#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/02/2010254.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2010254 loop_ _publ_author_name 'Cordes, A.W.' 'Folkert, S.' 'Bryan, C.D.' 'Chandrasekhar, V.' 'Thomas, K.R.J.' _publ_contact_author ; Dr. A.W. Cordes Department of Chemistry and Biochemistry University of Arkansas Fayetteville AR 72701 USA ; _publ_section_title ;2,2,4,4-Tetrakis(3,5-dimethylpyrazol-1-yl)-2\l^5^,4\l^5^,6\l^5^-cyclotriphosphaza-1,3,5-triene-6-spiro-2'-1',3'-diaza-2'-phosphacyclohexane, C~23~H~36~N~13~P~3~ ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1976 _journal_page_last 1978 _journal_volume 50 _journal_year 1994 _chemical_formula_moiety 'C23 H36 N13 P3' _chemical_formula_sum 'C23 H36 N13 P3' _chemical_formula_weight 587.54 _chemical_name_systematic ; Spiro [2,2,3,3-tetrakis (3,5-dimethylpyrazolyl)cyclotriphosphazene - 1-phospha-2,5- diazacyclohexane] ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _cell_angle_alpha 90.0 _cell_angle_beta 111.557(17) _cell_angle_gamma 90.0 _cell_formula_units_Z 8 _cell_length_a 31.998(8) _cell_length_b 10.1595(11) _cell_length_c 20.373(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 9.50 _cell_measurement_theta_min 9.00 _cell_volume 6160(2) _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, year?)' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, year?)' _computing_data_reduction ' NRCVAX (Gabe, Le Page, Charland, Lee & White, 1989)' _computing_molecular_graphics NRCVAX _computing_publication_material NRCVAX _computing_structure_refinement NRCVAX _computing_structure_solution NRCVAX _diffrn_ambient_temperature 293 _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method '\q/2\q [speed 4-16\% min^-1^, width (1.0 + 0.35tan\q)\%]' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'xray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.70930 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 5507 _diffrn_reflns_theta_max 24.91 _diffrn_reflns_theta_min 0.00 _diffrn_standards_decay_% '1.8 in 44.4 h' _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.22 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_type '\y scans (3 reflections)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.267 _exptl_crystal_description block _exptl_crystal_F_000 2482.95 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.29 _refine_diff_density_min -0.29 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.15 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 352 _refine_ls_number_reflns 2506 _refine_ls_R_factor_all 0.135 _refine_ls_R_factor_obs 0.052 _refine_ls_shift/esd_max 0.019 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/[\s^2^(F) + 0.0025F^2^]' _refine_ls_wR_factor_all 0.092 _refine_ls_wR_factor_obs 0.073 _reflns_number_observed 2506 _reflns_number_total 5404 _reflns_observed_criterion 'Inet > 3.0\s(Inet)' _[local]_cod_data_source_file bk1057.cif _[local]_cod_data_source_block global _[local]_cod_cif_authors_sg_H-M 'C 2/c' _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. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 39 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 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. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 6159.7(19) _cod_database_code 2010254 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 1/2+x,1/2+y,z 1/2-x,1/2-y,-z -x,y,1/2-z x,-y,1/2+z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol P1 0.0415(9) 0.0462(10) 0.0572(10) -0.0137(15) -0.0004(15) 0.0283(15) P P2 0.0406(9) 0.0597(10) 0.0372(7) -0.0124(15) 0.0092(12) 0.0056(14) P P3 0.0416(8) 0.0394(8) 0.0351(7) -0.0084(14) 0.0059(12) 0.0021(13) P N1 0.052(3) 0.051(3) 0.041(3) -0.025(5) -0.006(4) 0.002(5) N N2 0.053(3) 0.065(3) 0.053(3) -0.017(5) 0.034(5) 0.019(5) N N3 0.048(3) 0.059(3) 0.035(2) -0.038(5) 0.017(4) -0.013(4) N N4 0.065(4) 0.050(3) 0.085(4) -0.017(5) -0.005(6) 0.048(6) N N5 0.044(3) 0.074(4) 0.086(4) -0.020(6) -0.001(6) 0.064(6) N N11 0.043(3) 0.040(3) 0.043(3) -0.004(4) 0.015(4) 0.008(4) N N12 0.042(3) 0.049(3) 0.047(3) 0.000(5) 0.001(4) 0.012(5) N N21 0.053(3) 0.043(3) 0.046(3) 0.005(5) 0.028(5) 0.004(5) N N22 0.054(3) 0.067(3) 0.054(3) -0.008(6) 0.035(5) -0.003(5) N N31 0.043(3) 0.096(4) 0.039(3) 0.015(6) 0.010(5) 0.016(6) N N32 0.086(5) 0.078(4) 0.070(4) 0.055(7) 0.040(7) 0.042(7) N N41 0.053(3) 0.076(4) 0.036(3) -0.004(5) 0.025(5) 0.002(5) N N42 0.063(4) 0.074(4) 0.042(3) 0.005(6) 0.011(5) 0.001(6) N C1 0.102(6) 0.050(4) 0.110(6) -0.040(8) 0.084(10) -0.008(8) C C2 0.139(8) 0.064(5) 0.150(8) -0.060(11) 0.178(14) -0.022(11) C C3 0.054(5) 0.116(7) 0.103(6) -0.026(9) 0.034(8) 0.062(10) C C11 0.072(5) 0.071(5) 0.075(5) 0.014(8) -0.004(8) 0.044(8) C C12 0.049(4) 0.054(4) 0.057(4) 0.020(6) 0.024(6) 0.028(6) C C13 0.061(4) 0.048(4) 0.063(4) 0.020(6) 0.041(7) 0.036(7) C C14 0.060(4) 0.042(4) 0.057(4) -0.010(6) 0.056(6) -0.001(6) C C15 0.093(5) 0.036(3) 0.075(4) -0.020(7) 0.051(8) -0.009(7) C C21 0.083(6) 0.163(9) 0.115(7) -0.012(12) 0.124(11) 0.006(13) C C22 0.052(4) 0.104(6) 0.057(4) 0.009(9) 0.040(7) -0.013(8) C C23 0.079(6) 0.104(7) 0.082(5) 0.053(10) 0.068(9) -0.024(10) C C24 0.064(4) 0.065(5) 0.047(4) 0.018(7) 0.009(7) -0.017(7) C C25 0.108(7) 0.062(5) 0.100(6) 0.056(9) 0.056(10) -0.001(8) C C31 0.194(12) 0.139(9) 0.202(12) 0.207(18) 0.16(2) 0.118(17) C C32 0.090(7) 0.132(8) 0.078(6) 0.106(13) 0.052(11) 0.053(11) C C33 0.062(5) 0.203(11) 0.059(5) 0.078(15) 0.011(8) 0.018(12) C C34 0.046(4) 0.128(7) 0.040(3) 0.005(10) 0.017(6) -0.019(8) C C35 0.053(5) 0.188(10) 0.082(6) -0.066(11) 0.031(8) -0.081(12) C C41 0.150(8) 0.099(7) 0.077(5) 0.045(12) 0.054(11) -0.035(10) C C42 0.061(4) 0.092(6) 0.056(4) 0.015(8) 0.018(7) -0.023(8) C C43 0.062(4) 0.109(6) 0.049(4) 0.006(8) 0.048(7) -0.035(8) C C44 0.068(5) 0.099(6) 0.047(4) 0.002(8) 0.056(7) 0.010(8) C C45 0.095(6) 0.135(7) 0.058(4) 0.015(11) 0.071(8) 0.033(10) C loop_ _atom_site_label _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_calc_flag _atom_site_refinement_flags _atom_site_type_symbol P1 0.44355(5) 0.40306(16) 0.12028(8) 0.0535(9) Uani . . P P2 0.37788(5) 0.23918(16) 0.03000(7) 0.0486(9) Uani . . P P3 0.39574(5) 0.22557(14) 0.17005(7) 0.0418(8) Uani . . P N1 0.42840(15) 0.3452(4) 0.1809(2) 0.053(3) Uani . . N N2 0.41949(16) 0.3301(5) 0.0454(2) 0.057(3) Uani . . N N3 0.36946(15) 0.1703(5) 0.0931(2) 0.049(3) Uani . . N N4 0.43328(18) 0.5605(5) 0.1070(3) 0.076(4) Uani . . N N5 0.49759(16) 0.3998(5) 0.1504(3) 0.075(4) Uani . . N N11 0.42237(14) 0.0981(4) 0.2211(2) 0.044(3) Uani . . N N12 0.45407(14) 0.1326(4) 0.2862(2) 0.051(3) Uani . . N N21 0.35819(15) 0.2656(4) 0.2079(2) 0.049(3) Uani . . N N22 0.33736(17) 0.1642(5) 0.2279(3) 0.059(3) Uani . . N N31 0.33020(16) 0.3232(6) -0.0181(2) 0.062(4) Uani . . N N32 0.3316(2) 0.4594(6) -0.0125(3) 0.080(4) Uani . . N N41 0.37748(15) 0.1240(5) -0.0298(2) 0.056(3) Uani . . N N42 0.38509(17) -0.0058(5) -0.0103(3) 0.064(4) Uani . . N C1 0.4688(3) 0.6547(6) 0.1227(4) 0.087(6) Uani . . C C2 0.5034(3) 0.6122(8) 0.0963(5) 0.108(8) Uani . . C C3 0.5262(2) 0.4827(9) 0.1280(4) 0.094(6) Uani . . C C11 0.5036(2) 0.0192(7) 0.3909(4) 0.081(5) Uani . . C C12 0.46933(19) 0.0208(6) 0.3180(3) 0.056(4) Uani . . C C13 0.4474(2) -0.0860(6) 0.2761(3) 0.058(4) Uani . . C C14 0.4177(2) -0.0360(5) 0.2157(3) 0.051(4) Uani . . C C15 0.3840(2) -0.1065(6) 0.1554(3) 0.070(5) Uani . . C C21 0.2773(3) 0.1370(10) 0.2736(5) 0.113(8) Uani . . C C22 0.3077(2) 0.2202(8) 0.2498(3) 0.071(5) Uani . . C C23 0.3090(3) 0.3559(9) 0.2444(4) 0.087(6) Uani . . C C24 0.3403(2) 0.3852(7) 0.2167(3) 0.063(4) Uani . . C C25 0.3534(3) 0.5146(7) 0.1952(4) 0.093(6) Uani . . C C31 0.2779(4) 0.6399(11) -0.0510(7) 0.177(11) Uani . . C C32 0.2899(4) 0.4929(10) -0.0462(5) 0.102(7) Uani . . C C33 0.2612(3) 0.3893(13) -0.0739(4) 0.113(8) Uani . . C C34 0.2874(2) 0.2765(9) -0.0542(3) 0.074(5) Uani . . C C35 0.2764(3) 0.1345(11) -0.0660(4) 0.111(7) Uani . . C C41 0.3958(3) -0.2106(9) -0.0655(4) 0.113(7) Uani . . C C42 0.3872(2) -0.0646(7) -0.0663(4) 0.073(5) Uani . . C C43 0.3816(2) 0.0226(8) -0.1213(3) 0.072(5) Uani . . C C44 0.3760(2) 0.1424(8) -0.0978(3) 0.069(5) Uani . . C C45 0.3690(3) 0.2754(9) -0.1328(4) 0.094(6) Uani . . C H1 0.457 0.736 0.101 0.0974 Uiso . . H H2 0.482 0.668 0.172 0.0974 Uiso . . H H3 0.491 0.603 0.047 0.1277 Uiso . . H H4 0.526 0.678 0.108 0.1277 Uiso . . H H5 0.553 0.501 0.168 0.1010 Uiso . . H H6 0.534 0.437 0.093 0.1010 Uiso . . H H11 0.502 0.100 0.414 0.0826 Uiso . . H H12 0.533 0.009 0.389 0.0826 Uiso . . H H13 0.498 -0.052 0.416 0.0826 Uiso . . H H14 0.453 -0.177 0.288 0.0673 Uiso . . H H15 0.388 -0.199 0.161 0.0780 Uiso . . H H16 0.387 -0.080 0.112 0.0780 Uiso . . H H17 0.355 -0.085 0.154 0.0780 Uiso . . H H21 0.280 0.048 0.261 0.1302 Uiso . . H H22 0.247 0.166 0.250 0.1302 Uiso . . H H23 0.285 0.144 0.323 0.1302 Uiso . . H H24 0.291 0.417 0.258 0.0985 Uiso . . H H25 0.384 0.534 0.224 0.0999 Uiso . . H H26 0.350 0.511 0.147 0.0999 Uiso . . H H27 0.334 0.582 0.201 0.0999 Uiso . . H H31 0.299 0.689 -0.064 0.1884 Uiso . . H H32 0.279 0.670 -0.006 0.1884 Uiso . . H H33 0.249 0.649 -0.086 0.1884 Uiso . . H H34 0.230 0.393 -0.101 0.1181 Uiso . . H H35 0.291 0.085 -0.024 0.1179 Uiso . . H H36 0.285 0.106 -0.103 0.1179 Uiso . . H H37 0.245 0.126 -0.080 0.1179 Uiso . . H H41 0.371 -0.251 -0.101 0.1187 Uiso . . H H42 0.399 -0.245 -0.021 0.1187 Uiso . . H H43 0.422 -0.226 -0.075 0.1187 Uiso . . H H44 0.382 0.002 -0.167 0.0833 Uiso . . H H45 0.378 0.271 -0.172 0.1060 Uiso . . H H46 0.338 0.302 -0.149 0.1060 Uiso . . H H47 0.387 0.339 -0.100 0.1060 Uiso . . H H7 0.509 0.329 0.178 0.0778 Uiso . . H H8 0.410 0.580 0.068 0.0770 Uiso . . H loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag P1 N1 . . 1.596(5) yes P1 N2 . . 1.614(5) yes P1 N4 . . 1.635(5) yes P1 N5 . . 1.609(5) yes P2 N2 . . 1.554(5) yes P2 N3 . . 1.571(4) yes P2 N31 . . 1.708(5) yes P2 N41 . . 1.686(5) yes P3 N1 . . 1.565(4) yes P3 N3 . . 1.585(4) yes P3 N11 . . 1.683(4) yes P3 N21 . . 1.698(5) yes N4 C1 . . 1.428(9) no N5 C3 . . 1.436(9) no N11 N12 . . 1.386(6) no N11 C14 . . 1.371(7) no N12 C12 . . 1.310(7) no N21 N22 . . 1.367(7) no N21 C24 . . 1.383(8) no N22 C22 . . 1.317(9) no N31 N32 . . 1.387(9) no N31 C34 . . 1.378(9) no N32 C32 . . 1.302(11) no N41 N42 . . 1.373(7) no N41 C44 . . 1.380(7) no N42 C42 . . 1.311(9) no C1 C2 . . 1.465(12) no C2 C3 . . 1.526(13) no C11 C12 . . 1.486(9) no C12 C13 . . 1.399(9) no C13 C14 . . 1.347(8) no C14 C15 . . 1.487(9) no C21 C22 . . 1.499(11) no C22 C23 . . 1.385(12) no C23 C24 . . 1.351(11) no C24 C25 . . 1.493(11) no C31 C32 . . 1.535(14) no C32 C33 . . 1.375(18) no C33 C34 . . 1.391(14) no C34 C35 . . 1.484(13) no C41 C42 . . 1.508(11) no C42 C43 . . 1.387(11) no C43 C44 . . 1.344(11) no C44 C45 . . 1.506(11) no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.090 0.095 'International Tables Vol. IV Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV Table 2.2B' H H 0.000 0.000 'International Tables Vol. IV Table 2.2B' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 8 4 0 5 1 7 2 2 -8 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N1 P1 N2 112.8(2) yes N1 P1 N4 112.8(3) yes N1 P1 N5 106.7(3) yes N2 P1 N4 107.2(3) yes N2 P1 N5 115.1(3) yes N4 P1 N5 101.9(3) yes N2 P2 N3 119.4(2) yes N2 P2 N31 109.7(3) yes N2 P2 N41 109.7(3) yes N3 P2 N31 107.8(2) yes N3 P2 N41 108.9(2) yes N31 P2 N41 99.4(2) yes N1 P3 N3 120.0(2) yes N1 P3 N11 110.5(2) yes N1 P3 N21 107.3(3) yes N3 P3 N11 107.6(2) yes N3 P3 N21 109.1(2) yes N11 P3 N21 100.7(2) yes P1 N1 P3 123.6(3) yes P1 N2 P2 122.7(3) yes P2 N3 P3 117.6(3) yes P1 N4 C1 121.6(5) yes P1 N5 C3 126.0(4) yes P3 N11 N12 115.0(3) no P3 N11 C14 134.4(4) no N12 N11 C14 110.3(4) no N11 N12 C12 105.3(4) no P3 N21 N22 117.3(4) no P3 N21 C24 131.7(4) no N22 N21 C24 110.6(5) no N21 N22 C22 105.5(5) no P2 N31 N32 117.2(4) no P2 N31 C34 129.5(5) no N32 N31 C34 112.5(6) no N31 N32 C32 102.9(7) no P2 N41 N42 120.2(3) no P2 N41 C44 128.3(5) no N42 N41 C44 111.0(5) no N41 N42 C42 104.2(5) no N4 C1 C2 111.5(6) no C1 C2 C3 114.0(7) no N5 C3 C2 112.3(6) no N12 C12 C11 120.5(6) no N12 C12 C13 111.0(5) no C11 C12 C13 128.4(5) no C12 C13 C14 107.0(5) no N11 C14 C13 106.4(5) no N11 C14 C15 124.7(5) no C13 C14 C15 128.8(5) no N22 C22 C21 120.0(7) no N22 C22 C23 110.9(6) no C21 C22 C23 129.0(7) no C22 C23 C24 107.5(6) no N21 C24 C23 105.5(6) no N21 C24 C25 124.2(6) no C23 C24 C25 130.3(7) no N32 C32 C31 118.1(10) no N32 C32 C33 114.6(8) no C31 C32 C33 127.2(9) no C32 C33 C34 105.7(7) no N31 C34 C33 104.3(8) no N31 C34 C35 123.5(7) no C33 C34 C35 132.2(8) no N42 C42 C41 120.4(7) no N42 C42 C43 112.3(6) no C41 C42 C43 127.2(7) no C42 C43 C44 106.5(6) no N41 C44 C43 106.0(6) no N41 C44 C45 122.8(6) no C43 C44 C45 131.2(6) no