# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 207/486 #Alkylation and addition to isocyanate of 2-(5-amino-3,4- #dicyano-2H-pyrrol-2-ylidene)-1,1,2-tricyanoethanide.X-ray #crystal and molecular structures of methyl-, dimethyl-, #dimethylformamidino- and propylcarboxamido-amino derivatives. # AUDIT ################################################## data_global _audit_creation_date ? _audit_creation_method ? _audit_update_record ? # PROCESSING SUMMARY (IUCr Office Use only) ############## _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _iucr_compatibility_tag ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # SUBMISSION DETAILS ##################################### _publ_contact_author 'Vincenzo Fares' _publ_contact_author_address ;Istituto di Chimica dei Materiali, C.N.R. Area della Ricerca di Roma C.P. 10 00016 Monterotondo Stazione (Roma) Italy ; _publ_contact_letter ; Please consider this CIF submission as crystallographic data for publication in Perkin Trans. 1 ; _publ_contact_author_phone ' [+39] 06 90672285 ' _publ_contact_author_fax ' [+39] 06 90672630 ' _publ_contact_author_email ' fares@mlib.cnr.it ' _publ_requested_journal ' Perkin Trans. 1 ' _publ_requested_category ? _publ_requested_coeditor_name ? # TITLE ################################################ _publ_section_title ; Alchylation and addition to isocyanate of 2-(5-amino-3,4-dicyano-2H-dicyano- 2H-pyrrol-2-ylidene)-1,1,2-tricyanoethanide. X-ray crystal and molecular structures of methyl-, dimethyl, dimethylformamido-, and propylcarboxamido- amino derivatives ; # AUTHOR LIST ############################################ loop_ _publ_author_name _publ_author_footnote _publ_author_address ? 'To whom correspondence should be addressed' ; ; ? . ; ; # TEXT ################################################### _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_acknowledgements ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; data_1 # DATA SECTION OF BLOCK ################################## _chemical_name_systematic ;tetraphenylarsonium 2-(5-methylamino-3,4-dicyano-2H-dicyano- 2H-pyrrol-2-ylidene)-1,1,2-tricyanoethanide ; _chemical_compound_source ; ; _chemical_formula_iucr ? _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum 'H24C36N7As1' _chemical_formula_weight 629.56 _chemical_melting_point ? _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ; SIR97(Cascarano et al.,Acta Cryst.,1996,A52,C-79) ; _computing_structure_refinement ; SHELXTL PC, Siemens Analytical X-Ray Instruments, Madison, WI, 1990 ; _computing_molecular_graphics ? _computing_publication_material ? _cell_length_a 9.458 _cell_length_b 13.658 _cell_length_c 23.889 _cell_angle_alpha 90.000 _cell_angle_beta 94.470 _cell_angle_gamma 90.000 _cell_volume 3076.531 _cell_formula_units_Z 4 _cell_measurement_radiation 'CuK\a' _cell_measurement_wavelength 1.54178 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 70 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '1/2-x,1/2+y,1/2-z' _exptl_crystal_description 'platelets' _exptl_crystal_colour 'violet' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 1.941 _exptl_absorpt_correction_type 'semiempirical via \y scans (TEXSAN, 1985)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_detector ? _diffrn_measurement_device 'MSC-AFC5 Diffractometer' _diffrn_measurement_method '\q-2\q scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_reduction_process ? _diffrn_reflns_number ? _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 50.05 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'h ' 96 'Hydrogen ' 0.0000 0.0000 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'c ' 144 'Carbon ' 0.0170 0.0090 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'n ' 28 'Nitrogen ' 0.0290 0.0180 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'as ' 4 'Arsenic ' -1.0110 1.0060 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _reflns_number_total 3698 _reflns_number_observed 3355 _reflns_observed_criterion 'F > 6.0 sigma(F)' _reflns_limit_h_max 9 _reflns_limit_h_min 0 _reflns_limit_k_max 13 _reflns_limit_k_min 0 _reflns_limit_l_max 23 _reflns_limit_l_min -23 _reflns_d_resolution_high 1.006 _reflns_d_resolution_low 11.908 _refine_ls_structure_factor_coef 'F' _refine_ls_extinction_method 'none' _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? _refine_ls_abs_structure_details ; ; _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment 'H atoms rigid to parent C atom' _refine_ls_weighting_scheme 'W=1/(\s^2(Fo)+0.0005Fo^2)' _refine_ls_number_reflns 1871 _refine_ls_number_parameters 229 _refine_ls_R_factor_all 0.0919 _refine_ls_R_factor_obs 0.0539 _refine_ls_wR_factor_all 0.0743 _refine_ls_wR_factor_obs 0.0665 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.43 _refine_ls_shift/esd_max 0.008 _refine_ls_shift/esd_mean 0.002 _refine_diff_density_max ? _refine_diff_density_min 0.68 _refine_diff_density_rms 0.00 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type As(1) -0.0995(1) 0.2952(1) 0.30063(4) 1.000 0.0495(4) uani C(101) -0.2857(5) 0.2745(5) 0.3199(3) 1.000 0.053(3) uiso C(102) -0.3555(5) 0.3444(5) 0.3502(3) 1.000 0.061(3) uiso C(103) -0.4976(5) 0.3310(5) 0.3602(3) 1.000 0.070(3) uiso C(104) -0.5699(5) 0.2477(5) 0.3399(3) 1.000 0.089(4) uiso C(105) -0.5001(5) 0.1778(5) 0.3095(3) 1.000 0.100(4) uiso C(106) -0.3580(5) 0.1912(5) 0.2996(3) 1.000 0.081(3) uiso H(102) -0.3057(5) 0.4017(5) 0.3642(3) 1.000 0.080 uiso H(103) -0.5456(5) 0.3791(5) 0.3811(3) 1.000 0.080 uiso H(104) -0.6676(5) 0.2385(5) 0.3468(3) 1.000 0.080 uiso H(105) -0.5498(5) 0.1205(5) 0.2956(3) 1.000 0.080 uiso H(106) -0.3100(5) 0.1431(5) 0.2787(3) 1.000 0.080 uiso C(201) -0.1066(6) 0.3547(4) 0.2292(2) 1.000 0.049(2) uiso C(202) 0.0119(6) 0.3534(4) 0.1979(2) 1.000 0.066(3) uiso C(203) 0.0059(6) 0.3982(4) 0.1453(2) 1.000 0.066(3) uiso C(204) -0.1185(6) 0.4443(4) 0.1240(2) 1.000 0.077(3) uiso C(205) -0.2370(6) 0.4456(4) 0.1554(2) 1.000 0.071(3) uiso C(206) -0.2310(6) 0.4008(4) 0.2080(2) 1.000 0.055(3) uiso H(202) 0.0975(6) 0.3217(4) 0.2125(2) 1.000 0.080 uiso H(203) 0.0874(6) 0.3974(4) 0.1237(2) 1.000 0.080 uiso H(204) -0.1226(6) 0.4752(4) 0.0878(2) 1.000 0.080 uiso H(205) -0.3226(6) 0.4773(4) 0.1407(2) 1.000 0.080 uiso H(206) -0.3125(6) 0.4016(4) 0.2295(2) 1.000 0.080 uiso C(301) -0.0042(6) 0.1745(3) 0.2957(2) 1.000 0.049(2) uiso C(302) -0.0089(6) 0.1236(3) 0.2449(2) 1.000 0.063(3) uiso C(303) 0.0560(6) 0.0322(3) 0.2423(2) 1.000 0.075(3) uiso C(304) 0.1256(6) -0.0084(3) 0.2905(2) 1.000 0.080(3) uiso C(305) 0.1303(6) 0.0424(3) 0.3412(2) 1.000 0.078(3) uiso C(306) 0.0654(6) 0.1339(3) 0.3438(2) 1.000 0.062(3) uiso H(302) -0.0568(6) 0.1515(3) 0.2118(2) 1.000 0.080 uiso H(303) 0.0528(6) -0.0028(3) 0.2074(2) 1.000 0.080 uiso H(304) 0.1703(6) -0.0713(3) 0.2887(2) 1.000 0.080 uiso H(305) 0.1782(6) 0.0145(3) 0.3744(2) 1.000 0.080 uiso H(306) 0.0686(6) 0.1689(3) 0.3788(2) 1.000 0.080 uiso C(401) 0.0017(6) 0.3719(4) 0.3556(2) 1.000 0.053(2) uiso C(402) 0.1041(6) 0.4379(4) 0.3400(2) 1.000 0.059(3) uiso C(403) 0.1837(6) 0.4917(4) 0.3809(2) 1.000 0.086(3) uiso C(404) 0.1610(6) 0.4794(4) 0.4374(2) 1.000 0.083(3) uiso C(405) 0.0587(6) 0.4134(4) 0.4531(2) 1.000 0.080(3) uiso C(406) -0.0210(6) 0.3597(4) 0.4122(2) 1.000 0.068(3) uiso H(402) 0.1197(6) 0.4464(4) 0.3010(2) 1.000 0.080 uiso H(403) 0.2541(6) 0.5371(4) 0.3701(2) 1.000 0.080 uiso H(404) 0.2158(6) 0.5164(4) 0.4656(2) 1.000 0.080 uiso H(405) 0.0430(6) 0.4050(4) 0.4921(2) 1.000 0.080 uiso H(406) -0.0914(6) 0.3142(4) 0.4230(2) 1.000 0.080 uiso N(1) 0.8769(8) 0.8129(6) 0.4766(3) 1.000 0.062(3) uani C(2) 1.001(1) 0.8176(7) 0.4532(4) 1.000 0.057(4) uani C(3) 1.004(1) 0.7544(7) 0.4063(4) 1.000 0.060(4) uani C(4) 0.876(1) 0.7068(8) 0.4022(4) 1.000 0.057(4) uani C(5) 0.796(1) 0.7429(7) 0.4464(4) 1.000 0.058(4) uani C(6) 0.658(1) 0.7209(8) 0.4579(4) 1.000 0.058(4) uani C(7) 0.575(1) 0.7709(8) 0.4941(4) 1.000 0.064(4) uani N(8) 1.1070(9) 0.8781(6) 0.4718(4) 1.000 0.074(4) uani H(8) 1.1724(9) 0.8934(6) 0.4494(4) 1.000 0.080 uiso C(81) 1.114(1) 0.9183(8) 0.5279(4) 1.000 0.085(5) uani H(811) 1.193(1) 0.9579(8) 0.5358(4) 1.000 0.080 uiso H(812) 1.035(1) 0.9566(8) 0.5323(4) 1.000 0.080 uiso H(813) 1.117(1) 0.8642(8) 0.5534(4) 1.000 0.080 uiso C(9) 1.115(1) 0.7461(7) 0.3701(5) 1.000 0.069(4) uani C(10) 0.838(1) 0.6345(9) 0.3616(5) 1.000 0.063(4) uani C(11) 0.591(1) 0.6379(9) 0.4298(5) 1.000 0.069(5) uani C(12) 0.436(1) 0.7359(9) 0.5013(5) 1.000 0.083(5) uani C(13) 0.616(1) 0.861(1) 0.5207(4) 1.000 0.077(5) uani N(14) 0.637(1) 0.9324(9) 0.5438(4) 1.000 0.105(5) uani N(15) 1.205(1) 0.7433(7) 0.3408(5) 1.000 0.102(5) uani N(16) 0.8096(9) 0.5754(7) 0.3269(4) 1.000 0.079(4) uani N(17) 0.536(1) 0.5735(9) 0.4071(4) 1.000 0.105(5) uani N(18) 0.323(1) 0.710(1) 0.5073(4) 1.000 0.113(5) uani loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 As(1) 0.0430(6) 0.0011(6) 0.0058(4) 0.0565(7) 0.0032(7) 0.0494(6) N(1) 0.053(5) -0.001(5) 0.008(5) 0.064(6) 0.002(5) 0.069(5) C(2) 0.054(7) 0.004(6) 0.004(6) 0.055(7) 0.007(6) 0.061(7) C(3) 0.059(7) -0.005(6) 0.004(6) 0.065(7) 0.002(6) 0.055(7) C(4) 0.052(6) -0.009(6) -0.002(5) 0.056(6) 0.005(6) 0.063(7) C(5) 0.058(7) -0.003(6) 0.002(6) 0.068(7) 0.007(5) 0.047(6) C(6) 0.052(7) -0.002(6) 0.004(5) 0.074(8) -0.002(6) 0.046(6) C(7) 0.054(7) 0.008(6) 0.014(6) 0.089(9) 0.003(6) 0.051(7) N(8) 0.080(6) -0.026(6) 0.010(5) 0.076(6) -0.012(5) 0.068(6) C(81) 0.080(8) -0.004(7) -0.002(7) 0.086(8) -0.015(7) 0.086(9) C(9) 0.072(8) -0.020(6) 0.013(7) 0.067(7) 0.006(6) 0.071(8) C(10) 0.041(6) -0.001(6) -0.003(6) 0.074(9) 0.013(7) 0.073(8) C(11) 0.055(7) 0.001(7) 0.006(6) 0.09(1) -0.010(7) 0.064(8) C(12) 0.077(9) 0.007(8) 0.011(7) 0.11(1) -0.000(7) 0.064(8) C(13) 0.081(8) 0.007(8) 0.014(6) 0.10(1) -0.017(7) 0.046(7) N(14) 0.100(8) 0.003(8) 0.020(6) 0.14(1) -0.034(7) 0.080(7) N(15) 0.080(7) -0.008(6) 0.053(7) 0.106(8) -0.004(7) 0.128(9) N(16) 0.066(6) 0.005(6) 0.001(5) 0.090(7) -0.011(6) 0.081(7) N(17) 0.079(8) -0.023(7) 0.018(6) 0.13(1) -0.037(8) 0.111(9) N(18) 0.065(7) 0.006(8) 0.025(6) 0.18(1) 0.006(8) 0.098(7) # GEOMETRY ############################################### loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) C(101) 1.876(5) . . yes As(1) C(201) 1.886(5) . . yes As(1) C(301) 1.888(5) . . yes As(1) C(401) 1.883(6) . . yes C(101) C(102) 1.395(8) . . yes C(101) C(106) 1.395(9) . . yes C(102) C(103) 1.395(7) . . yes C(102) H(102) 0.960(9) . . yes C(103) C(104) 1.395(9) . . yes C(103) H(103) 0.960(8) . . yes C(104) C(105) 1.395(8) . . yes C(104) H(104) 0.960(7) . . yes C(105) C(106) 1.395(7) . . yes C(105) H(105) 0.960(9) . . yes C(106) H(106) 0.960(8) . . yes C(201) C(202) 1.395(7) . . yes C(201) C(206) 1.395(8) . . yes C(202) C(203) 1.395(6) . . yes C(202) H(202) 0.960(8) . . yes C(203) C(204) 1.395(8) . . yes C(203) H(203) 0.960(7) . . yes C(204) C(205) 1.395(7) . . yes C(204) H(204) 0.960(6) . . yes C(205) C(206) 1.395(6) . . yes C(205) H(205) 0.960(8) . . yes C(206) H(206) 0.960(7) . . yes C(301) C(302) 1.395(8) . . yes C(301) C(306) 1.395(8) . . yes C(302) C(303) 1.395(7) . . yes C(302) H(302) 0.960(8) . . yes C(303) C(304) 1.395(8) . . yes C(303) H(303) 0.960(8) . . yes C(304) C(305) 1.395(8) . . yes C(304) H(304) 0.960(7) . . yes C(305) C(306) 1.395(7) . . yes C(305) H(305) 0.960(8) . . yes C(306) H(306) 0.960(8) . . yes C(401) C(402) 1.395(8) . . yes C(401) C(406) 1.395(7) . . yes C(402) C(403) 1.395(8) . . yes C(402) H(402) 0.960(7) . . yes C(403) C(404) 1.395(7) . . yes C(403) H(403) 0.960(8) . . yes C(404) C(405) 1.395(8) . . yes C(404) H(404) 0.960(8) . . yes C(405) C(406) 1.395(8) . . yes C(405) H(405) 0.960(7) . . yes C(406) H(406) 0.960(8) . . yes N(1) C(2) 1.34(1) . . yes N(1) C(5) 1.39(1) . . yes C(2) C(3) 1.42(1) . . yes C(2) N(8) 1.35(1) . . yes C(3) C(4) 1.37(1) . . yes C(3) C(9) 1.41(1) . . yes C(4) C(5) 1.43(1) . . yes C(4) C(10) 1.41(2) . . yes C(5) C(6) 1.39(1) . . yes C(6) C(7) 1.39(1) . . yes C(6) C(11) 1.44(2) . . yes C(7) C(12) 1.43(2) . . yes C(7) C(13) 1.42(2) . . yes N(8) H(8) 0.87(1) . . yes N(8) C(81) 1.45(1) . . yes C(81) H(811) 0.93(1) . . yes C(81) H(812) 0.93(1) . . yes C(81) H(813) 0.96(1) . . yes C(9) N(15) 1.15(1) . . yes C(10) N(16) 1.17(1) . . yes C(11) N(17) 1.14(2) . . yes C(12) N(18) 1.14(2) . . yes C(13) N(14) 1.14(2) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(201) As(1) C(101) 108.6(3) . . . yes C(301) As(1) C(101) 110.2(3) . . . yes C(301) As(1) C(201) 107.6(2) . . . yes C(401) As(1) C(101) 110.4(3) . . . yes C(401) As(1) C(201) 111.8(2) . . . yes C(401) As(1) C(301) 108.1(2) . . . yes C(102) C(101) As(1) 121.0(4) . . . yes C(106) C(101) As(1) 118.8(4) . . . yes C(106) C(101) C(102) 120.0(5) . . . yes C(103) C(102) C(101) 120.0(6) . . . yes H(102) C(102) C(101) 120.0(6) . . . yes H(102) C(102) C(103) 120.0(6) . . . yes C(104) C(103) C(102) 120.0(5) . . . yes H(103) C(103) C(102) 120.0(7) . . . yes H(103) C(103) C(104) 120.0(6) . . . yes H(104) C(104) C(105) 120.0(7) . . . yes C(103) C(104) C(105) 120.0(5) . . . yes C(103) C(104) H(104) 120.0(7) . . . yes C(104) C(105) C(106) 120.0(6) . . . yes H(105) C(105) C(106) 120.0(6) . . . yes H(105) C(105) C(104) 120.0(6) . . . yes C(105) C(106) C(101) 120.0(5) . . . yes H(106) C(106) C(101) 120.0(6) . . . yes H(106) C(106) C(105) 120.0(7) . . . yes C(202) C(201) C(206) 120.0(4) . . . yes As(1) C(201) C(206) 119.5(4) . . . yes As(1) C(201) C(202) 120.5(4) . . . yes C(201) C(202) C(203) 120.0(5) . . . yes H(202) C(202) C(203) 120.0(6) . . . yes H(202) C(202) C(201) 120.0(5) . . . yes H(203) C(203) C(202) 120.0(6) . . . yes C(204) C(203) C(202) 120.0(5) . . . yes C(204) C(203) H(203) 120.0(5) . . . yes C(205) C(204) C(203) 120.0(4) . . . yes H(204) C(204) C(203) 120.0(6) . . . yes H(204) C(204) C(205) 120.0(6) . . . yes C(206) C(205) C(204) 120.0(5) . . . yes H(205) C(205) C(204) 120.0(5) . . . yes H(205) C(205) C(206) 120.0(6) . . . yes C(205) C(206) C(201) 120.0(5) . . . yes H(206) C(206) C(201) 120.0(5) . . . yes H(206) C(206) C(205) 120.0(6) . . . yes C(306) C(301) As(1) 119.5(4) . . . yes C(302) C(301) As(1) 120.4(4) . . . yes C(302) C(301) C(306) 120.0(5) . . . yes H(302) C(302) C(301) 120.0(6) . . . yes C(303) C(302) C(301) 120.0(5) . . . yes C(303) C(302) H(302) 120.0(6) . . . yes H(303) C(303) C(302) 120.0(6) . . . yes C(304) C(303) C(302) 120.0(5) . . . yes C(304) C(303) H(303) 120.0(6) . . . yes H(304) C(304) C(303) 120.0(6) . . . yes C(305) C(304) C(303) 120.0(5) . . . yes C(305) C(304) H(304) 120.0(7) . . . yes H(305) C(305) C(304) 120.0(6) . . . yes C(306) C(305) C(304) 120.0(5) . . . yes C(306) C(305) H(305) 120.0(6) . . . yes C(305) C(306) C(301) 120.0(5) . . . yes H(306) C(306) C(301) 120.0(6) . . . yes H(306) C(306) C(305) 120.0(6) . . . yes C(402) C(401) As(1) 119.9(4) . . . yes C(406) C(401) As(1) 120.1(4) . . . yes C(406) C(401) C(402) 120.0(5) . . . yes C(403) C(402) C(401) 120.0(5) . . . yes H(402) C(402) C(401) 120.0(6) . . . yes H(402) C(402) C(403) 120.0(6) . . . yes C(404) C(403) C(402) 120.0(5) . . . yes H(403) C(403) C(402) 120.0(6) . . . yes H(403) C(403) C(404) 120.0(6) . . . yes C(405) C(404) C(403) 120.0(5) . . . yes H(404) C(404) C(403) 120.0(6) . . . yes H(404) C(404) C(405) 120.0(6) . . . yes C(406) C(405) C(404) 120.0(5) . . . yes H(405) C(405) C(404) 120.0(6) . . . yes H(405) C(405) C(406) 120.0(6) . . . yes C(405) C(406) C(401) 120.0(5) . . . yes H(406) C(406) C(401) 120.0(6) . . . yes H(406) C(406) C(405) 120.0(6) . . . yes C(5) N(1) C(2) 106.4(8) . . . yes C(3) C(2) N(1) 111.9(9) . . . yes N(8) C(2) N(1) 123.0(9) . . . yes N(8) C(2) C(3) 125.0(9) . . . yes C(4) C(3) C(2) 105.8(9) . . . yes C(9) C(3) C(2) 126.5(9) . . . yes C(9) C(3) C(4) 127(1) . . . yes C(5) C(4) C(3) 107.4(9) . . . yes C(10) C(4) C(3) 123.9(9) . . . yes C(10) C(4) C(5) 128.6(9) . . . yes C(4) C(5) N(1) 108.4(8) . . . yes C(6) C(5) N(1) 122.4(9) . . . yes C(6) C(5) C(4) 129.1(9) . . . yes C(7) C(6) C(5) 126(1) . . . yes C(11) C(6) C(5) 117.7(9) . . . yes C(11) C(6) C(7) 115.3(9) . . . yes C(6) C(7) C(13) 123.9(9) . . . yes C(12) C(7) C(13) 117.1(9) . . . yes C(12) C(7) C(6) 118(1) . . . yes C(2) N(8) C(81) 121.2(8) . . . yes H(8) N(8) C(81) 119(1) . . . yes H(8) N(8) C(2) 119(1) . . . yes H(812) C(81) N(8) 109(1) . . . yes H(811) C(81) N(8) 112(1) . . . yes H(811) C(81) H(812) 106(1) . . . yes H(813) C(81) N(8) 107(1) . . . yes H(813) C(81) H(812) 110(1) . . . yes H(813) C(81) H(811) 109(1) . . . yes N(15) C(9) C(3) 177(1) . . . yes C(4) C(10) N(16) 177(1) . . . yes C(6) C(11) N(17) 178(1) . . . yes C(7) C(12) N(18) 178(1) . . . yes N(14) C(13) C(7) 174(1) . . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? . . ? #===END data_2 # DATA SECTION OF BLOCK ################################## _chemical_name_systematic ;Tetraphenylarsonium 2-(5,5-dimethylamino-3,4-dicyano-2H-dicyano- 2H-pyrrol-2-ylidene)-1,1,2-tricyanoethanide ; _chemical_compound_source ; ; _chemical_formula_iucr ? _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum 'H26C37N7As1' _chemical_formula_weight 643.59 _chemical_melting_point ? _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ; SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79) ; _computing_structure_refinement ; SHELXTL PC Siemens Analytical X-ray Instrument, Madison, WI, 1990 ; _computing_molecular_graphics ; SHELXTL PC Siemens Analytical X-ray Instrument, Madison, WI, 1990 ; _computing_publication_material ? _cell_length_a 12.707 _cell_length_b 15.364 _cell_length_c 17.117 _cell_angle_alpha 90.000 _cell_angle_beta 104.380 _cell_angle_gamma 90.000 _cell_volume 3237.061 _cell_formula_units_Z 4 _cell_measurement_radiation 'CuK\a' _cell_measurement_wavelength 1.54178 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20 _cell_measurement_theta_max 40 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '1/2-x,1/2+y,1/2-z' _exptl_crystal_description 'exagonal platelets' _exptl_crystal_colour 'bronze metallic luster' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.856 _exptl_absorpt_correction_type 'semiempirical via \y scans' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_detector ? _diffrn_measurement_device 'MSC-AFC5 Diffractometer' _diffrn_measurement_method '\q-2\q scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time no _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_reduction_process ? _diffrn_reflns_number ? _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 62.11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'h ' 104 'Hydrogen ' 0.0000 0.0000 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'c ' 148 'Carbon ' 0.0170 0.0090 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'n ' 28 'Nitrogen ' 0.0290 0.0180 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'as ' 4 'Arsenic ' -1.0110 1.0060 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _reflns_number_total 5319 _reflns_number_observed 3845 _reflns_observed_criterion 'Fo > 8.0 \s(Fo)' _reflns_limit_h_max 14 _reflns_limit_h_min 0 _reflns_limit_k_max 17 _reflns_limit_k_min 0 _reflns_limit_l_max 19 _reflns_limit_l_min -19 _reflns_d_resolution_high 0.872 _reflns_d_resolution_low 16.581 _refine_ls_structure_factor_coef 'F' _refine_ls_extinction_method 'none' _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? _refine_ls_abs_structure_details ; ; _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment 'H atoms rigid to parent C atom' _refine_ls_weighting_scheme 'W=1/(\s^2(Fo)+0.008Fo^2)' _refine_ls_number_reflns 3845 _refine_ls_number_parameters 358 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_obs 0.0647 _refine_ls_wR_factor_all 0.1129 _refine_ls_wR_factor_obs 0.0874 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.92 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.62 _refine_diff_density_min -0.65 _refine_diff_density_rms ? loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type As(1) 0.22160(3) -0.05778(3) 0.12577(2) 1.000 0.0464(2) uani N(1) -0.0731(3) -0.0404(2) 0.3644(2) 1.000 0.058(1) uani C(2) -0.0728(4) 0.0428(3) 0.3837(3) 1.000 0.060(2) uani C(3) 0.0344(5) 0.0725(3) 0.4201(3) 1.000 0.064(2) uani C(4) 0.1032(4) -0.0002(3) 0.4225(3) 1.000 0.060(2) uani C(5) 0.0315(4) -0.0694(3) 0.3870(3) 1.000 0.056(2) uani C(6) 0.0577(4) -0.1549(3) 0.3744(3) 1.000 0.057(2) uani C(7) -0.0145(4) -0.2215(3) 0.3425(3) 1.000 0.063(2) uani N(8) -0.1657(4) 0.0893(3) 0.3655(3) 1.000 0.078(2) uani C(81) -0.1742(7) 0.1774(4) 0.3911(5) 1.000 0.103(3) uani H(811) -0.1018(7) 0.1954(4) 0.4168(5) 1.000 0.080 uiso H(812) -0.2034(7) 0.2149(4) 0.3462(5) 1.000 0.080 uiso H(813) -0.2187(7) 0.1807(4) 0.4289(5) 1.000 0.080 uiso C(82) -0.2638(5) 0.0508(4) 0.3215(5) 1.000 0.088(3) uani H(821) -0.2479(5) -0.0072(4) 0.3072(5) 1.000 0.080 uiso H(822) -0.3125(5) 0.0485(4) 0.3564(5) 1.000 0.080 uiso H(823) -0.2971(5) 0.0827(4) 0.2737(5) 1.000 0.080 uiso C(9) 0.0734(6) 0.1564(4) 0.4475(4) 1.000 0.087(3) uani C(10) 0.2175(5) -0.0018(4) 0.4562(3) 1.000 0.076(2) uani C(11) 0.1699(4) -0.1836(3) 0.3946(3) 1.000 0.067(2) uani C(12) 0.0248(4) -0.3078(3) 0.3344(3) 1.000 0.068(2) uani C(13) -0.1291(5) -0.2121(4) 0.3152(4) 1.000 0.093(3) uani N(14) -0.2203(5) -0.2149(4) 0.2919(6) 1.000 0.158(4) uani N(15) 0.1066(7) 0.2238(4) 0.4678(4) 1.000 0.128(3) uani N(16) 0.3070(5) 0.0008(4) 0.4846(4) 1.000 0.102(3) uani N(17) 0.2577(4) -0.2070(3) 0.4077(4) 1.000 0.097(2) uani N(18) 0.0542(4) -0.3767(3) 0.3275(4) 1.000 0.092(2) uani C(101) 0.1280(2) 0.0196(2) 0.1633(2) 1.000 0.053(1) uani C(102) 0.0231(2) -0.0068(2) 0.1637(2) 1.000 0.063(2) uani C(103) -0.0471(2) 0.0510(2) 0.1883(2) 1.000 0.075(2) uani C(104) -0.0124(2) 0.1352(2) 0.2124(2) 1.000 0.076(2) uani C(105) 0.0925(2) 0.1616(2) 0.2119(2) 1.000 0.078(2) uani C(106) 0.1627(2) 0.1038(2) 0.1873(2) 1.000 0.062(2) uani H(102) -0.0007(2) -0.0647(2) 0.1472(2) 1.000 0.080 uiso H(103) -0.1192(2) 0.0328(2) 0.1886(2) 1.000 0.080 uiso H(104) -0.0607(2) 0.1749(2) 0.2292(2) 1.000 0.080 uiso H(105) 0.1164(2) 0.2195(2) 0.2284(2) 1.000 0.080 uiso H(106) 0.2349(2) 0.1220(2) 0.1870(2) 1.000 0.080 uiso C(201) 0.2549(3) -0.0107(2) 0.0324(2) 1.000 0.052(1) uani C(202) 0.2189(3) 0.0727(2) 0.0065(2) 1.000 0.076(2) uani C(203) 0.2457(3) 0.1088(2) -0.0608(2) 1.000 0.104(3) uani C(204) 0.3085(3) 0.0615(2) -0.1022(2) 1.000 0.105(3) uani C(205) 0.3445(3) -0.0219(2) -0.0763(2) 1.000 0.112(3) uani C(206) 0.3177(3) -0.0580(2) -0.0090(2) 1.000 0.086(2) uani H(202) 0.1757(3) 0.1052(2) 0.0350(2) 1.000 0.080 uiso H(203) 0.2209(3) 0.1661(2) -0.0787(2) 1.000 0.080 uiso H(204) 0.3269(3) 0.0863(2) -0.1486(2) 1.000 0.080 uiso H(205) 0.3877(3) -0.0544(2) -0.1048(2) 1.000 0.080 uiso H(206) 0.3425(3) -0.1153(2) 0.0089(2) 1.000 0.080 uiso C(301) 0.1466(2) -0.1643(2) 0.0979(2) 1.000 0.050(1) uani C(302) 0.0820(2) -0.1760(2) 0.0199(2) 1.000 0.065(2) uani C(303) 0.0185(2) -0.2507(2) 0.0007(2) 1.000 0.076(2) uani C(304) 0.0197(2) -0.3138(2) 0.0595(2) 1.000 0.079(2) uani C(305) 0.0843(2) -0.3022(2) 0.1375(2) 1.000 0.090(2) uani C(306) 0.1478(2) -0.2274(2) 0.1568(2) 1.000 0.070(2) uani H(302) 0.0812(2) -0.1326(2) -0.0206(2) 1.000 0.080 uiso H(303) -0.0260(2) -0.2587(2) -0.0530(2) 1.000 0.080 uiso H(304) -0.0240(2) -0.3653(2) 0.0463(2) 1.000 0.080 uiso H(305) 0.0851(2) -0.3456(2) 0.1780(2) 1.000 0.080 uiso H(306) 0.1923(2) -0.2194(2) 0.2105(2) 1.000 0.080 uiso C(401) 0.3477(2) -0.0778(2) 0.2099(1) 1.000 0.049(1) uani C(402) 0.3521(2) -0.0505(2) 0.2883(1) 1.000 0.066(2) uani C(403) 0.4458(2) -0.0647(2) 0.3496(1) 1.000 0.081(2) uani C(404) 0.5351(2) -0.1062(2) 0.3325(1) 1.000 0.076(2) uani C(405) 0.5308(2) -0.1334(2) 0.2540(1) 1.000 0.071(2) uani C(406) 0.4371(2) -0.1193(2) 0.1927(1) 1.000 0.062(2) uani H(402) 0.2906(2) -0.0220(2) 0.3001(1) 1.000 0.080 uiso H(403) 0.4488(2) -0.0460(2) 0.4037(1) 1.000 0.080 uiso H(404) 0.5996(2) -0.1159(2) 0.3747(1) 1.000 0.080 uiso H(405) 0.5922(2) -0.1620(2) 0.2422(1) 1.000 0.080 uiso H(406) 0.4341(2) -0.1380(2) 0.1387(1) 1.000 0.080 uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 As(1) 0.0467(3) 0.0003(2) 0.0106(2) 0.0427(4) 0.0024(2) 0.0492(3) N(1) 0.062(2) 0.001(2) 0.016(2) 0.049(2) 0.000(2) 0.063(2) C(2) 0.080(3) 0.008(2) 0.022(2) 0.049(2) 0.006(2) 0.056(3) C(3) 0.093(4) -0.004(2) 0.021(2) 0.048(2) -0.000(2) 0.053(3) C(4) 0.067(3) -0.004(2) 0.011(2) 0.061(3) 0.004(2) 0.051(2) C(5) 0.069(3) 0.003(2) 0.017(2) 0.051(2) 0.003(2) 0.049(2) C(6) 0.057(3) 0.007(2) 0.012(2) 0.059(3) 0.006(2) 0.055(2) C(7) 0.059(3) 0.011(2) 0.009(2) 0.057(3) -0.006(2) 0.068(3) N(8) 0.086(3) 0.013(2) 0.028(3) 0.053(2) -0.005(2) 0.098(3) C(81) 0.142(6) 0.037(4) 0.035(4) 0.063(3) 0.003(3) 0.106(4) C(82) 0.073(4) 0.020(3) 0.022(3) 0.084(4) -0.001(3) 0.106(5) C(9) 0.124(5) -0.018(3) 0.029(3) 0.059(3) -0.002(3) 0.080(3) C(10) 0.081(4) -0.019(3) 0.016(3) 0.080(4) -0.013(3) 0.066(3) C(11) 0.056(3) 0.001(2) 0.010(2) 0.063(3) 0.006(2) 0.079(3) C(12) 0.063(3) 0.004(2) 0.012(2) 0.054(3) -0.008(2) 0.084(3) C(13) 0.063(3) 0.010(3) -0.012(3) 0.067(3) -0.037(3) 0.129(5) N(14) 0.067(4) 0.015(3) -0.027(5) 0.109(5) -0.073(6) 0.26(1) N(15) 0.167(6) -0.034(4) 0.022(4) 0.069(3) -0.020(4) 0.138(5) N(16) 0.070(3) -0.022(3) 0.012(3) 0.125(5) -0.026(3) 0.105(4) N(17) 0.055(3) 0.008(2) 0.014(3) 0.080(3) 0.008(3) 0.150(5) N(18) 0.085(3) 0.016(2) 0.021(3) 0.063(3) -0.004(3) 0.125(4) C(101) 0.049(2) 0.001(2) 0.012(2) 0.060(2) 0.005(2) 0.049(2) C(102) 0.054(3) -0.003(2) 0.016(2) 0.069(3) 0.002(2) 0.066(3) C(103) 0.058(3) 0.002(3) 0.031(3) 0.096(4) 0.001(3) 0.078(3) C(104) 0.078(4) 0.017(3) 0.030(3) 0.079(3) -0.006(3) 0.076(3) C(105) 0.086(4) 0.005(3) 0.033(3) 0.063(3) -0.018(3) 0.091(3) C(106) 0.055(3) -0.002(2) 0.018(2) 0.053(3) -0.013(2) 0.079(3) C(201) 0.053(2) -0.006(2) 0.015(2) 0.058(3) 0.002(2) 0.047(2) C(202) 0.116(5) -0.014(3) 0.027(3) 0.051(3) 0.009(2) 0.064(3) C(203) 0.158(7) -0.031(4) 0.049(5) 0.062(3) 0.014(3) 0.101(4) C(204) 0.111(5) -0.032(4) 0.044(4) 0.124(6) 0.021(4) 0.090(4) C(205) 0.096(5) 0.018(5) 0.047(4) 0.171(7) 0.008(5) 0.083(4) C(206) 0.082(4) 0.033(3) 0.029(3) 0.111(5) 0.011(3) 0.071(3) C(301) 0.051(2) -0.005(2) 0.008(2) 0.040(2) -0.002(2) 0.056(2) C(302) 0.075(3) -0.003(2) 0.003(2) 0.057(3) 0.002(2) 0.057(3) C(303) 0.074(3) -0.009(3) -0.003(2) 0.071(3) -0.011(3) 0.070(3) C(304) 0.073(3) -0.023(3) 0.009(3) 0.062(3) -0.008(3) 0.095(4) C(305) 0.115(5) -0.025(3) 0.013(3) 0.067(3) 0.016(3) 0.081(4) C(306) 0.090(4) -0.012(2) 0.004(2) 0.050(3) 0.007(2) 0.061(3) C(401) 0.049(2) -0.009(2) 0.009(2) 0.040(2) 0.009(2) 0.057(2) C(402) 0.069(3) 0.012(2) 0.007(2) 0.069(3) 0.003(2) 0.055(3) C(403) 0.090(4) -0.003(3) 0.001(3) 0.084(4) 0.001(2) 0.059(3) C(404) 0.060(3) -0.012(3) -0.007(3) 0.073(3) 0.019(3) 0.081(3) C(405) 0.051(3) 0.000(2) 0.017(2) 0.077(3) 0.014(3) 0.085(3) C(406) 0.058(3) -0.005(2) 0.016(2) 0.068(3) 0.002(2) 0.061(3) # GEOMETRY ############################################### loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) C(101) 1.902(2) . . yes As(1) C(201) 1.895(3) . . yes As(1) C(301) 1.895(3) . . yes As(1) C(401) 1.894(3) . . yes N(1) C(2) 1.321(6) . . yes N(1) C(5) 1.363(7) . . yes C(2) C(3) 1.424(9) . . yes C(2) N(8) 1.349(8) . . yes C(3) C(4) 1.413(7) . . yes C(3) C(9) 1.418(8) . . yes C(4) C(5) 1.434(7) . . yes C(4) C(10) 1.423(9) . . yes C(5) C(6) 1.385(6) . . yes C(6) C(7) 1.391(7) . . yes C(6) C(11) 1.450(7) . . yes C(7) C(12) 1.437(7) . . yes C(7) C(13) 1.421(9) . . yes N(8) C(81) 1.435(7) . . yes N(8) C(82) 1.416(9) . . yes C(81) H(811) 0.96(1) . . yes C(81) H(812) 0.96(1) . . yes C(81) H(813) 0.96(1) . . yes C(82) H(821) 0.959(8) . . yes C(82) H(822) 0.961(9) . . yes C(82) H(823) 0.96(1) . . yes C(9) N(15) 1.140(9) . . yes C(10) N(16) 1.12(1) . . yes C(11) N(17) 1.140(8) . . yes C(12) N(18) 1.138(7) . . yes C(13) N(14) 1.13(1) . . yes C(101) C(102) 1.395(4) . . yes C(101) C(106) 1.395(4) . . yes C(102) C(103) 1.395(3) . . yes C(102) H(102) 0.960(4) . . yes C(103) C(104) 1.395(4) . . yes C(103) H(103) 0.960(4) . . yes C(104) C(105) 1.395(4) . . yes C(104) H(104) 0.960(3) . . yes C(105) C(106) 1.395(3) . . yes C(105) H(105) 0.960(4) . . yes C(106) H(106) 0.960(4) . . yes C(201) C(202) 1.395(4) . . yes C(201) C(206) 1.395(4) . . yes C(202) C(203) 1.395(4) . . yes C(202) H(202) 0.960(4) . . yes C(203) C(204) 1.395(4) . . yes C(203) H(203) 0.960(4) . . yes C(204) C(205) 1.395(4) . . yes C(204) H(204) 0.960(4) . . yes C(205) C(206) 1.395(4) . . yes C(205) H(205) 0.960(4) . . yes C(206) H(206) 0.960(4) . . yes C(301) C(302) 1.395(4) . . yes C(301) C(306) 1.395(4) . . yes C(302) C(303) 1.395(4) . . yes C(302) H(302) 0.960(4) . . yes C(303) C(304) 1.395(4) . . yes C(303) H(303) 0.960(4) . . yes C(304) C(305) 1.395(4) . . yes C(304) H(304) 0.960(4) . . yes C(305) C(306) 1.395(4) . . yes C(305) H(305) 0.960(4) . . yes C(306) H(306) 0.960(4) . . yes C(401) C(402) 1.395(3) . . yes C(401) C(406) 1.395(3) . . yes C(402) C(403) 1.395(4) . . yes C(402) H(402) 0.960(3) . . yes C(403) C(404) 1.395(3) . . yes C(403) H(403) 0.960(3) . . yes C(404) C(405) 1.395(3) . . yes C(404) H(404) 0.960(4) . . yes C(405) C(406) 1.395(4) . . yes C(405) H(405) 0.960(3) . . yes C(406) H(406) 0.960(3) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(301) As(1) C(101) 107.9(1) . . . yes C(201) As(1) C(101) 109.6(1) . . . yes C(201) As(1) C(301) 108.8(1) . . . yes C(401) As(1) C(101) 109.1(1) . . . yes C(401) As(1) C(301) 109.2(1) . . . yes C(401) As(1) C(201) 112.2(1) . . . yes C(5) N(1) C(2) 107.6(4) . . . yes N(8) C(2) C(3) 128.3(4) . . . yes N(1) C(2) C(3) 111.2(5) . . . yes N(1) C(2) N(8) 120.4(5) . . . yes C(4) C(3) C(2) 106.2(4) . . . yes C(9) C(3) C(2) 130.8(5) . . . yes C(9) C(3) C(4) 123.0(6) . . . yes C(3) C(4) C(5) 104.4(5) . . . yes C(10) C(4) C(5) 129.5(5) . . . yes C(10) C(4) C(3) 126.0(5) . . . yes C(6) C(5) C(4) 128.1(5) . . . yes N(1) C(5) C(4) 110.5(4) . . . yes N(1) C(5) C(6) 121.4(5) . . . yes C(7) C(6) C(11) 112.5(4) . . . yes C(5) C(6) C(11) 120.8(5) . . . yes C(5) C(6) C(7) 126.6(5) . . . yes C(13) C(7) C(12) 114.4(5) . . . yes C(6) C(7) C(12) 120.4(5) . . . yes C(6) C(7) C(13) 125.2(5) . . . yes C(2) N(8) C(81) 123.8(6) . . . yes C(82) N(8) C(81) 115.7(6) . . . yes C(82) N(8) C(2) 120.5(4) . . . yes H(813) C(81) H(812) 109(1) . . . yes H(811) C(81) H(812) 109.3(9) . . . yes H(811) C(81) H(813) 109(1) . . . yes N(8) C(81) H(812) 111.4(8) . . . yes N(8) C(81) H(813) 110.9(6) . . . yes N(8) C(81) H(811) 106.0(8) . . . yes H(822) C(82) H(821) 109.5(8) . . . yes H(823) C(82) H(821) 109(1) . . . yes H(823) C(82) H(822) 109.5(9) . . . yes N(8) C(82) H(821) 108.0(7) . . . yes N(8) C(82) H(822) 107.6(8) . . . yes N(8) C(82) H(823) 112.6(6) . . . yes C(3) C(9) N(15) 178.0(7) . . . yes N(16) C(10) C(4) 176.5(6) . . . yes N(17) C(11) C(6) 177.6(6) . . . yes C(7) C(12) N(18) 178.9(6) . . . yes C(7) C(13) N(14) 171.9(7) . . . yes C(106) C(101) C(102) 120.0(2) . . . yes As(1) C(101) C(102) 119.9(2) . . . yes As(1) C(101) C(106) 120.1(2) . . . yes C(103) C(102) C(101) 120.0(2) . . . yes H(102) C(102) C(101) 120.0(3) . . . yes H(102) C(102) C(103) 120.0(3) . . . yes H(103) C(103) C(104) 120.0(3) . . . yes C(102) C(103) C(104) 120.0(2) . . . yes C(102) C(103) H(103) 120.0(3) . . . yes H(104) C(104) C(105) 120.0(3) . . . yes C(103) C(104) C(105) 120.0(2) . . . yes C(103) C(104) H(104) 120.0(3) . . . yes C(106) C(105) C(104) 120.0(2) . . . yes H(105) C(105) C(104) 120.0(3) . . . yes H(105) C(105) C(106) 120.0(3) . . . yes C(105) C(106) C(101) 120.0(2) . . . yes H(106) C(106) C(101) 120.0(3) . . . yes H(106) C(106) C(105) 120.0(3) . . . yes As(1) C(201) C(202) 119.6(2) . . . yes C(206) C(201) C(202) 120.0(3) . . . yes C(206) C(201) As(1) 120.3(2) . . . yes H(202) C(202) C(203) 120.0(3) . . . yes C(201) C(202) C(203) 120.0(3) . . . yes C(201) C(202) H(202) 120.0(3) . . . yes H(203) C(203) C(202) 120.0(3) . . . yes C(204) C(203) C(202) 120.0(3) . . . yes C(204) C(203) H(203) 120.0(3) . . . yes C(205) C(204) C(203) 120.0(3) . . . yes H(204) C(204) C(203) 120.0(3) . . . yes H(204) C(204) C(205) 120.0(3) . . . yes C(204) C(205) C(206) 120.0(3) . . . yes H(205) C(205) C(206) 120.0(3) . . . yes H(205) C(205) C(204) 120.0(3) . . . yes C(201) C(206) C(205) 120.0(3) . . . yes H(206) C(206) C(205) 120.0(3) . . . yes H(206) C(206) C(201) 120.0(3) . . . yes C(306) C(301) As(1) 120.3(2) . . . yes C(302) C(301) As(1) 119.4(2) . . . yes C(302) C(301) C(306) 120.0(2) . . . yes C(303) C(302) C(301) 120.0(2) . . . yes H(302) C(302) C(301) 120.0(3) . . . yes H(302) C(302) C(303) 120.0(4) . . . yes C(304) C(303) C(302) 120.0(3) . . . yes H(303) C(303) C(302) 120.0(3) . . . yes H(303) C(303) C(304) 120.0(3) . . . yes C(303) C(304) C(305) 120.0(2) . . . yes H(304) C(304) C(305) 120.0(3) . . . yes H(304) C(304) C(303) 120.0(3) . . . yes C(306) C(305) C(304) 120.0(2) . . . yes H(305) C(305) C(304) 120.0(3) . . . yes H(305) C(305) C(306) 120.0(4) . . . yes C(305) C(306) C(301) 120.0(3) . . . yes H(306) C(306) C(301) 120.0(3) . . . yes H(306) C(306) C(305) 120.0(3) . . . yes C(402) C(401) As(1) 120.4(2) . . . yes C(406) C(401) As(1) 119.6(2) . . . yes C(406) C(401) C(402) 120.0(2) . . . yes H(402) C(402) C(401) 120.0(3) . . . yes C(403) C(402) C(401) 120.0(2) . . . yes C(403) C(402) H(402) 120.0(3) . . . yes C(402) C(403) C(404) 120.0(2) . . . yes H(403) C(403) C(404) 120.0(3) . . . yes H(403) C(403) C(402) 120.0(3) . . . yes C(403) C(404) C(405) 120.0(2) . . . yes H(404) C(404) C(405) 120.0(3) . . . yes H(404) C(404) C(403) 120.0(3) . . . yes C(404) C(405) C(406) 120.0(2) . . . yes H(405) C(405) C(406) 120.0(3) . . . yes H(405) C(405) C(404) 120.0(3) . . . yes H(406) C(406) C(401) 120.0(3) . . . yes C(405) C(406) C(401) 120.0(2) . . . yes C(405) C(406) H(406) 120.0(3) . . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? . . ? #===END data_3 # DATA SECTION OF BLOCK ################################## _chemical_name_systematic ;Tetraphenylarsonium 2-(5-dimethylformamidinoamino-3,4-dicyano-2H-dicyano- 2H-pyrrol-2-ylidene)-1,1,2-tricyanoethanide ; _chemical_compound_source ; ; _chemical_formula_iucr ? _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum 'H27C38N8As1' _chemical_formula_weight 670.61 _chemical_melting_point ? _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)' _computing_structure_refinement ; SHELXTL PC Siemens Analytical X-ray Instrument, Madison, WI, 1990 ; _computing_molecular_graphics ? _computing_publication_material ? _cell_length_a 9.557 _cell_length_b 13.607 _cell_length_c 25.454 _cell_angle_alpha 90.000 _cell_angle_beta 92.350 _cell_angle_gamma 90.000 _cell_volume 3307.308 _cell_formula_units_Z 4 _cell_measurement_radiation 'CuK\a' _cell_measurement_wavelength 1.54178 _cell_measurement_temperature 293 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '1/2-x,1/2+y,1/2-z' _exptl_crystal_description 'needle-like' _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.849 _exptl_absorpt_correction_type 'semiempirical via \y scans' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_detector ? _diffrn_measurement_device 'MSC-AFC5 Diffractometer' _diffrn_measurement_method '\q-2\q scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_reduction_process ? _diffrn_reflns_number ? _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 62.10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min 0 loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'h ' 108 'Hydrogen ' 0.0000 0.0000 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'c ' 152 'Carbon ' 0.0170 0.0090 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'n ' 32 'Nitrogen ' 0.0290 0.0180 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'as ' 4 'Arsenic ' -1.0110 1.0060 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _reflns_number_total 5944 _reflns_number_observed 3004 _reflns_observed_criterion 'Fo > 6.0\s(Fo)' _reflns_limit_h_max 10 _reflns_limit_h_min -10 _reflns_limit_k_max 15 _reflns_limit_k_min 0 _reflns_limit_l_max 29 _reflns_limit_l_min 0 _reflns_d_resolution_high 0.872 _reflns_d_resolution_low 12.716 _refine_ls_structure_factor_coef 'F' _refine_ls_extinction_method 'none' _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? _refine_ls_abs_structure_details ; ; _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment 'H atoms rigid to parent C atom' _refine_ls_weighting_scheme 'W=1/(\s^2(Fo)+0.009Fo^2)' _refine_ls_number_reflns 3004 _refine_ls_number_parameters 304 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.068 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.107 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1. _refine_ls_shift/esd_max 0.175 _refine_ls_shift/esd_mean 0.039 _refine_diff_density_max 0.61 _refine_diff_density_min 0.00 _refine_diff_density_rms ? loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type N(1) 0.3879(7) 0.2659(5) -0.0513(2) 1.000 0.053(2) uani C(2) 0.5052(8) 0.2547(7) -0.0782(3) 1.000 0.053(3) uani C(3) 0.5003(7) 0.3138(6) -0.1233(3) 1.000 0.049(3) uani C(4) 0.3714(7) 0.3637(6) -0.1239(3) 1.000 0.047(2) uani C(5) 0.3066(7) 0.3313(6) -0.0787(3) 1.000 0.050(3) uani C(6) 0.1723(7) 0.3562(6) -0.0603(3) 1.000 0.052(3) uani C(7) 0.1103(9) 0.3172(7) -0.0168(4) 1.000 0.059(3) uani N(8) 0.6201(7) 0.1984(5) -0.0625(3) 1.000 0.055(2) uani C(9) 0.6022(9) 0.3204(7) -0.1623(4) 1.000 0.061(3) uani C(10) 0.3273(8) 0.4326(6) -0.1618(3) 1.000 0.052(3) uani C(11) 0.0893(8) 0.4240(7) -0.0923(3) 1.000 0.054(3) uani C(12) -0.0246(9) 0.3509(8) -0.0024(4) 1.000 0.070(3) uani C(13) 0.173(1) 0.2416(8) 0.0147(4) 1.000 0.068(3) uani N(14) 0.210(1) 0.1801(8) 0.0421(4) 1.000 0.091(4) uani N(15) 0.6816(9) 0.3249(7) -0.1943(4) 1.000 0.094(4) uani N(16) 0.2942(7) 0.4884(6) -0.1943(3) 1.000 0.066(3) uani N(17) 0.0193(8) 0.4763(7) -0.1173(4) 1.000 0.082(3) uani N(18) -0.1341(9) 0.3745(8) 0.0083(4) 1.000 0.104(4) uani C(19) 0.6085(9) 0.1489(8) -0.0196(4) 1.000 0.066(3) uani H(19) 0.5204(9) 0.1505(8) -0.0028(4) 1.000 0.080 uiso N(20) 0.7110(8) 0.0948(7) 0.0020(3) 1.000 0.079(3) uani C(21) 0.691(1) 0.036(1) 0.0471(5) 1.000 0.126(7) uani H(211) 0.598(1) 0.047(1) 0.0589(5) 1.000 0.080 uiso H(212) 0.701(1) -0.032(1) 0.0379(5) 1.000 0.080 uiso H(213) 0.758(1) 0.053(1) 0.0748(5) 1.000 0.080 uiso C(22) 0.8467(9) 0.091(1) -0.0199(5) 1.000 0.093(5) uani H(221) 0.8478(9) 0.135(1) -0.0495(5) 1.000 0.080 uiso H(222) 0.9190(9) 0.110(1) 0.0054(5) 1.000 0.080 uiso H(223) 0.8626(9) 0.025(1) -0.0314(5) 1.000 0.080 uiso As(1) 0.5996(1) 0.2442(1) 0.19597(3) 1.000 0.0443(3) uani C(101) 0.7897(8) 0.2190(6) 0.1787(3) 1.000 0.049(2) uiso C(102) 0.8465(9) 0.1295(7) 0.1913(4) 1.000 0.061(2) uiso H(102) 0.7915(9) 0.0788(7) 0.2066(4) 1.000 0.080 uiso C(103) 0.988(1) 0.1144(8) 0.1829(4) 1.000 0.075(3) uiso H(103) 1.030(1) 0.0522(8) 0.1919(4) 1.000 0.080 uiso C(104) 1.064(1) 0.1863(7) 0.1608(4) 1.000 0.073(3) uiso H(104) 1.161(1) 0.1747(7) 0.1544(4) 1.000 0.080 uiso C(105) 1.007(1) 0.2744(7) 0.1479(4) 1.000 0.070(2) uiso H(105) 1.062(1) 0.3250(7) 0.1326(4) 1.000 0.080 uiso C(106) 0.8664(9) 0.2948(7) 0.1576(4) 1.000 0.061(2) uiso H(106) 0.8246(9) 0.3571(7) 0.1487(4) 1.000 0.080 uiso C(201) 0.5083(8) 0.3295(6) 0.1460(3) 1.000 0.050(2) uiso C(202) 0.556(1) 0.3350(7) 0.0951(4) 1.000 0.067(2) uiso H(202) 0.635(1) 0.2974(7) 0.0850(4) 1.000 0.080 uiso C(203) 0.484(1) 0.3963(9) 0.0591(5) 1.000 0.093(3) uiso H(203) 0.516(1) 0.4007(9) 0.0239(5) 1.000 0.080 uiso C(204) 0.372(1) 0.4497(9) 0.0747(4) 1.000 0.082(3) uiso H(204) 0.324(1) 0.4917(9) 0.0495(4) 1.000 0.080 uiso C(205) 0.327(1) 0.4442(8) 0.1238(4) 1.000 0.079(3) uiso H(205) 0.248(1) 0.4818(8) 0.1338(4) 1.000 0.080 uiso C(206) 0.3949(9) 0.3839(7) 0.1607(4) 1.000 0.067(2) uiso H(206) 0.3631(9) 0.3796(7) 0.1959(4) 1.000 0.080 uiso C(301) 0.5002(8) 0.1229(6) 0.1949(3) 1.000 0.050(2) uiso C(302) 0.4288(9) 0.0948(7) 0.1479(4) 1.000 0.062(2) uiso H(302) 0.4275(9) 0.1368(7) 0.1176(4) 1.000 0.080 uiso C(303) 0.366(1) 0.0048(9) 0.1469(5) 1.000 0.085(3) uiso H(303) 0.318(1) -0.0157(9) 0.1148(5) 1.000 0.080 uiso C(304) 0.369(1) -0.0536(9) 0.1894(4) 1.000 0.082(3) uiso H(304) 0.323(1) -0.1160(9) 0.1877(4) 1.000 0.080 uiso C(305) 0.434(1) -0.0266(8) 0.2352(4) 1.000 0.077(3) uiso H(305) 0.435(1) -0.0685(8) 0.2655(4) 1.000 0.080 uiso C(306) 0.5017(9) 0.0635(7) 0.2386(4) 1.000 0.068(2) uiso H(306) 0.5497(9) 0.0840(7) 0.2706(4) 1.000 0.080 uiso C(401) 0.6002(8) 0.2949(6) 0.2661(3) 1.000 0.046(2) uiso C(402) 0.4814(8) 0.2819(6) 0.2955(3) 1.000 0.053(2) uiso H(402) 0.3985(8) 0.2521(6) 0.2800(3) 1.000 0.080 uiso C(403) 0.483(1) 0.3146(7) 0.3466(4) 1.000 0.066(2) uiso H(403) 0.402(1) 0.3068(7) 0.3670(4) 1.000 0.080 uiso C(404) 0.6026(9) 0.3564(7) 0.3693(4) 1.000 0.065(2) uiso H(404) 0.6039(9) 0.3784(7) 0.4052(4) 1.000 0.080 uiso C(405) 0.7205(9) 0.3683(6) 0.3393(3) 1.000 0.058(2) uiso H(405) 0.8033(9) 0.3981(6) 0.3548(3) 1.000 0.080 uiso C(406) 0.7187(8) 0.3362(6) 0.2883(3) 1.000 0.048(2) uiso H(406) 0.8003(8) 0.3440(6) 0.2679(3) 1.000 0.080 uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 N(1) 0.046(3) 0.013(3) 0.002(3) 0.067(5) 0.002(3) 0.045(3) C(2) 0.046(4) 0.004(4) 0.001(3) 0.064(5) -0.012(5) 0.049(4) C(3) 0.040(4) 0.010(3) 0.007(3) 0.054(5) 0.006(4) 0.054(5) C(4) 0.045(4) 0.007(3) 0.003(3) 0.044(4) -0.005(4) 0.052(5) C(5) 0.039(4) 0.010(3) 0.008(4) 0.042(4) -0.006(4) 0.069(6) C(6) 0.040(4) 0.009(3) 0.002(4) 0.055(5) -0.011(4) 0.061(5) C(7) 0.052(5) 0.014(4) 0.010(4) 0.069(6) -0.003(4) 0.057(5) N(8) 0.047(4) 0.014(3) 0.001(3) 0.065(4) -0.001(4) 0.052(4) C(9) 0.048(5) 0.016(4) 0.014(4) 0.064(6) 0.005(4) 0.072(6) C(10) 0.040(4) 0.004(4) 0.009(4) 0.058(5) -0.004(4) 0.058(5) C(11) 0.046(4) 0.009(4) 0.011(4) 0.063(5) -0.011(4) 0.054(5) C(12) 0.056(5) 0.009(5) 0.019(4) 0.083(7) -0.011(5) 0.070(6) C(13) 0.065(6) 0.007(5) 0.018(4) 0.078(7) 0.003(6) 0.062(6) N(14) 0.096(7) 0.021(6) 0.026(5) 0.102(7) 0.027(6) 0.077(6) N(15) 0.079(6) 0.026(5) 0.042(5) 0.094(7) 0.028(6) 0.111(8) N(16) 0.057(4) 0.010(4) 0.003(4) 0.073(5) 0.014(4) 0.068(5) N(17) 0.052(4) 0.029(4) 0.012(4) 0.093(6) 0.015(5) 0.103(7) N(18) 0.072(6) 0.029(6) 0.027(5) 0.134(9) 0.005(7) 0.107(8) C(19) 0.060(5) 0.030(5) 0.011(4) 0.086(7) -0.002(5) 0.053(5) N(20) 0.069(5) 0.041(5) 0.010(4) 0.104(7) 0.016(5) 0.067(5) C(21) 0.13(1) 0.08(1) 0.038(8) 0.16(1) 0.037(9) 0.091(9) C(22) 0.044(5) 0.016(6) 0.004(5) 0.12(1) 0.014(8) 0.113(9) As(1) 0.0357(5) -0.0011(4) 0.0080(3) 0.0500(6) -0.0028(4) 0.0478(3) # GEOMETRY ############################################### loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) C(101) 1.917(8) . . yes As(1) C(201) 1.908(8) . . yes As(1) C(301) 1.903(8) . . yes As(1) C(401) 1.913(7) . . yes C(101) C(102) 1.37(1) . . yes C(101) C(106) 1.39(1) . . yes C(102) H(102) 0.96(1) . . yes C(102) C(103) 1.39(1) . . yes C(103) H(103) 0.96(2) . . yes C(103) C(104) 1.36(1) . . yes C(104) H(104) 0.96(1) . . yes C(104) C(105) 1.35(1) . . yes C(105) H(105) 0.96(1) . . yes C(105) C(106) 1.40(1) . . yes C(106) H(106) 0.96(1) . . yes C(201) C(202) 1.39(1) . . yes C(201) C(206) 1.38(1) . . yes C(202) H(202) 0.96(1) . . yes C(202) C(203) 1.40(2) . . yes C(203) H(203) 0.96(2) . . yes C(203) C(204) 1.37(2) . . yes C(204) H(204) 0.96(2) . . yes C(204) C(205) 1.34(1) . . yes C(205) H(205) 0.96(1) . . yes C(205) C(206) 1.39(1) . . yes C(206) H(206) 0.96(1) . . yes C(301) C(302) 1.41(1) . . yes C(301) C(306) 1.37(1) . . yes C(302) H(302) 0.96(1) . . yes C(302) C(303) 1.36(1) . . yes C(303) H(303) 0.96(2) . . yes C(303) C(304) 1.34(2) . . yes C(304) H(304) 0.96(2) . . yes C(304) C(305) 1.35(2) . . yes C(305) H(305) 0.96(2) . . yes C(305) C(306) 1.39(1) . . yes C(306) H(306) 0.96(1) . . yes C(401) C(402) 1.40(1) . . yes C(401) C(406) 1.37(1) . . yes C(402) H(402) 0.96(1) . . yes C(402) C(403) 1.37(1) . . yes C(403) H(403) 0.96(1) . . yes C(403) C(404) 1.38(1) . . yes C(404) H(404) 0.96(1) . . yes C(404) C(405) 1.40(1) . . yes C(405) H(405) 0.96(1) . . yes C(405) C(406) 1.37(1) . . yes C(406) H(406) 0.96(1) . . yes N(1) C(2) 1.35(1) . . yes N(1) C(5) 1.36(1) . . yes C(2) C(3) 1.40(1) . . yes C(2) N(8) 1.39(1) . . yes C(3) C(4) 1.41(1) . . yes C(3) C(9) 1.42(1) . . yes C(4) C(5) 1.40(1) . . yes C(4) C(10) 1.40(1) . . yes C(5) C(6) 1.42(1) . . yes C(6) C(7) 1.38(1) . . yes C(6) C(11) 1.45(1) . . yes C(7) C(12) 1.43(1) . . yes C(7) C(13) 1.42(1) . . yes N(8) C(19) 1.29(1) . . yes C(9) N(15) 1.14(1) . . yes C(10) N(16) 1.16(1) . . yes C(11) N(17) 1.15(1) . . yes C(12) N(18) 1.14(1) . . yes C(13) N(14) 1.14(1) . . yes C(19) H(19) 0.96(1) . . yes C(19) N(20) 1.33(1) . . yes N(20) C(21) 1.42(2) . . yes N(20) C(22) 1.43(1) . . yes C(21) H(211) 0.96(2) . . yes C(21) H(212) 0.96(2) . . yes C(21) H(213) 0.96(2) . . yes C(22) H(221) 0.96(2) . . yes C(22) H(222) 0.96(2) . . yes C(22) H(223) 0.96(2) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(5) N(1) C(2) 106.5(6) . . . yes C(3) C(2) N(1) 110.6(7) . . . yes N(8) C(2) N(1) 125.6(7) . . . yes N(8) C(2) C(3) 123.6(7) . . . yes C(4) C(3) C(2) 106.6(7) . . . yes C(9) C(3) C(2) 127.5(7) . . . yes C(9) C(3) C(4) 125.9(8) . . . yes C(3) C(4) C(5) 104.8(7) . . . yes C(10) C(4) C(5) 130.4(7) . . . yes C(10) C(4) C(3) 124.7(7) . . . yes C(4) C(5) C(6) 129.1(7) . . . yes N(1) C(5) C(6) 119.5(7) . . . yes N(1) C(5) C(4) 111.4(6) . . . yes C(5) C(6) C(11) 116.6(7) . . . yes C(7) C(6) C(11) 116.9(7) . . . yes C(7) C(6) C(5) 126.4(8) . . . yes C(12) C(7) C(13) 116.8(8) . . . yes C(6) C(7) C(13) 122.9(8) . . . yes C(6) C(7) C(12) 120.3(8) . . . yes C(2) N(8) C(19) 116.0(7) . . . yes N(15) C(9) C(3) 178(1) . . . yes C(4) C(10) N(16) 177.8(8) . . . yes C(6) C(11) N(17) 177.7(9) . . . yes C(7) C(12) N(18) 177(1) . . . yes C(7) C(13) N(14) 172(1) . . . yes H(19) C(19) N(8) 118(1) . . . yes N(20) C(19) N(8) 123.5(8) . . . yes N(20) C(19) H(19) 118(1) . . . yes C(21) N(20) C(19) 121.7(8) . . . yes C(22) N(20) C(19) 121.4(9) . . . yes C(22) N(20) C(21) 116.9(9) . . . yes H(211) C(21) N(20) 108(1) . . . yes H(212) C(21) N(20) 109(1) . . . yes H(212) C(21) H(211) 109(1) . . . yes H(213) C(21) N(20) 110(1) . . . yes H(213) C(21) H(211) 109(1) . . . yes H(213) C(21) H(212) 109(1) . . . yes H(221) C(22) N(20) 108(1) . . . yes H(222) C(22) N(20) 111(1) . . . yes H(222) C(22) H(221) 109(1) . . . yes H(223) C(22) N(20) 107(1) . . . yes H(223) C(22) H(221) 109(1) . . . yes H(223) C(22) H(222) 109(1) . . . yes C(201) As(1) C(101) 111.6(3) . . . yes C(301) As(1) C(101) 108.6(3) . . . yes C(301) As(1) C(201) 107.7(3) . . . yes C(401) As(1) C(101) 108.2(3) . . . yes C(401) As(1) C(201) 112.7(3) . . . yes C(401) As(1) C(301) 108.0(3) . . . yes C(102) C(101) C(106) 122.9(8) . . . yes As(1) C(101) C(106) 118.5(6) . . . yes As(1) C(101) C(102) 118.5(6) . . . yes H(102) C(102) C(103) 120(1) . . . yes C(101) C(102) C(103) 118.3(8) . . . yes C(101) C(102) H(102) 121.1(9) . . . yes H(103) C(103) C(104) 120(1) . . . yes C(102) C(103) C(104) 120(1) . . . yes C(102) C(103) H(103) 119(1) . . . yes C(105) C(104) H(104) 119(1) . . . yes C(103) C(104) H(104) 119(1) . . . yes C(103) C(104) C(105) 121(1) . . . yes C(104) C(105) H(105) 120(1) . . . yes C(106) C(105) H(105) 118(1) . . . yes C(106) C(105) C(104) 120.9(9) . . . yes C(105) C(106) C(101) 116.4(9) . . . yes H(106) C(106) C(101) 121(1) . . . yes H(106) C(106) C(105) 121(1) . . . yes C(206) C(201) As(1) 119.3(6) . . . yes C(202) C(201) As(1) 119.7(6) . . . yes C(202) C(201) C(206) 121.0(8) . . . yes C(201) C(202) H(202) 120(1) . . . yes C(203) C(202) H(202) 121(1) . . . yes C(203) C(202) C(201) 118.2(9) . . . yes C(202) C(203) H(203) 118(1) . . . yes C(204) C(203) H(203) 121(1) . . . yes C(204) C(203) C(202) 119(1) . . . yes C(203) C(204) C(205) 121(1) . . . yes H(204) C(204) C(205) 119(1) . . . yes H(204) C(204) C(203) 118(1) . . . yes C(204) C(205) H(205) 120(1) . . . yes C(206) C(205) H(205) 119(1) . . . yes C(206) C(205) C(204) 120(1) . . . yes C(201) C(206) H(206) 120(1) . . . yes C(205) C(206) H(206) 120(1) . . . yes C(205) C(206) C(201) 118.9(9) . . . yes As(1) C(301) C(302) 118.2(6) . . . yes C(306) C(301) C(302) 121.1(8) . . . yes C(306) C(301) As(1) 120.7(6) . . . yes H(302) C(302) C(301) 120(1) . . . yes C(303) C(302) C(301) 117.3(9) . . . yes C(303) C(302) H(302) 121(1) . . . yes C(304) C(303) C(302) 121(1) . . . yes H(303) C(303) C(302) 118(1) . . . yes H(303) C(303) C(304) 120(1) . . . yes C(303) C(304) H(304) 119(1) . . . yes C(305) C(304) H(304) 118(1) . . . yes C(305) C(304) C(303) 122(1) . . . yes H(305) C(305) C(304) 121(1) . . . yes C(306) C(305) C(304) 119(1) . . . yes C(306) C(305) H(305) 119(1) . . . yes C(301) C(306) H(306) 120(1) . . . yes C(305) C(306) H(306) 120(1) . . . yes C(305) C(306) C(301) 118.7(9) . . . yes C(402) C(401) As(1) 118.9(6) . . . yes C(406) C(401) As(1) 120.4(5) . . . yes C(406) C(401) C(402) 120.5(7) . . . yes H(402) C(402) C(401) 120.5(9) . . . yes C(403) C(402) C(401) 119.2(8) . . . yes C(403) C(402) H(402) 120.3(9) . . . yes H(403) C(403) C(402) 119(1) . . . yes C(404) C(403) C(402) 120.5(8) . . . yes C(404) C(403) H(403) 119(1) . . . yes H(404) C(404) C(403) 120(1) . . . yes C(405) C(404) C(403) 119.4(9) . . . yes C(405) C(404) H(404) 120(1) . . . yes H(405) C(405) C(404) 119(1) . . . yes C(406) C(405) C(404) 120.2(8) . . . yes C(406) C(405) H(405) 120.2(9) . . . yes H(406) C(406) C(405) 119.8(9) . . . yes C(401) C(406) C(405) 120.2(7) . . . yes C(401) C(406) H(406) 120.0(9) . . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? . . ? #===END data_4 # DATA SECTION OF BLOCK ################################## _chemical_name_systematic ;Tetraphenylarsonium 2-(5-propylcarboxamidoamino-3,4-dicyano-2H-dicyano- 2H-pyrrol-2-ylidene)-1,1,2-tricyanoethanide ; _chemical_compound_source ; ; _chemical_formula_iucr ? _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum 'H29C39N8O1As1' _chemical_formula_weight 700.64 _chemical_melting_point ? _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)' _computing_structure_refinement ; SHELXTL PC, Siemens Analytical Instruments, Madison, WI, 1990 ; _computing_molecular_graphics ; SHELXTL PC, Siemens Analytical Instruments, Madison, WI, 1990 ; _computing_publication_material ? _cell_length_a 14.056 _cell_length_b 14.057 _cell_length_c 9.565 _cell_angle_alpha 103.560 _cell_angle_beta 109.670 _cell_angle_gamma 88.650 _cell_volume 1726.847 _cell_formula_units_Z 2 _cell_measurement_radiation 'CuK\a' _cell_measurement_wavelength 1.54178 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20 _cell_measurement_theta_max 40 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' _exptl_crystal_description 'platelets' _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 1.817 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_detector ? _diffrn_measurement_device 'MSG-AFC5 Diffractometer' _diffrn_measurement_method '\q-2\q scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_reduction_process ? _diffrn_reflns_number ? _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 62.13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'h ' 58 'Hydrogen ' 0.0000 0.0000 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'c ' 78 'Carbon ' 0.0170 0.0090 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'n ' 16 'Nitrogen ' 0.0290 0.0180 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'o ' 2 'Oxygen ' 0.0470 0.0320 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' 'as ' 2 'Arsenic ' -1.0110 1.0060 ' Int. Tab. C, 4.2.6.8, 6.1.1.4' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _reflns_number_total 5699 _reflns_number_observed 5446 _reflns_observed_criterion 'none' _reflns_limit_h_max 16 _reflns_limit_h_min 0 _reflns_limit_k_max 16 _reflns_limit_k_min -16 _reflns_limit_l_max 10 _reflns_limit_l_min -10 _reflns_d_resolution_high 0.872 _reflns_d_resolution_low 13.640 _refine_ls_structure_factor_coef 'F' _refine_ls_extinction_method 'none' _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? _refine_ls_abs_structure_details ; ; _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment 'H atoms rigid to parent C atom' _refine_ls_weighting_scheme 'W=1/(\s^2(Fo)+0.002Fo^2)' _refine_ls_number_reflns 4314 _refine_ls_number_parameters 442 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_obs 0.0438 _refine_ls_wR_factor_all 0.0708 _refine_ls_wR_factor_obs 0.0654 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.05 _refine_ls_shift/esd_max 0.098 _refine_ls_shift/esd_mean 0.02 _refine_diff_density_max 0.39 _refine_diff_density_min 0.00 _refine_diff_density_rms ? loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type N(1) 0.5665(2) 0.1850(2) -0.3876(4) 1.000 0.047(1) uani C(2) 0.5382(3) 0.2709(3) -0.4175(4) 1.000 0.045(1) uani C(3) 0.5888(3) 0.3003(3) -0.5068(4) 1.000 0.044(1) uani C(4) 0.6537(3) 0.2262(3) -0.5303(4) 1.000 0.046(1) uani C(5) 0.6373(3) 0.1557(3) -0.4554(4) 1.000 0.047(1) uani C(6) 0.6796(3) 0.0637(3) -0.4512(4) 1.000 0.047(1) uani C(7) 0.6546(3) -0.0048(3) -0.3845(5) 1.000 0.051(1) uani N(8) 0.4677(2) 0.3249(2) -0.3662(4) 1.000 0.050(1) uani H(8) 0.4525(2) 0.3809(2) -0.3968(4) 1.000 0.080 uiso C(9) 0.5751(3) 0.3857(3) -0.5651(4) 1.000 0.050(1) uani C(10) 0.7243(3) 0.2290(3) -0.6071(5) 1.000 0.059(2) uani C(11) 0.7555(3) 0.0362(3) -0.5210(5) 1.000 0.056(2) uani C(12) 0.7047(3) -0.0947(3) -0.3870(5) 1.000 0.059(2) uani C(13) 0.5812(3) 0.0055(3) -0.3103(5) 1.000 0.058(2) uani N(14) 0.5246(3) 0.0070(3) -0.2473(5) 1.000 0.078(2) uani N(15) 0.5629(3) 0.4552(3) -0.6096(5) 1.000 0.070(2) uani N(16) 0.7813(4) 0.2379(3) -0.6650(5) 1.000 0.084(2) uani N(17) 0.8173(3) 0.0105(3) -0.5699(5) 1.000 0.082(2) uani N(18) 0.7453(3) -0.1655(3) -0.3870(5) 1.000 0.083(2) uani C(19) 0.4178(3) 0.3047(3) -0.2720(5) 1.000 0.055(2) uani O(20) 0.3585(2) 0.3640(2) -0.2390(4) 1.000 0.071(1) uani N(21) 0.4370(3) 0.2216(3) -0.2265(4) 1.000 0.065(2) uani H(21) 0.4835(3) 0.1831(3) -0.2523(4) 1.000 0.080 uiso C(22) 0.3835(4) 0.1930(4) -0.1339(6) 1.000 0.069(2) uani H(221) 0.3837(4) 0.1232(4) -0.1467(6) 1.000 0.080 uiso H(222) 0.3144(4) 0.2102(4) -0.1682(6) 1.000 0.080 uiso C(23) 0.4313(5) 0.2405(5) 0.0330(6) 1.000 0.098(3) uani H(231) 0.4392(5) 0.3099(5) 0.0449(6) 1.000 0.080 uiso H(232) 0.4971(5) 0.2164(5) 0.0717(6) 1.000 0.080 uiso C(24) 0.3667(5) 0.2206(5) 0.1242(7) 1.000 0.111(4) uani H(241) 0.3981(5) 0.2522(5) 0.2305(7) 1.000 0.080 uiso H(242) 0.3012(5) 0.2453(5) 0.0856(7) 1.000 0.080 uiso H(243) 0.3595(5) 0.1512(5) 0.1126(7) 1.000 0.080 uiso As(1) 0.94478(3) 0.29874(3) 0.03614(4) 1.000 0.0440(2) uani C(101) 0.9155(3) 0.1747(3) 0.0680(4) 1.000 0.049(1) uani C(102) 0.9896(4) 0.1324(4) 0.1672(6) 1.000 0.082(2) uani H(102) 1.0559(4) 0.1643(4) 0.2197(6) 1.000 0.080 uiso C(103) 0.9663(4) 0.0433(4) 0.1887(7) 1.000 0.096(3) uani H(103) 1.0172(4) 0.0129(4) 0.2569(7) 1.000 0.080 uiso C(104) 0.8730(4) -0.0021(4) 0.1161(5) 1.000 0.078(2) uani H(104) 0.8585(4) -0.0649(4) 0.1304(5) 1.000 0.080 uiso C(105) 0.7998(4) 0.0408(4) 0.0202(6) 1.000 0.083(2) uani H(105) 0.7331(4) 0.0093(4) -0.0292(6) 1.000 0.080 uiso C(106) 0.8209(4) 0.1296(3) -0.0031(5) 1.000 0.071(2) uani H(106) 0.7689(4) 0.1603(3) -0.0691(5) 1.000 0.080 uiso C(201) 1.0368(3) 0.3813(3) 0.2195(4) 1.000 0.047(1) uani C(202) 1.1313(3) 0.3504(3) 0.2892(5) 1.000 0.068(2) uani H(202) 1.1522(3) 0.2889(3) 0.2439(5) 1.000 0.080 uiso C(203) 1.1958(4) 0.4092(4) 0.4220(5) 1.000 0.074(2) uani H(203) 1.2608(4) 0.3882(4) 0.4744(5) 1.000 0.080 uiso C(204) 1.1672(4) 0.4999(4) 0.4828(5) 1.000 0.069(2) uani H(204) 1.2106(4) 0.5415(4) 0.5766(5) 1.000 0.080 uiso C(205) 1.0747(4) 0.5311(3) 0.4093(5) 1.000 0.063(2) uani H(205) 1.0561(4) 0.5953(3) 0.4489(5) 1.000 0.080 uiso C(206) 1.0085(3) 0.4717(3) 0.2783(4) 1.000 0.051(1) uani H(206) 0.9430(3) 0.4929(3) 0.2283(4) 1.000 0.080 uiso C(301) 1.0055(3) 0.2791(3) -0.1191(4) 1.000 0.047(1) uani C(302) 1.0929(3) 0.3328(3) -0.0963(5) 1.000 0.058(2) uani H(302) 1.1223(3) 0.3822(3) -0.0032(5) 1.000 0.080 uiso C(303) 1.1359(3) 0.3161(4) -0.2096(6) 1.000 0.069(2) uani H(303) 1.1971(3) 0.3526(4) -0.1931(6) 1.000 0.080 uiso C(304) 1.0927(4) 0.2474(4) -0.3428(6) 1.000 0.071(2) uani H(304) 1.1236(4) 0.2364(4) -0.4203(6) 1.000 0.080 uiso C(305) 1.0051(4) 0.1951(4) -0.3670(6) 1.000 0.074(2) uani H(305) 0.9746(4) 0.1478(4) -0.4621(6) 1.000 0.080 uiso C(306) 0.9606(3) 0.2098(3) -0.2554(5) 1.000 0.061(2) uani H(306) 0.9001(3) 0.1724(3) -0.2708(5) 1.000 0.080 uiso C(401) 0.8219(3) 0.3630(3) -0.0217(4) 1.000 0.045(1) uani C(402) 0.7601(3) 0.3693(3) 0.0664(5) 1.000 0.058(2) uani H(402) 0.7766(3) 0.3368(3) 0.1486(5) 1.000 0.080 uiso C(403) 0.6756(3) 0.4236(3) 0.0359(5) 1.000 0.066(2) uani H(403) 0.6323(3) 0.4283(3) 0.0962(5) 1.000 0.080 uiso C(404) 0.6529(3) 0.4708(3) -0.0803(5) 1.000 0.066(2) uani H(404) 0.5941(3) 0.5085(3) -0.1012(5) 1.000 0.080 uiso C(405) 0.7125(3) 0.4635(3) -0.1687(5) 1.000 0.065(2) uani H(405) 0.6963(3) 0.4974(3) -0.2493(5) 1.000 0.080 uiso C(406) 0.7983(3) 0.4096(3) -0.1408(4) 1.000 0.053(1) uani H(406) 0.8400(3) 0.4030(3) -0.2036(4) 1.000 0.080 uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 N(1) 0.051(2) 0.014(1) 0.025(1) 0.044(2) 0.022(1) 0.055(2) C(2) 0.044(2) 0.010(1) 0.016(2) 0.040(2) 0.017(2) 0.054(2) C(3) 0.049(2) 0.009(1) 0.017(2) 0.039(2) 0.018(2) 0.049(2) C(4) 0.051(2) 0.008(2) 0.021(2) 0.043(2) 0.016(2) 0.049(2) C(5) 0.051(2) 0.010(2) 0.016(2) 0.043(2) 0.019(2) 0.050(2) C(6) 0.047(2) 0.010(2) 0.014(2) 0.044(2) 0.015(2) 0.051(2) C(7) 0.050(2) 0.016(2) 0.016(2) 0.046(2) 0.024(2) 0.060(2) N(8) 0.048(2) 0.015(1) 0.023(1) 0.046(2) 0.026(1) 0.065(2) C(9) 0.051(2) 0.009(2) 0.021(2) 0.049(2) 0.017(2) 0.053(2) C(10) 0.072(3) 0.018(2) 0.034(2) 0.054(2) 0.024(2) 0.065(3) C(11) 0.066(2) 0.013(2) 0.026(2) 0.044(2) 0.020(2) 0.064(2) C(12) 0.060(2) 0.016(2) 0.022(2) 0.054(2) 0.029(2) 0.070(3) C(13) 0.061(2) 0.015(2) 0.022(2) 0.048(2) 0.033(2) 0.072(3) N(14) 0.078(3) 0.024(2) 0.047(2) 0.079(3) 0.051(2) 0.103(3) N(15) 0.077(2) 0.020(2) 0.037(2) 0.058(2) 0.044(2) 0.093(3) N(16) 0.109(3) 0.026(2) 0.071(3) 0.082(3) 0.046(2) 0.100(3) N(17) 0.091(3) 0.027(2) 0.063(3) 0.073(3) 0.026(2) 0.107(3) N(18) 0.094(3) 0.030(2) 0.035(3) 0.058(2) 0.039(2) 0.106(3) C(19) 0.051(2) 0.011(2) 0.024(2) 0.057(2) 0.023(2) 0.065(2) O(20) 0.072(2) 0.031(2) 0.052(2) 0.068(2) 0.035(2) 0.097(2) N(21) 0.076(2) 0.027(2) 0.051(2) 0.064(2) 0.040(2) 0.085(3) C(22) 0.069(3) 0.013(2) 0.036(2) 0.073(3) 0.033(2) 0.082(3) C(23) 0.106(5) -0.014(4) 0.030(3) 0.112(5) 0.032(3) 0.080(4) C(24) 0.129(5) -0.008(4) 0.049(4) 0.133(5) 0.041(4) 0.089(4) As(1) 0.0444(3) 0.0079(2) 0.0142(1) 0.0447(3) 0.0136(2) 0.0436(2) C(101) 0.057(2) 0.005(2) 0.021(2) 0.047(2) 0.012(2) 0.047(2) C(102) 0.065(3) 0.005(2) 0.012(3) 0.073(3) 0.045(3) 0.105(4) C(103) 0.095(4) 0.004(3) 0.009(3) 0.073(3) 0.058(3) 0.117(5) C(104) 0.113(4) -0.011(3) 0.028(3) 0.059(3) 0.019(2) 0.064(3) C(105) 0.085(3) -0.022(3) 0.011(3) 0.071(3) 0.022(3) 0.083(3) C(106) 0.066(3) -0.006(2) 0.002(2) 0.064(3) 0.024(2) 0.072(3) C(201) 0.050(2) 0.006(2) 0.009(2) 0.048(2) 0.014(2) 0.040(2) C(202) 0.061(3) 0.010(2) 0.001(2) 0.051(2) 0.020(2) 0.075(3) C(203) 0.064(3) -0.002(2) -0.009(2) 0.071(3) 0.030(2) 0.071(3) C(204) 0.077(3) -0.018(2) 0.011(2) 0.076(3) 0.012(2) 0.046(2) C(205) 0.075(3) -0.005(2) 0.032(2) 0.055(2) 0.003(2) 0.061(3) C(206) 0.054(2) 0.007(2) 0.021(2) 0.051(2) 0.014(2) 0.051(2) C(301) 0.050(2) 0.012(2) 0.021(2) 0.043(2) 0.018(2) 0.053(2) C(302) 0.053(2) 0.006(2) 0.028(2) 0.057(2) 0.020(2) 0.070(3) C(303) 0.058(2) 0.015(2) 0.042(2) 0.075(3) 0.033(3) 0.093(3) C(304) 0.074(3) 0.024(2) 0.048(3) 0.080(3) 0.027(3) 0.079(3) C(305) 0.086(3) 0.011(3) 0.039(2) 0.077(3) 0.008(2) 0.064(3) C(306) 0.060(2) 0.002(2) 0.027(2) 0.066(3) 0.012(2) 0.060(2) C(401) 0.041(2) 0.009(2) 0.009(1) 0.051(2) 0.015(2) 0.042(2) C(402) 0.053(2) 0.016(2) 0.025(2) 0.072(3) 0.027(2) 0.058(2) C(403) 0.051(2) 0.014(2) 0.026(2) 0.075(3) 0.015(2) 0.074(3) C(404) 0.053(2) 0.018(2) 0.007(2) 0.062(3) 0.014(2) 0.071(3) C(405) 0.066(3) 0.007(2) 0.001(2) 0.060(3) 0.024(2) 0.060(2) C(406) 0.053(2) 0.003(2) 0.012(2) 0.059(2) 0.017(2) 0.045(2) # GEOMETRY ############################################### loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) C(101) 1.916(4) . . yes As(1) C(201) 1.919(5) . . yes As(1) C(301) 1.913(4) . . yes As(1) C(401) 1.903(4) . . yes C(101) C(102) 1.381(8) . . yes C(101) C(106) 1.364(8) . . yes C(102) H(102) 0.960(9) . . yes C(102) C(103) 1.379(7) . . yes C(103) H(103) 0.96(1) . . yes C(103) C(104) 1.35(1) . . yes C(104) H(104) 0.960(7) . . yes C(104) C(105) 1.363(9) . . yes C(105) H(105) 0.96(1) . . yes C(105) C(106) 1.375(7) . . yes C(106) H(106) 0.960(8) . . yes C(201) C(202) 1.381(7) . . yes C(201) C(206) 1.372(6) . . yes C(202) H(202) 0.960(7) . . yes C(202) C(203) 1.374(9) . . yes C(203) H(203) 0.960(8) . . yes C(203) C(204) 1.382(7) . . yes C(204) H(204) 0.960(9) . . yes C(204) C(205) 1.371(8) . . yes C(205) H(205) 0.960(7) . . yes C(205) C(206) 1.376(8) . . yes C(206) H(206) 0.960(6) . . yes C(301) C(302) 1.383(6) . . yes C(301) C(306) 1.388(7) . . yes C(302) H(302) 0.960(8) . . yes C(302) C(303) 1.382(7) . . yes C(303) H(303) 0.960(7) . . yes C(303) C(304) 1.36(1) . . yes C(304) H(304) 0.960(7) . . yes C(304) C(305) 1.372(8) . . yes C(305) H(305) 0.960(9) . . yes C(305) C(306) 1.382(6) . . yes C(306) H(306) 0.960(7) . . yes C(401) C(402) 1.388(5) . . yes C(401) C(406) 1.387(5) . . yes C(402) H(402) 0.960(6) . . yes C(402) C(403) 1.381(7) . . yes C(403) H(403) 0.960(6) . . yes C(403) C(404) 1.370(7) . . yes C(404) H(404) 0.960(7) . . yes C(404) C(405) 1.364(6) . . yes C(405) H(405) 0.960(6) . . yes C(405) C(406) 1.391(6) . . yes C(406) H(406) 0.960(5) . . yes N(1) C(2) 1.326(5) . . yes N(1) C(5) 1.368(5) . . yes C(2) C(3) 1.413(4) . . yes C(2) N(8) 1.383(5) . . yes C(3) C(4) 1.396(5) . . yes C(3) C(9) 1.422(5) . . yes C(4) C(5) 1.416(5) . . yes C(4) C(10) 1.425(5) . . yes C(5) C(6) 1.414(5) . . yes C(6) C(7) 1.383(5) . . yes C(6) C(11) 1.439(5) . . yes C(7) C(12) 1.432(6) . . yes C(7) C(13) 1.424(5) . . yes N(8) H(8) 0.900(4) . . yes N(8) C(19) 1.392(5) . . yes C(9) N(15) 1.142(5) . . yes C(10) N(16) 1.141(6) . . yes C(11) N(17) 1.133(6) . . yes C(12) N(18) 1.135(6) . . yes C(13) N(14) 1.144(6) . . yes C(19) O(20) 1.229(5) . . yes C(19) N(21) 1.332(5) . . yes N(21) H(21) 0.900(5) . . yes N(21) C(22) 1.462(6) . . yes C(22) H(221) 0.960(7) . . yes C(22) H(222) 0.960(8) . . yes C(22) C(23) 1.50(1) . . yes C(23) H(231) 0.96(1) . . yes C(23) H(232) 0.96(1) . . yes C(23) C(24) 1.524(8) . . yes C(24) H(241) 0.96(1) . . yes C(24) H(242) 0.96(1) . . yes C(24) H(243) 0.96(1) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(5) N(1) C(2) 106.3(3) . . . yes C(3) C(2) N(8) 124.4(3) . . . yes N(1) C(2) N(8) 123.6(3) . . . yes N(1) C(2) C(3) 111.9(3) . . . yes C(2) C(3) C(4) 105.6(3) . . . yes C(9) C(3) C(4) 126.7(3) . . . yes C(9) C(3) C(2) 127.6(3) . . . yes C(3) C(4) C(5) 105.6(3) . . . yes C(10) C(4) C(5) 129.8(4) . . . yes C(10) C(4) C(3) 124.6(3) . . . yes C(4) C(5) C(6) 128.7(3) . . . yes N(1) C(5) C(6) 120.7(3) . . . yes N(1) C(5) C(4) 110.5(3) . . . yes C(11) C(6) C(5) 119.1(3) . . . yes C(7) C(6) C(5) 125.6(3) . . . yes C(7) C(6) C(11) 115.3(3) . . . yes C(13) C(7) C(12) 114.9(3) . . . yes C(6) C(7) C(12) 119.6(3) . . . yes C(6) C(7) C(13) 125.5(4) . . . yes C(19) N(8) H(8) 115.5(4) . . . yes C(2) N(8) H(8) 115.8(3) . . . yes C(2) N(8) C(19) 128.7(3) . . . yes C(3) C(9) N(15) 178.4(4) . . . yes C(4) C(10) N(16) 175.4(5) . . . yes N(17) C(11) C(6) 175.6(5) . . . yes N(18) C(12) C(7) 179.1(7) . . . yes N(14) C(13) C(7) 174.5(5) . . . yes O(20) C(19) N(8) 117.8(3) . . . yes N(21) C(19) N(8) 117.2(4) . . . yes N(21) C(19) O(20) 125.0(4) . . . yes H(21) N(21) C(19) 119.7(4) . . . yes C(22) N(21) C(19) 120.4(4) . . . yes C(22) N(21) H(21) 120.0(4) . . . yes H(221) C(22) N(21) 109.2(5) . . . yes H(222) C(22) N(21) 109.7(5) . . . yes H(222) C(22) H(221) 108.0(7) . . . yes C(23) C(22) N(21) 112.5(5) . . . yes C(23) C(22) H(221) 108.3(6) . . . yes C(23) C(22) H(222) 109.0(6) . . . yes H(231) C(23) C(24) 109.4(7) . . . yes H(232) C(23) C(24) 109.4(6) . . . yes H(232) C(23) H(231) 108.3(9) . . . yes C(22) C(23) C(24) 111.5(6) . . . yes C(22) C(23) H(231) 108.5(7) . . . yes C(22) C(23) H(232) 109.6(7) . . . yes H(241) C(24) C(23) 110.3(8) . . . yes H(242) C(24) C(23) 109.0(7) . . . yes H(242) C(24) H(241) 109(1) . . . yes H(243) C(24) C(23) 109.1(7) . . . yes H(243) C(24) H(241) 109.5(9) . . . yes H(243) C(24) H(242) 109(1) . . . yes C(201) As(1) C(401) 108.1(2) . . . yes C(101) As(1) C(401) 108.6(2) . . . yes C(101) As(1) C(201) 111.4(2) . . . yes C(301) As(1) C(401) 110.9(2) . . . yes C(301) As(1) C(201) 108.2(2) . . . yes C(301) As(1) C(101) 109.7(2) . . . yes As(1) C(101) C(102) 119.9(4) . . . yes C(106) C(101) C(102) 119.9(4) . . . yes C(106) C(101) As(1) 120.2(3) . . . yes C(103) C(102) H(102) 120.8(7) . . . yes C(101) C(102) H(102) 120.5(6) . . . yes C(101) C(102) C(103) 118.7(6) . . . yes C(104) C(103) C(102) 121.4(6) . . . yes H(103) C(103) C(102) 119.6(8) . . . yes H(103) C(103) C(104) 119.1(6) . . . yes C(103) C(104) H(104) 120.3(8) . . . yes C(105) C(104) H(104) 119.9(8) . . . yes C(105) C(104) C(103) 119.7(5) . . . yes C(106) C(105) H(105) 120.2(7) . . . yes C(104) C(105) H(105) 119.7(6) . . . yes C(104) C(105) C(106) 120.1(6) . . . yes H(106) C(106) C(105) 120.0(7) . . . yes C(101) C(106) C(105) 120.2(5) . . . yes C(101) C(106) H(106) 119.8(5) . . . yes C(202) C(201) As(1) 120.1(3) . . . yes C(206) C(201) As(1) 119.3(3) . . . yes C(206) C(201) C(202) 120.6(5) . . . yes C(203) C(202) H(202) 120.2(6) . . . yes C(201) C(202) H(202) 120.1(7) . . . yes C(201) C(202) C(203) 119.7(4) . . . yes H(203) C(203) C(204) 119.0(7) . . . yes C(202) C(203) C(204) 120.0(5) . . . yes C(202) C(203) H(203) 121.1(6) . . . yes C(205) C(204) C(203) 119.7(6) . . . yes H(204) C(204) C(203) 121.2(6) . . . yes H(204) C(204) C(205) 119.0(6) . . . yes C(206) C(205) H(205) 119.6(6) . . . yes C(204) C(205) H(205) 119.7(7) . . . yes C(204) C(205) C(206) 120.7(5) . . . yes C(201) C(206) C(205) 119.3(4) . . . yes H(206) C(206) C(205) 120.7(5) . . . yes H(206) C(206) C(201) 120.0(6) . . . yes C(302) C(301) As(1) 120.7(4) . . . yes C(306) C(301) As(1) 119.0(3) . . . yes C(306) C(301) C(302) 120.3(4) . . . yes C(301) C(302) H(302) 119.9(5) . . . yes C(303) C(302) H(302) 120.7(5) . . . yes C(303) C(302) C(301) 119.4(5) . . . yes C(304) C(303) H(303) 120.1(6) . . . yes C(302) C(303) H(303) 119.4(7) . . . yes C(302) C(303) C(304) 120.5(5) . . . yes H(304) C(304) C(305) 120.2(8) . . . yes C(303) C(304) C(305) 120.3(5) . . . yes C(303) C(304) H(304) 119.5(7) . . . yes H(305) C(305) C(306) 119.9(6) . . . yes C(304) C(305) C(306) 120.6(6) . . . yes C(304) C(305) H(305) 119.5(6) . . . yes C(301) C(306) C(305) 118.9(5) . . . yes H(306) C(306) C(305) 121.0(6) . . . yes H(306) C(306) C(301) 120.1(5) . . . yes C(402) C(401) As(1) 118.3(3) . . . yes C(406) C(401) As(1) 121.1(3) . . . yes C(406) C(401) C(402) 120.3(4) . . . yes H(402) C(402) C(403) 120.5(5) . . . yes C(401) C(402) C(403) 119.5(4) . . . yes C(401) C(402) H(402) 120.1(5) . . . yes C(404) C(403) H(403) 119.7(6) . . . yes C(402) C(403) H(403) 120.1(5) . . . yes C(402) C(403) C(404) 120.3(4) . . . yes C(403) C(404) C(405) 120.5(4) . . . yes H(404) C(404) C(405) 119.4(5) . . . yes H(404) C(404) C(403) 120.1(5) . . . yes C(406) C(405) H(405) 119.5(5) . . . yes C(404) C(405) H(405) 119.8(5) . . . yes C(404) C(405) C(406) 120.7(4) . . . yes C(405) C(406) C(401) 118.8(3) . . . yes H(406) C(406) C(401) 119.9(5) . . . yes H(406) C(406) C(405) 121.3(5) . . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? . . ? #===END