Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bhargava, Suresh K.' 'Mohr, Fabian' 'Papadopoulos, Stavroula' 'Raston, Colin' 'Skelton, Brian W.' 'van den Ancker, Tania R.' 'White, Allan H.' # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Prof Suresh K Bhargava' _publ_contact_author_address ; Department of Applied Chemistry RMIT University GPO Box 2476V Melbourne Victoria 3001 AUSTRALIA ; _publ_contact_author_email SURESH.BHARGAVA@RMIT.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 ? _publ_requested_category ? _publ_section_title ; #<< paper title text Syntheses and Crystal Structures of Binuclear Gold(I), Silver(I) and Copper(I) Complexes Containing Bulky Pyridyl Functionalised Alkyl Lignds ; _publ_section_title_footnote ; ? #<< paper footnote 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. ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_ausi _database_code_CSD 165353 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C13 H24 Au1 N1 Si2' _chemical_formula_moiety ? _chemical_formula_weight 447.48 _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 11.953(2) _cell_length_b 8.732(8) _cell_length_c 8.416(7) _cell_angle_alpha 81.40(7) _cell_angle_beta 76.82(5) _cell_angle_gamma 72.22(5) _cell_volume 811.4(11) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.832 _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 23.0 _cell_measurement_theta_max 28.5 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 9.195 _exptl_crystal_description block _exptl_crystal_size_max .58 _exptl_crystal_size_mid .42 _exptl_crystal_size_min .14 _exptl_crystal_size_rad ? _exptl_crystal_colour light_brown _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .072 _exptl_absorpt_correction_T_max .29 _diffrn_reflns_number 6489 _reflns_number_total 4722 _reflns_Friedel_coverage ? _reflns_number_gt 4722 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 32.47 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .067 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .038 _refine_ls_wR_factor_ref .045 _refine_ls_goodness_of_fit_ref 1.93 _refine_ls_number_reflns 4188 _refine_ls_number_parameters 155 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .045 _refine_diff_density_min -1.634 _refine_diff_density_max 2.917 _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 ADDREF' _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 26 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 0 .007996 .005981 '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' Si ? 0 4 .072021 .070984 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 2 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 2 -2.688 8.798 '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 Au .96586(2) .89631(2) .62292(3) .03250(18) Uani ? ? 1.00000 ? ? N1 1.1495(5) .7704(6) .5979(6) .034(3) Uani ? ? 1.00000 ? ? C2 1.2356(6) .8314(7) .4962(8) .037(4) Uani ? ? 1.00000 ? ? C2' 1.2098(5) .9560(7) .3534(7) .034(4) Uani ? ? 1.00000 ? ? Si1 1.29677(17) 1.1100(2) .3172(2) .0431(14) Uani ? ? 1.00000 ? ? C11 1.4649(8) 1.0354(12) .2542(13) .071(8) Uani ? ? 1.00000 ? ? C12 1.2583(9) 1.2629(10) .1450(13) .071(8) Uani ? ? 1.00000 ? ? C13 1.2633(10) 1.2130(12) .5095(13) .079(10) Uani ? ? 1.00000 ? ? Si2 1.22098(17) .8394(2) .1754(2) .0404(13) Uani ? ? 1.00000 ? ? C21 1.3716(8) .6880(10) .1279(12) .071(8) Uani ? ? 1.00000 ? ? C22 1.1950(9) .9687(10) -.0183(10) .066(8) Uani ? ? 1.00000 ? ? C23 1.1092(9) .7187(10) .2263(11) .064(8) Uani ? ? 1.00000 ? ? C3 1.3538(7) .7630(9) .5167(10) .052(6) Uani ? ? 1.00000 ? ? C4 1.3853(7) .6369(9) .6318(10) .055(6) Uani ? ? 1.00000 ? ? C5 1.2986(7) .5727(8) .7248(9) .050(6) Uani ? ? 1.00000 ? ? C6 1.1816(6) .6398(7) .7063(8) .041(5) Uani ? ? 1.00000 ? ? C6' 1.0853(7) .5709(9) .8042(11) .060(7) Uani ? ? 1.00000 ? ? H11a 1.49472 .95675 .33592 .10500 Uiso ? ? 1.00000 ? ? H11b 1.48261 .98618 .15343 .10500 Uiso ? ? 1.00000 ? ? H11c 1.50979 1.11270 .23489 .10500 Uiso ? ? 1.00000 ? ? H12a 1.27653 1.20846 .05138 .10400 Uiso ? ? 1.00000 ? ? H12b 1.17587 1.31601 .17257 .10400 Uiso ? ? 1.00000 ? ? H12c 1.30269 1.33916 .13058 .10400 Uiso ? ? 1.00000 ? ? H13a 1.17775 1.26596 .53507 .13600 Uiso ? ? 1.00000 ? ? H13b 1.28393 1.13670 .59693 .13600 Uiso ? ? 1.00000 ? ? H13c 1.30485 1.29118 .49141 .13600 Uiso ? ? 1.00000 ? ? H21a 1.43153 .74501 .10040 .09600 Uiso ? ? 1.00000 ? ? H21b 1.38471 .61593 .22171 .09600 Uiso ? ? 1.00000 ? ? H21c 1.37767 .63023 .03865 .09600 Uiso ? ? 1.00000 ? ? H22a 1.11589 1.04100 .00367 .10000 Uiso ? ? 1.00000 ? ? H22b 1.25147 1.02763 -.04744 .10000 Uiso ? ? 1.00000 ? ? H22c 1.19983 .90931 -.10617 .10000 Uiso ? ? 1.00000 ? ? H23a 1.12138 .64743 .32038 .10300 Uiso ? ? 1.00000 ? ? H23b 1.02904 .79294 .24942 .10300 Uiso ? ? 1.00000 ? ? H23c 1.11296 .66153 .13758 .10300 Uiso ? ? 1.00000 ? ? H3 1.41371 .80566 .45115 .06100 Uiso ? ? 1.00000 ? ? H4 1.46592 .59409 .64532 .06700 Uiso ? ? 1.00000 ? ? H5 1.31986 .48108 .80131 .05600 Uiso ? ? 1.00000 ? ? H6'a 1.03413 .64485 .87863 .08600 Uiso ? ? 1.00000 ? ? H6'b 1.12075 .47220 .86270 .08600 Uiso ? ? 1.00000 ? ? H6'c 1.03951 .55114 .73258 .08600 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 Au .03108(13) .02850(12) .03237(13) -.00523(8) -.00589(8) .00732(8) N1 .035(2) .032(2) .032(2) -.007(2) -.008(2) .0053(18) C2 .038(3) .032(2) .037(3) -.009(2) -.005(3) .000(2) C2' .028(3) .037(3) .034(3) -.008(2) -.005(2) .004(2) Si1 .0408(9) .0409(8) .0481(10) -.0166(8) -.0084(8) .0048(7) C11 .043(4) .079(6) .087(6) -.025(4) -.008(4) .017(5) C12 .063(5) .056(4) .094(7) -.025(4) -.029(5) .035(4) C13 .085(7) .085(6) .078(6) -.036(6) -.008(5) -.027(5) Si2 .0403(9) .0373(8) .0391(9) -.0050(7) -.0084(7) -.0008(7) C21 .058(5) .064(5) .073(6) .014(4) -.013(4) -.020(4) C22 .086(7) .062(5) .045(4) -.010(4) -.024(4) .003(4) C23 .073(6) .063(4) .066(5) -.034(4) -.005(4) -.020(4) C3 .038(3) .052(4) .058(4) -.009(3) -.014(3) .018(3) C4 .041(4) .052(4) .067(5) -.003(3) -.027(4) .018(3) C5 .055(4) .037(3) .044(4) .004(3) -.015(3) .011(3) C6 .047(4) .037(3) .035(3) -.008(3) -.011(3) .008(2) C6' .050(4) .053(4) .065(5) -.012(3) -.011(4) .026(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 Au N1 . . 2.111(5) ? Au Au . '2 776' 2.6904(16) ? Au C2' . '2 776' 2.084(5) ? N1 C2 . . 1.368(9) ? N1 C6 . . 1.364(8) ? C2 C2' . . 1.515(8) ? C2 C3 . . 1.396(11) ? C2' Si1 . . 1.889(7) ? C2' Si2 . . 1.892(7) ? Si1 C11 . . 1.887(9) ? Si1 C12 . . 1.856(10) ? Si1 C13 . . 1.873(12) ? C11 H11a . . .945 ? C11 H11b . . .959 ? C11 H11c . . .958 ? C12 H12a . . .930 ? C12 H12b . . .943 ? C12 H12c . . .950 ? C13 H13a . . .973 ? C13 H13b . . .939 ? C13 H13c . . .937 ? Si2 C21 . . 1.878(8) ? Si2 C22 . . 1.869(8) ? Si2 C23 . . 1.882(11) ? C21 H21a . . .960 ? C21 H21b . . .944 ? C21 H21c . . .943 ? C22 H22a . . .958 ? C22 H22b . . .938 ? C22 H22c . . .947 ? C23 H23a . . .941 ? C23 H23b . . .974 ? C23 H23c . . .944 ? C3 C4 . . 1.374(11) ? C3 H3 . . .937 ? C4 C5 . . 1.362(11) ? C4 H4 . . .948 ? C5 C6 . . 1.377(10) ? C5 H5 . . .957 ? C6 C6' . . 1.486(11) ? C6' H6'a . . .943 ? C6' H6'b . . .954 ? C6' H6'c . . .965 ? 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 N1 Au Au . . '2 776' 86.12(14) ? N1 Au C2' . . '2 776' 173.6(2) ? Au Au C2' '2 776' . '2 776' 89.47(16) ? Au N1 C2 . . . 121.6(4) ? Au N1 C6 . . . 117.6(4) ? C2 N1 C6 . . . 119.9(6) ? N1 C2 C2' . . . 122.9(6) ? N1 C2 C3 . . . 117.6(6) ? C2' C2 C3 . . . 119.2(6) ? C2 C2' Si1 . . . 114.2(5) ? C2 C2' Si2 . . . 106.2(4) ? C2 C2' Au . . '2 776' 115.4(4) ? Si1 C2' Si2 . . . 117.7(3) ? Si1 C2' Au . . '2 776' 101.5(3) ? Si2 C2' Au . . '2 776' 101.4(3) ? C2' Si1 C11 . . . 117.6(4) ? C2' Si1 C12 . . . 112.3(4) ? C2' Si1 C13 . . . 108.4(4) ? C11 Si1 C12 . . . 101.3(4) ? C11 Si1 C13 . . . 107.4(5) ? C12 Si1 C13 . . . 109.5(4) ? Si1 C11 H11a . . . 108.5 ? Si1 C11 H11b . . . 107.7 ? Si1 C11 H11c . . . 118.2 ? H11a C11 H11b . . . 109.1 ? H11a C11 H11c . . . 107.1 ? H11b C11 H11c . . . 105.9 ? Si1 C12 H12a . . . 107.5 ? Si1 C12 H12b . . . 107.2 ? Si1 C12 H12c . . . 110.3 ? H12a C12 H12b . . . 111.9 ? H12a C12 H12c . . . 110.5 ? H12b C12 H12c . . . 109.4 ? Si1 C13 H13a . . . 108.6 ? Si1 C13 H13b . . . 110.1 ? Si1 C13 H13c . . . 108.7 ? H13a C13 H13b . . . 108.4 ? H13a C13 H13c . . . 109.0 ? H13b C13 H13c . . . 112.0 ? C2' Si2 C21 . . . 111.5(4) ? C2' Si2 C22 . . . 114.1(4) ? C2' Si2 C23 . . . 110.8(3) ? C21 Si2 C22 . . . 107.2(4) ? C21 Si2 C23 . . . 105.5(4) ? C22 Si2 C23 . . . 107.2(5) ? Si2 C21 H21a . . . 108.2 ? Si2 C21 H21b . . . 109.1 ? Si2 C21 H21c . . . 111.7 ? H21a C21 H21b . . . 109.1 ? H21a C21 H21c . . . 108.6 ? H21b C21 H21c . . . 110.0 ? Si2 C22 H22a . . . 107.4 ? Si2 C22 H22b . . . 108.4 ? Si2 C22 H22c . . . 113.4 ? H22a C22 H22b . . . 109.8 ? H22a C22 H22c . . . 108.0 ? H22b C22 H22c . . . 109.7 ? Si2 C23 H23a . . . 110.4 ? Si2 C23 H23b . . . 108.5 ? Si2 C23 H23c . . . 111.6 ? H23a C23 H23b . . . 108.2 ? H23a C23 H23c . . . 110.5 ? H23b C23 H23c . . . 107.6 ? C2 C3 C4 . . . 122.3(7) ? C2 C3 H3 . . . 119.0 ? C4 C3 H3 . . . 118.7 ? C3 C4 C5 . . . 118.7(8) ? C3 C4 H4 . . . 120.8 ? C5 C4 H4 . . . 120.5 ? C4 C5 C6 . . . 119.5(6) ? C4 C5 H5 . . . 119.6 ? C6 C5 H5 . . . 120.9 ? N1 C6 C5 . . . 121.8(6) ? N1 C6 C6' . . . 117.5(6) ? C5 C6 C6' . . . 120.7(6) ? C6 C6' H6'a . . . 109.2 ? C6 C6' H6'b . . . 109.0 ? C6 C6' H6'c . . . 109.8 ? H6'a C6' H6'b . . . 109.8 ? H6'a C6' H6'c . . . 109.1 ? H6'b C6' H6'c . . . 109.9 ? 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 #-------------------------------------------------------------------------- _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_000 432 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 9 6 7 -9 -6 -7 15 0 0 -15 0 0 0 10 0 0 -10 0 0 0 9 0 0 -9 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min -11 _reflns_limit_k_max 12 _reflns_limit_l_min -12 _reflns_limit_l_max 12 _reflns_number_observed ? _reflns_d_resolution_high .662 _reflns_d_resolution_low 11.167 _diffrn_reflns_av_sigmaI/netI .059 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .042 _refine_ls_wR_factor_all .046 _refine_ls_goodness_of_fit_all 1.85 _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 #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_cusi _database_code_CSD 165354 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C32 H64 Cu2 N2 Si6' _chemical_formula_moiety ? _chemical_formula_weight 772.49 _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 12.156(5) _cell_length_b 20.980(10) _cell_length_c 18.848(6) _cell_angle_alpha 90.00000 _cell_angle_beta 110.78(3) _cell_angle_gamma 90.00000 _cell_volume 4494(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 12.4 _cell_measurement_theta_max 18.4 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.127 _exptl_crystal_description block _exptl_crystal_size_max .58 _exptl_crystal_size_mid .45 _exptl_crystal_size_min .36 _exptl_crystal_size_rad ? _exptl_crystal_colour green _diffrn_measurement_device_type ; CAD4 diffractometer ; _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 .60 _exptl_absorpt_correction_T_max .73 _diffrn_reflns_number 12497 _reflns_number_total 7892 _reflns_Friedel_coverage ? _reflns_number_gt 4838 _reflns_threshold_expression 'I > 3.00 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 .053 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 10 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .048 _refine_ls_wR_factor_ref .051 _refine_ls_goodness_of_fit_ref 1.999 _refine_ls_number_reflns 4838 _refine_ls_number_parameters 408 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .042 _refine_diff_density_min -.41 _refine_diff_density_max .40 _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 ? 0 128 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 0 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 256 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 24 .072 .071 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 8 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 8 .263 1.266 '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 Cu1 .26164(5) .75790(3) .53975(3) .0585(3) Uani ? ? 1.00000 ? ? N11 .1808(3) .83879(16) .5185(2) .054(2) Uani ? ? 1.00000 ? ? C12 .0596(4) .8369(2) .4924(2) .054(3) Uani ? ? 1.00000 ? ? C12' -.0020(4) .77989(19) .5073(2) .049(2) Uani ? ? 1.00000 ? ? Si11 -.11750(12) .75001(7) .41803(8) .0652(8) Uani ? ? 1.00000 ? ? C111 -.0601(7) .7504(4) .3404(4) .145(6) Uani ? ? 1.00000 ? ? C112 -.2591(6) .7950(3) .3804(4) .140(5) Uani ? ? 1.00000 ? ? C113 -.1652(6) .6676(3) .4262(4) .114(4) Uani ? ? 1.00000 ? ? Si12 -.05143(13) .80033(7) .58781(8) .0675(8) Uani ? ? 1.00000 ? ? C121 -.1402(7) .7365(3) .6107(4) .127(5) Uani ? ? 1.00000 ? ? C122 -.1464(7) .8717(3) .5730(4) .142(6) Uani ? ? 1.00000 ? ? C123 .0780(6) .8155(5) .6753(4) .168(7) Uani ? ? 1.00000 ? ? C13 -.0014(4) .8907(2) .4553(3) .068(3) Uani ? ? 1.00000 ? ? C14 .0568(5) .9442(2) .4452(3) .085(3) Uani ? ? 1.00000 ? ? C15 .1760(5) .9455(2) .4736(3) .077(3) Uani ? ? 1.00000 ? ? C16 .2356(4) .8931(2) .5101(3) .071(3) Uani ? ? 1.00000 ? ? C16' .3678(5) .8940(3) .5499(4) .096(4) Uani ? ? 1.00000 ? ? Si13 .42482(18) .94943(10) .63389(14) .1283(15) Uani ? ? 1.00000 ? ? C131 .5940(13) .9457(11) .6524(14) .25(2) Uani ? ? .50000 ? ? C131' .5576(17) .9224(10) .7071(13) .24(2) Uani ? ? .50000 ? ? C132 .3783(17) 1.0317(7) .6062(12) .248(16) Uani ? ? .50000 ? ? C132' .4642(18) 1.0259(8) .6111(12) .212(17) Uani ? ? .50000 ? ? C133 .3860(16) .9125(9) .7060(9) .173(15) Uani ? ? .50000 ? ? C133' .3064(15) .9629(10) .6808(11) .203(17) Uani ? ? .50000 ? ? Cu2 .08949(5) .70238(3) .54546(3) .0510(3) Uani ? ? 1.00000 ? ? N21 .1715(3) .62185(16) .56998(19) .052(2) Uani ? ? 1.00000 ? ? C22' .3410(4) .6753(2) .5499(3) .059(3) Uani ? ? 1.00000 ? ? Si21 .38140(16) .67346(9) .46235(10) .0925(11) Uani ? ? 1.00000 ? ? C211 .2574(7) .6401(5) .3827(4) .164(7) Uani ? ? 1.00000 ? ? C212 .4085(7) .7527(4) .4302(5) .158(7) Uani ? ? 1.00000 ? ? C213 .5139(7) .6246(4) .4673(5) .147(6) Uani ? ? 1.00000 ? ? Si22 .46333(13) .68607(8) .64287(9) .0808(10) Uani ? ? 1.00000 ? ? C221 .5701(5) .7484(4) .6417(4) .133(5) Uani ? ? 1.00000 ? ? C222 .5518(7) .6125(4) .6772(5) .178(6) Uani ? ? 1.00000 ? ? C223 .4018(6) .7086(4) .7173(4) .144(6) Uani ? ? 1.00000 ? ? C22 .2748(4) .6168(2) .5560(3) .063(3) Uani ? ? 1.00000 ? ? C23 .3177(5) .5554(2) .5514(3) .079(3) Uani ? ? 1.00000 ? ? C24 .2601(5) .5027(2) .5610(4) .091(4) Uani ? ? 1.00000 ? ? C25 .1604(5) .5088(2) .5770(3) .078(3) Uani ? ? 1.00000 ? ? C26 .1192(4) .5689(2) .5833(3) .058(3) Uani ? ? 1.00000 ? ? C26' .0122(4) .5770(2) .6041(3) .065(3) Uani ? ? 1.00000 ? ? Si23 .03295(15) .55900(8) .70631(10) .0853(11) Uani ? ? 1.00000 ? ? C231 -.1075(6) .5720(4) .7189(4) .132(6) Uani ? ? 1.00000 ? ? C232 .0759(7) .4750(4) .7287(4) .155(6) Uani ? ? 1.00000 ? ? C233 .1469(6) .6132(4) .7677(4) .156(6) Uani ? ? 1.00000 ? ? H111a -.10990 .73550 .29492 .21600 Uiso ? ? 1.00000 ? ? H111b .01332 .72156 .35494 .21600 Uiso ? ? 1.00000 ? ? H111c -.02767 .79142 .33476 .21600 Uiso ? ? 1.00000 ? ? H112a -.29575 .79544 .41988 .18600 Uiso ? ? 1.00000 ? ? H112b -.24498 .83862 .37211 .18600 Uiso ? ? 1.00000 ? ? H112c -.32127 .78080 .33588 .18600 Uiso ? ? 1.00000 ? ? H113a -.09854 .63844 .43999 .15100 Uiso ? ? 1.00000 ? ? H113b -.19609 .66453 .46738 .15100 Uiso ? ? 1.00000 ? ? H113c -.22365 .65046 .38241 .15100 Uiso ? ? 1.00000 ? ? H121a -.21230 .72768 .56578 .16700 Uiso ? ? 1.00000 ? ? H121b -.09918 .69669 .62219 .16700 Uiso ? ? 1.00000 ? ? H121c -.16957 .74505 .65078 .16700 Uiso ? ? 1.00000 ? ? H122a -.10857 .90852 .56177 .20000 Uiso ? ? 1.00000 ? ? H122b -.21831 .86538 .52722 .20000 Uiso ? ? 1.00000 ? ? H122c -.17536 .88348 .61185 .20000 Uiso ? ? 1.00000 ? ? H123a .12913 .77946 .68864 .22700 Uiso ? ? 1.00000 ? ? H123b .12422 .85098 .66684 .22700 Uiso ? ? 1.00000 ? ? H123c .05577 .82674 .71703 .22700 Uiso ? ? 1.00000 ? ? H13 -.08925 .88897 .43582 .08200 Uiso ? ? 1.00000 ? ? H14 .01046 .98053 .41840 .10200 Uiso ? ? 1.00000 ? ? H15 .21609 .98481 .46738 .08400 Uiso ? ? 1.00000 ? ? H16'a .41753 .84733 .57308 .12000 Uiso ? ? 1.00000 ? ? H16'b .39377 .90835 .50757 .12000 Uiso ? ? 1.00000 ? ? H131a .62419 .90549 .66429 .30000 Uiso ? ? .50000 ? ? H131b .60980 .96291 .60988 .30000 Uiso ? ? .50000 ? ? H131c .62135 .97509 .69455 .30000 Uiso ? ? .50000 ? ? H132a .40830 1.04770 .56705 .22500 Uiso ? ? .50000 ? ? H132b .29411 1.03680 .58436 .22500 Uiso ? ? .50000 ? ? H132c .40604 1.06261 .64700 .22500 Uiso ? ? .50000 ? ? H133a .30072 .90751 .69045 .23900 Uiso ? ? .50000 ? ? H133b .41945 .87103 .71846 .23900 Uiso ? ? .50000 ? ? H133c .41222 .93968 .74872 .23900 Uiso ? ? .50000 ? ? H131'a .54827 .88095 .72343 .26700 Uiso ? ? .50000 ? ? H131'b .62002 .91813 .68337 .26700 Uiso ? ? .50000 ? ? H131'c .59029 .94951 .74839 .26700 Uiso ? ? .50000 ? ? H132'a .51790 1.02548 .58288 .24700 Uiso ? ? .50000 ? ? H132'b .39021 1.04749 .56933 .24700 Uiso ? ? .50000 ? ? H132'c .48800 1.05764 .64766 .24700 Uiso ? ? .50000 ? ? H133'a .23627 .97985 .64344 .30000 Uiso ? ? .50000 ? ? H133'b .28568 .92189 .69627 .30000 Uiso ? ? .50000 ? ? H133'c .33318 .98975 .72237 .30000 Uiso ? ? .50000 ? ? H211a .23605 .59551 .39309 .18000 Uiso ? ? 1.00000 ? ? H211b .18290 .66311 .37167 .18000 Uiso ? ? 1.00000 ? ? H211c .27182 .63705 .33645 .18000 Uiso ? ? 1.00000 ? ? H212a .34708 .78301 .42299 .16700 Uiso ? ? 1.00000 ? ? H212b .47842 .77462 .47341 .16700 Uiso ? ? 1.00000 ? ? H212c .43547 .75635 .38863 .16700 Uiso ? ? 1.00000 ? ? H213a .58315 .64110 .50861 .16500 Uiso ? ? 1.00000 ? ? H213b .50478 .58139 .47955 .16500 Uiso ? ? 1.00000 ? ? H213c .53888 .62355 .42412 .16500 Uiso ? ? 1.00000 ? ? H221a .60474 .73811 .60231 .18300 Uiso ? ? 1.00000 ? ? H221b .53136 .78911 .62544 .18300 Uiso ? ? 1.00000 ? ? H221c .63512 .75572 .68654 .18300 Uiso ? ? 1.00000 ? ? H222a .50395 .57731 .68336 .18600 Uiso ? ? 1.00000 ? ? H222b .58632 .59708 .64037 .18600 Uiso ? ? 1.00000 ? ? H222c .61711 .61566 .72448 .18600 Uiso ? ? 1.00000 ? ? H223a .35971 .75034 .70359 .15400 Uiso ? ? 1.00000 ? ? H223b .35001 .67940 .72381 .15400 Uiso ? ? 1.00000 ? ? H223c .46438 .71729 .76545 .15400 Uiso ? ? 1.00000 ? ? H23 .39134 .55173 .54111 .09600 Uiso ? ? 1.00000 ? ? H24 .29119 .46100 .55612 .10800 Uiso ? ? 1.00000 ? ? H25 .11857 .47062 .58469 .09300 Uiso ? ? 1.00000 ? ? H26'a -.01979 .62059 .59130 .07900 Uiso ? ? 1.00000 ? ? H26'b -.05327 .54993 .57022 .07900 Uiso ? ? 1.00000 ? ? H231a -.13261 .61578 .70101 .17900 Uiso ? ? 1.00000 ? ? H231b -.16645 .54517 .67979 .17900 Uiso ? ? 1.00000 ? ? H231c -.14334 .56943 .75786 .17900 Uiso ? ? 1.00000 ? ? H232a .03828 .44522 .68855 .19500 Uiso ? ? 1.00000 ? ? H232b .16004 .46714 .74449 .19500 Uiso ? ? 1.00000 ? ? H232c .04948 .46999 .77012 .19500 Uiso ? ? 1.00000 ? ? H233a .22810 .60228 .78212 .20000 Uiso ? ? 1.00000 ? ? H233b .14311 .65890 .74940 .20000 Uiso ? ? 1.00000 ? ? H233c .12170 .61373 .81080 .20000 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 Cu2 .0475(3) .0531(3) .0515(3) .0057(3) .0164(3) .0041(3) N11 .051(2) .054(2) .057(2) -.0061(18) .019(2) -.006(2) C12 .071(3) .046(3) .047(3) .000(2) .022(2) -.005(2) C12' .044(3) .053(3) .045(3) .007(2) .011(2) .004(2) Si11 .0709(10) .0580(9) .0537(8) .0006(7) .0061(7) .0017(7) C111 .169(7) .205(8) .078(5) -.051(6) .065(5) -.046(5) C112 .101(5) .107(5) .144(7) .024(4) -.039(5) -.005(5) C113 .115(5) .086(4) .099(5) -.032(4) -.014(4) .015(4) Si12 .0724(10) .0735(10) .0613(9) .0039(8) .0297(8) -.0039(8) C121 .176(7) .093(5) .175(7) -.002(5) .142(6) -.004(5) C122 .233(9) .095(5) .128(6) .071(5) .102(6) .007(5) C123 .116(6) .314(12) .069(5) -.034(7) .027(4) -.072(6) C13 .066(3) .053(3) .078(4) .000(2) .017(3) .002(3) C14 .111(5) .051(3) .087(4) .003(3) .028(4) .010(3) C15 .091(4) .062(3) .079(4) -.015(3) .031(3) -.003(3) C16 .073(4) .064(3) .084(4) -.008(3) .038(3) -.007(3) C16' .068(4) .085(4) .136(6) -.018(3) .038(4) -.008(4) Si13 .0965(15) .1107(16) .149(2) -.0333(12) .0081(14) -.0192(15) C131 .070(11) .29(2) .36(3) -.087(14) .030(15) -.09(2) C131' .18(2) .22(2) .24(2) -.026(16) -.032(16) -.10(2) C132 .27(2) .082(11) .25(2) .024(13) -.081(18) -.087(14) C132' .27(2) .152(16) .20(2) -.113(16) .057(17) -.005(15) C133 .224(19) .203(18) .105(13) -.066(15) .072(13) -.058(13) C133' .158(16) .27(2) .22(2) -.091(15) .120(15) -.148(18) Cu1 .0508(4) .0632(4) .0629(4) .0010(3) .0220(3) -.0000(3) N21 .049(2) .053(2) .050(2) .0101(18) .0129(18) .0046(19) C22' .042(3) .076(3) .057(3) .007(2) .016(2) .001(3) Si21 .0983(13) .1210(15) .0726(11) .0250(11) .0482(10) .0066(11) C211 .162(7) .238(10) .078(5) .035(7) .024(5) -.019(6) C212 .207(9) .178(8) .154(7) .041(6) .144(7) .044(6) C213 .154(7) .165(7) .177(8) .045(6) .127(6) .005(6) Si22 .0566(9) .1041(13) .0708(11) .0040(9) .0091(8) .0043(10) C221 .077(5) .167(7) .132(6) -.026(5) .010(4) .015(6) C222 .146(7) .149(7) .149(7) .054(6) -.060(5) -.003(6) C223 .112(6) .247(9) .069(4) -.036(6) .030(4) -.035(5) C22 .066(3) .066(3) .057(3) .014(3) .022(3) .004(3) C23 .066(3) .077(4) .103(4) .021(3) .041(3) -.006(3) C24 .100(5) .055(3) .125(5) .019(3) .049(4) -.001(3) C25 .084(4) .055(3) .097(4) .006(3) .034(3) .002(3) C26 .065(3) .056(3) .049(3) .007(2) .014(2) .006(2) C26' .058(3) .063(3) .071(4) .003(2) .019(3) .007(3) Si23 .0873(12) .0990(13) .0754(11) -.0013(10) .0362(10) .0229(10) C231 .115(6) .164(7) .150(7) .001(5) .090(5) .024(6) C232 .201(9) .139(7) .135(7) .052(6) .072(7) .077(6) C233 .143(7) .239(9) .085(5) -.086(7) .040(5) .003(6) # 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 Cu2 C12' . . 1.957(4) ? Cu2 Cu1 . . 2.4305(12) ? Cu2 N21 . . 1.933(3) ? N11 C12 . . 1.378(6) ? N11 C16 . . 1.357(6) ? N11 Cu1 . . 1.931(3) ? C12 C12' . . 1.490(6) ? C12 C13 . . 1.394(6) ? C12' Si11 . . 1.875(4) ? C12' Si12 . . 1.870(5) ? Si11 C111 . . 1.831(9) ? Si11 C112 . . 1.868(7) ? Si11 C113 . . 1.848(6) ? C111 H111a . . .912 ? C111 H111b . . 1.031 ? C111 H111c . . .968 ? C112 H112a . . .994 ? C112 H112b . . .953 ? C112 H112c . . .956 ? C113 H113a . . .974 ? C113 H113b . . .977 ? C113 H113c . . .948 ? Si12 C121 . . 1.864(8) ? Si12 C122 . . 1.851(8) ? Si12 C123 . . 1.858(6) ? C121 H121a . . .996 ? C121 H121b . . .957 ? C121 H121c . . .960 ? C122 H122a . . .961 ? C122 H122b . . .996 ? C122 H122c . . .950 ? C123 H123a . . .955 ? C123 H123b . . .978 ? C123 H123c . . .948 ? C13 C14 . . 1.375(7) ? C13 H13 . . .999 ? C14 C15 . . 1.355(8) ? C14 H14 . . .976 ? C15 C16 . . 1.362(7) ? C15 H15 . . .986 ? C16 C16' . . 1.513(7) ? C16' Si13 . . 1.888(6) ? C16' H16'a . . 1.152 ? C16' H16'b . . 1.003 ? Si13 C131 . . 1.962(16) ? Si13 C131' . . 1.803(18) ? Si13 C132 . . 1.833(15) ? Si13 C132' . . 1.77(2) ? Si13 C133 . . 1.77(2) ? Si13 C133' . . 1.96(2) ? C131 H131a . . .91 ? C131 H131b . . .96 ? C131 H131c . . .97 ? C131' H131'a . . .94 ? C131' H131'b . . 1.01 ? C131' H131'c . . .93 ? C132 H132a . . .99 ? C132 H132b . . .96 ? C132 H132c . . .971 ? C132' H132'a . . .98 ? C132' H132'b . . 1.063 ? C132' H132'c . . .927 ? C133 H133a . . .977 ? C133 H133b . . .953 ? C133 H133c . . .945 ? C133' H133'a . . .961 ? C133' H133'b . . .97 ? C133' H133'c . . .93 ? Cu1 C22' . . 1.959(5) ? N21 C22 . . 1.375(7) ? N21 C26 . . 1.348(6) ? C22' Si21 . . 1.882(6) ? C22' Si22 . . 1.866(4) ? C22' C22 . . 1.495(7) ? Si21 C211 . . 1.847(7) ? Si21 C212 . . 1.838(9) ? Si21 C213 . . 1.884(8) ? C211 H211a . . 1.008 ? C211 H211b . . .982 ? C211 H211c . . .950 ? C212 H212a . . .953 ? C212 H212b . . 1.051 ? C212 H212c . . .954 ? C213 H213a . . .985 ? C213 H213b . . .951 ? C213 H213c . . .965 ? Si22 C221 . . 1.848(7) ? Si22 C222 . . 1.862(8) ? Si22 C223 . . 1.870(8) ? C221 H221a . . .999 ? C221 H221b . . .971 ? C221 H221c . . .942 ? C222 H222a . . .972 ? C222 H222b . . .983 ? C222 H222c . . .963 ? C223 H223a . . 1.000 ? C223 H223b . . .918 ? C223 H223c . . .972 ? C22 C23 . . 1.405(7) ? C23 C24 . . 1.354(8) ? C23 H23 . . .983 ? C24 C25 . . 1.355(9) ? C24 H24 . . .971 ? C25 C26 . . 1.376(7) ? C25 H25 . . .986 ? C26 C26' . . 1.496(8) ? C26' Si23 . . 1.890(6) ? C26' H26'a . . .990 ? C26' H26'b . . 1.001 ? Si23 C231 . . 1.826(8) ? Si23 C232 . . 1.845(8) ? Si23 C233 . . 1.847(7) ? C231 H231a . . .988 ? C231 H231b . . 1.000 ? C231 H231c . . .979 ? C232 H232a . . .962 ? C232 H232b . . .972 ? C232 H232c . . .950 ? C233 H233a . . .955 ? C233 H233b . . 1.014 ? C233 H233c . . .965 ? 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 C12' Cu2 Cu1 . . . 88.36(14) ? C12' Cu2 N21 . . . 172.66(16) ? Cu1 Cu2 N21 . . . 92.87(12) ? C12 N11 C16 . . . 119.3(4) ? C12 N11 Cu1 . . . 116.8(3) ? C16 N11 Cu1 . . . 121.8(3) ? N11 C12 C12' . . . 120.1(3) ? N11 C12 C13 . . . 117.9(4) ? C12' C12 C13 . . . 122.0(4) ? Cu2 C12' C12 . . . 118.6(3) ? Cu2 C12' Si11 . . . 101.5(2) ? Cu2 C12' Si12 . . . 101.3(2) ? C12 C12' Si11 . . . 111.5(3) ? C12 C12' Si12 . . . 107.2(3) ? Si11 C12' Si12 . . . 116.8(2) ? C12' Si11 C111 . . . 109.8(3) ? C12' Si11 C112 . . . 117.9(3) ? C12' Si11 C113 . . . 113.3(2) ? C111 Si11 C112 . . . 104.8(4) ? C111 Si11 C113 . . . 106.9(4) ? C112 Si11 C113 . . . 103.3(3) ? Si11 C111 H111a . . . 115.8 ? Si11 C111 H111b . . . 108.9 ? Si11 C111 H111c . . . 112.2 ? H111a C111 H111b . . . 105.8 ? H111a C111 H111c . . . 111.2 ? H111b C111 H111c . . . 101.7 ? Si11 C112 H112a . . . 108.5 ? Si11 C112 H112b . . . 110.6 ? Si11 C112 H112c . . . 120.7 ? H112a C112 H112b . . . 105.6 ? H112a C112 H112c . . . 103.6 ? H112b C112 H112c . . . 106.7 ? Si11 C113 H113a . . . 110.7 ? Si11 C113 H113b . . . 110.3 ? Si11 C113 H113c . . . 116.2 ? H113a C113 H113b . . . 105.4 ? H113a C113 H113c . . . 106.9 ? H113b C113 H113c . . . 106.7 ? C12' Si12 C121 . . . 113.7(3) ? C12' Si12 C122 . . . 115.2(3) ? C12' Si12 C123 . . . 110.2(3) ? C121 Si12 C122 . . . 103.6(4) ? C121 Si12 C123 . . . 107.2(4) ? C122 Si12 C123 . . . 106.3(4) ? Si12 C121 H121a . . . 110.1 ? Si12 C121 H121b . . . 112.4 ? Si12 C121 H121c . . . 117.0 ? H121a C121 H121b . . . 105.2 ? H121a C121 H121c . . . 104.0 ? H121b C121 H121c . . . 107.1 ? Si12 C122 H122a . . . 111.2 ? Si12 C122 H122b . . . 109.4 ? Si12 C122 H122c . . . 118.4 ? H122a C122 H122b . . . 104.9 ? H122a C122 H122c . . . 107.3 ? H122b C122 H122c . . . 104.6 ? Si12 C123 H123a . . . 111.4 ? Si12 C123 H123b . . . 109.9 ? Si12 C123 H123c . . . 112.2 ? H123a C123 H123b . . . 106.7 ? H123a C123 H123c . . . 109.1 ? H123b C123 H123c . . . 107.2 ? C12 C13 C14 . . . 121.4(4) ? C12 C13 H13 . . . 117.7 ? C14 C13 H13 . . . 120.9 ? C13 C14 C15 . . . 119.5(4) ? C13 C14 H14 . . . 118.6 ? C15 C14 H14 . . . 121.9 ? C14 C15 C16 . . . 119.0(5) ? C14 C15 H15 . . . 118.4 ? C16 C15 H15 . . . 122.6 ? N11 C16 C15 . . . 122.8(4) ? N11 C16 C16' . . . 115.6(4) ? C15 C16 C16' . . . 121.4(5) ? C16 C16' Si13 . . . 115.7(4) ? C16 C16' H16'a . . . 120.0 ? C16 C16' H16'b . . . 100.8 ? Si13 C16' H16'a . . . 102.6 ? Si13 C16' H16'b . . . 110.8 ? H16'a C16' H16'b . . . 106.6 ? C16' Si13 C131 . . . 100.0 ? C16' Si13 C131' . . . 114.3(7) ? C16' Si13 C132 . . . 110.9(6) ? C16' Si13 C132' . . . 114.0(7) ? C16' Si13 C133 . . . 104.8(6) ? C16' Si13 C133' . . . 110.9(6) ? C131 Si13 C132 . . . 106.7(10) ? C131 Si13 C133 . . . 113.2(9) ? C131' Si13 C132' . . . 103.0(9) ? C131' Si13 C133' . . . 107.6(10) ? C132 Si13 C133 . . . 119.5(10) ? C132' Si13 C133' . . . 106.5(10) ? Si13 C131 H131a . . . 112.6 ? Si13 C131 H131b . . . 110.1 ? Si13 C131 H131c . . . 98.8 ? H131a C131 H131b . . . 112 ? H131a C131 H131c . . . 113 ? H131b C131 H131c . . . 109 ? Si13 C131' H131'a . . . 111.1 ? Si13 C131' H131'b . . . 107.3 ? Si13 C131' H131'c . . . 116.6 ? H131'a C131' H131'b . . . 105 ? H131'a C131' H131'c . . . 111 ? H131'b C131' H131'c . . . 105.0 ? Si13 C132 H132a . . . 111.9 ? Si13 C132 H132b . . . 113.6 ? Si13 C132 H132c . . . 114.8 ? H132a C132 H132b . . . 105.0 ? H132a C132 H132c . . . 104.3 ? H132b C132 H132c . . . 106 ? Si13 C132' H132'a . . . 114.4 ? Si13 C132' H132'b . . . 109.6 ? Si13 C132' H132'c . . . 121 ? H132'a C132' H132'b . . . 98.8 ? H132'a C132' H132'c . . . 109 ? H132'b C132' H132'c . . . 101.8 ? Si13 C133 H133a . . . 111.1 ? Si13 C133 H133b . . . 112.4 ? Si13 C133 H133c . . . 106.7 ? H133a C133 H133b . . . 107.0 ? H133a C133 H133c . . . 109 ? H133b C133 H133c . . . 110.9 ? Si13 C133' H133'a . . . 109.0 ? Si13 C133' H133'b . . . 108.6 ? Si13 C133' H133'c . . . 112.1 ? H133'a C133' H133'b . . . 106.9 ? H133'a C133' H133'c . . . 110 ? H133'b C133' H133'c . . . 110 ? Cu2 Cu1 N11 . . . 92.72(12) ? Cu2 Cu1 C22' . . . 88.49(15) ? N11 Cu1 C22' . . . 174.00(19) ? Cu2 N21 C22 . . . 116.8(3) ? Cu2 N21 C26 . . . 121.9(3) ? C22 N21 C26 . . . 119.7(4) ? Cu1 C22' Si21 . . . 101.8(2) ? Cu1 C22' Si22 . . . 100.7(2) ? Cu1 C22' C22 . . . 118.3(3) ? Si21 C22' Si22 . . . 117.2(3) ? Si21 C22' C22 . . . 111.4(3) ? Si22 C22' C22 . . . 107.4(3) ? C22' Si21 C211 . . . 109.2(3) ? C22' Si21 C212 . . . 113.8(3) ? C22' Si21 C213 . . . 116.9(3) ? C211 Si21 C212 . . . 105.4(4) ? C211 Si21 C213 . . . 105.7(4) ? C212 Si21 C213 . . . 105.0(4) ? Si21 C211 H211a . . . 112.7 ? Si21 C211 H211b . . . 114.2 ? Si21 C211 H211c . . . 114.1 ? H211a C211 H211b . . . 102.5 ? H211a C211 H211c . . . 105.1 ? H211b C211 H211c . . . 107.2 ? Si21 C212 H212a . . . 115.3 ? Si21 C212 H212b . . . 109.3 ? Si21 C212 H212c . . . 119.8 ? H212a C212 H212b . . . 101.3 ? H212a C212 H212c . . . 108.0 ? H212b C212 H212c . . . 100.5 ? Si21 C213 H213a . . . 108.9 ? Si21 C213 H213b . . . 111.1 ? Si21 C213 H213c . . . 119.3 ? H213a C213 H213b . . . 106.5 ? H213a C213 H213c . . . 103.8 ? H213b C213 H213c . . . 106.4 ? C22' Si22 C221 . . . 113.8(3) ? C22' Si22 C222 . . . 113.3(3) ? C22' Si22 C223 . . . 109.7(3) ? C221 Si22 C222 . . . 105.6(3) ? C221 Si22 C223 . . . 107.4(4) ? C222 Si22 C223 . . . 106.6(4) ? Si22 C221 H221a . . . 109.8 ? Si22 C221 H221b . . . 111.2 ? Si22 C221 H221c . . . 118.3 ? H221a C221 H221b . . . 103.9 ? H221a C221 H221c . . . 105.2 ? H221b C221 H221c . . . 107.4 ? Si22 C222 H222a . . . 112.0 ? Si22 C222 H222b . . . 111.5 ? Si22 C222 H222c . . . 116.6 ? H222a C222 H222b . . . 105.0 ? H222a C222 H222c . . . 105.9 ? H222b C222 H222c . . . 105.0 ? Si22 C223 H223a . . . 109.4 ? Si22 C223 H223b . . . 114.0 ? Si22 C223 H223c . . . 111.0 ? H223a C223 H223b . . . 107.9 ? H223a C223 H223c . . . 103.7 ? H223b C223 H223c . . . 110.3 ? N21 C22 C22' . . . 120.3(4) ? N21 C22 C23 . . . 117.9(4) ? C22' C22 C23 . . . 121.8(5) ? C22 C23 C24 . . . 121.2(6) ? C22 C23 H23 . . . 117.9 ? C24 C23 H23 . . . 120.9 ? C23 C24 C25 . . . 120.0(5) ? C23 C24 H24 . . . 119.0 ? C25 C24 H24 . . . 121.0 ? C24 C25 C26 . . . 119.1(5) ? C24 C25 H25 . . . 120.3 ? C26 C25 H25 . . . 120.6 ? N21 C26 C25 . . . 121.9(5) ? N21 C26 C26' . . . 117.8(4) ? C25 C26 C26' . . . 120.2(5) ? C26 C26' Si23 . . . 115.5(3) ? C26 C26' H26'a . . . 110.1 ? C26 C26' H26'b . . . 109.7 ? Si23 C26' H26'a . . . 109.4 ? Si23 C26' H26'b . . . 109.0 ? H26'a C26' H26'b . . . 102.3 ? C26' Si23 C231 . . . 108.0(3) ? C26' Si23 C232 . . . 110.4(3) ? C26' Si23 C233 . . . 108.3(3) ? C231 Si23 C232 . . . 108.4(4) ? C231 Si23 C233 . . . 110.7(4) ? C232 Si23 C233 . . . 110.9(3) ? Si23 C231 H231a . . . 106.5 ? Si23 C231 H231b . . . 106.1 ? Si23 C231 H231c . . . 140.8 ? H231a C231 H231b . . . 102.6 ? H231a C231 H231c . . . 98.2 ? H231b C231 H231c . . . 97.4 ? Si23 C232 H232a . . . 115.0 ? Si23 C232 H232b . . . 114.4 ? Si23 C232 H232c . . . 98.2 ? H232a C232 H232b . . . 106.7 ? H232a C232 H232c . . . 111.7 ? H232b C232 H232c . . . 110.8 ? Si23 C233 H233a . . . 120.0 ? Si23 C233 H233b . . . 115.9 ? Si23 C233 H233c . . . 98.2 ? H233a C233 H233b . . . 104.0 ? H233a C233 H233c . . . 111.5 ? H233b C233 H233c . . . 106.6 ? 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 #-------------------------------------------------------------------------- _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 1672 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 6 9 10 -6 -9 -10 6 -9 10 -6 9 -10 11 0 0 -11 0 0 0 22 0 0 -22 0 0 0 16 0 0 -16 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min -22 _reflns_limit_l_max 22 _reflns_number_observed 4838 _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 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .076 _refine_ls_wR_factor_all .055 _refine_ls_goodness_of_fit_all 1.675 _refine_ls_shift/su_mean .001 #========================================================================== # 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_cusii _database_code_CSD 165355 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C13 H24 Cu1 N1 Si2' _chemical_formula_moiety ? _chemical_formula_weight 314.06 _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 11.494(5) _cell_length_b 9.257(3) _cell_length_c 9.058(4) _cell_angle_alpha 113.53(3) _cell_angle_beta 97.07(4) _cell_angle_gamma 104.56(3) _cell_volume 827.7(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.26 _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 17.2 _cell_measurement_theta_max 20.7 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.446 _exptl_crystal_description block _exptl_crystal_size_max .60 _exptl_crystal_size_mid .34 _exptl_crystal_size_min .24 _exptl_crystal_size_rad ? _exptl_crystal_colour green _diffrn_measurement_device_type ; CAD4 diffractometer ; _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 .60 _exptl_absorpt_correction_T_max .72 _diffrn_reflns_number 4953 _reflns_number_total 4803 _reflns_Friedel_coverage ? _reflns_number_gt 4803 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 29.99 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .135 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _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 _refine_ls_R_factor_gt .065 _refine_ls_wR_factor_ref .073 _refine_ls_goodness_of_fit_ref 1.542 _refine_ls_number_reflns 3349 _refine_ls_number_parameters 155 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .019 _refine_diff_density_min -1.168 _refine_diff_density_max 1.334 _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 ADDREF' _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 26 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 0 .007996 .005981 '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' Si ? 0 4 .072021 .070984 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 2 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 2 .263001 1.266 '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 Cu 1.07683(4) .92908(6) .97519(6) .0510(2) Uani ? ? 1.00000 ? ? N1 .9541(3) .7171(4) .8181(4) .0537(14) Uani ? ? 1.00000 ? ? C2 .8335(4) .7094(5) .7827(5) .0578(12) Uani ? ? 1.00000 ? ? C2' .7942(4) .8602(5) .8650(5) .0511(13) Uani ? ? 1.00000 ? ? Si1 .73739(13) .9224(2) .70546(17) .0682(6) Uani ? ? 1.00000 ? ? C11 .6037(7) .7609(12) .5259(9) .155(5) Uani ? ? 1.00000 ? ? C12 .6817(7) 1.1044(10) .7958(9) .121(4) Uani ? ? 1.00000 ? ? C13 .8647(6) .9796(9) .6109(8) .104(4) Uani ? ? 1.00000 ? ? Si2 .69223(12) .81423(16) .99777(17) .0590(6) Uani ? ? 1.00000 ? ? C21 .5259(5) .6872(8) .8883(8) .099(3) Uani ? ? 1.00000 ? ? C22 .6862(6) 1.0058(7) 1.1736(7) .087(3) Uani ? ? 1.00000 ? ? C23 .7552(6) .6985(8) 1.0970(8) .096(3) Uani ? ? 1.00000 ? ? C3 .7451(5) .5552(7) .6692(7) .087(2) Uani ? ? 1.00000 ? ? C4 .7767(6) .4168(7) .5955(8) .103(3) Uani ? ? 1.00000 ? ? C5 .8976(6) .4276(6) .6327(8) .092(3) Uani ? ? 1.00000 ? ? C6 .9852(5) .5777(6) .7453(7) .070(2) Uani ? ? 1.00000 ? ? C6' 1.1177(6) .5900(8) .7912(10) .114(4) Uani ? ? 1.00000 ? ? H11a .62903 .66267 .46704 .16600 Uiso ? ? 1.00000 ? ? H11b .53481 .72340 .56403 .16600 Uiso ? ? 1.00000 ? ? H11c .57390 .78715 .43923 .16600 Uiso ? ? 1.00000 ? ? H12a .61320 1.07715 .84463 .19000 Uiso ? ? 1.00000 ? ? H12b .74555 1.19921 .88249 .19000 Uiso ? ? 1.00000 ? ? H12c .65056 1.13843 .71611 .19000 Uiso ? ? 1.00000 ? ? H13a .93436 1.06919 .69218 .15800 Uiso ? ? 1.00000 ? ? H13b .89300 .88507 .55778 .15800 Uiso ? ? 1.00000 ? ? H13c .83774 1.01009 .52688 .15800 Uiso ? ? 1.00000 ? ? H21a .48964 .74873 .83827 .12600 Uiso ? ? 1.00000 ? ? H21b .51938 .58474 .79878 .12600 Uiso ? ? 1.00000 ? ? H21c .47147 .66375 .95291 .12600 Uiso ? ? 1.00000 ? ? H22a .76815 1.07284 1.24323 .12900 Uiso ? ? 1.00000 ? ? H22b .65474 1.07143 1.12976 .12900 Uiso ? ? 1.00000 ? ? H22c .63508 .98452 1.24313 .12900 Uiso ? ? 1.00000 ? ? H23a .75752 .59689 1.01478 .15300 Uiso ? ? 1.00000 ? ? H23b .83756 .76514 1.16532 .15300 Uiso ? ? 1.00000 ? ? H23c .70459 .67439 1.16613 .15300 Uiso ? ? 1.00000 ? ? H3 .65691 .55838 .63672 .11500 Uiso ? ? 1.00000 ? ? H4 .71629 .31420 .51111 .12100 Uiso ? ? 1.00000 ? ? H5 .92015 .33056 .60060 .11200 Uiso ? ? 1.00000 ? ? H6'a 1.17031 .70685 .83825 .16200 Uiso ? ? 1.00000 ? ? H6'b 1.14266 .53166 .69210 .16200 Uiso ? ? 1.00000 ? ? H6'c 1.14584 .55343 .86678 .16200 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 Cu .0482(3) .0351(3) .0504(3) .0102(2) .0051(2) .0049(2) N1 .059(2) .0366(18) .050(2) .0096(16) .0093(17) .0095(16) C2 .053(2) .045(2) .046(2) .000(2) .012(2) .002(2) C2' .042(2) .045(2) .046(2) .0064(18) .0093(18) .0061(19) Si1 .0588(8) .0751(10) .0507(8) .0058(7) .0048(6) .0213(7) C11 .119(6) .176(8) .092(5) -.045(6) -.046(4) .063(5) C12 .146(6) .156(7) .103(5) .098(6) .034(5) .070(5) C13 .100(5) .132(6) .087(5) .025(4) .037(4) .059(5) Si2 .0607(8) .0486(7) .0570(8) .0142(6) .0207(6) .0140(6) C21 .066(3) .085(4) .105(5) .000(3) .036(3) .015(4) C22 .104(4) .070(4) .079(4) .030(3) .046(3) .018(3) C23 .138(6) .088(4) .081(4) .050(4) .038(4) .045(4) C3 .059(3) .057(3) .081(4) .000(2) .012(3) -.017(3) C4 .086(4) .047(3) .104(5) -.004(3) .028(4) -.020(3) C5 .103(4) .037(3) .100(5) .016(3) .030(4) .000(3) C6 .080(3) .039(2) .078(4) .021(2) .018(3) .013(2) C6' .105(5) .064(4) .147(7) .048(4) .003(5) .018(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 Cu N1 . . 1.936(3) ? Cu Cu . '2 777' 2.4363(11) ? Cu C2' . '2 777' 1.965(3) ? N1 C2 . . 1.361(6) ? N1 C6 . . 1.356(7) ? C2 C2' . . 1.509(7) ? C2 C3 . . 1.403(5) ? C2' Si1 . . 1.862(6) ? C2' Si2 . . 1.872(5) ? Si1 C11 . . 1.879(6) ? Si1 C12 . . 1.868(9) ? Si1 C13 . . 1.854(8) ? C11 H11a . . .990 ? C11 H11b . . .944 ? C11 H11c . . .960 ? C12 H12a . . .977 ? C12 H12b . . .954 ? C12 H12c . . .961 ? C13 H13a . . .951 ? C13 H13b . . .974 ? C13 H13c . . .955 ? Si2 C21 . . 1.869(5) ? Si2 C22 . . 1.876(6) ? Si2 C23 . . 1.865(9) ? C21 H21a . . .991 ? C21 H21b . . .948 ? C21 H21c . . .951 ? C22 H22a . . .958 ? C22 H22b . . .962 ? C22 H22c . . .955 ? C23 H23a . . .948 ? C23 H23b . . .958 ? C23 H23c . . .957 ? C3 C4 . . 1.353(9) ? C3 H3 . . 1.031 ? C4 C5 . . 1.357(10) ? C4 H4 . . .963 ? C5 C6 . . 1.377(6) ? C5 H5 . . .941 ? C6 C6' . . 1.491(9) ? C6' H6'a . . .978 ? C6' H6'b . . .966 ? C6' H6'c . . .935 ? 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 N1 Cu Cu . . '2 777' 93.20(12) ? N1 Cu C2' . . '2 777' 177.9(2) ? Cu Cu C2' '2 777' . '2 777' 88.87(15) ? Cu N1 C2 . . . 118.4(3) ? Cu N1 C6 . . . 121.8(3) ? C2 N1 C6 . . . 119.8(3) ? N1 C2 C2' . . . 121.6(3) ? N1 C2 C3 . . . 118.0(4) ? C2' C2 C3 . . . 120.4(4) ? C2 C2' Si1 . . . 109.3(3) ? C2 C2' Si2 . . . 107.0(3) ? C2 C2' Cu . . '2 777' 118.0(3) ? Si1 C2' Si2 . . . 120.2(3) ? Si1 C2' Cu . . '2 777' 100.4(2) ? Si2 C2' Cu . . '2 777' 102.5(2) ? C2' Si1 C11 . . . 116.8(4) ? C2' Si1 C12 . . . 112.1(3) ? C2' Si1 C13 . . . 109.6(3) ? C11 Si1 C12 . . . 104.0(4) ? C11 Si1 C13 . . . 105.5(3) ? C12 Si1 C13 . . . 108.4(4) ? Si1 C11 H11a . . . 108.4 ? Si1 C11 H11b . . . 110.8 ? Si1 C11 H11c . . . 119.1 ? H11a C11 H11b . . . 106.6 ? H11a C11 H11c . . . 103.8 ? H11b C11 H11c . . . 107.3 ? Si1 C12 H12a . . . 110.3 ? Si1 C12 H12b . . . 111.6 ? Si1 C12 H12c . . . 114.1 ? H12a C12 H12b . . . 106.9 ? H12a C12 H12c . . . 105.8 ? H12b C12 H12c . . . 107.7 ? Si1 C13 H13a . . . 111.6 ? Si1 C13 H13b . . . 110.3 ? Si1 C13 H13c . . . 111.4 ? H13a C13 H13b . . . 107.4 ? H13a C13 H13c . . . 108.9 ? H13b C13 H13c . . . 107.0 ? C2' Si2 C21 . . . 116.0(3) ? C2' Si2 C22 . . . 113.8(3) ? C2' Si2 C23 . . . 109.1(3) ? C21 Si2 C22 . . . 104.6(3) ? C21 Si2 C23 . . . 107.0(3) ? C22 Si2 C23 . . . 105.7(3) ? Si2 C21 H21a . . . 108.3 ? Si2 C21 H21b . . . 110.8 ? Si2 C21 H21c . . . 117.9 ? H21a C21 H21b . . . 106.3 ? H21a C21 H21c . . . 104.7 ? H21b C21 H21c . . . 108.2 ? Si2 C22 H22a . . . 109.9 ? Si2 C22 H22b . . . 109.6 ? Si2 C22 H22c . . . 114.8 ? H22a C22 H22b . . . 107.8 ? H22a C22 H22c . . . 107.4 ? H22b C22 H22c . . . 107.1 ? Si2 C23 H23a . . . 110.5 ? Si2 C23 H23b . . . 109.9 ? Si2 C23 H23c . . . 110.4 ? H23a C23 H23b . . . 109.0 ? H23a C23 H23c . . . 108.9 ? H23b C23 H23c . . . 108.1 ? C2 C3 C4 . . . 122.0(5) ? C2 C3 H3 . . . 115.1 ? C4 C3 H3 . . . 122.6 ? C3 C4 C5 . . . 118.9(4) ? C3 C4 H4 . . . 121.0 ? C5 C4 H4 . . . 119.9 ? C4 C5 C6 . . . 119.7(6) ? C4 C5 H5 . . . 120.6 ? C6 C5 H5 . . . 118.4 ? N1 C6 C5 . . . 121.5(5) ? N1 C6 C6' . . . 118.2(4) ? C5 C6 C6' . . . 120.3(6) ? C6 C6' H6'a . . . 109.2 ? C6 C6' H6'b . . . 109.7 ? C6 C6' H6'c . . . 122.0 ? H6'a C6' H6'b . . . 105.8 ? H6'a C6' H6'c . . . 104.0 ? H6'b C6' H6'c . . . 104.9 ? 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 #-------------------------------------------------------------------------- _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_000 332 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 4 4 9 0 0 0 8 0 0 0 9 -5 -4 -4 -9 0 0 0 -8 0 0 0 -9 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min -13 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _reflns_number_observed ? _reflns_d_resolution_high .711 _reflns_d_resolution_low 10.766 _diffrn_reflns_av_sigmaI/netI 0 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .08 _refine_ls_wR_factor_all .075 _refine_ls_goodness_of_fit_all 1.988 _refine_ls_shift/su_mean .002 #========================================================================== # 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 #===END