(2) 0.006(2) 0.001(2) O9 0.022(2) 0.010(2) 0.011(2) -0.004(1) 0.007(1) 0.000(1) O10 0.022(2) 0.012(2) 0.018(2) -0.006(1) 0.011(1) -0.000(1) O11 0.040(2) 0.005(2) 0.020(2) 0.001(1) 0.013(2) -0.003(2) N1 0.037(3) 0.020(2) 0.023(3) 0.001(2) 0.017(2) 0.003(2) N2 0.050(3) 0.027(3) 0.017(2) 0.003(2) 0.016(2) 0.017(2) C1 0.033(3) 0.032(3) 0.033(4) -0.010(3) 0.006(3) 0.000(3) C2 0.036(3) 0.040(4) 0.027(3) 0.004(3) 0.011(3) 0.007(3) _refine_ls_extinction_coef 13.1(15) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag GA1 . O1 . 2.003(4) yes GA1 . O2 . 1.961(4) yes GA1 . O5 . 1.931(4) yes GA1 . O6 . 1.998(4) yes GA1 . O9 . 1.984(4) yes GA1 . O10 . 1.951(4) yes P1 . O1 . 1.498(4) yes P1 . O2 3_565 1.504(4) yes P1 . O3 3_665 1.549(4) yes P1 . O4 . 1.579(4) yes P2 . O5 . 1.522(4) yes P2 . O6 3_564 1.508(4) yes P2 . O7 . 1.498(4) yes P2 . O8 . 1.615(4) yes P3 . O8 . 1.613(4) yes P3 . O9 . 1.542(4) yes P3 . O10 3_564 1.506(4) yes P3 . O11 . 1.510(4) yes O3 . H3 . 1.00(1) no O4 . H4 3_665 1.00(1) no N1 . C1 . 1.502(8) yes N1 . H111 . 1.000(5) no N1 . H112 . 1.000(5) no N1 . H113 . 1.000(5) no N2 . C2 2_555 1.507(9) yes N2 . H121 . 1.000(6) no N2 . H122 . 1.000(5) no N2 . H123 . 1.000(6) no C1 . C2 . 1.50(1) yes C1 . H11 . 1.000(7) no C1 . H12 . 1.000(7) no C2 . H21 . 1.000(8) no C2 . H22 . 1.000(7) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . GA1 . O2 . 87.8(2) no O1 . GA1 . O5 . 179.4(2) no O2 . GA1 . O5 . 91.7(2) no O1 . GA1 . O6 . 87.1(2) no O2 . GA1 . O6 . 171.5(2) no O5 . GA1 . O6 . 93.4(2) no O1 . GA1 . O9 . 84.8(1) no O2 . GA1 . O9 . 88.7(2) no O5 . GA1 . O9 . 95.2(2) no O6 . GA1 . O9 . 84.0(1) no O1 . GA1 . O10 . 92.0(2) no O2 . GA1 . O10 . 92.2(2) no O5 . GA1 . O10 . 88.1(2) no O6 . GA1 . O10 . 94.7(2) no O9 . GA1 . O10 . 176.6(2) no O1 . P1 . O2 3_565 117.5(2) no O1 . P1 . O3 3_665 111.1(2) no O2 3_565 P1 . O3 3_665 107.2(2) no O1 . P1 . O4 . 106.6(2) no O2 3_565 P1 . O4 . 106.4(2) no O3 3_665 P1 . O4 . 107.5(2) no O5 . P2 . O6 3_564 111.0(2) no O5 . P2 . O7 . 113.7(2) no O6 3_564 P2 . O7 . 112.7(2) no O5 . P2 . O8 . 105.6(2) no O6 3_564 P2 . O8 . 106.7(2) no O7 . P2 . O8 . 106.6(2) no O8 . P3 . O9 . 107.5(2) no O8 . P3 . O10 3_564 108.1(2) no O9 . P3 . O10 3_564 110.7(2) no O8 . P3 . O11 . 105.0(2) no O9 . P3 . O11 . 110.9(2) no O10 3_564 P3 . O11 . 114.2(2) no GA1 . O1 . P1 . 140.5(2) no GA1 . O2 . P1 3_564 148.3(3) no P1 3_464 O3 . H3 . 112.6(56) no P1 . O4 . H4 3_665 118.6(55) no GA1 . O5 . P2 . 135.2(3) no GA1 . O6 . P2 3_565 127.0(2) no P2 . O8 . P3 . 121.5(2) no GA1 . O9 . P3 . 125.2(2) no GA1 . O10 . P3 3_565 133.3(2) no C1 . N1 . H111 . 109.5(5) no C1 . N1 . H112 . 109.5(5) no H111 . N1 . H112 . 109.5(5) no C1 . N1 . H113 . 109.5(5) no H111 . N1 . H113 . 109.4(5) no H112 . N1 . H113 . 109.5(5) no C2 2_555 N2 . H121 . 109.5(5) no C2 2_555 N2 . H122 . 109.5(5) no H121 . N2 . H122 . 109.5(5) no C2 2_555 N2 . H123 . 109.5(5) no H121 . N2 . H123 . 109.4(5) no H122 . N2 . H123 . 109.5(5) no N1 . C1 . C2 . 107.3(5) no N1 . C1 . H11 . 110.0(6) no C2 . C1 . H11 . 110.0(6) no N1 . C1 . H12 . 110.0(6) no C2 . C1 . H12 . 110.0(6) no H11 . C1 . H12 . 109.5(6) no N2 2_445 C2 . C1 . 108.7(6) no N2 2_445 C2 . H21 . 109.7(6) no C1 . C2 . H21 . 109.7(6) no N2 2_445 C2 . H22 . 109.7(6) no C1 . C2 . H22 . 109.7(6) no H21 . C2 . H22 . 109.5(6) no #===END