# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1477 data_[NbOPO4]4 _publ_contact_author ; Allan J. Jacobson Department of Chemistry University of Houston Houston, TX 77204-5641 phone: 713-7432785 E-mail:ajjacob@uh.edu ; _publ_requested_journal 'JCS Chemical Communications' _publ_section_title ; The synthesis and single crystal structure of an amino acid intercalated layered niobium phosphate:[NbOPO4]4.(H3NCH2COOH)2(H2PO4)(OH,F) ; _publ_author_name ; Xiqu Wang, Lumei Liu, Heidi Cheng and Allan J. Jacobson ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[NbOPO4]4.(H3NCH2COOH)2(H2PO4)(OH,F)' _chemical_formula_analytical ? _chemical_formula_sum 'C4 N2 H14.6 O28.6 F0.4 Nb4 P5' _chemical_formula_weight 1082.3 _chemical_melting_point ? _chemical_compound_source 'hydrothermal synthesis' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'C2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 17.020(2) _cell_length_b 6.4973(7) _cell_length_c 6.4992(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.304(2) _cell_angle_gamma 90.00 _cell_volume 678.30(12) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.650 _exptl_crystal_density_method ? _exptl_crystal_F_000 475 _exptl_absorpt_coefficient_mu 1.988 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2117 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 28.34 _reflns_number_total 850 _reflns_number_observed 814 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+7.1436P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ignored _refine_ls_hydrogen_treatment ignored _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0032(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 850 _refine_ls_number_parameters 74 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_obs 0.0345 _refine_ls_wR_factor_all 0.0892 _refine_ls_wR_factor_obs 0.0883 _refine_ls_goodness_of_fit_all 1.173 _refine_ls_goodness_of_fit_obs 1.189 _refine_ls_restrained_S_all 1.172 _refine_ls_restrained_S_obs 1.188 _refine_ls_shift/esd_max 0.008 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nb Nb 0.20870(3) 0.0000 0.21561(8) 0.0093(2) Uani 1 d S . P P 0.24991(9) 0.0000 -0.2504(2) 0.0114(3) Uani 1 d S . O1 O 0.3151(3) 0.0000 0.3090(8) 0.0223(10) Uani 1 d S . O2 O 0.1929(2) 0.3099(5) 0.2025(5) 0.0166(6) Uani 1 d . . O3 O 0.1921(3) 0.0000 -0.4887(7) 0.0163(9) Uani 1 d S . O4 O 0.1942(3) 0.0000 -0.1069(7) 0.0175(9) Uani 1 d S . O5 O 0.0706(3) 0.0000 0.0920(8) 0.0248(10) Uani 1 d S . C1 C -0.0040(9) 0.0826(25) 0.0805(25) 0.013(3) Uiso 0.25 d PD -1 C2 C -0.0230(24) 0.2433(49) 0.2201(56) 0.076(11) Uiso 0.25 d PD -1 N N 0.0179(30) 0.3904(75) 0.3982(74) 0.156(24) Uiso 0.25 d PD -1 P2 P 0.0094(25) 0.4427(51) -0.0535(59) 0.085(14) Uiso 0.06 d PG -2 O21 O -0.0217(47) 0.3274(122) 0.1136(112) 0.077(10) Uiso 0.06 d PG -2 O22 O 0.0019(58) 0.6744(56) -0.0226(135) 0.077(10) Uiso 0.06 d PG -2 O23 O 0.1027(26) 0.3786(123) 0.0015(124) 0.077(10) Uiso 0.06 d PG -2 O24 O -0.0408(42) 0.3752(118) -0.2808(77) 0.077(10) Uiso 0.06 d PG -2 P3 P -0.0120(33) -0.1700(75) 0.4701(80) 0.230(46) Uiso 0.06 d PG -3 O31 O 0.0335(54) -0.1702(119) 0.7196(81) 0.077(10) Uiso 0.06 d PG -3 O32 O -0.0127(46) 0.0497(83) 0.3848(108) 0.077(10) Uiso 0.06 d PG -3 O33 O 0.0402(50) -0.3153(114) 0.3730(136) 0.077(10) Uiso 0.06 d PG -3 O34 O -0.0988(38) -0.2531(121) 0.4223(142) 0.077(10) Uiso 0.06 d PG -3 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 Nb 0.0149(3) 0.0073(3) 0.0066(3) 0.000 0.0046(2) 0.000 P 0.0221(8) 0.0066(6) 0.0067(6) 0.000 0.0063(5) 0.000 O1 0.019(2) 0.024(2) 0.023(2) 0.000 0.005(2) 0.000 O2 0.026(2) 0.0079(13) 0.0169(14) -0.0004(11) 0.0080(12) -0.0010(11) O3 0.028(2) 0.017(2) 0.006(2) 0.000 0.007(2) 0.000 O4 0.026(2) 0.018(2) 0.011(2) 0.000 0.009(2) 0.000 O5 0.024(2) 0.027(3) 0.022(2) 0.000 0.005(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb O1 1.708(5) . ? Nb O4 2.028(4) . ? Nb O2 2.029(3) 6 ? Nb O2 2.029(3) . ? Nb O3 2.033(4) 1_556 ? Nb O5 2.219(5) . ? P O4 1.535(4) . ? P O3 1.536(4) . ? P O2 1.539(3) 7 ? P O2 1.539(3) 4_545 ? O2 P 1.539(3) 7 ? O2 O23 1.71(5) . ? O3 Nb 2.033(4) 1_554 ? O5 C1 1.36(2) . ? O5 C1 1.36(2) 6 ? O5 C1 1.41(2) 5 ? O5 C1 1.41(2) 2 ? C1 O5 1.41(2) 5 ? C1 C2 1.488(10) . ? C2 N 1.485(10) . ? P2 O24 1.51 . ? P2 O22 1.53 . ? P2 O21 1.55 . ? P2 O23 1.56 . ? P3 O34 1.51 . ? P3 O32 1.53 . ? P3 O31 1.55 . ? P3 O33 1.56 . ? 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_3 _geom_angle_publ_flag O1 Nb O4 96.9(2) . . ? O1 Nb O2 97.16(9) . 6 ? O4 Nb O2 89.27(9) . 6 ? O1 Nb O2 97.16(9) . . ? O4 Nb O2 89.27(9) . . ? O2 Nb O2 165.7(2) 6 . ? O1 Nb O3 97.2(2) . 1_556 ? O4 Nb O3 165.8(2) . 1_556 ? O2 Nb O3 88.97(9) 6 1_556 ? O2 Nb O3 88.97(9) . 1_556 ? O1 Nb O5 179.6(2) . . ? O4 Nb O5 82.7(2) . . ? O2 Nb O5 82.84(9) 6 . ? O2 Nb O5 82.84(9) . . ? O3 Nb O5 83.1(2) 1_556 . ? O4 P O3 107.1(2) . . ? O4 P O2 110.7(2) . 7 ? O3 P O2 110.83(15) . 7 ? O4 P O2 110.7(2) . 4_545 ? O3 P O2 110.83(15) . 4_545 ? O2 P O2 106.8(2) 7 4_545 ? P O2 O23 107.0(27) 7 . ? P O2 Nb 136.2(2) 7 . ? O23 O2 Nb 111.3(28) . . ? P O3 Nb 135.2(3) . 1_554 ? P O4 Nb 137.7(3) . . ? C1 O5 C1 46.6(14) . 6 ? C1 O5 C1 67.4(11) . 5 ? C1 O5 C1 46.7(12) 6 5 ? C1 O5 C1 46.7(12) . 2 ? C1 O5 C1 67.4(11) 6 2 ? C1 O5 C1 44.7(13) 5 2 ? C1 O5 Nb 151.6(7) . . ? C1 O5 Nb 151.6(7) 6 . ? C1 O5 Nb 139.9(7) 5 . ? C1 O5 Nb 139.9(7) 2 . ? O5 C1 O5 112.6(11) . 5 ? O5 C1 C2 129.2(19) . . ? O5 C1 C2 118.1(18) 5 . ? N C2 C1 141.8(35) . . ? O24 P2 O22 111.7 . . ? O24 P2 O21 109.4 . . ? O22 P2 O21 108.7 . . ? O24 P2 O23 110.5 . . ? O22 P2 O23 110.8 . . ? O21 P2 O23 105.5 . . ? P2 O23 O2 146.1(48) . . ? O34 P3 O32 111.7 . . ? O34 P3 O31 109.4 . . ? O32 P3 O31 108.7 . . ? O34 P3 O33 110.5 . . ? O32 P3 O33 110.8 . . ? O31 P3 O33 105.5 . . ? _refine_diff_density_max 1.007 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.194