Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Vassilyeva, Olga' 'Gatteschi, Dante' 'Kokozay, Volodymyr N.' 'Makhankova, V. G.' 'Skelton, Brian W.' 'Sorace, Lorenzo' _publ_contact_author_name 'Dr Olga Vassilyeva' _publ_contact_author_address ; Chemistry National Taras Shevchenko University Volodimirska str 64 Kyiv 01033 UKRAINE ; _publ_contact_author_email 'VASSILYEVA@CHEM.UNIV.KIEV.UA' _publ_section_title ; Reaction of zerovalent copper with cobalt(II) salts in the presence of 2-dimethylaminoethanol as an access to novel polynuclear CuII/CoII complexes constructed from one and two Cu2Co triangles with antiferromagnetic exchange coupling ; data_LE410 _database_code_CSD 187030 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C16 H31.5 Co1 Cu2 N6.5 O3 S3' _chemical_formula_moiety ? _chemical_formula_weight 645.19 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M C_m_c_21 _symmetry_space_group_name_Hall c_2c_-2 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,1/2+z -x,+y,+z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2-y,1/2+z 1/2-x,1/2+y,+z 1/2+x,1/2-y,1/2+z _cell_length_a 14.036(2) _cell_length_b 20.009(3) _cell_length_c 10.097(2) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 2835.7(8) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 3427 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 2.313 _exptl_crystal_description prism _exptl_crystal_size_max .2 _exptl_crystal_size_mid .07 _exptl_crystal_size_min .05 _exptl_crystal_size_rad ? _exptl_crystal_colour dark _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .631 _exptl_absorpt_correction_T_max .831 _diffrn_reflns_number 17013 _reflns_number_total 2046 _reflns_Friedel_coverage .898 _reflns_number_gt 1531 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.36 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .043 _refine_ls_wR_factor_ref .048 _refine_ls_goodness_of_fit_ref 1.388 _refine_ls_number_reflns 1492 _refine_ls_number_parameters 169 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .009 _refine_diff_density_min -.564 _refine_diff_density_max 1.117 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack xabs refined' _refine_ls_abs_structure_Flack .05(4) # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _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 64 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 126 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Co ? 0 4 .299 .973 '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' N ? 0 26 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 12 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 12 .11 .124 '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 Co .00000 .07743(8) .00000 .0324(8) Uani ? ? 1.00000 ? ? Cu .12157(8) .17089(4) .17763(17) .0399(5) Uani ? ? 1.00000 ? ? O11 .1174(4) .0850(3) .0979(7) .041(3) Uani ? ? 1.00000 ? ? C12 .1987(7) .0464(4) .1145(10) .042(5) Uani ? ? 1.00000 ? ? C13 .2439(6) .0659(4) .2449(13) .049(5) Uani ? ? 1.00000 ? ? N14 .2479(6) .1402(3) .2528(10) .051(4) Uani ? ? 1.00000 ? ? C141 .3264(8) .1665(5) .1692(15) .061(6) Uani ? ? 1.00000 ? ? C142 .2647(9) .1607(5) .3923(11) .062(7) Uani ? ? 1.00000 ? ? O21 .00000 .1829(4) .0806(9) .038(5) Uani ? ? 1.00000 ? ? C22 .00000 .2284(6) -.0296(13) .047(8) Uani ? ? 1.00000 ? ? C23 .0438(13) .1981(8) -.1440(17) .041(9) Uani ? ? .50000 ? ? N24 .00000 .1314(5) -.1766(10) .041(6) Uani ? ? 1.00000 ? ? C241 .0751(17) .0971(11) -.267(2) .052(13) Uani ? ? .50000 ? ? C241' -.0864(14) .1334(10) -.240(3) .045(11) Uani ? ? .50000 ? ? N01 .1429(6) .2640(3) .2112(8) .055(5) Uani ? ? 1.00000 ? ? C01 .1491(6) .3199(4) .2409(11) .041(5) Uani ? ? 1.00000 ? ? S01 .1601(2) .39754(12) .2816(4) .070(2) Uani ? ? 1.00000 ? ? N02 .00000 -.0178(5) -.0647(11) .041(6) Uani ? ? 1.00000 ? ? C02 .00000 -.0751(6) -.0865(14) .036(7) Uani ? ? 1.00000 ? ? S02 .00000 -.15569(15) -.1108(3) .044(2) Uani ? ? 1.00000 ? ? N0 .00000 .4345(15) -.176(4) .085(9) Uiso ? ? .50000 ? ? C10 .00000 .4439(17) -.057(6) .19(3) Uiso ? ? .50000 ? ? C20 .00000 .4608(17) .098(4) .070(10) Uiso ? ? .50000 ? ? H12a .24255 .05433 .04403 .05300 Uiso ? ? 1.00000 ? ? H12b .18260 .00021 .11585 .05300 Uiso ? ? 1.00000 ? ? H13a .30792 .04808 .24849 .07400 Uiso ? ? 1.00000 ? ? H13b .20876 .04826 .31635 .07400 Uiso ? ? 1.00000 ? ? H141a .32490 .21457 .17757 .09300 Uiso ? ? 1.00000 ? ? H141b .31361 .15482 .08091 .09300 Uiso ? ? 1.00000 ? ? H141c .38382 .14988 .19917 .09300 Uiso ? ? 1.00000 ? ? H142a .26624 .20802 .39931 .09200 Uiso ? ? 1.00000 ? ? H142b .32275 .14259 .42435 .09200 Uiso ? ? 1.00000 ? ? H142c .21348 .14430 .44712 .09200 Uiso ? ? 1.00000 ? ? H22a .03483 .26716 -.00741 .03100 Uiso ? ? .50000 ? ? H22b -.06383 .23997 -.05095 .03100 Uiso ? ? .50000 ? ? H23a .10904 .19138 -.12687 .02700 Uiso ? ? .50000 ? ? H23b .03536 .22650 -.21783 .02700 Uiso ? ? .50000 ? ? H241a .13605 .11729 -.25606 .05900 Uiso ? ? .50000 ? ? H241b .05682 .09912 -.35694 .05900 Uiso ? ? .50000 ? ? H241c .08114 .05036 -.24235 .05900 Uiso ? ? .50000 ? ? H241'a -.10980 .08782 -.25261 .05600 Uiso ? ? .50000 ? ? H241'b -.08031 .15272 -.32598 .05600 Uiso ? ? .50000 ? ? H241'c -.13226 .15699 -.19062 .05600 Uiso ? ? .50000 ? ? H20a .00000 .50853 .10165 .10400 Uiso ? ? .50000 ? ? H20b .05585 .44460 .14245 .10400 Uiso ? ? .50000 ? ? 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 Co .0474(9) .0248(7) .0251(7) .00000 .00000 -.0021(7) Cu .0626(7) .0237(4) .0336(5) -.0074(5) -.0068(6) -.0012(5) O11 .049(4) .026(3) .047(4) .002(3) -.012(3) -.008(3) C12 .052(6) .029(4) .047(5) -.004(4) -.005(4) .007(4) C13 .053(5) .039(5) .054(5) -.004(4) -.013(6) .004(5) N14 .067(5) .041(4) .044(4) -.021(3) -.008(5) .002(5) C141 .064(6) .047(5) .073(7) -.017(5) -.006(7) .003(6) C142 .084(8) .056(7) .048(6) -.015(6) -.024(6) -.009(5) O21 .065(6) .022(4) .026(4) .00000 .00000 .004(3) C22 .074(10) .031(7) .036(8) .00000 .00000 .012(5) C23 .061(12) .030(8) .030(9) -.003(8) .007(8) .011(7) N24 .061(7) .037(6) .025(5) .00000 .00000 .002(5) C241 .062(14) .057(13) .037(12) .022(12) -.002(11) -.005(11) C241' .035(10) .057(12) .042(12) -.000(10) -.007(10) -.005(12) N01 .088(6) .028(3) .050(6) -.016(4) -.002(4) -.000(3) C01 .049(5) .036(4) .040(5) -.006(3) -.005(5) .002(4) S01 .0704(18) .0331(11) .108(3) .0008(12) -.0103(19) -.0246(15) N02 .052(7) .036(7) .036(6) .00000 .00000 -.012(5) C02 .039(7) .033(7) .038(7) .00000 .00000 .000(6) S02 .078(3) .0269(16) .0282(17) .00000 .00000 -.0014(12) # 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 Co O11 . . 1.928(6) ? Co O21 . . 2.262(8) ? Co N24 . . 2.085(10) ? Co N02 . . 2.015(10) ? Co O11 . 3 1.928(6) ? Cu O11 . . 1.899(6) ? Cu N14 . . 2.024(8) ? Cu O21 . . 1.982(5) ? Cu N01 . . 1.917(7) ? Cu S02 . 2 2.751(3) ? O11 C12 . . 1.388(11) ? C12 C13 . . 1.513(16) ? C12 H12a . . .954 ? C12 H12b . . .951 ? C13 N14 . . 1.489(11) ? C13 H13a . . .968 ? C13 H13b . . .942 ? N14 C141 . . 1.485(15) ? N14 C142 . . 1.486(15) ? C141 H141a . . .966 ? C141 H141b . . .939 ? C141 H141c . . .922 ? C142 H142a . . .949 ? C142 H142b . . .949 ? C142 H142c . . .965 ? O21 C22 . . 1.437(15) ? C22 C23 . . 1.44(2) ? C22 H22a . . .944 ? C22 H22b . . .950 ? C22 C23 . 3 1.44(2) ? C22 H22a . 3 .944 ? C22 H22b . 3 .950 ? C23 N24 . . 1.51(2) ? C23 H23a . . .942 ? C23 H23b . . .945 ? N24 C241 . . 1.56(2) ? N24 C241' . . 1.37(2) ? N24 C241 . 3 1.56(2) ? N24 C241' . 3 1.37(2) ? C241 H241a . . .95 ? C241 H241b . . .94 ? C241 H241c . . .97 ? C241' H241'a . . .98 ? C241' H241'b . . .96 ? C241' H241'c . . .94 ? N01 C01 . . 1.161(11) ? C01 S01 . . 1.615(8) ? N02 C02 . . 1.167(16) ? C02 S02 . . 1.631(13) ? N0 C10 . . 1.21(7) ? C10 C20 . . 1.61(7) ? C20 H20a . . .96 ? C20 H20b . . .96 ? C20 H20b . 3 .96 ? 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 O11 Co O21 . . . 75.1(2) ? O11 Co N24 . . . 113.5(2) ? O11 Co N02 . . . 103.9(2) ? O11 Co O11 . . 3 117.5(3) ? O21 Co N24 . . . 79.9(4) ? O21 Co N02 . . . 177.8(4) ? O21 Co O11 . . 3 75.1(2) ? N24 Co N02 . . . 102.3(4) ? N24 Co O11 . . 3 113.5(2) ? N02 Co O11 . . 3 103.9(2) ? O11 Cu N14 . . . 84.9(3) ? O11 Cu O21 . . . 82.8(3) ? O11 Cu N01 . . . 163.6(3) ? O11 Cu S02 . . 2 102.1(2) ? N14 Cu O21 . . . 167.5(3) ? N14 Cu N01 . . . 95.3(3) ? N14 Cu S02 . . 2 102.6(3) ? O21 Cu N01 . . . 96.0(3) ? O21 Cu S02 . . 2 82.1(2) ? N01 Cu S02 . . 2 93.9(3) ? Co O11 Cu . . . 108.3(3) ? Co O11 C12 . . . 136.2(5) ? Cu O11 C12 . . . 115.3(5) ? O11 C12 C13 . . . 107.8(7) ? O11 C12 H12a . . . 110.3 ? O11 C12 H12b . . . 110.3 ? C13 C12 H12a . . . 109.6 ? C13 C12 H12b . . . 109.8 ? H12a C12 H12b . . . 109.0 ? C12 C13 N14 . . . 108.7(8) ? C12 C13 H13a . . . 109.0 ? C12 C13 H13b . . . 110.5 ? N14 C13 H13a . . . 109.3 ? N14 C13 H13b . . . 110.7 ? H13a C13 H13b . . . 108.6 ? Cu N14 C13 . . . 104.4(6) ? Cu N14 C141 . . . 109.2(7) ? Cu N14 C142 . . . 114.2(7) ? C13 N14 C141 . . . 110.6(8) ? C13 N14 C142 . . . 109.4(9) ? C141 N14 C142 . . . 108.9(9) ? N14 C141 H141a . . . 106.7 ? N14 C141 H141b . . . 108.0 ? N14 C141 H141c . . . 109.5 ? H141a C141 H141b . . . 109.1 ? H141a C141 H141c . . . 110.5 ? H141b C141 H141c . . . 112.9 ? N14 C142 H142a . . . 110.5 ? N14 C142 H142b . . . 110.7 ? N14 C142 H142c . . . 109.4 ? H142a C142 H142b . . . 109.6 ? H142a C142 H142c . . . 108.3 ? H142b C142 H142c . . . 108.3 ? Co O21 Cu . . . 93.7(2) ? Co O21 C22 . . . 108.2(7) ? Co O21 Cu . . 3 93.7(2) ? Cu O21 C22 . . . 117.4(3) ? Cu O21 Cu . . 3 118.8(4) ? C22 O21 Cu . . 3 117.4(3) ? O21 C22 C23 . . . 110.8(10) ? O21 C22 H22a . . . 109.7 ? O21 C22 H22b . . . 109.3 ? O21 C22 C23 . . 3 110.8(10) ? O21 C22 H22a . . 3 109.7 ? O21 C22 H22b . . 3 109.3 ? C23 C22 H22a . . . 108.4 ? C23 C22 H22b . . . 108.8 ? H22a C22 H22b . . . 109.9 ? C23 C22 H22a 3 . 3 108.4 ? C23 C22 H22b 3 . 3 108.8 ? H22a C22 H22b 3 . 3 109.9 ? C22 C23 N24 . . . 112.0(12) ? C22 C23 H23a . . . 109.1 ? C22 C23 H23b . . . 109.0 ? N24 C23 H23a . . . 108.1 ? N24 C23 H23b . . . 108.0 ? H23a C23 H23b . . . 110.6 ? Co N24 C23 . . . 105.8(8) ? Co N24 C241 . . . 106.0(10) ? Co N24 C241' . . . 114.4(11) ? Co N24 C23 . . 3 105.8(8) ? Co N24 C241 . . 3 106.0(10) ? Co N24 C241' . . 3 114.4(11) ? C23 N24 C241 . . . 104.0(11) ? C23 N24 C241' . . . 115.9(13) ? C241 N24 C241' . . . 109.8(15) ? C23 N24 C241 3 . 3 104.0(11) ? C23 N24 C241' 3 . 3 115.9(13) ? C241 N24 C241' 3 . 3 109.8(15) ? N24 C241 H241a . . . 110.6 ? N24 C241 H241b . . . 111 ? N24 C241 H241c . . . 109 ? H241a C241 H241b . . . 110 ? H241a C241 H241c . . . 107 ? H241b C241 H241c . . . 108 ? N24 C241' H241'a . . . 109.4 ? N24 C241' H241'b . . . 110.9 ? N24 C241' H241'c . . . 112 ? H241'a C241' H241'b . . . 107 ? H241'a C241' H241'c . . . 108 ? H241'b C241' H241'c . . . 110 ? Cu N01 C01 . . . 173.3(8) ? N01 C01 S01 . . . 178.7(9) ? Co N02 C02 . . . 172.0(11) ? N02 C02 S02 . . . 177.8(13) ? C02 S02 Cu . . '2 554' 103.1(4) ? C02 S02 Cu . . '4 554' 103.1(4) ? Cu S02 Cu '2 554' . '4 554' 76.68(10) ? N0 C10 C20 . . . 177(3) ? C10 C20 H20a . . . 104 ? C10 C20 H20b . . . 112 ? C10 C20 H20b . . 3 112 ? H20a C20 H20b . . . 109 ? H20a C20 H20b . . 3 109 ? H20b C20 H20b . . 3 110 ? 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 1320 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _reflns_number_observed ? _reflns_d_resolution_high .725 _reflns_d_resolution_low 7.573 _diffrn_reflns_av_sigmaI/netI .081 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 3 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .065 _refine_ls_wR_factor_all .053 _refine_ls_goodness_of_fit_all 1.31 _refine_ls_shift/su_mean .001 data_LE503 _database_code_CSD 187031 _audit_creation_method Xtal3.6 _audit_creation_date 00-05-16 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C32 H74 Co2 Cu4 I4 N10 O8' _chemical_formula_moiety ? _chemical_formula_weight 1606.68 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 15.372(2) _cell_length_b 10.781(2) _cell_length_c 16.487(3) _cell_angle_alpha 90.00000 _cell_angle_beta 95.647(2) _cell_angle_gamma 90.00000 _cell_volume 2719.1(8) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.962 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 4.452 _exptl_crystal_description bar _exptl_crystal_size_max .45 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .15 _exptl_crystal_size_rad ? _exptl_crystal_colour dark-green _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .491 _exptl_absorpt_correction_T_max .720 _diffrn_reflns_number 25794 _reflns_number_total 6782 _reflns_Friedel_coverage 0 _reflns_number_gt 5367 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.03 _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 -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .073 _refine_ls_wR_factor_ref .083 _refine_ls_goodness_of_fit_ref 2.019 _refine_ls_number_reflns 5367 _refine_ls_number_parameters 271 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .023 _refine_diff_density_min -3.519 _refine_diff_density_max 3.518 _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 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _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 64 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 148 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Co ? 0 4 .299 .973 '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' I ? 0 8 -.726 1.812 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 20 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 16 .008 .006 '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 I1 .10616(4) .76458(6) .20830(4) .0273(3) Uani ? ? 1.00000 ? ? I2 -.16602(4) .82484(6) .09862(4) .0287(3) Uani ? ? 1.00000 ? ? Cu1 -.07203(8) .64700(10) .17492(7) .0229(5) Uani ? ? 1.00000 ? ? Cu2 .09484(7) .59797(10) .05736(7) .0201(5) Uani ? ? 1.00000 ? ? Co3 -.00597(8) .38200(11) .13002(8) .0199(6) Uani ? ? 1.00000 ? ? O1 -.0590(5) .4747(6) .2123(4) .027(3) Uani ? ? 1.00000 ? ? O2 -.0679(4) .2977(5) .0359(4) .023(3) Uani ? ? 1.00000 ? ? O3 .1105(4) .4371(6) .1095(4) .026(3) Uani ? ? 1.00000 ? ? O4 -.0294(4) .5783(6) .0762(4) .021(3) Uani ? ? 1.00000 ? ? N1 -.1131(6) .6748(7) .2872(5) .029(4) Uani ? ? 1.00000 ? ? N2 .0089(5) .1956(7) .1756(5) .024(4) Uani ? ? 1.00000 ? ? N3 .2252(5) .5861(7) .0461(5) .024(4) Uani ? ? 1.00000 ? ? N4 .4973(9) .4316(12) -.0909(8) .063(8) Uani ? ? 1.00000 ? ? N5 .3940(7) -.0538(10) .0482(7) .048(6) Uani ? ? 1.00000 ? ? C1 -.0672(7) .4565(10) .2954(6) .032(5) Uani ? ? 1.00000 ? ? C2 -.0599(7) .5828(9) .3380(6) .028(5) Uani ? ? 1.00000 ? ? C3 -.2065(8) .6449(12) .2849(7) .040(6) Uani ? ? 1.00000 ? ? C4 -.0956(8) .8000(10) .3235(7) .038(6) Uani ? ? 1.00000 ? ? C5 -.0539(7) .1659(8) .0325(6) .024(4) Uani ? ? 1.00000 ? ? C6 .0178(7) .1292(9) .0976(7) .029(5) Uani ? ? 1.00000 ? ? C7 .0852(7) .1674(10) .2344(7) .032(5) Uani ? ? 1.00000 ? ? C8 -.0711(7) .1553(9) .2101(7) .034(5) Uani ? ? 1.00000 ? ? C9 .1986(6) .3974(9) .1238(6) .026(5) Uani ? ? 1.00000 ? ? C10 .2582(6) .5093(9) .1175(7) .028(5) Uani ? ? 1.00000 ? ? C11 .2413(7) .5243(9) -.0319(6) .029(5) Uani ? ? 1.00000 ? ? C12 .2703(6) .7071(9) .0499(7) .030(5) Uani ? ? 1.00000 ? ? C13 .4257(9) .2627(14) -.0086(8) .053(8) Uani ? ? 1.00000 ? ? C14 .4653(8) .3579(11) -.0538(8) .040(6) Uani ? ? 1.00000 ? ? C15 .2672(9) .0381(11) .1220(7) .043(6) Uani ? ? 1.00000 ? ? C16 .3402(8) -.0152(10) .0808(8) .040(6) Uani ? ? 1.00000 ? ? H1A -.02194 .40227 .31870 .04000 Uiso ? ? 1.00000 ? ? H1B -.12235 .41962 .30287 .04000 Uiso ? ? 1.00000 ? ? H2A -.08065 .57682 .39102 .03600 Uiso ? ? 1.00000 ? ? H2B -.00006 .60831 .34513 .03600 Uiso ? ? 1.00000 ? ? H3A -.24031 .70278 .25192 .06000 Uiso ? ? 1.00000 ? ? H3B -.22468 .64527 .33838 .06000 Uiso ? ? 1.00000 ? ? H3C -.21689 .56331 .26210 .06000 Uiso ? ? 1.00000 ? ? H4A -.12824 .86122 .29195 .05600 Uiso ? ? 1.00000 ? ? H4B -.03448 .81926 .32367 .05600 Uiso ? ? 1.00000 ? ? H4C -.11062 .80231 .37784 .05600 Uiso ? ? 1.00000 ? ? H5A -.10688 .12325 .04110 .03000 Uiso ? ? 1.00000 ? ? H5B -.03786 .14380 -.02017 .03000 Uiso ? ? 1.00000 ? ? H6A .01599 .04197 .10781 .03600 Uiso ? ? 1.00000 ? ? H6B .07378 .14891 .08012 .03600 Uiso ? ? 1.00000 ? ? H7A .07962 .20935 .28453 .04700 Uiso ? ? 1.00000 ? ? H7B .13743 .19263 .21330 .04700 Uiso ? ? 1.00000 ? ? H7C .08759 .08002 .24468 .04700 Uiso ? ? 1.00000 ? ? H8A -.07697 .19886 .25991 .05100 Uiso ? ? 1.00000 ? ? H8B -.06836 .06862 .22149 .05100 Uiso ? ? 1.00000 ? ? H8C -.12107 .17184 .17299 .05100 Uiso ? ? 1.00000 ? ? H9A .21086 .33649 .08476 .03200 Uiso ? ? 1.00000 ? ? H9B .20851 .36164 .17717 .03200 Uiso ? ? 1.00000 ? ? H10A .25878 .55828 .16601 .03400 Uiso ? ? 1.00000 ? ? H10B .31622 .48268 .11154 .03400 Uiso ? ? 1.00000 ? ? H11A .21995 .57463 -.07698 .04500 Uiso ? ? 1.00000 ? ? H11B .21259 .44596 -.03607 .04500 Uiso ? ? 1.00000 ? ? H11C .30266 .51140 -.03396 .04500 Uiso ? ? 1.00000 ? ? H12A .24932 .75638 .00420 .04500 Uiso ? ? 1.00000 ? ? H12B .33159 .69532 .04959 .04500 Uiso ? ? 1.00000 ? ? H12C .25931 .74949 .09865 .04500 Uiso ? ? 1.00000 ? ? H13A .45803 .18709 -.01041 .04000 Uiso ? ? 1.00000 ? ? H13B .36721 .24782 -.03183 .04000 Uiso ? ? 1.00000 ? ? H13C .42404 .28650 .04676 .04600 Uiso ? ? 1.00000 ? ? H15A .22500 .05758 .06494 .03500 Uiso ? ? 1.00000 ? ? H15B .24077 -.01946 .15679 .03500 Uiso ? ? 1.00000 ? ? H15C .28215 .11142 .15309 .03500 Uiso ? ? 1.00000 ? ? H4O -.07104 .61438 .03714 .02700 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 I1 .0319(3) .0160(3) .0339(3) -.0028(2) .0025(3) -.0040(2) I2 .0352(4) .0125(3) .0378(4) .0036(2) .0015(3) -.0009(2) Cu1 .0308(6) .0107(5) .0277(6) .0017(4) .0059(5) -.0010(4) Cu2 .0240(5) .0089(5) .0277(6) -.0010(4) .0031(4) .0023(4) Co3 .0258(6) .0081(5) .0260(6) -.0008(5) .0037(5) -.0004(5) O1 .043(4) .014(3) .026(3) .001(3) .006(3) .005(3) O2 .035(4) .004(3) .030(3) -.000(2) .002(3) -.001(2) O3 .025(3) .013(3) .039(4) -.001(3) -.001(3) .004(3) O4 .026(3) .013(3) .022(3) .001(2) .002(2) -.000(2) N1 .038(5) .013(4) .037(5) .007(3) .010(4) -.001(3) N2 .030(4) .010(4) .033(4) -.001(3) .006(3) .004(3) N3 .032(4) .009(3) .032(4) -.001(3) .007(3) .001(3) N4 .087(10) .043(7) .061(8) -.007(7) .012(7) -.006(6) N5 .050(6) .032(6) .065(7) -.010(5) .022(5) -.008(5) C1 .044(6) .023(5) .029(5) .001(4) .007(4) .006(4) C2 .043(6) .019(5) .024(5) .005(4) .008(4) -.002(4) C3 .036(6) .049(7) .037(6) .001(5) .010(5) .002(5) C4 .056(7) .023(5) .035(6) .006(5) .008(5) -.007(4) C5 .037(5) .004(4) .031(5) -.002(3) .000(4) -.001(3) C6 .038(5) .010(4) .040(6) .005(4) .003(4) -.005(4) C7 .031(5) .022(5) .044(6) .001(4) .003(4) .013(4) C8 .040(6) .017(5) .045(6) -.006(4) .010(5) .005(4) C9 .023(4) .012(4) .043(6) -.003(3) .001(4) .005(4) C10 .018(4) .018(5) .047(6) -.001(3) -.003(4) .008(4) C11 .032(5) .022(5) .034(5) .009(4) .005(4) -.004(4) C12 .025(5) .010(4) .056(7) -.006(3) .008(5) -.004(4) C13 .053(8) .056(9) .048(7) .002(7) .002(6) -.011(6) C14 .046(7) .030(6) .044(7) .009(5) .003(5) -.007(5) C15 .058(8) .026(6) .045(7) -.002(5) .012(6) -.007(5) C16 .050(7) .019(5) .050(7) -.010(5) .004(6) -.006(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 I1 Cu1 . . 3.0191(14) ? I1 Cu2 . . 3.0600(13) ? I2 Cu1 . . 2.6436(13) ? Cu1 O1 . . 1.961(7) ? Cu1 O4 . . 1.958(6) ? Cu1 N1 . . 2.036(9) ? Cu2 O3 . . 1.940(7) ? Cu2 O4 . . 1.976(7) ? Cu2 N3 . . 2.035(8) ? Cu2 O2 . '3 565' 1.917(6) ? Cu2 O4 . '3 565' 3.007(6) ? Co3 O1 . . 1.930(7) ? Co3 O2 . . 1.963(6) ? Co3 O3 . . 1.947(7) ? Co3 O4 . . 2.309(6) ? Co3 N2 . . 2.149(8) ? O1 C1 . . 1.401(12) ? O2 C5 . . 1.439(10) ? O3 C9 . . 1.418(11) ? O4 H4O . . .946 ? N1 C2 . . 1.490(13) ? N1 C3 . . 1.467(15) ? N1 C4 . . 1.491(14) ? N2 C6 . . 1.490(13) ? N2 C7 . . 1.479(13) ? N2 C8 . . 1.470(14) ? N3 C10 . . 1.487(13) ? N3 C11 . . 1.491(13) ? N3 C12 . . 1.476(12) ? N4 C14 . . 1.143(19) ? N5 C16 . . 1.110(17) ? C1 C2 . . 1.531(14) ? C1 H1A . . .960 ? C1 H1B . . .956 ? C2 H2A . . .961 ? C2 H2B . . .956 ? C3 H3A . . .949 ? C3 H3B . . .951 ? C3 H3C . . .963 ? C4 H4A . . .952 ? C4 H4B . . .962 ? C4 H4C . . .947 ? C5 C6 . . 1.514(14) ? C5 H5A . . .957 ? C5 H5B . . .957 ? C6 H6A . . .956 ? C6 H6B . . .957 ? C7 H7A . . .953 ? C7 H7B . . .946 ? C7 H7C . . .957 ? C8 H8A . . .959 ? C8 H8B . . .953 ? C8 H8C . . .950 ? C9 C10 . . 1.525(13) ? C9 H9A . . .952 ? C9 H9B . . .959 ? C10 H10A . . .958 ? C10 H10B . . .951 ? C11 H11A . . .952 ? C11 H11B . . .952 ? C11 H11C . . .958 ? C12 H12A . . .952 ? C12 H12B . . .951 ? C12 H12C . . .954 ? C13 C14 . . 1.44(2) ? C13 H13A . . .957 ? C13 H13B . . .955 ? C13 H13C . . .951 ? C15 C16 . . 1.484(18) ? C15 H15A . . 1.109 ? C15 H15B . . .962 ? C15 H15C . . .957 ? 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 Cu1 I1 Cu2 . . . 68.12(3) ? I1 Cu1 I2 . . . 103.05(4) ? I1 Cu1 O1 . . . 106.1(2) ? I1 Cu1 O4 . . . 86.47(19) ? I1 Cu1 N1 . . . 97.5(2) ? I2 Cu1 O1 . . . 150.5(2) ? I2 Cu1 O4 . . . 95.22(18) ? I2 Cu1 N1 . . . 97.0(2) ? O1 Cu1 O4 . . . 82.6(3) ? O1 Cu1 N1 . . . 83.4(3) ? O4 Cu1 N1 . . . 166.0(3) ? I1 Cu2 O3 . . . 99.8(2) ? I1 Cu2 O4 . . . 85.03(18) ? I1 Cu2 N3 . . . 97.7(2) ? I1 Cu2 O2 . . '3 565' 107.35(19) ? I1 Cu2 O4 . . '3 565' 162.74(13) ? O3 Cu2 O4 . . . 85.1(3) ? O3 Cu2 N3 . . . 84.5(3) ? O3 Cu2 O2 . . '3 565' 152.6(3) ? O3 Cu2 O4 . . '3 565' 77.1(2) ? O4 Cu2 N3 . . . 169.5(3) ? O4 Cu2 O2 . . '3 565' 93.1(3) ? O4 Cu2 O4 . . '3 565' 77.8(2) ? N3 Cu2 O2 . . '3 565' 95.8(3) ? N3 Cu2 O4 . . '3 565' 98.9(3) ? O2 Cu2 O4 '3 565' . '3 565' 75.7(2) ? O1 Co3 O2 . . . 126.2(3) ? O1 Co3 O3 . . . 115.0(3) ? O1 Co3 O4 . . . 74.6(3) ? O1 Co3 N2 . . . 106.1(3) ? O2 Co3 O3 . . . 112.8(3) ? O2 Co3 O4 . . . 94.3(2) ? O2 Co3 N2 . . . 82.5(3) ? O3 Co3 O4 . . . 76.4(2) ? O3 Co3 N2 . . . 106.1(3) ? O4 Co3 N2 . . . 176.5(3) ? Cu1 O1 Co3 . . . 107.9(3) ? Cu1 O1 C1 . . . 115.1(6) ? Co3 O1 C1 . . . 134.4(6) ? Co3 O2 C5 . . . 115.2(5) ? Co3 O2 Cu2 . . '3 565' 114.3(3) ? C5 O2 Cu2 . . '3 565' 124.7(6) ? Cu2 O3 Co3 . . . 105.9(3) ? Cu2 O3 C9 . . . 114.7(6) ? Co3 O3 C9 . . . 139.3(6) ? Cu1 O4 Cu2 . . . 119.9(3) ? Cu1 O4 Co3 . . . 94.6(3) ? Cu1 O4 H4O . . . 98.7 ? Cu1 O4 Cu2 . . '3 565' 137.1(3) ? Cu2 O4 Co3 . . . 92.4(2) ? Cu2 O4 H4O . . . 116.6 ? Cu2 O4 Cu2 . . '3 565' 102.2(2) ? Co3 O4 H4O . . . 135.0 ? Co3 O4 Cu2 . . '3 565' 74.35(17) ? H4O O4 Cu2 . . '3 565' 66.8(3) ? Cu1 N1 C2 . . . 102.2(6) ? Cu1 N1 C3 . . . 109.5(7) ? Cu1 N1 C4 . . . 116.0(7) ? C2 N1 C3 . . . 110.5(8) ? C2 N1 C4 . . . 108.0(8) ? C3 N1 C4 . . . 110.3(9) ? Co3 N2 C6 . . . 99.4(5) ? Co3 N2 C7 . . . 118.1(6) ? Co3 N2 C8 . . . 110.3(6) ? C6 N2 C7 . . . 109.4(8) ? C6 N2 C8 . . . 110.1(8) ? C7 N2 C8 . . . 108.9(8) ? Cu2 N3 C10 . . . 103.0(6) ? Cu2 N3 C11 . . . 110.8(6) ? Cu2 N3 C12 . . . 113.8(6) ? C10 N3 C11 . . . 111.2(7) ? C10 N3 C12 . . . 109.7(7) ? C11 N3 C12 . . . 108.3(8) ? O1 C1 C2 . . . 108.3(8) ? O1 C1 H1A . . . 110.3 ? O1 C1 H1B . . . 110.6 ? C2 C1 H1A . . . 109.9 ? C2 C1 H1B . . . 109.6 ? H1A C1 H1B . . . 108.2 ? N1 C2 C1 . . . 108.8(8) ? N1 C2 H2A . . . 110.1 ? N1 C2 H2B . . . 110.2 ? C1 C2 H2A . . . 110.0 ? C1 C2 H2B . . . 109.7 ? H2A C2 H2B . . . 108.0 ? N1 C3 H3A . . . 110.5 ? N1 C3 H3B . . . 110.5 ? N1 C3 H3C . . . 109.6 ? H3A C3 H3B . . . 109.5 ? H3A C3 H3C . . . 108.5 ? H3B C3 H3C . . . 108.2 ? N1 C4 H4A . . . 110.1 ? N1 C4 H4B . . . 109.5 ? N1 C4 H4C . . . 110.6 ? H4A C4 H4B . . . 108.3 ? H4A C4 H4C . . . 109.6 ? H4B C4 H4C . . . 108.7 ? O2 C5 C6 . . . 109.4(7) ? O2 C5 H5A . . . 109.7 ? O2 C5 H5B . . . 109.5 ? C6 C5 H5A . . . 109.9 ? C6 C5 H5B . . . 110.0 ? H5A C5 H5B . . . 108.3 ? N2 C6 C5 . . . 111.3(8) ? N2 C6 H6A . . . 108.3 ? N2 C6 H6B . . . 108.4 ? C5 C6 H6A . . . 110.5 ? C5 C6 H6B . . . 110.0 ? H6A C6 H6B . . . 108.3 ? N2 C7 H7A . . . 109.8 ? N2 C7 H7B . . . 110.3 ? N2 C7 H7C . . . 109.4 ? H7A C7 H7B . . . 109.6 ? H7A C7 H7C . . . 108.6 ? H7B C7 H7C . . . 109.2 ? N2 C8 H8A . . . 109.9 ? N2 C8 H8B . . . 110.1 ? N2 C8 H8C . . . 110.4 ? H8A C8 H8B . . . 108.5 ? H8A C8 H8C . . . 108.7 ? H8B C8 H8C . . . 109.2 ? O3 C9 C10 . . . 108.7(7) ? O3 C9 H9A . . . 110.2 ? O3 C9 H9B . . . 109.7 ? C10 C9 H9A . . . 109.8 ? C10 C9 H9B . . . 109.8 ? H9A C9 H9B . . . 108.6 ? N3 C10 C9 . . . 109.6(7) ? N3 C10 H10A . . . 109.2 ? N3 C10 H10B . . . 109.7 ? C9 C10 H10A . . . 109.5 ? C9 C10 H10B . . . 110.2 ? H10A C10 H10B . . . 108.7 ? N3 C11 H11A . . . 110.2 ? N3 C11 H11B . . . 110.1 ? N3 C11 H11C . . . 110.0 ? H11A C11 H11B . . . 109.2 ? H11A C11 H11C . . . 108.7 ? H11B C11 H11C . . . 108.7 ? N3 C12 H12A . . . 109.8 ? N3 C12 H12B . . . 110.1 ? N3 C12 H12C . . . 109.7 ? H12A C12 H12B . . . 109.2 ? H12A C12 H12C . . . 109.0 ? H12B C12 H12C . . . 109.1 ? C14 C13 H13A . . . 110.1 ? C14 C13 H13B . . . 110.0 ? C14 C13 H13C . . . 110.9 ? H13A C13 H13B . . . 108.4 ? H13A C13 H13C . . . 108.8 ? H13B C13 H13C . . . 108.5 ? N4 C14 C13 . . . 178.5(14) ? C16 C15 H15A . . . 95.2 ? C16 C15 H15B . . . 113.9 ? C16 C15 H15C . . . 114.3 ? H15A C15 H15B . . . 112.5 ? H15A C15 H15C . . . 112.8 ? H15B C15 H15C . . . 107.9 ? N5 C16 C15 . . . 178.2(13) ? #-------------------------------------------------------------------------- # 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 1564 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min -22 _reflns_limit_l_max 22 _reflns_number_observed ? _reflns_d_resolution_high .732 _reflns_d_resolution_low 11.754 _diffrn_reflns_av_sigmaI/netI .055 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .097 _refine_ls_wR_factor_all .086 _refine_ls_goodness_of_fit_all 1.858 _refine_ls_shift/su_mean .001 data_LE351 _database_code_CSD 187032 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H68 Br4 Co2 Cu4 N8 O8' _chemical_formula_weight 1336.56 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.408(2) _cell_length_b 10.631(2) _cell_length_c 22.474(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.54(3) _cell_angle_gamma 90.00 _cell_volume 2485.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method ? _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 5.593 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4630 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.1487 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4371 _reflns_number_observed 2220 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 711 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3660 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1761 _refine_ls_R_factor_obs 0.0796 _refine_ls_wR_factor_all 0.1840 _refine_ls_wR_factor_obs 0.1445 _refine_ls_goodness_of_fit_all 1.053 _refine_ls_goodness_of_fit_obs 1.213 _refine_ls_restrained_S_all 1.077 _refine_ls_restrained_S_obs 1.213 _refine_ls_shift/esd_max -0.104 _refine_ls_shift/esd_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Br1 Br 0.21060(14) 0.94581(14) 0.86019(6) 0.0445(4) Uani 1 d . . Br2 Br 0.2100(2) 1.2908(2) 0.94466(7) 0.0584(5) Uani 1 d . . Cu1 Cu 0.3484(2) 1.1612(2) 0.88278(7) 0.0360(4) Uani 1 d . . Cu2 Cu 0.3721(2) 0.8966(2) 0.95794(7) 0.0364(4) Uani 1 d . . Co3 Co 0.6099(2) 1.0203(2) 0.90262(8) 0.0373(5) Uani 1 d . . O1 O 0.5121(8) 1.1254(9) 0.8475(4) 0.047(3) Uani 1 d . . O2 O 0.7190(8) 1.0728(9) 0.9704(4) 0.040(2) Uani 1 d . . O3 O 0.5284(9) 0.8594(9) 0.9175(4) 0.046(3) Uani 1 d . . O4 O 0.4271(8) 1.0723(8) 0.9504(4) 0.032(2) Uani 1 d . . N1 N 0.3126(12) 1.2498(11) 0.8043(5) 0.045(3) Uani 1 d . . N2 N 0.7903(12) 0.9804(13) 0.8644(5) 0.057(4) Uani 1 d . . N3 N 0.3486(11) 0.7070(10) 0.9592(6) 0.049(3) Uani 1 d . . C1 C 0.5216(14) 1.1548(16) 0.7867(6) 0.058(5) Uani 1 d . . H1A H 0.5627 1.0838 0.7652 0.080 Uiso 1 d R . H1B H 0.5748 1.2323 0.7818 0.080 Uiso 1 d R . C2 C 0.3873(14) 1.1794(14) 0.7626(6) 0.046(4) Uani 1 d . . H2A H 0.3887 1.2248 0.7237 0.080 Uiso 1 d R . H2B H 0.3439 1.0965 0.7559 0.080 Uiso 1 d R . C3 C 0.3581(15) 1.3805(13) 0.8094(6) 0.056(4) Uani 1 d . . H3A H 0.4483 1.3807 0.8259 0.080 Uiso 1 d R . H3B H 0.3029 1.4305 0.8365 0.080 Uiso 1 d R . H3C H 0.3568 1.4214 0.7693 0.080 Uiso 1 d R . C4 C 0.1758(14) 1.2532(15) 0.7854(7) 0.057(4) Uani 1 d . . H4A H 0.1223 1.2934 0.8164 0.080 Uiso 1 d R . H4B H 0.1468 1.1649 0.7777 0.080 Uiso 1 d R . H4C H 0.1675 1.3005 0.7470 0.080 Uiso 1 d R . C5 C 0.8469(14) 1.0361(18) 0.9692(7) 0.064(5) Uani 1 d . . H5A H 0.8741 1.0000 1.0087 0.080 Uiso 1 d R . H5B H 0.9021 1.1110 0.9614 0.080 Uiso 1 d R . C6 C 0.8650(17) 0.9392(20) 0.9186(7) 0.090(7) Uani 1 d . . H6A H 0.9579 0.9304 0.9091 0.080 Uiso 1 d R . H6B H 0.8321 0.8555 0.9317 0.080 Uiso 1 d R . C7 C 0.8027(18) 0.8828(23) 0.8207(8) 0.110(8) Uani 1 d . . H7A H 0.7664 0.8035 0.8374 0.080 Uiso 1 d R . H7B H 0.8951 0.8695 0.8113 0.080 Uiso 1 d R . H7C H 0.7549 0.9054 0.7830 0.080 Uiso 1 d R . C8 C 0.8444(17) 1.0873(21) 0.8375(10) 0.114(9) Uani 1 d . . H8A H 0.9326 1.0690 0.8233 0.080 Uiso 1 d R . H8B H 0.8482 1.1558 0.8680 0.080 Uiso 1 d R . H8C H 0.7879 1.1163 0.8035 0.080 Uiso 1 d R . C9 C 0.5438(16) 0.7330(16) 0.9024(7) 0.068(5) Uani 1 d . . H9A H 0.6068 0.6930 0.9309 0.080 Uiso 1 d R . H9B H 0.5779 0.7252 0.8614 0.080 Uiso 1 d R . C10 C 0.4181(17) 0.6665(15) 0.9066(8) 0.072(5) Uani 1 d . . H10A H 0.3652 0.6856 0.8700 0.080 Uiso 1 d R . H10B H 0.4319 0.5735 0.9085 0.080 Uiso 1 d R . C11 C 0.4016(17) 0.6506(14) 1.0157(7) 0.069(5) Uani 1 d . . H11A H 0.3696 0.5627 1.0206 0.080 Uiso 1 d R . H11B H 0.3765 0.7029 1.0505 0.080 Uiso 1 d R . H11C H 0.4976 0.6503 1.0141 0.080 Uiso 1 d R . C12 C 0.2118(15) 0.6672(17) 0.9540(8) 0.080(6) Uani 1 d . . H12A H 0.1593 0.7140 0.9833 0.080 Uiso 1 d R . H12B H 0.2062 0.5745 0.9609 0.080 Uiso 1 d R . H12C H 0.1796 0.6840 0.9124 0.080 Uiso 1 d R . N4 N 0.2730(23) 0.5359(25) 1.1606(10) 0.151(9) Uani 1 d . . C13 C 0.1839(25) 0.5107(23) 1.1325(13) 0.103(8) Uani 1 d . . C14 C 0.0795(21) 0.4728(25) 1.0948(10) 0.136(10) Uani 1 d . . H14A H 0.0026 0.5274 1.1007 0.080 Uiso 1 d R . H14B H 0.1050 0.4771 1.0523 0.080 Uiso 1 d R . H14C H 0.0580 0.3839 1.1052 0.080 Uiso 1 d R . H4O H 0.4167(118) 1.1150(116) 0.9782(50) 0.034(43) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0473(9) 0.0432(9) 0.0421(8) -0.0026(7) -0.0132(7) -0.0037(8) Br2 0.0704(12) 0.0485(10) 0.0559(10) -0.0024(8) -0.0052(9) 0.0237(9) Cu1 0.0407(11) 0.0360(10) 0.0306(9) 0.0050(8) -0.0079(8) 0.0054(9) Cu2 0.0393(11) 0.0287(9) 0.0411(10) -0.0017(8) -0.0038(8) -0.0012(8) Co3 0.0336(11) 0.0432(12) 0.0349(10) 0.0032(9) -0.0025(8) 0.0057(9) O1 0.041(6) 0.062(7) 0.038(5) 0.033(5) -0.011(5) 0.001(5) O2 0.030(6) 0.052(6) 0.039(5) 0.003(5) -0.006(4) -0.002(5) O3 0.046(6) 0.036(6) 0.057(6) -0.003(5) -0.003(5) 0.002(5) O4 0.040(6) 0.026(5) 0.029(5) -0.001(4) -0.012(5) 0.002(4) N1 0.055(8) 0.047(8) 0.033(7) 0.010(6) -0.010(6) 0.000(7) N2 0.062(9) 0.078(10) 0.032(7) 0.002(7) 0.016(7) -0.009(8) N3 0.045(8) 0.032(7) 0.070(9) -0.008(7) 0.001(7) -0.005(6) C1 0.045(10) 0.080(12) 0.049(10) 0.013(9) 0.006(8) 0.006(9) C2 0.058(10) 0.052(10) 0.029(8) 0.011(7) -0.001(7) 0.005(8) C3 0.084(12) 0.031(9) 0.051(10) 0.017(8) -0.018(9) -0.001(9) C4 0.054(11) 0.052(10) 0.064(11) 0.017(9) -0.008(9) 0.010(8) C5 0.036(9) 0.107(15) 0.049(10) -0.009(10) -0.003(8) -0.005(10) C6 0.070(13) 0.142(20) 0.057(12) 0.023(13) -0.004(10) 0.022(13) C7 0.074(15) 0.179(25) 0.079(14) -0.033(16) 0.013(11) 0.031(16) C8 0.044(12) 0.147(22) 0.154(21) 0.072(19) 0.035(12) 0.020(13) C9 0.059(12) 0.067(13) 0.079(13) -0.029(10) 0.004(10) 0.032(10) C10 0.092(15) 0.038(10) 0.084(13) -0.008(10) -0.018(12) 0.010(10) C11 0.101(14) 0.033(9) 0.073(12) 0.018(9) -0.021(11) -0.008(9) C12 0.056(12) 0.065(12) 0.117(16) 0.020(11) -0.005(11) -0.019(10) N4 0.150(22) 0.189(25) 0.112(18) -0.015(16) -0.023(16) -0.020(20) C13 0.093(19) 0.081(17) 0.134(24) 0.013(16) -0.001(16) -0.009(14) C14 0.108(20) 0.148(25) 0.149(23) -0.020(20) -0.042(18) 0.011(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Cu1 2.742(2) . ? Br1 Cu2 2.780(2) . ? Br2 Cu1 2.453(2) . ? Cu1 O1 1.936(9) . ? Cu1 O4 1.951(8) . ? Cu1 N1 2.025(10) . ? Cu2 O3 1.925(9) . ? Cu2 O2 1.918(9) 3_677 ? Cu2 O4 1.963(9) . ? Cu2 N3 2.030(11) . ? Co3 O1 1.936(8) . ? Co3 O3 1.943(9) . ? Co3 O2 1.957(8) . ? Co3 N2 2.129(13) . ? Co3 O4 2.277(10) . ? O1 C1 1.407(15) . ? O2 C5 1.39(2) . ? O2 Cu2 1.918(9) 3_677 ? O3 C9 1.40(2) . ? O4 H4O 0.78(11) . ? N1 C2 1.44(2) . ? N1 C3 1.47(2) . ? N1 C4 1.48(2) . ? N2 C8 1.41(2) . ? N2 C7 1.44(2) . ? N2 C6 1.49(2) . ? N3 C10 1.47(2) . ? N3 C11 1.50(2) . ? N3 C12 1.49(2) . ? C1 C2 1.51(2) . ? C1 H1A 1.00 . ? C1 H1B 1.00 . ? C2 H2A 1.00 . ? C2 H2B 1.00 . ? C3 H3A 1.00 . ? C3 H3B 1.00 . ? C3 H3C 1.00 . ? C4 H4A 1.00 . ? C4 H4B 1.00 . ? C4 H4C 1.00 . ? C5 C6 1.55(2) . ? C5 H5A 1.00 . ? C5 H5B 1.00 . ? C6 H6A 1.00 . ? C6 H6B 1.00 . ? C7 H7A 1.00 . ? C7 H7B 1.00 . ? C7 H7C 1.00 . ? C8 H8A 1.00 . ? C8 H8B 1.00 . ? C8 H8C 1.00 . ? C9 C10 1.49(2) . ? C9 H9A 1.00 . ? C9 H9B 1.00 . ? C10 H10A 1.00 . ? C10 H10B 1.00 . ? C11 H11A 1.00 . ? C11 H11B 1.00 . ? C11 H11C 1.00 . ? C12 H12A 1.00 . ? C12 H12B 1.00 . ? C12 H12C 1.00 . ? N4 C13 1.14(3) . ? C13 C14 1.42(3) . ? C14 H14A 1.00 . ? C14 H14B 1.00 . ? C14 H14C 1.00 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 Br1 Cu2 73.07(6) . . ? O1 Cu1 O4 82.4(4) . . ? O1 Cu1 N1 83.0(4) . . ? O4 Cu1 N1 165.3(5) . . ? O1 Cu1 Br2 151.6(3) . . ? O4 Cu1 Br2 94.1(3) . . ? N1 Cu1 Br2 97.8(4) . . ? O1 Cu1 Br1 102.8(3) . . ? O4 Cu1 Br1 86.9(3) . . ? N1 Cu1 Br1 98.3(3) . . ? Br2 Cu1 Br1 105.17(8) . . ? O3 Cu2 O2 150.9(4) . 3_677 ? O3 Cu2 O4 84.4(4) . . ? O2 Cu2 O4 93.6(4) 3_677 . ? O3 Cu2 N3 84.6(5) . . ? O2 Cu2 N3 95.4(5) 3_677 . ? O4 Cu2 N3 169.0(5) . . ? O3 Cu2 Br1 99.6(3) . . ? O2 Cu2 Br1 109.2(3) 3_677 . ? O4 Cu2 Br1 85.7(2) . . ? N3 Cu2 Br1 97.3(4) . . ? O1 Co3 O3 113.2(4) . . ? O1 Co3 O2 128.1(4) . . ? O3 Co3 O2 111.3(4) . . ? O1 Co3 N2 108.1(4) . . ? O3 Co3 N2 106.7(5) . . ? O2 Co3 N2 82.6(4) . . ? O1 Co3 O4 74.4(3) . . ? O3 Co3 O4 76.0(4) . . ? O2 Co3 O4 92.2(3) . . ? N2 Co3 O4 174.7(4) . . ? C1 O1 Cu1 116.1(8) . . ? C1 O1 Co3 134.4(9) . . ? Cu1 O1 Co3 107.7(4) . . ? C5 O2 Cu2 124.0(8) . 3_677 ? C5 O2 Co3 116.2(8) . . ? Cu2 O2 Co3 114.3(4) 3_677 . ? C9 O3 Cu2 114.6(9) . . ? C9 O3 Co3 138.8(10) . . ? Cu2 O3 Co3 106.2(4) . . ? Cu1 O4 Cu2 114.2(4) . . ? Cu1 O4 Co3 95.1(4) . . ? Cu2 O4 Co3 93.4(4) . . ? Cu1 O4 H4O 106.1(90) . . ? Cu2 O4 H4O 115.9(94) . . ? Co3 O4 H4O 130.7(96) . . ? C2 N1 C3 111.2(12) . . ? C2 N1 C4 111.0(11) . . ? C3 N1 C4 107.8(12) . . ? C2 N1 Cu1 103.6(8) . . ? C3 N1 Cu1 108.7(8) . . ? C4 N1 Cu1 114.6(9) . . ? C8 N2 C7 104.2(15) . . ? C8 N2 C6 112.4(15) . . ? C7 N2 C6 106.9(15) . . ? C8 N2 Co3 112.3(11) . . ? C7 N2 Co3 121.1(11) . . ? C6 N2 Co3 100.0(9) . . ? C10 N3 C11 112.8(12) . . ? C10 N3 C12 110.2(13) . . ? C11 N3 C12 106.5(12) . . ? C10 N3 Cu2 102.6(9) . . ? C11 N3 Cu2 111.5(9) . . ? C12 N3 Cu2 113.4(10) . . ? O1 C1 C2 107.4(11) . . ? O1 C1 H1A 110.2 . . ? C2 C1 H1A 111.2 . . ? O1 C1 H1B 110.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 108.9 . . ? N1 C2 C1 111.5(11) . . ? N1 C2 H2A 109.8 . . ? C1 C2 H2A 111.3 . . ? N1 C2 H2B 107.8 . . ? C1 C2 H2B 108.2 . . ? H2A C2 H2B 108.1 . . ? N1 C3 H3A 109.1 . . ? N1 C3 H3B 111.1 . . ? H3A C3 H3B 108.9 . . ? N1 C3 H3C 110.1 . . ? H3A C3 H3C 108.9 . . ? H3B C3 H3C 108.8 . . ? N1 C4 H4A 111.2 . . ? N1 C4 H4B 108.1 . . ? H4A C4 H4B 110.5 . . ? N1 C4 H4C 108.8 . . ? H4A C4 H4C 110.5 . . ? H4B C4 H4C 107.7 . . ? O2 C5 C6 109.6(12) . . ? O2 C5 H5A 109.8 . . ? C6 C5 H5A 111.0 . . ? O2 C5 H5B 109.6 . . ? C6 C5 H5B 108.6 . . ? H5A C5 H5B 108.2 . . ? N2 C6 C5 109.4(15) . . ? N2 C6 H6A 109.8 . . ? C5 C6 H6A 110.8 . . ? N2 C6 H6B 109.0 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 108.7 . . ? N2 C7 H7A 108.2 . . ? N2 C7 H7B 110.6 . . ? H7A C7 H7B 109.6 . . ? N2 C7 H7C 110.7 . . ? H7A C7 H7C 109.6 . . ? H7B C7 H7C 108.3 . . ? N2 C8 H8A 111.2 . . ? N2 C8 H8B 107.6 . . ? H8A C8 H8B 109.93 . . ? N2 C8 H8C 110.0 . . ? H8A C8 H8C 109.9 . . ? H8B C8 H8C 108.1 . . ? O3 C9 C10 109.5(12) . . ? O3 C9 H9A 109.3 . . ? C10 C9 H9A 108.6 . . ? O3 C9 H9B 110.5 . . ? C10 C9 H9B 110.7 . . ? H9A C9 H9B 108.2 . . ? N3 C10 C9 111.4(13) . . ? N3 C10 H10A 109.3 . . ? C9 C10 H10A 108.4 . . ? N3 C10 H10B 109.3 . . ? C9 C10 H10B 110.3 . . ? H10A C10 H10B 108.2 . . ? N3 C11 H11A 110.6 . . ? N3 C11 H11B 110.1 . . ? H11A C11 H11B 109.7 . . ? N3 C11 H11C 108.5 . . ? H11A C11 H11C 109.7 . . ? H11B C11 H11C 108.2 . . ? N3 C12 H12A 110.2 . . ? N3 C12 H12B 109.1 . . ? H12A C12 H12B 110.7 . . ? N3 C12 H12C 108.6 . . ? H12A C12 H12C 110.6 . . ? H12B C12 H12C 107.6 . . ? N4 C13 C14 175.4(31) . . ? C13 C14 H14A 111.1 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 107.5 . . ? H14A C14 H14C 109.47 . . ? H14B C14 H14C 109.5 . . ? _refine_diff_density_max 1.194 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.165