data_rgr191 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H7 Ba O8 P' _chemical_formula_weight 327.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ba' 'Ba' -0.3244 2.2819 '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' '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.427(6) _cell_length_b 11.786(15) _cell_length_c 10.615(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.47(10) _cell_angle_gamma 90.00 _cell_volume 803.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 5.149 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4735 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.63 _reflns_number_total 1715 _reflns_number_gt 1688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+1.3467P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1715 _refine_ls_number_parameters 125 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 2.943 _refine_ls_shift/su_mean 0.024 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba1 Ba 0.05201(3) 0.578552(15) 0.195174(18) 0.01392(11) Uani 1 1 d . . . C1 C 0.2336(5) 0.8022(3) 0.4335(3) 0.0154(6) Uani 1 1 d . . . C2 C 0.1747(5) 0.7139(3) 0.5326(3) 0.0159(6) Uani 1 1 d . . . H2A H 0.2515 0.6436 0.5173 0.019 Uiso 1 1 calc R . . O1 O 0.1883(5) 0.7743(2) 0.3202(2) 0.0247(6) Uani 1 1 d . . . O2 O 0.3163(4) 0.8927(2) 0.4654(2) 0.0221(5) Uani 1 1 d . . . O3 O 0.2357(5) 0.7575(2) 0.6538(3) 0.0249(6) Uani 1 1 d . . . H3A H 0.2410 0.7055 0.7051 0.037 Uiso 1 1 calc R . . O4 O -0.2181(4) 0.7958(2) 0.5370(2) 0.0228(6) Uani 1 1 d . . . O5 O -0.1459(4) 0.6124(2) 0.6480(2) 0.0186(5) Uani 1 1 d . . . H5A H -0.1998 0.6530 0.7007 0.028 Uiso 1 1 calc R . . O6 O -0.1560(4) 0.6130(3) 0.4123(3) 0.0236(6) Uani 1 1 d . . . O7 O -0.2526(5) 0.4111(2) 0.1775(3) 0.0237(6) Uani 1 1 d D . . O8 O 0.4767(6) 0.5718(3) 0.2673(5) 0.0436(9) Uani 1 1 d D . . P1 P -0.10737(13) 0.68318(7) 0.52530(8) 0.01418(19) Uani 1 1 d . . . H7A H -0.380(6) 0.447(6) 0.193(6) 0.055(18) Uiso 1 1 d D . . H8B H 0.461(6) 0.536(3) 0.344(2) 0.000(8) Uiso 1 1 d D . . H7B H -0.271(10) 0.378(6) 0.098(3) 0.057(18) Uiso 1 1 d D . . H8A H 0.60(3) 0.61(2) 0.23(3) 0.35(15) Uiso 1 1 d D . . 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 Ba1 0.01767(16) 0.01235(15) 0.01178(15) -0.00046(6) 0.00141(10) -0.00045(6) C1 0.0185(16) 0.0175(15) 0.0104(14) 0.0011(12) 0.0032(12) 0.0011(12) C2 0.0202(16) 0.0159(15) 0.0118(15) 0.0013(12) 0.0009(12) -0.0005(12) O1 0.0383(16) 0.0250(14) 0.0109(11) -0.0025(10) 0.0030(11) -0.0112(12) O2 0.0323(15) 0.0173(11) 0.0168(12) 0.0007(11) 0.0000(11) -0.0070(11) O3 0.0367(16) 0.0242(14) 0.0135(12) 0.0036(10) -0.0052(11) -0.0084(12) O4 0.0301(14) 0.0209(13) 0.0179(12) 0.0035(10) 0.0075(11) 0.0101(10) O5 0.0267(13) 0.0175(12) 0.0120(11) 0.0027(10) 0.0077(10) 0.0038(11) O6 0.0269(14) 0.0252(14) 0.0188(13) -0.0078(12) 0.0008(11) -0.0044(12) O7 0.0294(16) 0.0233(14) 0.0183(14) -0.0024(10) 0.0002(12) -0.0060(11) O8 0.033(2) 0.042(2) 0.056(2) 0.0013(16) -0.0064(18) 0.0021(14) P1 0.0185(4) 0.0149(4) 0.0093(4) 0.0000(3) 0.0032(3) 0.0008(3) _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 Ba1 O4 2.706(4) 4_675 ? Ba1 O6 2.724(4) . ? Ba1 O7 2.782(4) . ? Ba1 O1 2.791(4) . ? Ba1 O8 2.817(5) . ? Ba1 O3 2.831(4) 4_575 ? Ba1 O5 2.855(4) 3_566 ? Ba1 O2 2.858(4) 4_575 ? Ba1 O2 2.915(4) 2_545 ? Ba1 Ba1 4.572(5) 3_565 ? C1 O2 1.235(5) . ? C1 O1 1.273(4) . ? C1 C2 1.534(5) . ? C2 O3 1.431(4) . ? C2 P1 1.848(4) . ? C2 H2A 0.9800 . ? O2 Ba1 2.858(4) 4_676 ? O2 Ba1 2.915(4) 2 ? O3 Ba1 2.831(4) 4_676 ? O3 H3A 0.8200 . ? O4 P1 1.513(3) . ? O4 Ba1 2.706(4) 4_576 ? O5 P1 1.572(3) . ? O5 Ba1 2.855(4) 3_566 ? O5 H5A 0.8200 . ? O6 P1 1.484(3) . ? O7 H7A 0.94(2) . ? O7 H7B 0.94(2) . ? O8 H8B 0.926(18) . ? O8 H8A 0.95(2) . ? 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 O4 Ba1 O6 136.97(10) 4_675 . ? O4 Ba1 O7 137.79(10) 4_675 . ? O6 Ba1 O7 78.63(11) . . ? O4 Ba1 O1 70.92(11) 4_675 . ? O6 Ba1 O1 68.25(9) . . ? O7 Ba1 O1 146.08(10) . . ? O4 Ba1 O8 69.11(13) 4_675 . ? O6 Ba1 O8 105.52(15) . . ? O7 Ba1 O8 132.34(11) . . ? O1 Ba1 O8 66.66(11) . . ? O4 Ba1 O3 86.08(12) 4_675 4_575 ? O6 Ba1 O3 70.32(11) . 4_575 ? O7 Ba1 O3 88.42(13) . 4_575 ? O1 Ba1 O3 74.04(12) . 4_575 ? O8 Ba1 O3 138.45(11) . 4_575 ? O4 Ba1 O5 133.06(9) 4_675 3_566 ? O6 Ba1 O5 74.04(10) . 3_566 ? O7 Ba1 O5 67.54(12) . 3_566 ? O1 Ba1 O5 108.36(13) . 3_566 ? O8 Ba1 O5 68.32(11) . 3_566 ? O3 Ba1 O5 140.24(10) 4_575 3_566 ? O4 Ba1 O2 72.01(11) 4_675 4_575 ? O6 Ba1 O2 116.32(11) . 4_575 ? O7 Ba1 O2 70.75(11) . 4_575 ? O1 Ba1 O2 117.44(10) . 4_575 ? O8 Ba1 O2 136.36(14) . 4_575 ? O3 Ba1 O2 54.83(9) 4_575 4_575 ? O5 Ba1 O2 133.69(9) 3_566 4_575 ? O4 Ba1 O2 82.95(12) 4_675 2_545 ? O6 Ba1 O2 139.71(9) . 2_545 ? O7 Ba1 O2 69.01(12) . 2_545 ? O1 Ba1 O2 143.81(9) . 2_545 ? O8 Ba1 O2 81.02(12) . 2_545 ? O3 Ba1 O2 129.84(10) 4_575 2_545 ? O5 Ba1 O2 71.83(12) 3_566 2_545 ? O2 Ba1 O2 75.27(10) 4_575 2_545 ? O4 Ba1 Ba1 74.26(10) 4_675 3_565 ? O6 Ba1 Ba1 139.77(8) . 3_565 ? O7 Ba1 Ba1 64.25(9) . 3_565 ? O1 Ba1 Ba1 143.37(6) . 3_565 ? O8 Ba1 Ba1 110.67(13) . 3_565 ? O3 Ba1 Ba1 92.76(10) 4_575 3_565 ? O5 Ba1 Ba1 103.48(10) 3_566 3_565 ? O2 Ba1 Ba1 38.06(7) 4_575 3_565 ? O2 Ba1 Ba1 37.20(6) 2_545 3_565 ? O2 C1 O1 124.6(3) . . ? O2 C1 C2 120.6(3) . . ? O1 C1 C2 114.7(3) . . ? O3 C2 C1 107.8(3) . . ? O3 C2 P1 110.7(2) . . ? C1 C2 P1 111.3(2) . . ? O3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? P1 C2 H2A 109.0 . . ? C1 O1 Ba1 136.4(2) . . ? C1 O2 Ba1 123.5(2) . 4_676 ? C1 O2 Ba1 128.2(2) . 2 ? Ba1 O2 Ba1 104.73(10) 4_676 2 ? C2 O3 Ba1 124.3(2) . 4_676 ? C2 O3 H3A 109.5 . . ? Ba1 O3 H3A 113.0 4_676 . ? P1 O4 Ba1 142.80(15) . 4_576 ? P1 O5 Ba1 150.04(14) . 3_566 ? P1 O5 H5A 109.5 . . ? Ba1 O5 H5A 98.6 3_566 . ? P1 O6 Ba1 132.01(17) . . ? Ba1 O7 H7A 107(5) . . ? Ba1 O7 H7B 115(4) . . ? H7A O7 H7B 105(6) . . ? Ba1 O8 H8B 97(2) . . ? Ba1 O8 H8A 133(10) . . ? H8B O8 H8A 129(10) . . ? O6 P1 O4 117.74(18) . . ? O6 P1 O5 109.86(19) . . ? O4 P1 O5 108.27(16) . . ? O6 P1 C2 109.22(18) . . ? O4 P1 C2 106.73(17) . . ? O5 P1 C2 104.13(17) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.870 _refine_diff_density_min -1.739 _refine_diff_density_rms 0.238