#------------------------------------------------------------------------------ #$Date: 2025-08-18 13:40:47 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301773 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100936.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 loop_ _publ_author_name 'Becker, Gerd' 'Brombach, Heike' 'Horner, Stephen T.' 'Niecke, Edgar' 'Schwarz, Wolfgang' 'Streubel, Rainer' 'W\"urthwein, Ernst-Ulrich' _publ_contact_author ; Gerd Becker Institut fuer Anorganische Chemie Universitaet Stuttgart 70569 Stuttgart Germany ; _publ_contact_author_email becker@iac.uni-stuttgart.de _publ_contact_author_fax '(+49 711) 685 4241' _publ_contact_author_phone '(+49 711) 685 4221' _publ_section_title ; Synthesis and Structure of K^+^[^i^PrN\\db C\\db P]^-^, a 1-Aza-3\l^3^-phospha-3-allenide ; _journal_coden_ASTM INOCAJ _journal_issue 9 _journal_name_full 'Inorganic Chemistry' _journal_page_first 3080 _journal_page_last 3086 _journal_paper_doi 10.1021/ic048162+ _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C7 H16 N P Si' _chemical_formula_weight 173.27 _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 112.21(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 7.285(3) _cell_length_b 10.067(4) _cell_length_c 8.103(2) _cell_measurement_reflns_used 45 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 18 _cell_measurement_theta_min 14 _cell_volume 550.2(3) _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method Wyckoff-Scan _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 3887 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 30.02 _diffrn_reflns_theta_min 2.72 _diffrn_standards_decay_% ? _diffrn_standards_interval_count 98 _diffrn_standards_interval_time ? _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.302 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.046 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description cylinder _exptl_crystal_F_000 188 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_size_rad 0.15 _refine_diff_density_max 0.412 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.044 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 89 _refine_ls_number_reflns 1689 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0296 _refine_ls_shift/su_max 0.061 _refine_ls_shift/su_mean 0.009 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.0442P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0858 _refine_ls_wR_factor_ref 0.0889 _reflns_number_gt 1555 _reflns_number_total 1689 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'PSI-SCAN' changed to 'psi-scan' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P21/m _cod_database_code 1100936 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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) 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' 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) . . ? 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_ _cod_changelog_entry_id _cod_changelog_entry_author _cod_changelog_entry_date _cod_changelog_entry_text 1 'Vaitkus, Antanas' 2021-10-24T01:00:00+03:00 'Updated bibliographic information.' loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 14319342