data_b26381m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Guanidinium tetramethoxyborate hexafluorophosphate solvate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H68 B3 F6 N12 O14 P' _chemical_formula_weight 854.24 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 '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' 'B' 'B' 0.0013 0.0007 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' _symmetry_cell_setting 'cubic' _symmetry_space_group_name_H-M 'P-43m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' _cell_length_a 10.5722(4) _cell_length_b 10.5722(4) _cell_length_c 10.5722(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1181.67(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2424 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 26.97 _exptl_crystal_description 'tetrahedron' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 0.142 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The crystal was sealed in a Lindeman tube along with a small amount mother liquor. ; _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 7442 _diffrn_reflns_av_R_equivalents 0.1625 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.36 _reflns_number_total 563 _reflns_number_gt 452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Although the atoms of the {[C(NH2)3]4[B(OCH3)4]3} hydrogen-bonded network are well defined, the hexafluorophosphate ion and the methanol are highly disordered within the intraframework voids. Attempts to model this disorder were unsuccessful. This disorder leads to elevation of the agreement values. On the basis of the PLATON program (Spek, A. L., 1998), we estimate that the void in each unit cell is occupied by two methanol molecules in addition to the hexafluorophosphate ion. When the contribution of the disordered regions of the crystal are subtracted from the intensity data using the SQUEEZE routine in PLATON, much more satisfactory agreement values are obtained (R1 = 4.69%). 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^)+(0.1630P)^2^+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(5) _refine_ls_number_reflns 563 _refine_ls_number_parameters 24 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1103 _refine_ls_R_factor_gt 0.1048 _refine_ls_wR_factor_ref 0.2476 _refine_ls_wR_factor_gt 0.2414 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.199 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 O1 O 0.42355(15) 0.42355(15) 0.0880(2) 0.0655(8) Uani 1 2 d S . . B1 B 0.5000 0.5000 0.0000 0.0570(16) Uani 1 8 d S . . C1 C 0.3355(3) 0.3355(3) 0.0344(4) 0.0948(16) Uani 1 2 d S . . H1A H 0.2919 0.2919 0.1011 0.114 Uiso 1 2 calc SR . . H1B H 0.3802 0.2754 -0.0169 0.114 Uiso 1 1 calc R . . H1C H 0.2754 0.3802 -0.0169 0.114 Uiso 0.00 1 calc PR . . N1 N 0.6981(2) 0.4550(2) 0.3019(2) 0.0725(9) Uani 1 2 d S . . H1D H 0.7638 0.4889 0.3358 0.087 Uiso 1 1 calc R . . H1E H 0.6653 0.4878 0.2351 0.087 Uiso 0.00 1 calc PR . . C2 C 0.6477(3) 0.3523(3) 0.3523(3) 0.0640(14) Uani 1 6 d S . . 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 O1 0.0682(10) 0.0682(10) 0.0599(12) 0.0012(7) 0.0012(7) -0.0083(10) B1 0.058(2) 0.058(2) 0.056(3) 0.000 0.000 0.000 C1 0.102(2) 0.102(2) 0.080(3) 0.0003(15) 0.0003(15) -0.027(3) N1 0.0757(12) 0.0660(16) 0.0757(12) 0.0090(10) -0.0123(16) -0.0090(10) C2 0.0640(14) 0.0640(14) 0.0640(14) -0.0010(14) 0.0010(14) 0.0010(14) _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 O1 C1 1.433(5) . ? O1 B1 1.474(2) . ? B1 O1 1.474(2) 2_665 ? B1 O1 1.474(2) 4_565 ? B1 O1 1.474(2) 3_655 ? N1 C2 1.322(3) . ? C2 N1 1.322(3) 7_665 ? C2 N1 1.322(3) 10_656 ? 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 C1 O1 B1 117.6(2) . . ? O1 B1 O1 113.49(10) 2_665 4_565 ? O1 B1 O1 113.49(10) 2_665 3_655 ? O1 B1 O1 101.71(18) 4_565 3_655 ? O1 B1 O1 101.71(18) 2_665 . ? O1 B1 O1 113.49(10) 4_565 . ? O1 B1 O1 113.49(10) 3_655 . ? N1 C2 N1 119.994(9) . 7_665 ? N1 C2 N1 119.994(9) . 10_656 ? N1 C2 N1 119.994(9) 7_665 10_656 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.36 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.769 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.211