# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1858 data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-09-23 _audit_update_record ? #============================================================================== # (Publishing Staff 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 ? _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 ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal 'J.Chem.Soc.Dalton' _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; data_vtb57 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C12 H12 As2 Cl2 N4' _chemical_formula_moiety ? _chemical_formula_weight 433.01 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 9.926(4) _cell_length_b 13.005(3) _cell_length_c 14.224(4) _cell_angle_alpha 90.00000 _cell_angle_beta 122.61(2) _cell_angle_gamma 90.00000 _cell_volume 1546.7(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.859 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 16.6 _cell_measurement_theta_max 18.9 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 4.66 _exptl_crystal_description prism _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type Cad4 _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAl absorb ; _exptl_absorpt_correction_T_min .28 _exptl_absorpt_correction_T_max .38 _diffrn_reflns_number 4021 _reflns_number_total 3540 _reflns_Friedel_coverage ? _reflns_number_gt 2144 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .024 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .055 _refine_ls_wR_factor_ref .051 _refine_ls_goodness_of_fit_ref 2.01 _refine_ls_number_reflns 2144 _refine_ls_number_parameters 182 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref #<< use NfA code _refine_ls_shift/su_max .080 _refine_diff_density_min -.78 _refine_diff_density_max .80 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 48 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' As ? 0 8 -.03 2.007 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 48 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group As1 .61991(9) .62803(6) .66152(7) .0513(4) Uani ? ? 1.00000 ? ? As2 .74843(8) .62864(6) .52203(7) .0493(4) Uani ? ? 1.00000 ? ? Cl1 .7625(2) .79537(15) .49087(16) .0599(11) Uani ? ? 1.00000 ? ? Cl2 .5959(2) .79433(16) .68729(17) .0627(11) Uani ? ? 1.00000 ? ? N11 1.0704(7) .6051(4) .7213(5) .045(3) Uani ? ? 1.00000 ? ? C12 .9710(8) .6132(5) .7565(6) .043(4) Uani ? ? 1.00000 ? ? N12 .8114(6) .6298(5) .6674(5) .051(3) Uani ? ? 1.00000 ? ? C13 1.0168(10) .6065(6) .8664(7) .054(4) Uani ? ? 1.00000 ? ? C14 1.1768(12) .5921(7) .9439(7) .070(5) Uani ? ? 1.00000 ? ? C15 1.2828(9) .5823(7) .9114(7) .066(5) Uani ? ? 1.00000 ? ? C16 1.2290(8) .5899(6) .8003(7) .050(4) Uani ? ? 1.00000 ? ? C161 1.3379(8) .5824(7) .7581(7) .065(5) Uani ? ? 1.00000 ? ? N21 .2985(6) .6279(4) .4665(5) .044(3) Uani ? ? 1.00000 ? ? C22 .3961(8) .6329(5) .4286(6) .042(3) Uani ? ? 1.00000 ? ? N22 .5565(6) .6294(5) .5152(5) .051(3) Uani ? ? 1.00000 ? ? C23 .3451(9) .6412(6) .3169(7) .056(4) Uani ? ? 1.00000 ? ? C24 .1826(10) .6445(6) .2405(6) .055(4) Uani ? ? 1.00000 ? ? C25 .0793(9) .6394(6) .2782(7) .050(4) Uani ? ? 1.00000 ? ? C26 .1387(8) .6317(5) .3893(6) .042(3) Uani ? ? 1.00000 ? ? C261 .0348(8) .6270(6) .4350(7) .058(4) Uani ? ? 1.00000 ? ? H13 .93691 .61041 .88737 .06500 Uiso ? ? 1.00000 ? ? H14 1.21078 .58792 1.02171 .08500 Uiso ? ? 1.00000 ? ? H15 1.39580 .57179 .96527 .08000 Uiso ? ? 1.00000 ? ? H161a 1.29842 .62040 .69044 .07200 Uiso ? ? 1.00000 ? ? H161b 1.34754 .51069 .74053 .07200 Uiso ? ? 1.00000 ? ? H161c 1.44942 .60922 .82185 .07200 Uiso ? ? 1.00000 ? ? H23 .41613 .64380 .28990 .06500 Uiso ? ? 1.00000 ? ? H24 .13867 .65078 .15949 .06700 Uiso ? ? 1.00000 ? ? H25 -.03700 .64243 .22530 .06200 Uiso ? ? 1.00000 ? ? H261a -.04146 .68180 .40138 .07400 Uiso ? ? 1.00000 ? ? H261b -.02485 .56299 .40783 .07400 Uiso ? ? 1.00000 ? ? H261c .08016 .62911 .52609 .07400 Uiso ? ? 1.00000 ? ? 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 As1 .0425(5) .0550(5) .0733(6) .0033(4) .0424(5) .0055(5) As2 .0370(4) .0547(5) .0694(6) -.0018(4) .0374(4) -.0067(5) Cl1 .0552(13) .0611(13) .0660(14) -.0054(10) .0344(12) .0009(11) Cl2 .0615(13) .0629(13) .0705(15) .0112(11) .0400(12) -.0030(11) N11 .038(3) .044(4) .060(4) -.001(3) .031(3) -.002(3) C12 .043(4) .030(4) .065(5) -.001(3) .034(4) -.003(4) N12 .032(3) .050(4) .077(4) .005(3) .034(3) .002(4) C13 .060(5) .053(5) .065(5) .004(4) .044(5) -.003(4) C14 .080(7) .077(6) .055(6) .010(5) .038(5) -.001(5) C15 .040(5) .084(6) .063(6) .012(4) .020(5) -.004(5) C16 .033(4) .051(5) .064(5) .003(4) .024(4) -.003(4) C161 .036(4) .085(6) .078(6) .006(4) .032(4) -.006(5) N21 .034(3) .048(3) .057(4) .000(3) .028(3) .004(3) C22 .034(4) .037(4) .061(5) -.000(3) .029(4) -.003(4) N22 .031(3) .061(4) .076(5) -.004(3) .038(3) -.011(4) C23 .053(5) .052(5) .081(6) -.003(4) .048(5) -.003(5) C24 .061(5) .060(5) .057(5) .000(4) .040(5) .002(4) C25 .045(4) .043(4) .059(5) .005(4) .025(4) .004(4) C26 .038(4) .037(4) .054(5) .003(4) .027(4) .004(4) C261 .038(4) .066(5) .087(6) .005(4) .045(4) .005(5) # 5. Molecular Geometry #---------------------- 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 #<< enter YES for value to be published As1 As2 . . 2.8796(18) ? As1 Cl2 . . 2.228(2) ? As1 N12 . . 1.857(7) ? As1 N22 . . 1.821(7) ? As2 Cl1 . . 2.233(2) ? As2 N12 . . 1.809(7) ? As2 N22 . . 1.854(7) ? N11 C12 . . 1.330(13) ? N11 C16 . . 1.368(8) ? C12 N12 . . 1.414(7) ? C12 C13 . . 1.376(13) ? C13 C14 . . 1.373(11) ? C13 H13 . . .987(12) ? C14 C15 . . 1.364(17) ? C14 H14 . . .970(10) ? C15 C16 . . 1.372(13) ? C15 H15 . . .968(7) ? C16 C161 . . 1.497(15) ? C161 H161a . . .957(9) ? C161 H161b . . .984(9) ? C161 H161c . . 1.042(6) ? N21 C22 . . 1.339(13) ? N21 C26 . . 1.358(8) ? C22 N22 . . 1.393(7) ? C22 C23 . . 1.389(13) ? C23 C24 . . 1.376(10) ? C23 H23 . . .968(12) ? C24 C25 . . 1.390(16) ? C24 H24 . . .992(9) ? C25 C26 . . 1.361(12) ? C25 H25 . . .982(7) ? C26 C261 . . 1.487(15) ? C261 H261a . . .959(7) ? C261 H261b . . .972(7) ? C261 H261c . . 1.120(9) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published As2 As1 Cl2 . . . 103.72(9) ? As2 As1 N12 . . . 37.6(2) ? As2 As1 N22 . . . 38.8(2) ? Cl2 As1 N12 . . . 100.2(2) ? Cl2 As1 N22 . . . 100.2(2) ? N12 As1 N22 . . . 76.5(3) ? As1 As2 Cl1 . . . 103.75(8) ? As1 As2 N12 . . . 38.8(2) ? As1 As2 N22 . . . 38.0(2) ? Cl1 As2 N12 . . . 101.4(2) ? Cl1 As2 N22 . . . 99.0(2) ? N12 As2 N22 . . . 76.8(3) ? C12 N11 C16 . . . 117.5(7) ? N11 C12 N12 . . . 112.0(7) ? N11 C12 C13 . . . 124.4(6) ? N12 C12 C13 . . . 123.6(9) ? As1 N12 As2 . . . 103.5(2) ? As1 N12 C12 . . . 131.5(7) ? As2 N12 C12 . . . 123.6(7) ? C12 C13 C14 . . . 116.9(10) ? C12 C13 H13 . . . 120.8(7) ? C14 C13 H13 . . . 122.3(10) ? C13 C14 C15 . . . 120.7(9) ? C13 C14 H14 . . . 117.6(12) ? C15 C14 H14 . . . 121.7(8) ? C14 C15 C16 . . . 119.4(7) ? C14 C15 H15 . . . 121.4(9) ? C16 C15 H15 . . . 119.2(11) ? N11 C16 C15 . . . 121.2(9) ? N11 C16 C161 . . . 116.1(8) ? C15 C16 C161 . . . 122.7(6) ? C16 C161 H161a . . . 112.1(7) ? C16 C161 H161b . . . 110.6(8) ? C16 C161 H161c . . . 106.7(8) ? H161a C161 H161b . . . 106.1(9) ? H161a C161 H161c . . . 111.7(9) ? H161b C161 H161c . . . 109.6(7) ? C22 N21 C26 . . . 117.1(7) ? N21 C22 N22 . . . 111.9(7) ? N21 C22 C23 . . . 124.6(6) ? N22 C22 C23 . . . 123.5(9) ? As1 N22 As2 . . . 103.2(2) ? As1 N22 C22 . . . 122.4(7) ? As2 N22 C22 . . . 134.4(7) ? C22 C23 C24 . . . 117.0(10) ? C22 C23 H23 . . . 124.2(7) ? C24 C23 H23 . . . 118.7(9) ? C23 C24 C25 . . . 119.2(8) ? C23 C24 H24 . . . 120.9(11) ? C25 C24 H24 . . . 119.9(7) ? C24 C25 C26 . . . 120.2(6) ? C24 C25 H25 . . . 120.7(8) ? C26 C25 H25 . . . 119.1(10) ? N21 C26 C25 . . . 121.8(9) ? N21 C26 C261 . . . 115.4(7) ? C25 C26 C261 . . . 122.8(6) ? C26 C261 H261a . . . 107.3(8) ? C26 C261 H261b . . . 106.2(8) ? C26 C261 H261c . . . 124.3(6) ? H261a C261 H261b . . . 106.8(6) ? H261a C261 H261c . . . 106.0(9) ? H261b C261 H261c . . . 105.1(8) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 As1 C12 2.988(8) . . ? As1 N21 2.887(5) . . ? As1 C22 2.825(7) . . ? As2 N11 2.929(5) . . ? As2 C12 2.847(7) . . ? As2 C22 2.999(8) . . ? Cl1 N12 3.140(7) . . ? Cl1 N22 3.118(7) . . ? Cl2 N12 3.144(7) . . ? Cl2 N22 3.117(7) . . ? N11 N12 2.276(9) . . ? N11 C13 2.393(14) . . ? N11 C14 2.750(12) . . ? N11 C15 2.387(9) . . ? N11 C161 2.432(11) . . ? N11 H161a 2.535(8) . . ? C12 C14 2.342(10) . . ? C12 C15 2.692(9) . . ? C12 C16 2.307(12) . . ? C12 H13 2.064(10) . . ? N12 C13 2.459(9) . . ? N12 N22 2.276(6) . . ? N12 H13 2.684(7) . . ? C13 C15 2.378(13) . . ? C13 C16 2.739(16) . . ? C13 H14 2.015(7) . . ? C14 C16 2.362(17) . . ? C14 H13 2.076(11) . . ? C14 H15 2.043(12) . . ? C15 C161 2.518(16) . . ? C15 H14 2.046(12) . . ? C15 H161c 2.598(12) . . ? C16 H15 2.029(7) . . ? C16 H161a 2.058(11) . . ? C16 H161b 2.061(10) . . ? C16 H161c 2.055(9) . . ? C161 H15 2.685(10) . . ? N21 N22 2.264(9) . . ? N21 C23 2.415(14) . . ? N21 C24 2.777(11) . . ? N21 C25 2.377(8) . . ? N21 C261 2.406(11) . . ? C22 C24 2.358(9) . . ? C22 C25 2.687(9) . . ? C22 C26 2.301(12) . . ? C22 H23 2.092(10) . . ? N22 C23 2.451(9) . . ? C23 C25 2.387(13) . . ? C23 C26 2.747(16) . . ? C23 H24 2.069(7) . . ? C24 C26 2.385(15) . . ? C24 H23 2.028(9) . . ? C24 H25 2.071(10) . . ? C25 C261 2.502(15) . . ? C25 H24 2.071(11) . . ? C25 H261a 2.660(11) . . ? C26 H25 2.030(6) . . ? C26 H261a 1.996(9) . . ? C26 H261b 1.991(9) . . ? C26 H261c 2.311(10) . . ? C261 H25 2.675(9) . . ? H13 H14 2.3512(8) . . ? H14 H15 2.3771(7) . . ? H161a H161b 1.5513(3) . . ? H161a H161c 1.6558(4) . . ? H161a H261c 2.1708(6) . '1 655' ? H161b H161c 1.6558(3) . . ? H23 H24 2.3511(9) . . ? H24 H25 2.3849(7) . . ? H261a H261b 1.5514(4) . . ? H261a H261c 1.6630(4) . . ? H261b H261c 1.6630(4) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 848 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 6 5 4 -6 5 -4 6 -5 -4 -6 -5 5 6 -9 -5 6 9 -5 -6 9 5 -6 -9 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min -16 _reflns_limit_l_max 16 _reflns_number_observed ? _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min ? _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CAD4 diffracometer' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .101 _refine_ls_wR_factor_all .055 _refine_ls_goodness_of_fit_all 1.67 _refine_ls_shift/su_mean .004 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_vtb70 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C27 H45 Bi1 N6 Si3' _chemical_formula_moiety ? _chemical_formula_weight 746.94 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 14.912(5) _cell_length_b 11.812(4) _cell_length_c 11.389(4) _cell_angle_alpha 116.11(2) _cell_angle_beta 94.03(3) _cell_angle_gamma 104.73(2) _cell_volume 1703.4(11) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 16.2 _cell_measurement_theta_max 18.8 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 5.3 _exptl_crystal_description prism _exptl_crystal_size_max .28 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .2 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type CAD4 _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'XTAL absorb' _exptl_absorpt_correction_T_min .3 _exptl_absorpt_correction_T_max .38 _diffrn_reflns_number 6143 _reflns_number_total 5986 _reflns_Friedel_coverage ? _reflns_number_gt 5176 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .024 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 1778(121) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack ? #ActaC _refine_ls_number_reflns 5176 #ActaC _refine_ls_number_parameters 335 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .049 #ActaC _refine_ls_R_factor_gt .038 #ActaC _refine_ls_wR_factor_all .039 #ActaC _refine_ls_wR_factor_ref .038 #ActaC _refine_ls_goodness_of_fit_all 1.392 #ActaC _refine_ls_goodness_of_fit_ref 1.45 #ActaC _refine_ls_shift/su_max .073 #ActaC _refine_ls_shift/su_mean .001 #ActaC _refine_diff_density_min -1.092 #ActaC _refine_diff_density_max 1.063 #ActaC # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 54 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' Bi ? 0 2 -4.861 10.559 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 6 .072021 .070984 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 90 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Bi .18598(2) .15048(2) .14019(3) .03671(12) Uani ? ? 1.00000 ? ? N11 .2163(4) -.0791(5) .0106(5) .045(2) Uani ? ? 1.00000 ? ? C12 .2559(5) -.0604(7) .1313(7) .046(3) Uani ? ? 1.00000 ? ? N12 .2718(4) .0650(5) .2361(5) .041(2) Uani ? ? 1.00000 ? ? Si1 .31982(15) .1096(2) .3996(2) .0514(9) Uani ? ? 1.00000 ? ? C121 .4338(6) .0723(9) .4140(9) .082(5) Uani ? ? 1.00000 ? ? C122 .2344(6) .0220(10) .4662(9) .083(5) Uani ? ? 1.00000 ? ? C123 .3490(6) .2901(9) .5090(8) .080(4) Uani ? ? 1.00000 ? ? C13 .2748(6) -.1680(7) .1402(8) .062(4) Uani ? ? 1.00000 ? ? C14 .2578(6) -.2840(7) .0264(9) .066(4) Uani ? ? 1.00000 ? ? C15 .2179(6) -.3007(7) -.0965(8) .064(4) Uani ? ? 1.00000 ? ? C16 .1965(5) -.1966(7) -.1003(7) .052(3) Uani ? ? 1.00000 ? ? C161 .1480(7) -.2070(8) -.2255(8) .077(4) Uani ? ? 1.00000 ? ? N21 .1621(4) .2794(5) .0091(5) .045(3) Uani ? ? 1.00000 ? ? C22 .2425(5) .2636(6) -.0338(6) .042(3) Uani ? ? 1.00000 ? ? N22 .2943(4) .2214(5) .0348(6) .047(3) Uani ? ? 1.00000 ? ? Si2 .40036(16) .1910(2) -.0031(2) .0597(10) Uani ? ? 1.00000 ? ? C221 .4893(7) .3408(11) .0082(12) .112(6) Uani ? ? 1.00000 ? ? C222 .3821(7) .0500(10) -.1709(10) .100(6) Uani ? ? 1.00000 ? ? C223 .4571(6) .1571(10) .1215(9) .082(5) Uani ? ? 1.00000 ? ? C23 .2661(6) .2939(8) -.1353(8) .065(4) Uani ? ? 1.00000 ? ? C24 .2056(7) .3371(8) -.1903(8) .071(4) Uani ? ? 1.00000 ? ? C25 .1240(6) .3519(8) -.1462(8) .066(4) Uani ? ? 1.00000 ? ? C26 .1026(5) .3199(7) -.0478(8) .055(3) Uani ? ? 1.00000 ? ? C261 .0142(6) .3288(9) .0049(10) .084(5) Uani ? ? 1.00000 ? ? N31 .0980(4) .1937(5) .3416(5) .043(2) Uani ? ? 1.00000 ? ? C32 .1425(4) .3247(6) .3865(6) .039(3) Uani ? ? 1.00000 ? ? N32 .2120(4) .3515(5) .3241(5) .042(2) Uani ? ? 1.00000 ? ? Si3 .28073(16) .5157(2) .3696(2) .0610(10) Uani ? ? 1.00000 ? ? C321 .3355(7) .6122(8) .5524(9) .092(5) Uani ? ? 1.00000 ? ? C322 .2077(8) .6052(8) .3285(11) .098(6) Uani ? ? 1.00000 ? ? C323 .3791(7) .5195(9) .2807(10) .110(5) Uani ? ? 1.00000 ? ? C33 .1126(5) .4187(6) .4912(7) .047(3) Uani ? ? 1.00000 ? ? C34 .0417(5) .3738(8) .5466(7) .058(4) Uani ? ? 1.00000 ? ? C35 -.0020(5) .2387(8) .4997(8) .056(4) Uani ? ? 1.00000 ? ? C36 .0271(5) .1523(7) .3957(7) .049(3) Uani ? ? 1.00000 ? ? C361 -.0192(6) .0024(7) .3280(8) .068(4) Uani ? ? 1.00000 ? ? H121a .42515 -.01940 .36012 .12000 Uiso ? ? 1.00000 ? ? H121b .48044 .12173 .38370 .12000 Uiso ? ? 1.00000 ? ? H121c .46252 .09734 .50384 .12000 Uiso ? ? 1.00000 ? ? H122a .17591 .04120 .46392 .11600 Uiso ? ? 1.00000 ? ? H122b .21848 -.07461 .41172 .11600 Uiso ? ? 1.00000 ? ? H122c .25875 .04276 .55542 .11600 Uiso ? ? 1.00000 ? ? H123a .39607 .34083 .47772 .11500 Uiso ? ? 1.00000 ? ? H123b .29536 .32048 .50896 .11500 Uiso ? ? 1.00000 ? ? H123c .37730 .31992 .59993 .11500 Uiso ? ? 1.00000 ? ? H13 .29809 -.15992 .22709 .07500 Uiso ? ? 1.00000 ? ? H14 .27335 -.35667 .03214 .08000 Uiso ? ? 1.00000 ? ? H15 .20644 -.38423 -.17825 .07900 Uiso ? ? 1.00000 ? ? H161a .08974 -.28141 -.26708 .11200 Uiso ? ? 1.00000 ? ? H161b .18719 -.22000 -.29105 .11200 Uiso ? ? 1.00000 ? ? H161c .13228 -.12660 -.20585 .11200 Uiso ? ? 1.00000 ? ? H221a .46578 .37083 -.04988 .15000 Uiso ? ? 1.00000 ? ? H221b .50358 .41683 .09960 .15000 Uiso ? ? 1.00000 ? ? H221c .54859 .32959 -.00946 .15000 Uiso ? ? 1.00000 ? ? H222a .33801 -.02991 -.17822 .14000 Uiso ? ? 1.00000 ? ? H222b .35371 .06691 -.23832 .14000 Uiso ? ? 1.00000 ? ? H222c .43814 .03067 -.19460 .14000 Uiso ? ? 1.00000 ? ? H223a .47042 .23055 .20987 .12000 Uiso ? ? 1.00000 ? ? H223b .41533 .08012 .12313 .12000 Uiso ? ? 1.00000 ? ? H223c .51487 .13922 .10330 .12000 Uiso ? ? 1.00000 ? ? H23 .32610 .28573 -.16534 .08200 Uiso ? ? 1.00000 ? ? H24 .22070 .35693 -.26263 .08300 Uiso ? ? 1.00000 ? ? H25 .08259 .38611 -.18242 .08100 Uiso ? ? 1.00000 ? ? H261a .02336 .36275 .10164 .11700 Uiso ? ? 1.00000 ? ? H261b -.01615 .38352 -.01450 .11700 Uiso ? ? 1.00000 ? ? H261c -.03409 .24335 -.03396 .11700 Uiso ? ? 1.00000 ? ? H321a .28836 .61494 .60614 .13200 Uiso ? ? 1.00000 ? ? H321b .37648 .56859 .57636 .13200 Uiso ? ? 1.00000 ? ? H321c .37425 .70082 .58112 .13200 Uiso ? ? 1.00000 ? ? H322a .18076 .56105 .23584 .13600 Uiso ? ? 1.00000 ? ? H322b .15677 .60948 .37672 .13600 Uiso ? ? 1.00000 ? ? H322c .24388 .69537 .35381 .13600 Uiso ? ? 1.00000 ? ? H323a .42074 .47684 .30129 .13000 Uiso ? ? 1.00000 ? ? H323b .35627 .47384 .18626 .13000 Uiso ? ? 1.00000 ? ? H323c .41854 .60827 .30447 .13000 Uiso ? ? 1.00000 ? ? H33 .14167 .51299 .52276 .05900 Uiso ? ? 1.00000 ? ? H34 .02193 .43836 .62025 .07300 Uiso ? ? 1.00000 ? ? H35 -.05146 .20570 .53965 .06900 Uiso ? ? 1.00000 ? ? H361a -.08636 -.02568 .31569 .09900 Uiso ? ? 1.00000 ? ? H361b .00523 -.03951 .37346 .09900 Uiso ? ? 1.00000 ? ? H361c -.00796 -.03803 .23843 .09900 Uiso ? ? 1.00000 ? ? 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 Bi .04157(16) .03231(15) .03994(15) .01448(11) .00849(10) .01884(11) N11 .059(4) .042(3) .042(3) .023(3) .014(3) .023(3) C12 .046(4) .048(4) .059(5) .020(3) .014(4) .034(4) N12 .047(3) .035(3) .046(3) .016(3) .007(3) .022(3) Si1 .0543(13) .0575(13) .0471(12) .0225(11) .0052(10) .0270(11) C121 .067(6) .095(7) .093(7) .039(5) .006(5) .044(6) C122 .084(7) .115(8) .075(6) .032(6) .019(5) .065(6) C123 .091(7) .080(6) .056(5) .039(5) -.009(5) .018(5) C13 .080(6) .046(5) .061(5) .024(4) .001(4) .028(4) C14 .073(6) .045(5) .091(7) .033(4) .016(5) .035(5) C15 .080(6) .043(5) .060(5) .031(4) .006(4) .012(4) C16 .061(5) .047(4) .049(4) .022(4) .013(4) .019(4) C161 .111(7) .064(6) .045(5) .036(5) .004(5) .016(4) N21 .053(4) .053(4) .050(3) .029(3) .014(3) .034(3) C22 .054(4) .029(3) .043(4) .020(3) .017(3) .013(3) N22 .053(4) .049(4) .056(4) .026(3) .017(3) .035(3) Si2 .0582(14) .0686(15) .0800(16) .0340(12) .0324(12) .0489(13) C221 .081(7) .111(8) .192(12) .038(6) .078(8) .102(9) C222 .123(9) .120(9) .088(7) .080(7) .059(7) .049(7) C223 .055(5) .114(8) .102(7) .043(5) .030(5) .062(6) C23 .086(6) .065(5) .075(6) .039(5) .041(5) .049(5) C24 .111(8) .061(5) .065(5) .037(5) .029(5) .044(5) C25 .087(6) .058(5) .071(6) .031(5) .004(5) .043(5) C26 .058(5) .043(4) .063(5) .013(4) .004(4) .027(4) C261 .064(6) .095(7) .119(8) .040(5) .020(6) .066(7) N31 .044(3) .035(3) .050(3) .013(3) .008(3) .021(3) C32 .034(4) .042(4) .044(4) .016(3) .004(3) .022(3) N32 .044(3) .039(3) .047(3) .010(3) .013(3) .023(3) Si3 .0635(14) .0355(12) .0695(15) .0043(10) .0179(12) .0182(11) C321 .086(7) .057(6) .076(6) -.009(5) -.002(5) .003(5) C322 .132(9) .051(6) .120(8) .029(6) .029(7) .048(6) C323 .092(7) .064(6) .115(8) -.022(5) .044(6) .016(6) C33 .054(4) .036(4) .043(4) .012(3) .011(3) .012(3) C34 .062(5) .060(5) .051(5) .029(4) .020(4) .018(4) C35 .058(5) .063(5) .057(5) .020(4) .021(4) .036(4) C36 .050(4) .045(4) .055(5) .012(4) .006(4) .029(4) C361 .074(6) .046(5) .075(6) -.002(4) .015(5) .033(4) # 5. Molecular Geometry #---------------------- 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 #<< enter YES for value to be published Bi N11 . . 2.632(6) ? Bi N12 . . 2.298(7) ? Bi N21 . . 2.623(8) ? Bi N22 . . 2.285(6) ? Bi N31 . . 2.641(6) ? Bi N32 . . 2.284(5) ? N11 C12 . . 1.357(10) ? N11 C16 . . 1.343(8) ? C12 N12 . . 1.378(8) ? C12 C13 . . 1.413(14) ? N12 Si1 . . 1.736(6) ? Si1 C121 . . 1.875(11) ? Si1 C122 . . 1.851(11) ? Si1 C123 . . 1.844(9) ? C121 H121a . . .948(9) ? C121 H121b . . .974(11) ? C121 H121c . . .962(10) ? C122 H122a . . .957(11) ? C122 H122b . . .980(10) ? C122 H122c . . .952(10) ? C123 H123a . . .994(10) ? C123 H123b . . .956(11) ? C123 H123c . . .957(9) ? C13 C14 . . 1.355(10) ? C13 H13 . . .981(9) ? C14 C15 . . 1.390(14) ? C14 H14 . . .971(10) ? C15 C16 . . 1.364(14) ? C15 H15 . . .976(7) ? C16 C161 . . 1.493(13) ? C161 H161a . . .969(8) ? C161 H161b . . .963(10) ? C161 H161c . . .970(10) ? N21 C22 . . 1.350(10) ? N21 C26 . . 1.358(12) ? C22 N22 . . 1.382(11) ? C22 C23 . . 1.395(13) ? N22 Si2 . . 1.750(7) ? Si2 C221 . . 1.868(12) ? Si2 C222 . . 1.843(9) ? Si2 C223 . . 1.841(13) ? C221 H221a . . .960(16) ? C221 H221b . . .992(10) ? C221 H221c . . .950(11) ? C222 H222a . . .968(11) ? C222 H222b . . .971(13) ? C222 H222c . . .948(12) ? C223 H223a . . .960(8) ? C223 H223b . . .971(11) ? C223 H223c . . .953(9) ? C23 C24 . . 1.380(16) ? C23 H23 . . .993(9) ? C24 C25 . . 1.372(14) ? C24 H24 . . .976(11) ? C25 C26 . . 1.365(14) ? C25 H25 . . .975(11) ? C26 C261 . . 1.495(13) ? C261 H261a . . .978(11) ? C261 H261b . . .965(13) ? C261 H261c . . .962(8) ? N31 C32 . . 1.353(8) ? N31 C36 . . 1.352(10) ? C32 N32 . . 1.347(9) ? C32 C33 . . 1.419(9) ? N32 Si3 . . 1.763(6) ? Si3 C321 . . 1.871(9) ? Si3 C322 . . 1.864(13) ? Si3 C323 . . 1.843(11) ? C321 H321a . . .961(10) ? C321 H321b . . .987(12) ? C321 H321c . . .949(9) ? C322 H322a . . .947(10) ? C322 H322b . . .967(12) ? C322 H322c . . .961(9) ? C323 H323a . . .968(12) ? C323 H323b . . .953(10) ? C323 H323c . . .965(10) ? C33 C34 . . 1.378(12) ? C33 H33 . . .969(7) ? C34 C35 . . 1.389(11) ? C34 H34 . . .979(8) ? C35 C36 . . 1.366(10) ? C35 H35 . . .980(9) ? C36 C361 . . 1.519(10) ? C361 H361a . . .950(8) ? C361 H361b . . .968(11) ? C361 H361c . . .966(9) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N11 Bi N12 . . . 55.26(18) ? N11 Bi N21 . . . 118.43(19) ? N11 Bi N22 . . . 84.6(2) ? N11 Bi N31 . . . 119.9(2) ? N11 Bi N32 . . . 152.8(2) ? N12 Bi N21 . . . 154.6(2) ? N12 Bi N22 . . . 99.8(2) ? N12 Bi N31 . . . 85.5(2) ? N12 Bi N32 . . . 97.8(2) ? N21 Bi N22 . . . 55.0(2) ? N21 Bi N31 . . . 114.8(2) ? N21 Bi N32 . . . 83.6(2) ? N22 Bi N31 . . . 151.87(16) ? N22 Bi N32 . . . 97.5(2) ? N31 Bi N32 . . . 54.40(19) ? Bi N11 C12 . . . 87.1(4) ? Bi N11 C16 . . . 149.6(6) ? C12 N11 C16 . . . 121.3(7) ? N11 C12 N12 . . . 114.9(8) ? N11 C12 C13 . . . 118.9(6) ? N12 C12 C13 . . . 126.1(7) ? Bi N12 C12 . . . 101.2(5) ? Bi N12 Si1 . . . 134.2(3) ? C12 N12 Si1 . . . 122.6(6) ? N12 Si1 C121 . . . 112.3(4) ? N12 Si1 C122 . . . 110.3(3) ? N12 Si1 C123 . . . 111.1(4) ? C121 Si1 C122 . . . 109.1(5) ? C121 Si1 C123 . . . 105.7(4) ? C122 Si1 C123 . . . 108.2(4) ? Si1 C121 H121a . . . 111.3(6) ? Si1 C121 H121b . . . 109.8(9) ? Si1 C121 H121c . . . 114.1(7) ? H121a C121 H121b . . . 107.6(9) ? H121a C121 H121c . . . 107.9(12) ? H121b C121 H121c . . . 105.9(7) ? Si1 C122 H122a . . . 111.7(10) ? Si1 C122 H122b . . . 110.5(7) ? Si1 C122 H122c . . . 112.7(6) ? H122a C122 H122b . . . 106.4(7) ? H122a C122 H122c . . . 108.6(9) ? H122b C122 H122c . . . 106.6(13) ? Si1 C123 H123a . . . 110.7(6) ? Si1 C123 H123b . . . 112.8(6) ? Si1 C123 H123c . . . 114.2(9) ? H123a C123 H123b . . . 105.4(11) ? H123a C123 H123c . . . 105.1(7) ? H123b C123 H123c . . . 108.0(8) ? C12 C13 C14 . . . 118.7(9) ? C12 C13 H13 . . . 120.8(6) ? C14 C13 H13 . . . 120.4(10) ? C13 C14 C15 . . . 121.3(9) ? C13 C14 H14 . . . 118.6(10) ? C15 C14 H14 . . . 120.1(7) ? C14 C15 C16 . . . 118.3(6) ? C14 C15 H15 . . . 120.9(10) ? C16 C15 H15 . . . 120.8(9) ? N11 C16 C15 . . . 121.3(8) ? N11 C16 C161 . . . 116.3(8) ? C15 C16 C161 . . . 122.5(6) ? C16 C161 H161a . . . 111.6(9) ? C16 C161 H161b . . . 111.9(9) ? C16 C161 H161c . . . 110.1(6) ? H161a C161 H161b . . . 106.8(6) ? H161a C161 H161c . . . 107.9(10) ? H161b C161 H161c . . . 108.4(10) ? Bi N21 C22 . . . 87.7(5) ? Bi N21 C26 . . . 148.5(5) ? C22 N21 C26 . . . 121.3(7) ? N21 C22 N22 . . . 113.5(7) ? N21 C22 C23 . . . 119.1(8) ? N22 C22 C23 . . . 127.3(7) ? Bi N22 C22 . . . 101.7(4) ? Bi N22 Si2 . . . 133.1(4) ? C22 N22 Si2 . . . 122.5(5) ? N22 Si2 C221 . . . 111.5(4) ? N22 Si2 C222 . . . 112.3(4) ? N22 Si2 C223 . . . 110.4(4) ? C221 Si2 C222 . . . 108.8(5) ? C221 Si2 C223 . . . 104.7(5) ? C222 Si2 C223 . . . 108.9(5) ? Si2 C221 H221a . . . 112.1(7) ? Si2 C221 H221b . . . 110.4(11) ? Si2 C221 H221c . . . 114.4(10) ? H221a C221 H221b . . . 105.2(12) ? H221a C221 H221c . . . 108.3(14) ? H221b C221 H221c . . . 105.8(9) ? Si2 C222 H222a . . . 110.4(9) ? Si2 C222 H222b . . . 110.2(9) ? Si2 C222 H222c . . . 114.5(7) ? H222a C222 H222b . . . 106.3(9) ? H222a C222 H222c . . . 107.6(12) ? H222b C222 H222c . . . 107.4(11) ? Si2 C223 H223a . . . 111.2(9) ? Si2 C223 H223b . . . 110.5(6) ? Si2 C223 H223c . . . 112.6(9) ? H223a C223 H223b . . . 106.9(11) ? H223a C223 H223c . . . 108.2(7) ? H223b C223 H223c . . . 107.2(11) ? C22 C23 C24 . . . 118.8(9) ? C22 C23 H23 . . . 119.9(10) ? C24 C23 H23 . . . 121.3(10) ? C23 C24 C25 . . . 121.3(10) ? C23 C24 H24 . . . 119.6(10) ? C25 C24 H24 . . . 119.1(11) ? C24 C25 C26 . . . 118.3(10) ? C24 C25 H25 . . . 121.3(10) ? C26 C25 H25 . . . 120.4(9) ? N21 C26 C25 . . . 121.1(8) ? N21 C26 C261 . . . 116.3(9) ? C25 C26 C261 . . . 122.6(9) ? C26 C261 H261a . . . 113.9(8) ? C26 C261 H261b . . . 114.5(11) ? C26 C261 H261c . . . 111.8(8) ? H261a C261 H261b . . . 106.0(9) ? H261a C261 H261c . . . 105.8(12) ? H261b C261 H261c . . . 104.0(8) ? Bi N31 C32 . . . 86.5(4) ? Bi N31 C36 . . . 150.4(4) ? C32 N31 C36 . . . 121.1(6) ? N31 C32 N32 . . . 114.7(6) ? N31 C32 C33 . . . 118.6(6) ? N32 C32 C33 . . . 126.7(6) ? Bi N32 C32 . . . 102.6(3) ? Bi N32 Si3 . . . 133.7(3) ? C32 N32 Si3 . . . 122.1(4) ? N32 Si3 C321 . . . 111.5(4) ? N32 Si3 C322 . . . 111.1(4) ? N32 Si3 C323 . . . 111.8(4) ? C321 Si3 C322 . . . 108.6(5) ? C321 Si3 C323 . . . 106.6(4) ? C322 Si3 C323 . . . 107.0(6) ? Si3 C321 H321a . . . 111.7(6) ? Si3 C321 H321b . . . 110.3(6) ? Si3 C321 H321c . . . 114.4(9) ? H321a C321 H321b . . . 105.6(11) ? H321a C321 H321c . . . 108.2(8) ? H321b C321 H321c . . . 106.2(8) ? Si3 C322 H322a . . . 111.0(8) ? Si3 C322 H322b . . . 109.9(10) ? Si3 C322 H322c . . . 112.3(8) ? H322a C322 H322b . . . 108.3(10) ? H322a C322 H322c . . . 108.4(13) ? H322b C322 H322c . . . 106.8(9) ? Si3 C323 H323a . . . 110.4(10) ? Si3 C323 H323b . . . 111.3(7) ? Si3 C323 H323c . . . 113.6(8) ? H323a C323 H323b . . . 107.7(9) ? H323a C323 H323c . . . 106.1(9) ? H323b C323 H323c . . . 107.4(13) ? C32 C33 C34 . . . 119.1(6) ? C32 C33 H33 . . . 120.2(7) ? C34 C33 H33 . . . 120.7(7) ? C33 C34 C35 . . . 121.1(7) ? C33 C34 H34 . . . 119.3(8) ? C35 C34 H34 . . . 119.5(8) ? C34 C35 C36 . . . 117.5(8) ? C34 C35 H35 . . . 121.8(7) ? C36 C35 H35 . . . 120.7(8) ? N31 C36 C35 . . . 122.6(7) ? N31 C36 C361 . . . 114.3(6) ? C35 C36 C361 . . . 123.1(7) ? C36 C361 H361a . . . 114.4(8) ? C36 C361 H361b . . . 113.4(7) ? C36 C361 H361c . . . 110.4(8) ? H361a C361 H361b . . . 107.9(9) ? H361a C361 H361c . . . 104.0(7) ? H361b C361 H361c . . . 106.1(9) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Bi C12 2.901(9) . . ? Bi Si1 3.723(3) . . ? Bi C123 4.087(9) . . ? Bi C16 3.852(7) . . ? Bi C22 2.900(8) . . ? Bi Si2 3.708(3) . . ? Bi C223 4.046(9) . . ? Bi C26 3.846(10) . . ? Bi C32 2.894(6) . . ? Bi Si3 3.727(2) . . ? Bi C323 4.085(9) . . ? Bi C36 3.875(8) . . ? Bi H123b 3.7789(13) . . ? Bi H161c 3.7088(10) . . ? Bi H223b 3.7178(12) . . ? Bi H323b 3.7985(11) . . ? Bi H361c 3.7345(9) . . ? N11 N12 2.306(7) . . ? N11 C13 2.386(13) . . ? N11 C14 2.721(13) . . ? N11 C15 2.359(10) . . ? N11 C161 2.410(9) . . ? N11 H161c 2.439(6) . . ? C12 Si1 2.737(7) . . ? C12 C14 2.382(11) . . ? C12 C15 2.757(9) . . ? C12 C16 2.354(9) . . ? C12 H13 2.092(10) . . ? C12 H223b 2.565(7) . . ? N12 C122 2.945(13) . . ? N12 C123 2.953(8) . . ? N12 C13 2.488(10) . . ? N12 H223b 2.581(6) . . ? Si1 C13 3.163(7) . . ? Si1 H121a 2.388(3) . . ? Si1 H121b 2.387(2) . . ? Si1 H121c 2.431(3) . . ? Si1 H122a 2.378(2) . . ? Si1 H122b 2.379(3) . . ? Si1 H122c 2.387(3) . . ? Si1 H123a 2.384(2) . . ? Si1 H123b 2.384(2) . . ? Si1 H123c 2.4014(18) . . ? Si1 H13 2.825(2) . . ? C121 C123 2.964(15) . . ? C122 C123 2.994(14) . . ? C13 C15 2.393(10) . . ? C13 C16 2.741(13) . . ? C13 H14 2.010(8) . . ? C14 C16 2.364(15) . . ? C14 H13 2.036(8) . . ? C14 H15 2.068(9) . . ? C15 C161 2.504(15) . . ? C15 H14 2.056(10) . . ? C16 H15 2.044(8) . . ? C16 H161a 2.058(7) . . ? C16 H161b 2.056(8) . . ? C16 H161c 2.040(10) . . ? C161 H15 2.699(11) . . ? N21 N22 2.286(9) . . ? N21 C23 2.367(11) . . ? N21 C24 2.718(13) . . ? N21 C25 2.371(13) . . ? N21 C261 2.424(12) . . ? N21 H261a 2.606(6) . . ? C22 Si2 2.753(8) . . ? C22 C24 2.388(14) . . ? C22 C25 2.765(14) . . ? C22 C26 2.360(12) . . ? C22 H23 2.076(8) . . ? C22 H323b 2.666(5) . . ? N22 C221 2.991(12) . . ? N22 C222 2.984(12) . . ? N22 C223 2.950(13) . . ? N22 C23 2.488(13) . . ? N22 H323b 2.563(5) . . ? Si2 C23 3.191(11) . . ? Si2 H221a 2.401(3) . . ? Si2 H221b 2.402(2) . . ? Si2 H221c 2.421(2) . . ? Si2 H222a 2.361(2) . . ? Si2 H222b 2.361(2) . . ? Si2 H222c 2.396(2) . . ? Si2 H223a 2.364(3) . . ? Si2 H223b 2.364(3) . . ? Si2 H223c 2.377(3) . . ? Si2 H23 2.839(3) . . ? C221 C223 2.94(2) . . ? C222 C223 2.998(14) . . ? C23 C25 2.398(14) . . ? C23 C26 2.735(12) . . ? C23 H24 2.046(11) . . ? C24 C26 2.350(14) . . ? C24 H23 2.077(11) . . ? C24 H25 2.056(11) . . ? C25 C261 2.510(15) . . ? C25 H24 2.034(10) . . ? C25 H261b 2.664(10) . . ? C26 H25 2.040(10) . . ? C26 H261a 2.092(8) . . ? C26 H261b 2.089(9) . . ? C26 H261c 2.056(8) . . ? C261 H25 2.698(12) . . ? N31 N32 2.274(8) . . ? N31 C33 2.383(8) . . ? N31 C34 2.737(9) . . ? N31 C35 2.384(10) . . ? N31 C361 2.414(10) . . ? N31 H361c 2.465(5) . . ? C32 Si3 2.729(7) . . ? C32 C34 2.412(11) . . ? C32 C35 2.787(11) . . ? C32 C36 2.355(11) . . ? C32 H123b 2.611(7) . . ? C32 H33 2.082(6) . . ? N32 C322 2.992(13) . . ? N32 C323 2.986(12) . . ? N32 C33 2.472(9) . . ? N32 H123b 2.580(7) . . ? Si3 C33 3.153(8) . . ? Si3 H321a 2.398(3) . . ? Si3 H321b 2.398(3) . . ? Si3 H321c 2.4227(19) . . ? Si3 H322a 2.374(3) . . ? Si3 H322b 2.374(3) . . ? Si3 H322c 2.399(3) . . ? Si3 H323a 2.361(3) . . ? Si3 H323b 2.362(3) . . ? Si3 H323c 2.399(3) . . ? Si3 H33 2.805(3) . . ? C321 C323 2.977(15) . . ? C322 C323 2.980(16) . . ? C33 C35 2.409(11) . . ? C33 C36 2.731(10) . . ? C33 H34 2.045(8) . . ? C34 C36 2.355(10) . . ? C34 H33 2.050(9) . . ? C34 H35 2.079(9) . . ? C35 C361 2.538(10) . . ? C35 H34 2.056(8) . . ? C36 H35 2.048(8) . . ? C36 H361a 2.098(6) . . ? C36 H361b 2.101(9) . . ? C36 H361c 2.065(6) . . ? H121a H121b 1.5514(5) . . ? H121a H121c 1.5445(4) . . ? H121a H13 2.1034(5) . . ? H121b H121c 1.5446(5) . . ? H122a H122b 1.5513(4) . . ? H122a H122c 1.5501(4) . . ? H122b H122c 1.5500(4) . . ? H123a H123b 1.5513(5) . . ? H123a H123c 1.5488(5) . . ? H123b H123c 1.5488(4) . . ? H13 H14 2.3182(6) . . ? H14 H15 2.3781(8) . . ? H161a H161b 1.5513(4) . . ? H161a H161c 1.5678(5) . . ? H161b H161c 1.5678(3) . . ? H221a H221b 1.5513(6) . . ? H221a H221c 1.5484(4) . . ? H221a H23 2.1130(6) . . ? H221b H221c 1.5484(3) . . ? H222a H222b 1.5513(4) . . ? H222a H222c 1.5458(4) . . ? H222b H222c 1.5459(4) . . ? H223a H223b 1.5513(5) . . ? H223a H223c 1.5494(3) . . ? H223b H223c 1.5494(4) . . ? H23 H24 2.3776(5) . . ? H24 H25 2.3544(7) . . ? H261a H261b 1.5513(4) . . ? H261a H261c 1.5461(4) . . ? H261b H261c 1.5184(6) . . ? H321a H321b 1.5513(4) . . ? H321a H321c 1.5478(4) . . ? H321a H33 2.1210(6) . . ? H321b H321c 1.5478(5) . . ? H322a H322b 1.5513(5) . . ? H322a H322c 1.5475(3) . . ? H322b H322c 1.5476(4) . . ? H322b H33 2.3889(6) . . ? H323a H323b 1.5513(4) . . ? H323a H323c 1.5457(5) . . ? H323b H323c 1.5456(3) . . ? H33 H34 2.3533(5) . . ? H34 H35 2.3878(8) . . ? H361a H361b 1.5514(4) . . ? H361a H361c 1.5102(4) . . ? H361b H361c 1.5450(5) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 748 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 4 4 -8 5 5 9 -6 5 9 5 -7 -5 -4 -4 8 -5 -5 -9 6 -5 -9 -5 7 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min -14 _reflns_limit_k_max 13 _reflns_limit_l_min -13 _reflns_limit_l_max 13 _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI .04 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_reduction_process perpendicular_monochr_Lp _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_vtlasc _audit_creation_date 97-10-21 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural ? #ActaC _chemical_formula_sum 'C6 H6 As2 Cl4 N2' #ActaC _chemical_formula_weight 397.78 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf Nonius software' #ActaC _computing_cell_refinement 'Enraf Nonius software' #ActaC _computing_data_reduction xtal_DIFDAT_ABSORB_SORTRF_ADDREF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 10.608(6) #ActaC _cell_length_b 8.296(3) #ActaC _cell_length_c 8.073(4) #ActaC _cell_angle_alpha 78.75(3) #ActaC _cell_angle_beta 68.12(4) #ActaC _cell_angle_gamma 68.91(4) #ActaC _cell_volume 613.6(6) #ActaC _cell_formula_units_Z 2 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 8 #ActaC _cell_measurement_theta_min 10.9 #ActaC _cell_measurement_theta_max 15.0 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting triclinic #ActaC _symmetry_space_group_name_H-M p_-1 #ActaC _symmetry_space_group_name_Hall -p_1 #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,-y,-z _exptl_crystal_description prism #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour colourless #ActaC _exptl_crystal_size_max 0.55 #ActaC _exptl_crystal_size_mid 0.38 #ActaC _exptl_crystal_size_min 0.28 #ActaC _exptl_crystal_density_diffrn 2.153 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 380 #ActaC _exptl_absorpt_process_details 'XTAL absorb' _exptl_absorpt_coefficient_mu 6.2 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min .17 #ActaC _exptl_absorpt_correction_T_max .39 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type 'Mo K\a' #ActaC _diffrn_radiation_source 'seled tuble' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method '2\q-\w scans' #ActaC _diffrn_standards_number 8 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 60 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 5 5 4 5 0 0 0 5 0 0 0 5 -5 -5 -4 -5 0 0 0 -5 0 0 0 -5 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 4342 #ActaC _diffrn_reflns_av_R_equivalents .101 #ActaC _diffrn_reflns_av_sigmaI/netI .107 #ActaC _diffrn_reflns_limit_h_min -12 #ActaC _diffrn_reflns_limit_h_max 12 #ActaC _diffrn_reflns_limit_k_min -9 #ActaC _diffrn_reflns_limit_k_max 9 #ActaC _diffrn_reflns_limit_l_min -9 #ActaC _diffrn_reflns_limit_l_max 9 #ActaC _diffrn_reflns_theta_min 2.18 #ActaC _diffrn_reflns_theta_max 25.04 #ActaC _diffrn_reflns_reduction_process equatorial_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 12 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 4 .004 .003 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 12 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 As ? 0 4 -.03 2.007 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Cl ? 0 8 .132 .159 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC As1 .19977(8) .79194(11) .01980(12) .0388(9) Uani ? ? Cl11 .0281(2) .9606(3) .2254(3) .061(3) Uani ? ? Cl12 .3067(3) .9964(3) -.1175(4) .069(3) Uani ? ? N1 .1693(6) .5483(9) .2179(9) .039(7) Uani ? ? C2 .2922(8) .5429(11) .2365(11) .039(8) Uani ? ? N2 .3323(7) .6877(8) .1430(9) .041(7) Uani ? ? As2 .42339(9) .80798(11) .19528(13) .0443(10) Uani ? ? Cl21 .3252(3) .7947(3) .4870(3) .065(3) Uani ? ? Cl22 .6244(2) .6015(3) .1861(4) .060(3) Uani ? ? C3 .3629(9) .4041(11) .3323(12) .048(10) Uani ? ? C4 .3032(11) .2761(12) .4039(14) .061(12) Uani ? ? C5 .1795(10) .2776(14) .3808(13) .059(11) Uani ? ? C6 .1158(8) .4179(11) .2845(12) .043(9) Uani ? ? C61 -.0167(10) .4335(15) .2470(15) .068(13) Uani ? ? H3 .44921 .40126 .34583 .05900 Uiso ? ? H4 .34891 .18158 .47082 .07700 Uiso ? ? H5 .14183 .18460 .42934 .07500 Uiso ? ? H61a -.06683 .55150 .22055 .10200 Uiso ? ? H61b .00529 .36850 .14860 .10200 Uiso ? ? H61c -.06492 .38712 .35648 .10200 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC As1 .0424(5) .0359(5) .0453(6) -.0146(4) -.0237(4) .0042(4) Cl11 .0546(13) .0511(14) .0653(17) .0002(11) -.0209(12) -.0098(13) Cl12 .0843(17) .0651(16) .0778(19) -.0468(15) -.0468(15) .0323(14) N1 .037(3) .037(4) .046(4) -.014(3) -.013(3) -.007(3) C2 .045(4) .043(5) .036(5) -.021(4) -.018(4) .006(4) N2 .044(4) .040(4) .049(4) -.020(3) -.029(3) .015(3) As2 .0505(5) .0389(5) .0552(6) -.0204(4) -.0287(5) .0057(4) Cl21 .0713(15) .0640(16) .0561(16) -.0064(13) -.0272(12) -.0156(13) Cl22 .0409(11) .0646(16) .0804(18) -.0132(11) -.0240(11) -.0137(14) C3 .054(5) .036(5) .060(6) -.019(4) -.029(5) .010(4) C4 .078(7) .039(5) .071(7) -.019(5) -.037(6) .013(5) C5 .064(6) .052(6) .058(6) -.032(5) -.009(5) .006(5) C6 .045(5) .038(5) .049(5) -.017(4) -.012(4) -.006(4) C61 .062(6) .078(7) .082(8) -.046(6) -.027(5) .009(6) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme calc #ActaC _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 341(166) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack ? #ActaC _refine_ls_number_reflns 1448 #ActaC _refine_ls_number_parameters 128 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .081 #ActaC _refine_ls_R_factor_gt .044 #ActaC _refine_ls_wR_factor_all .064 #ActaC _refine_ls_wR_factor_ref .051 #ActaC _refine_ls_goodness_of_fit_all .996 #ActaC _refine_ls_goodness_of_fit_ref .99 #ActaC _refine_ls_shift/su_max .041 #ActaC _refine_ls_shift/su_mean .004 #ActaC _refine_diff_density_min -.618 #ActaC _refine_diff_density_max .807 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC As1 Cl11 2.202(2) . . ? As1 Cl12 2.260(3) . . ? As1 N1 2.361(7) . . ? As1 N2 1.883(8) . . ? N1 C2 1.352(13) . . ? N1 C6 1.329(12) . . ? C2 N2 1.403(11) . . ? C2 C3 1.396(12) . . ? N2 As2 1.808(9) . . ? As2 Cl21 2.190(3) . . ? As2 Cl22 2.188(2) . . ? C3 C4 1.355(15) . . ? C3 H3 .954(11) . . ? C4 C5 1.388(18) . . ? C4 H4 .948(10) . . ? C5 C6 1.374(13) . . ? C5 H5 .946(12) . . ? C6 C61 1.502(17) . . ? C61 H61a .957(11) . . ? C61 H61b .956(13) . . ? C61 H61c .929(10) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC As1 Cl11 3.520(3) . 2_575 ? As1 C2 2.588(8) . . ? As1 As2 3.234(2) . . ? As1 Cl22 3.510(3) . 2_665 ? Cl11 Cl12 3.271(4) . . ? Cl11 N2 3.116(6) . . ? Cl12 N2 2.979(7) . . ? Cl12 As2 3.122(3) . . ? Cl12 As2 3.582(4) . 2_675 ? N1 N2 2.255(11) . . ? N1 C3 2.390(12) . . ? N1 C4 2.707(12) . . ? N1 C5 2.358(12) . . ? N1 C61 2.403(16) . . ? N1 H61a 2.487(8) . . ? C2 As2 2.907(10) . . ? C2 C4 2.347(12) . . ? C2 C5 2.737(15) . . ? C2 C6 2.330(15) . . ? C2 H3 2.053(9) . . ? N2 Cl21 3.043(9) . . ? N2 Cl22 3.056(8) . . ? N2 C3 2.528(11) . . ? As2 C3 3.526(10) . . ? Cl21 Cl22 3.264(3) . . ? C3 C5 2.405(17) . . ? C3 C6 2.748(15) . . ? C3 H4 1.987(9) . . ? C4 C6 2.359(15) . . ? C4 H3 2.031(12) . . ? C4 H5 2.040(13) . . ? C5 C61 2.523(16) . . ? C5 H4 2.028(12) . . ? C5 H61c 2.490(11) . . ? C6 H5 2.040(8) . . ? C6 H61a 2.056(9) . . ? C6 H61b 2.056(12) . . ? C6 H61c 1.883(9) . . ? H61a H61b 1.5506(5) . . ? H61a H61c 1.5739(5) . . ? H61b H61c 1.5754(8) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC Cl11 As1 Cl12 94.29(11) . . . ? Cl11 As1 N1 89.19(16) . . . ? Cl11 As1 N2 99.1(2) . . . ? Cl12 As1 N1 154.5(2) . . . ? Cl12 As1 N2 91.5(2) . . . ? N1 As1 N2 63.0(3) . . . ? As1 N1 C2 83.7(5) . . . ? As1 N1 C6 153.8(7) . . . ? C2 N1 C6 120.7(7) . . . ? N1 C2 N2 109.9(7) . . . ? N1 C2 C3 120.9(8) . . . ? N2 C2 C3 129.2(9) . . . ? As1 N2 C2 103.0(6) . . . ? As1 N2 As2 122.3(4) . . . ? C2 N2 As2 129.3(7) . . . ? N2 As2 Cl21 98.7(2) . . . ? N2 As2 Cl22 99.3(2) . . . ? Cl21 As2 Cl22 96.41(11) . . . ? C2 C3 C4 117.1(10) . . . ? C2 C3 H3 120.7(9) . . . ? C4 C3 H3 122.3(9) . . . ? C3 C4 C5 122.5(9) . . . ? C3 C4 H4 118.3(12) . . . ? C5 C4 H4 119.3(11) . . . ? C4 C5 C6 117.3(10) . . . ? C4 C5 H5 120.6(10) . . . ? C6 C5 H5 122.1(12) . . . ? N1 C6 C5 121.5(10) . . . ? N1 C6 C61 116.0(8) . . . ? C5 C6 C61 122.5(10) . . . ? C6 C61 H61a 111.5(12) . . . ? C6 C61 H61b 111.5(8) . . . ? C6 C61 H61c 98.7(10) . . . ? H61a C61 H61b 108.3(12) . . . ? H61a C61 H61c 113.2(9) . . . ? H61b C61 H61c 113.4(14) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min -8 _reflns_limit_k_max 9 _reflns_limit_l_min -8 _reflns_limit_l_max 9 _reflns_number_total 2172 #ActaC _reflns_number_gt 1448 #ActaC _reflns_observed_criterion refl_observed_if_I____>2.000_sigma(I___) _reflns_d_resolution_high .84 _reflns_d_resolution_low 9.341 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? .72716 #end---------------------------- data_vtb38 _audit_creation_date 97-01-24 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural ? #ActaC _chemical_formula_sum 'C27 H45 N6 Sb Si3' #ActaC _chemical_formula_weight 659.72 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf Nonius software' #ActaC _computing_cell_refinement 'Enraf Nonius software' #ActaC _computing_data_reduction xtal_DIFDAT_ABSORB_SORTRF_ADDREF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 14.865(6) #ActaC _cell_length_b 11.682(17) #ActaC _cell_length_c 11.296(10) #ActaC _cell_angle_alpha 116.13(9) #ActaC _cell_angle_beta 94.04(5) #ActaC _cell_angle_gamma 104.01(7) #ActaC _cell_volume 1673(3) #ActaC _cell_formula_units_Z 2 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 8 #ActaC _cell_measurement_theta_min 18.6 #ActaC _cell_measurement_theta_max 23.1 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting triclinic #ActaC _symmetry_space_group_name_H-M p_-1 #ActaC _symmetry_space_group_name_Hall -p_1 #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,-y,-z _exptl_crystal_description fragmant #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour colourless #ActaC _exptl_crystal_size_max 0.65 #ActaC _exptl_crystal_size_mid 0.50 #ActaC _exptl_crystal_size_min 0.25 #ActaC _exptl_crystal_density_diffrn 1.31 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 684 #ActaC _exptl_absorpt_process_details 'XTAL absorb' _exptl_absorpt_coefficient_mu 0.96 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min .68 #ActaC _exptl_absorpt_correction_T_max .81 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'sealed tube' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method '2\q-\w scans' #ActaC _diffrn_standards_number 8 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 60 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 7 6 5 13 0 0 0 9 0 0 0 11 -7 -6 -5 -13 0 0 0 -9 0 0 0 -11 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 6511 #ActaC _diffrn_reflns_av_R_equivalents .021 #ActaC _diffrn_reflns_av_sigmaI/netI .021 #ActaC _diffrn_reflns_limit_h_min -16 #ActaC _diffrn_reflns_limit_h_max 16 #ActaC _diffrn_reflns_limit_k_min -12 #ActaC _diffrn_reflns_limit_k_max 12 #ActaC _diffrn_reflns_limit_l_min -12 #ActaC _diffrn_reflns_limit_l_max 4 #ActaC _diffrn_reflns_theta_min 1.44 #ActaC _diffrn_reflns_theta_max 22.51 #ActaC _diffrn_reflns_reduction_process equatorial_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 54 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 12 .004 .003 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Sb ? 0 2 -.816 1.546 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Si ? 0 6 .072 .071 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 90 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Sb .189321(13) .152869(19) .14247(2) .03408(12) Uani ? ? N11 .22008(18) -.0757(2) .0061(3) .0422(12) Uani ? ? C12 .2569(2) -.0571(3) .1268(3) .0406(14) Uani ? ? N12 .27253(17) .0706(2) .2302(3) .0382(11) Uani ? ? Si1 .32004(7) .11196(10) .39564(10) .0478(4) Uani ? ? C121 .4343(3) .0727(4) .4068(4) .072(2) Uani ? ? C122 .2349(3) .0200(5) .4617(5) .077(2) Uani ? ? C123 .3509(3) .2928(4) .5113(4) .075(2) Uani ? ? C13 .2750(3) -.1660(3) .1377(4) .0552(17) Uani ? ? C14 .2571(3) -.2850(3) .0247(4) .0611(18) Uani ? ? C15 .2183(3) -.3022(3) -.0987(4) .0580(17) Uani ? ? C16 .1983(2) -.1955(3) -.1048(4) .0503(15) Uani ? ? C161 .1493(3) -.2052(4) -.2298(4) .071(2) Uani ? ? N21 .16127(18) .2865(2) .0184(3) .0428(12) Uani ? ? C22 .2402(2) .2669(3) -.0260(3) .0422(14) Uani ? ? N22 .29072(17) .2210(2) .0416(3) .0418(12) Uani ? ? Si2 .39725(7) .18992(11) .00069(12) .0547(5) Uani ? ? C221 .4837(3) .3380(5) .0035(6) .098(3) Uani ? ? C222 .3763(3) .0465(5) -.1709(5) .083(2) Uani ? ? C223 .4581(3) .1553(5) .1236(5) .079(2) Uani ? ? C23 .2622(3) .2908(4) -.1334(4) .0591(18) Uani ? ? C24 .2022(3) .3346(4) -.1891(4) .066(2) Uani ? ? C25 .1210(3) .3521(4) -.1427(4) .0609(18) Uani ? ? C26 .1015(2) .3246(3) -.0406(4) .0489(15) Uani ? ? C261 .0126(3) .3323(4) .0118(5) .077(2) Uani ? ? Si3 .28065(7) .50980(9) .36523(12) .0571(5) Uani ? ? N31 .10253(17) .1884(2) .3441(3) .0397(11) Uani ? ? C32 .1453(2) .3195(3) .3857(3) .0378(13) Uani ? ? N32 .21559(16) .3442(2) .3203(3) .0388(11) Uani ? ? C321 .3346(3) .6065(4) .5496(5) .080(2) Uani ? ? C322 .2053(4) .5996(4) .3249(5) .091(3) Uani ? ? C323 .3798(3) .5190(4) .2783(5) .101(3) Uani ? ? C33 .1140(2) .4152(3) .4885(4) .0456(14) Uani ? ? C34 .0432(2) .3734(3) .5430(4) .0509(15) Uani ? ? C35 -.0002(2) .2384(4) .4983(4) .0512(16) Uani ? ? C36 .0304(2) .1478(3) .3950(3) .0432(14) Uani ? ? C361 -.0168(3) -.0006(4) .3294(4) .0623(18) Uani ? ? H121a .42656 -.01875 .34740 .10600 Uiso ? ? H121b .48024 .12419 .37294 .10600 Uiso ? ? H121c .46280 .09743 .49338 .10600 Uiso ? ? H122a .17630 .03926 .46069 .11700 Uiso ? ? H122b .22140 -.07605 .40703 .11700 Uiso ? ? H122c .25958 .04070 .55235 .11700 Uiso ? ? H123a .39765 .34215 .48026 .09900 Uiso ? ? H123b .29684 .32316 .51189 .09900 Uiso ? ? H123c .37803 .31946 .60189 .09900 Uiso ? ? H13 .29858 -.15443 .22365 .06700 Uiso ? ? H14 .27374 -.35719 .02851 .07300 Uiso ? ? H15 .20476 -.38659 -.17821 .07000 Uiso ? ? H161a .16205 -.27738 -.30405 .10400 Uiso ? ? H161b .08255 -.23164 -.23174 .10400 Uiso ? ? H161c .16591 -.11861 -.24715 .10400 Uiso ? ? H221a .45948 .36699 -.05167 .15800 Uiso ? ? H221b .49936 .41576 .09880 .15800 Uiso ? ? H221c .54382 .32636 -.01202 .15800 Uiso ? ? H222a .33274 -.03234 -.17547 .12600 Uiso ? ? H222b .34677 .06592 -.23535 .12600 Uiso ? ? H222c .43224 .02793 -.19419 .12600 Uiso ? ? H223a .47162 .23406 .20919 .12600 Uiso ? ? H223b .41774 .08237 .12522 .12600 Uiso ? ? H223c .51542 .14073 .10089 .12600 Uiso ? ? H23 .32146 .28443 -.16830 .08500 Uiso ? ? H24 .21474 .34047 -.26903 .09100 Uiso ? ? H25 .07770 .37837 -.18359 .07600 Uiso ? ? H261a -.01090 .39713 .00423 .11700 Uiso ? ? H261b .02556 .35772 .10867 .11700 Uiso ? ? H261c -.03748 .25187 -.02586 .11700 Uiso ? ? H321a .28673 .60506 .60346 .09200 Uiso ? ? H321b .37643 .56088 .57247 .09200 Uiso ? ? H321c .37069 .69386 .57783 .09200 Uiso ? ? H322a .17967 .55540 .23052 .12900 Uiso ? ? H322b .15486 .60334 .37226 .12900 Uiso ? ? H322c .24026 .69122 .34901 .12900 Uiso ? ? H323a .42235 .47831 .30296 .11700 Uiso ? ? H323b .35785 .47247 .18504 .11700 Uiso ? ? H323c .41658 .60895 .30402 .11700 Uiso ? ? H33 .14087 .51101 .51311 .05600 Uiso ? ? H34 .02401 .43678 .61970 .06300 Uiso ? ? H35 -.05249 .20904 .53630 .05500 Uiso ? ? H361a -.07963 -.02117 .26013 .09000 Uiso ? ? H361b -.03500 -.02954 .39530 .09000 Uiso ? ? H361c .02340 -.05025 .28305 .09000 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Sb .03768(14) .03075(14) .03140(16) .01105(9) .00655(10) .01239(11) N11 .0547(16) .0373(15) .0360(18) .0200(12) .0084(14) .0156(14) C12 .0415(17) .0405(18) .042(2) .0147(14) .0103(16) .0205(17) N12 .0459(14) .0343(14) .0339(17) .0151(12) .0063(13) .0144(13) Si1 .0499(5) .0562(6) .0375(6) .0195(5) .0040(5) .0213(5) C121 .062(2) .093(3) .066(3) .033(2) -.001(2) .038(3) C122 .077(3) .112(4) .062(3) .029(3) .017(2) .057(3) C123 .082(3) .071(3) .047(3) .027(2) -.018(2) .009(2) C13 .075(2) .045(2) .052(3) .0262(18) .004(2) .026(2) C14 .076(2) .041(2) .073(3) .0282(18) .012(2) .027(2) C15 .074(2) .040(2) .053(3) .0243(18) .011(2) .013(2) C16 .059(2) .043(2) .043(2) .0188(16) .0108(19) .0135(18) C161 .103(3) .058(2) .039(3) .030(2) .000(2) .011(2) N21 .0511(15) .0394(15) .0448(19) .0200(12) .0134(14) .0220(14) C22 .0523(19) .0341(17) .041(2) .0149(15) .0124(17) .0165(17) N22 .0472(15) .0452(16) .0429(19) .0194(12) .0173(14) .0252(15) Si2 .0520(6) .0639(7) .0665(8) .0290(5) .0284(6) .0383(6) C221 .074(3) .097(4) .155(6) .031(3) .058(3) .080(4) C222 .100(3) .095(3) .071(3) .057(3) .042(3) .036(3) C223 .048(2) .115(4) .097(4) .033(2) .022(2) .066(3) C23 .075(2) .067(2) .060(3) .034(2) .030(2) .042(2) C24 .102(3) .064(3) .053(3) .034(2) .027(2) .040(2) C25 .080(3) .051(2) .060(3) .026(2) .004(2) .031(2) C26 .058(2) .0369(18) .050(2) .0168(16) .0040(19) .0190(18) C261 .059(2) .091(3) .101(4) .039(2) .022(2) .055(3) Si3 .0597(6) .0339(5) .0578(8) .0016(4) .0164(6) .0105(5) N31 .0440(14) .0315(14) .0377(18) .0090(11) .0089(13) .0125(13) C32 .0405(17) .0357(17) .032(2) .0128(14) .0017(15) .0122(16) N32 .0395(14) .0343(14) .0346(17) .0085(11) .0086(13) .0107(13) C321 .076(3) .050(2) .067(3) -.002(2) .002(2) .000(2) C322 .130(4) .051(2) .096(4) .025(3) .025(3) .039(3) C323 .087(3) .060(3) .098(4) -.019(2) .038(3) .005(3) C33 .054(2) .0355(18) .041(2) .0152(15) .0121(17) .0110(17) C34 .059(2) .055(2) .035(2) .0277(17) .0170(18) .0125(19) C35 .050(2) .062(2) .046(2) .0178(17) .0176(18) .027(2) C36 .0450(18) .046(2) .037(2) .0106(15) .0044(16) .0210(18) C361 .067(2) .048(2) .069(3) .0058(18) .016(2) .030(2) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type atomblock #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 6127(287) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack ? #ActaC _refine_ls_number_reflns 4017 #ActaC _refine_ls_number_parameters 336 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .028 #ActaC _refine_ls_R_factor_gt .025 #ActaC _refine_ls_wR_factor_all .032 #ActaC _refine_ls_wR_factor_ref .032 #ActaC _refine_ls_goodness_of_fit_all 1.378 #ActaC _refine_ls_goodness_of_fit_ref 1.458 #ActaC _refine_ls_shift/su_max .087 #ActaC _refine_ls_shift/su_mean .007 #ActaC _refine_diff_density_min -.542 #ActaC _refine_diff_density_max .441 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Sb N11 2.604(4) . . ? Sb N12 2.163(4) . . ? Sb N21 2.595(4) . . ? Sb N22 2.159(3) . . ? Sb N31 2.620(3) . . ? Sb N32 2.167(3) . . ? N11 C12 1.335(5) . . ? N11 C16 1.346(4) . . ? C12 N12 1.379(4) . . ? C12 C13 1.416(6) . . ? N12 Si1 1.755(4) . . ? Si1 C121 1.873(5) . . ? Si1 C122 1.869(6) . . ? Si1 C123 1.842(5) . . ? C121 H121a .951(4) . . ? C121 H121b 1.008(5) . . ? C121 H121c .923(5) . . ? C122 H122a .951(5) . . ? C122 H122b .971(5) . . ? C122 H122c .964(5) . . ? C123 H123a .978(5) . . ? C123 H123b .954(5) . . ? C123 H123c .952(5) . . ? C13 C14 1.358(5) . . ? C13 H13 .947(5) . . ? C14 C15 1.379(7) . . ? C14 H14 .952(5) . . ? C15 C16 1.377(7) . . ? C15 H15 .958(3) . . ? C16 C161 1.488(7) . . ? C161 H161a .963(4) . . ? C161 H161b .961(4) . . ? C161 H161c 1.087(5) . . ? N21 C22 1.339(4) . . ? N21 C26 1.342(6) . . ? C22 N22 1.382(6) . . ? C22 C23 1.403(7) . . ? N22 Si2 1.757(3) . . ? Si2 C221 1.875(6) . . ? Si2 C222 1.861(4) . . ? Si2 C223 1.845(6) . . ? C221 H221a .920(7) . . ? C221 H221b 1.019(5) . . ? C221 H221c .953(5) . . ? C222 H222a .967(5) . . ? C222 H222b .960(6) . . ? C222 H222c .936(5) . . ? C223 H223a .960(4) . . ? C223 H223b .924(5) . . ? C223 H223c .939(4) . . ? C23 C24 1.370(7) . . ? C23 H23 .996(4) . . ? C24 C25 1.373(6) . . ? C24 H24 .963(5) . . ? C25 C26 1.359(7) . . ? C25 H25 .949(5) . . ? C26 C261 1.492(6) . . ? C261 H261a .940(6) . . ? C261 H261b .989(6) . . ? C261 H261c .940(4) . . ? Si3 N32 1.759(4) . . ? Si3 C321 1.874(5) . . ? Si3 C322 1.865(6) . . ? Si3 C323 1.836(6) . . ? N31 C32 1.350(4) . . ? N31 C36 1.337(5) . . ? C32 N32 1.369(5) . . ? C32 C33 1.413(5) . . ? C321 H321a .969(5) . . ? C321 H321b .998(5) . . ? C321 H321c .925(4) . . ? C322 H322a .955(5) . . ? C322 H322b .950(6) . . ? C322 H322c .971(5) . . ? C323 H323a .970(6) . . ? C323 H323b .935(5) . . ? C323 H323c .958(5) . . ? C33 C34 1.355(6) . . ? C33 H33 .992(4) . . ? C34 C35 1.385(5) . . ? C34 H34 .975(4) . . ? C35 C36 1.382(5) . . ? C35 H35 .976(4) . . ? C36 C361 1.501(5) . . ? C361 H361a 1.079(4) . . ? C361 H361b .973(5) . . ? C361 H361c .956(4) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Sb C12 2.810(5) . . ? Sb C22 2.814(5) . . ? Sb C32 2.815(4) . . ? N11 N12 2.280(4) . . ? N11 C13 2.369(6) . . ? N11 C14 2.722(7) . . ? N11 C15 2.367(6) . . ? N11 C161 2.405(5) . . ? C12 Si1 2.724(4) . . ? C12 C14 2.391(6) . . ? C12 C15 2.755(5) . . ? C12 C16 2.343(5) . . ? C12 H13 2.053(5) . . ? C12 H223b 2.553(3) . . ? N12 C122 2.985(7) . . ? N12 C123 2.989(5) . . ? N12 C13 2.498(6) . . ? N12 H223b 2.539(3) . . ? Si1 H121a 2.386(2) . . ? Si1 H121b 2.3897(14) . . ? Si1 H121c 2.4001(14) . . ? Si1 H122a 2.3914(14) . . ? Si1 H122b 2.389(3) . . ? Si1 H122c 2.407(2) . . ? Si1 H123a 2.357(4) . . ? Si1 H123b 2.356(3) . . ? Si1 H123c 2.404(2) . . ? C121 C123 2.934(7) . . ? C13 C15 2.380(6) . . ? C13 C16 2.731(7) . . ? C13 H14 2.015(4) . . ? C14 C16 2.367(7) . . ? C14 H13 2.022(4) . . ? C14 H15 2.043(4) . . ? C15 C161 2.521(8) . . ? C15 H14 2.015(5) . . ? C15 H161a 2.569(5) . . ? C16 H15 2.040(5) . . ? C16 H161a 1.989(4) . . ? C16 H161b 1.990(4) . . ? C16 H161c 2.236(5) . . ? N21 N22 2.275(4) . . ? N21 C23 2.366(6) . . ? N21 C24 2.716(7) . . ? N21 C25 2.357(7) . . ? N21 C261 2.400(5) . . ? N21 H261b 2.481(3) . . ? C22 Si2 2.740(4) . . ? C22 C24 2.386(7) . . ? C22 C25 2.747(7) . . ? C22 C26 2.336(5) . . ? C22 H23 2.128(4) . . ? C22 H323b 2.617(3) . . ? N22 C222 2.986(6) . . ? N22 C223 2.978(6) . . ? N22 C23 2.495(7) . . ? N22 H323b 2.532(4) . . ? Si2 H221a 2.390(3) . . ? Si2 H221b 2.396(3) . . ? Si2 H221c 2.4233(18) . . ? Si2 H222a 2.365(3) . . ? Si2 H222b 2.358(2) . . ? Si2 H222c 2.380(2) . . ? Si2 H223a 2.307(2) . . ? Si2 H223b 2.309(2) . . ? Si2 H223c 2.3406(17) . . ? C221 C223 2.962(10) . . ? C23 C25 2.385(6) . . ? C23 C26 2.721(6) . . ? C23 H24 2.002(5) . . ? C24 C26 2.347(7) . . ? C24 H23 2.027(5) . . ? C24 H25 2.034(5) . . ? C25 C261 2.504(7) . . ? C25 H24 2.048(5) . . ? C25 H261a 2.659(5) . . ? C26 H25 2.012(5) . . ? C26 H261a 2.048(4) . . ? C26 H261b 2.042(4) . . ? C26 H261c 2.084(4) . . ? C261 H25 2.682(6) . . ? Si3 C32 2.720(4) . . ? Si3 H321a 2.402(3) . . ? Si3 H321b 2.398(2) . . ? Si3 H321c 2.4057(19) . . ? Si3 H322a 2.3731(18) . . ? Si3 H322b 2.3728(17) . . ? Si3 H322c 2.414(3) . . ? Si3 H323a 2.3288(14) . . ? Si3 H323b 2.332(2) . . ? Si3 H323c 2.3815(16) . . ? N31 N32 2.286(4) . . ? N31 C33 2.375(5) . . ? N31 C34 2.725(5) . . ? N31 C35 2.370(5) . . ? N31 C361 2.406(5) . . ? N31 H361c 2.497(4) . . ? C32 C34 2.391(5) . . ? C32 C35 2.766(5) . . ? C32 C36 2.346(5) . . ? C32 H123b 2.560(4) . . ? C32 H33 2.081(4) . . ? N32 C321 2.994(5) . . ? N32 C323 2.993(6) . . ? N32 C33 2.490(5) . . ? N32 H123b 2.540(4) . . ? C321 C323 2.959(8) . . ? C322 C323 2.972(8) . . ? C33 C35 2.386(6) . . ? C33 C36 2.729(6) . . ? C33 H34 2.041(4) . . ? C34 C36 2.369(5) . . ? C34 H33 2.055(4) . . ? C34 H35 2.061(4) . . ? C35 C361 2.530(6) . . ? C35 H34 2.027(4) . . ? C36 H35 2.068(4) . . ? C36 H361a 2.080(3) . . ? C36 H361b 2.066(5) . . ? C36 H361c 2.061(4) . . ? H121a H121b 1.551(2) . . ? H121a H121c 1.5495(12) . . ? H121a H13 2.0735(11) . . ? H121b H121c 1.5495(12) . . ? H122a H122b 1.5514(16) . . ? H122a H122c 1.5488(7) . . ? H122b H122c 1.5488(12) . . ? H122b H13 2.3703(14) . . ? H123a H123b 1.5514(6) . . ? H123a H123c 1.5436(12) . . ? H123b H123c 1.5437(7) . . ? H13 H14 2.339(2) . . ? H14 H15 2.3255(19) . . ? H161a H161b 1.5513(6) . . ? H161a H161c 1.658(3) . . ? H161a H33 2.347(2) . 1_544 ? H161b H161c 1.6583(14) . . ? H161c H222a 2.3684(10) . . ? H161c H361a 2.352(2) . 2 ? H221a H221b 1.5513(14) . . ? H221a H221c 1.5472(7) . . ? H221a H23 2.1017(9) . . ? H221b H221c 1.5472(9) . . ? H222a H222b 1.5513(16) . . ? H222a H222c 1.5489(7) . . ? H222b H222c 1.5488(6) . . ? H223a H223b 1.551(2) . . ? H223a H223c 1.5461(10) . . ? H223b H223c 1.5462(6) . . ? H23 H24 2.2682(10) . . ? H24 H25 2.3695(9) . . ? H261a H261a 2.392(3) . 2_565 ? H261a H261b 1.5513(10) . . ? H261a H261c 1.516(2) . . ? H261b H261c 1.5165(10) . . ? H321a H321b 1.5514(6) . . ? H321a H321c 1.5512(10) . . ? H321a H33 2.1206(9) . . ? H321b H321c 1.551(2) . . ? H322a H322b 1.5513(13) . . ? H322a H322c 1.5452(13) . . ? H322b H322c 1.5453(10) . . ? H322b H33 2.2776(18) . . ? H323a H323b 1.5513(10) . . ? H323a H323c 1.544(2) . . ? H323b H323c 1.5440(13) . . ? H33 H34 2.3884(11) . . ? H34 H35 2.331(3) . . ? H361a H361b 1.6737(12) . . ? H361a H361c 1.6738(7) . . ? H361b H361b 2.2409(19) . 2_556 ? H361b H361c 1.5513(9) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC N11 Sb N12 56.25(11) . . . ? N11 Sb N21 118.60(12) . . . ? N11 Sb N22 83.84(13) . . . ? N11 Sb N31 119.30(11) . . . ? N11 Sb N32 152.91(11) . . . ? N12 Sb N21 155.14(10) . . . ? N12 Sb N22 99.28(12) . . . ? N12 Sb N31 84.82(11) . . . ? N12 Sb N32 97.14(14) . . . ? N21 Sb N22 56.28(11) . . . ? N21 Sb N31 114.75(11) . . . ? N21 Sb N32 82.97(15) . . . ? N22 Sb N31 153.13(9) . . . ? N22 Sb N32 97.05(13) . . . ? N31 Sb N32 56.09(11) . . . ? Sb N11 C12 84.5(2) . . . ? Sb N11 C16 150.3(3) . . . ? C12 N11 C16 121.8(4) . . . ? N11 C12 N12 114.3(4) . . . ? N11 C12 C13 118.9(3) . . . ? N12 C12 C13 126.7(4) . . . ? Sb N12 C12 102.7(2) . . . ? Sb N12 Si1 134.26(15) . . . ? C12 N12 Si1 120.3(3) . . . ? N12 Si1 C121 111.69(18) . . . ? N12 Si1 C122 110.85(17) . . . ? N12 Si1 C123 112.4(2) . . . ? C121 Si1 C122 108.8(3) . . . ? C121 Si1 C123 104.34(19) . . . ? C122 Si1 C123 108.5(2) . . . ? Si1 C121 H121a 111.1(3) . . . ? Si1 C121 H121b 108.3(4) . . . ? Si1 C121 H121c 113.9(4) . . . ? H121a C121 H121b 104.7(4) . . . ? H121a C121 H121c 111.6(6) . . . ? H121b C121 H121c 106.6(3) . . . ? Si1 C122 H122a 111.8(5) . . . ? Si1 C122 H122b 110.5(4) . . . ? Si1 C122 H122c 112.4(3) . . . ? H122a C122 H122b 107.6(4) . . . ? H122a C122 H122c 108.0(5) . . . ? H122b C122 H122c 106.4(6) . . . ? Si1 C123 H123a 109.5(3) . . . ? Si1 C123 H123b 110.8(3) . . . ? Si1 C123 H123c 114.9(4) . . . ? H123a C123 H123b 106.8(5) . . . ? H123a C123 H123c 106.2(3) . . . ? H123b C123 H123c 108.2(4) . . . ? C12 C13 C14 119.1(4) . . . ? C12 C13 H13 119.3(3) . . . ? C14 C13 H13 121.6(5) . . . ? C13 C14 C15 120.9(4) . . . ? C13 C14 H14 120.5(5) . . . ? C15 C14 H14 118.6(3) . . . ? C14 C15 C16 118.4(3) . . . ? C14 C15 H15 120.9(5) . . . ? C16 C15 H15 120.7(5) . . . ? N11 C16 C15 120.7(4) . . . ? N11 C16 C161 116.0(4) . . . ? C15 C16 C161 123.2(3) . . . ? C16 C161 H161a 106.5(4) . . . ? C16 C161 H161b 106.8(4) . . . ? C16 C161 H161c 119.7(3) . . . ? H161a C161 H161b 107.5(3) . . . ? H161a C161 H161c 107.8(5) . . . ? H161b C161 H161c 108.0(5) . . . ? Sb N21 C22 84.9(2) . . . ? Sb N21 C26 149.7(2) . . . ? C22 N21 C26 121.2(4) . . . ? N21 C22 N22 113.5(4) . . . ? N21 C22 C23 119.3(4) . . . ? N22 C22 C23 127.3(3) . . . ? Sb N22 C22 103.0(2) . . . ? Sb N22 Si2 133.4(2) . . . ? C22 N22 Si2 121.1(3) . . . ? N22 Si2 C221 112.1(2) . . . ? N22 Si2 C222 111.19(18) . . . ? N22 Si2 C223 111.5(2) . . . ? C221 Si2 C222 107.2(3) . . . ? C221 Si2 C223 105.5(2) . . . ? C222 Si2 C223 109.1(3) . . . ? Si2 C221 H221a 113.1(3) . . . ? Si2 C221 H221b 108.1(5) . . . ? Si2 C221 H221c 113.9(5) . . . ? H221a C221 H221b 106.2(5) . . . ? H221a C221 H221c 111.5(7) . . . ? H221b C221 H221c 103.3(4) . . . ? Si2 C222 H222a 109.4(4) . . . ? Si2 C222 H222b 109.2(4) . . . ? Si2 C222 H222c 112.4(3) . . . ? H222a C222 H222b 107.2(4) . . . ? H222a C222 H222c 109.0(5) . . . ? H222b C222 H222c 109.5(6) . . . ? Si2 C223 H223a 106.3(5) . . . ? Si2 C223 H223b 108.3(3) . . . ? Si2 C223 H223c 110.1(5) . . . ? H223a C223 H223b 110.9(6) . . . ? H223a C223 H223c 109.0(3) . . . ? H223b C223 H223c 112.1(6) . . . ? C22 C23 C24 118.7(4) . . . ? C22 C23 H23 124.1(5) . . . ? C24 C23 H23 117.0(5) . . . ? C23 C24 C25 120.8(5) . . . ? C23 C24 H24 117.2(5) . . . ? C25 C24 H24 121.5(5) . . . ? C24 C25 C26 118.4(5) . . . ? C24 C25 H25 121.2(5) . . . ? C26 C25 H25 120.3(4) . . . ? N21 C26 C25 121.5(4) . . . ? N21 C26 C261 115.7(4) . . . ? C25 C26 C261 122.8(4) . . . ? C26 C261 H261a 112.7(5) . . . ? C26 C261 H261b 109.1(4) . . . ? C26 C261 H261c 116.1(4) . . . ? H261a C261 H261b 107.0(4) . . . ? H261a C261 H261c 107.6(4) . . . ? H261b C261 H261c 103.6(6) . . . ? N32 Si3 C321 111.0(2) . . . ? N32 Si3 C322 111.80(18) . . . ? N32 Si3 C323 112.70(18) . . . ? C321 Si3 C322 108.4(2) . . . ? C321 Si3 C323 105.8(2) . . . ? C322 Si3 C323 106.8(3) . . . ? Sb N31 C32 83.8(2) . . . ? Sb N31 C36 150.58(17) . . . ? C32 N31 C36 121.7(3) . . . ? N31 C32 N32 114.5(3) . . . ? N31 C32 C33 118.5(3) . . . ? N32 C32 C33 127.0(3) . . . ? Sb N32 Si3 134.1(2) . . . ? Sb N32 C32 103.23(17) . . . ? Si3 N32 C32 120.3(2) . . . ? Si3 C321 H321a 111.3(3) . . . ? Si3 C321 H321b 109.4(3) . . . ? Si3 C321 H321c 114.2(5) . . . ? H321a C321 H321b 104.1(5) . . . ? H321a C321 H321c 109.9(4) . . . ? H321b C321 H321c 107.4(4) . . . ? Si3 C322 H322a 110.4(4) . . . ? Si3 C322 H322b 110.6(5) . . . ? Si3 C322 H322c 112.8(4) . . . ? H322a C322 H322b 109.0(5) . . . ? H322a C322 H322c 106.7(6) . . . ? H322b C322 H322c 107.1(4) . . . ? Si3 C323 H323a 108.2(5) . . . ? Si3 C323 H323b 110.4(3) . . . ? Si3 C323 H323c 113.2(4) . . . ? H323a C323 H323b 109.1(5) . . . ? H323a C323 H323c 106.5(4) . . . ? H323b C323 H323c 109.3(7) . . . ? C32 C33 C34 119.5(3) . . . ? C32 C33 H33 118.7(4) . . . ? C34 C33 H33 121.6(3) . . . ? C33 C34 C35 121.1(3) . . . ? C33 C34 H34 121.5(3) . . . ? C35 C34 H34 117.3(4) . . . ? C34 C35 C36 117.8(4) . . . ? C34 C35 H35 120.6(3) . . . ? C36 C35 H35 121.6(4) . . . ? N31 C36 C35 121.3(3) . . . ? N31 C36 C361 115.9(3) . . . ? C35 C36 C361 122.7(4) . . . ? C36 C361 H361a 106.4(4) . . . ? C36 C361 H361b 111.5(3) . . . ? C36 C361 H361c 112.2(3) . . . ? H361a C361 H361b 109.2(4) . . . ? H361a C361 H361c 110.5(4) . . . ? H361b C361 H361c 107.1(5) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min -12 _reflns_limit_k_max 12 _reflns_limit_l_min -12 _reflns_limit_l_max 12 _reflns_number_total 4362 #ActaC _reflns_number_gt 4017 #ActaC _reflns_threshold_expression refl_observed_if_I____>3.000_sigma(I___) _reflns_d_resolution_high .928 _reflns_d_resolution_low 14.122 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? .63541 #end--------------------------