#------------------------------------------------------------------------------ #$Date: 2008-01-13 23:15:36 +0100 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100936.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_1100936 _publ_section_title ; Synthesis and Structure of K[iPrNCP], a 1-Aza-3lambda3- phospha-3-allenide ; loop_ _publ_author_name 'Becker, Gerd' 'Brombach, Heike' 'Horner, Stephen Thomas' 'Niecke, Edgar' 'Schwarz, Wolfgang' 'Streubel, Rainer' 'Wurthwein, Ernst-Ulrich' _chemical_formula_sum 'C7 H16 N P Si' _chemical_formula_weight 173.27 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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 Monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.285(3) _cell_length_b 10.067(4) _cell_length_c 8.103(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.21(2) _cell_angle_gamma 90.00 _cell_volume 550.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 14 _cell_measurement_theta_max 18 _exptl_crystal_description cylinder _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_size_rad 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.046 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 188 _exptl_absorpt_coefficient_mu 0.302 _exptl_absorpt_correction_type PSI-SCAN _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.860 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method 'Wyckoff-Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 98 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3887 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 30.02 _reflns_number_total 1689 _reflns_number_gt 1555 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.0442P] 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 1689 _refine_ls_number_parameters 89 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.061 _refine_ls_shift/su_mean 0.009 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 P P 0.19698(5) 0.2500 -0.20981(5) 0.03990(13) Uani 1 2 d S . . C C 0.39322(18) 0.2500 -0.04174(15) 0.0280(2) Uani 1 2 d S . . N N 0.56125(15) 0.2500 0.09777(13) 0.0294(2) Uani 1 2 d S . . C1 C 0.74870(18) 0.2500 0.06212(17) 0.0328(3) Uani 1 2 d S . . H1A H 0.848(3) 0.2500 0.180(2) 0.034(4) Uiso 1 2 d S . . Si Si 0.57488(5) 0.2500 0.32101(4) 0.02920(12) Uani 1 2 d S . . C11 C 0.7631(2) 0.12446(12) -0.0360(2) 0.0488(3) Uani 1 1 d . . . H11A H 0.886(2) 0.1252(17) -0.0507(19) 0.056(4) Uiso 1 1 d . . . H11B H 0.657(3) 0.1207(18) -0.144(2) 0.062(5) Uiso 1 1 d . . . H11C H 0.754(3) 0.0456(19) 0.029(2) 0.070(5) Uiso 1 1 d . . . C21 C 0.3173(2) 0.2500 0.3126(2) 0.0466(4) Uani 1 2 d S . . H21A H 0.247(2) 0.329(2) 0.256(2) 0.078(6) Uiso 1 1 d . . . H21B H 0.310(4) 0.2500 0.424(4) 0.072(8) Uiso 1 2 d S . . C22 C 0.71175(19) 0.09784(11) 0.43133(14) 0.0430(2) Uani 1 1 d . . . H22A H 0.842(3) 0.099(2) 0.432(2) 0.064(5) Uiso 1 1 d . . . H22B H 0.645(2) 0.0191(19) 0.376(2) 0.068(5) Uiso 1 1 d . . . H22C H 0.722(2) 0.096(2) 0.552(2) 0.068(5) Uiso 1 1 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 P 0.03051(19) 0.0522(2) 0.02985(19) 0.000 0.00327(14) 0.000 C 0.0288(5) 0.0303(5) 0.0258(5) 0.000 0.0113(4) 0.000 N 0.0249(4) 0.0397(5) 0.0239(4) 0.000 0.0098(4) 0.000 C1 0.0257(5) 0.0425(7) 0.0324(6) 0.000 0.0133(5) 0.000 Si 0.03068(19) 0.03395(19) 0.02281(17) 0.000 0.00993(13) 0.000 C11 0.0492(6) 0.0433(5) 0.0667(8) -0.0030(5) 0.0364(6) 0.0057(5) C21 0.0394(7) 0.0668(11) 0.0411(8) 0.000 0.0239(6) 0.000 C22 0.0517(6) 0.0379(5) 0.0335(5) 0.0055(4) 0.0094(4) 0.0023(4) _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 P C 1.5578(14) . ? C N 1.3154(15) . ? N C1 1.4988(16) . ? N Si 1.7738(11) . ? C1 C11 1.5180(14) . ? C1 C11 1.5180(14) 4_565 ? C1 H1A 0.956(18) . ? Si C21 1.8521(17) . ? Si C22 1.8617(12) 4_565 ? Si C22 1.8617(12) . ? C11 H11A 0.947(16) . ? C11 H11B 0.926(17) . ? C11 H11C 0.970(18) . ? C21 H21A 0.96(2) . ? C21 H21B 0.92(3) . ? C22 H22A 0.945(17) . ? C22 H22B 0.949(19) . ? C22 H22C 0.956(17) . ? 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 N C P 178.68(10) . . ? C N C1 117.00(10) . . ? C N Si 123.48(9) . . ? C1 N Si 119.52(8) . . ? N C1 C11 110.47(7) . . ? N C1 C11 110.47(7) . 4_565 ? C11 C1 C11 112.73(13) . 4_565 ? N C1 H1A 102.1(11) . . ? C11 C1 H1A 110.3(5) . . ? C11 C1 H1A 110.3(5) 4_565 . ? N Si C21 107.29(7) . . ? N Si C22 107.64(4) . 4_565 ? C21 Si C22 111.65(5) . 4_565 ? N Si C22 107.64(4) . . ? C21 Si C22 111.65(5) . . ? C22 Si C22 110.73(8) 4_565 . ? C1 C11 H11A 108.4(10) . . ? C1 C11 H11B 109.3(11) . . ? H11A C11 H11B 112.1(14) . . ? C1 C11 H11C 111.3(10) . . ? H11A C11 H11C 109.8(15) . . ? H11B C11 H11C 106.0(16) . . ? Si C21 H21A 111.3(11) . . ? Si C21 H21B 113.3(16) . . ? H21A C21 H21B 104.4(13) . . ? Si C22 H22A 110.5(12) . . ? Si C22 H22B 112.0(10) . . ? H22A C22 H22B 110.4(16) . . ? Si C22 H22C 109.4(11) . . ? H22A C22 H22C 107.5(14) . . ? H22B C22 H22C 106.9(16) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.412 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.044