# Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Leigh Jones' _publ_contact_author_email LEIGH.JONES@NUIGALWAY.IE _publ_section_title ; Planar [Ni7] Discs as Double-Bowl, Pseudo Metallacalix[6]arene Host Cavities. ; loop_ _publ_author_name 'Leigh Jones' 'Euan Brechin' 'Peter W. Dunne' 'Georgios Karotsis' 'Patrick McArdle' 'Sean Meally' ; G.S.Papaefstathioi ; # Attachment '[Ni7](1).cif' data_lfj50a-1 _database_code_depnum_ccdc_archive 'CCDC 741051' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ni7(OH)6(L1)6)(NO3)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H66 N8 Ni7 O24' _chemical_formula_weight 1622.12 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' _cell_length_a 13.806(2) _cell_length_b 13.806(2) _cell_length_c 23.270(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3841.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 1.749 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _exptl_absorpt_correction_T_min 0.57946 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 8234 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.1183 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.6239 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0349664281 _diffrn_orient_matrix_UB_12 0.0096677209 _diffrn_orient_matrix_UB_13 0.0187042266 _diffrn_orient_matrix_UB_21 -0.0078340246 _diffrn_orient_matrix_UB_22 -0.0457483366 _diffrn_orient_matrix_UB_23 0.0173695959 _diffrn_orient_matrix_UB_31 0.0473800140 _diffrn_orient_matrix_UB_32 0.0366962609 _diffrn_orient_matrix_UB_33 0.0167299896 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -33.00 79.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 19.5780 0.0000 -90.0000 112 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 2306 _reflns_number_gt 1376 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1573P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -10(10) _refine_ls_number_reflns 2306 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1209 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.2662 _refine_ls_wR_factor_gt 0.2446 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.0000 0.0000 0.0270(7) Uani 1 6 d S . . Ni2 Ni 0.10310(10) 0.25718(10) -0.00763(5) 0.0289(5) Uani 1 1 d . . . O1 O 0.1252(5) 0.1349(5) -0.0442(3) 0.0255(14) Uani 1 1 d . . . H1 H 0.1306 0.1314 -0.0869 0.031 Uiso 1 1 calc R . . O2 O 0.2407(5) 0.2819(5) 0.0336(3) 0.0261(14) Uani 1 1 d . . . O3 O 0.1427(6) 0.3972(5) 0.0564(3) 0.0381(17) Uani 1 1 d . . . O4 O 0.6484(8) 0.4125(8) 0.2044(4) 0.072(3) Uani 1 1 d . . . N1 N 0.3820(7) 0.2033(7) 0.0694(4) 0.038(2) Uani 1 1 d . . . N2 N 0.6667 0.3333 0.2027(6) 0.045(4) Uani 1 3 d S . . C1 C 0.4400(12) 0.1341(12) 0.0734(7) 0.077(5) Uani 1 1 d . . . H1A H 0.4925 0.1608 0.1058 0.116 Uiso 1 1 calc R . . H1B H 0.4808 0.1417 0.0377 0.116 Uiso 1 1 calc R . . H1C H 0.3839 0.0552 0.0794 0.116 Uiso 1 1 calc R . . C2 C 0.4066(9) 0.2756(9) 0.1097(5) 0.041(3) Uani 1 1 d . . . H2 H 0.4634 0.2852 0.1359 0.049 Uiso 1 1 calc R . . C3 C 0.3557(9) 0.3434(9) 0.1184(4) 0.036(2) Uiso 1 1 d . . . C4 C 0.3873(9) 0.4115(9) 0.1688(5) 0.046(3) Uani 1 1 d . . . H4 H 0.4420 0.4126 0.1940 0.056 Uiso 1 1 calc R . . C5 C 0.3399(10) 0.4746(9) 0.1809(5) 0.047(3) Uani 1 1 d . . . H5 H 0.3623 0.5205 0.2143 0.057 Uiso 1 1 calc R . . C6 C 0.2589(10) 0.4723(9) 0.1449(4) 0.044(3) Uani 1 1 d . . . H6 H 0.2243 0.5150 0.1541 0.053 Uiso 1 1 calc R . . C7 C 0.2284(9) 0.4080(8) 0.0959(4) 0.035(2) Uani 1 1 d . . . C8 C 0.1345(11) 0.4935(10) 0.0481(6) 0.063(4) Uani 1 1 d . . . H8A H 0.0887 0.4989 0.0787 0.094 Uiso 1 1 calc R . . H8B H 0.0996 0.4890 0.0108 0.094 Uiso 1 1 calc R . . H8C H 0.2094 0.5597 0.0490 0.094 Uiso 1 1 calc R . . C9 C 0.2740(8) 0.3411(8) 0.0806(4) 0.031(2) Uani 1 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 Ni1 0.0161(9) 0.0161(9) 0.0489(19) 0.000 0.000 0.0080(5) Ni2 0.0219(7) 0.0206(7) 0.0433(8) 0.0002(5) -0.0039(5) 0.0099(6) O1 0.023(3) 0.018(3) 0.030(3) 0.001(3) 0.002(3) 0.006(3) O2 0.028(3) 0.023(3) 0.030(4) -0.012(3) -0.010(3) 0.015(3) O3 0.042(4) 0.029(4) 0.053(4) -0.001(3) -0.004(3) 0.024(3) O4 0.072(6) 0.055(6) 0.099(7) 0.019(5) 0.026(5) 0.039(5) N1 0.032(5) 0.039(5) 0.047(5) -0.007(4) -0.007(4) 0.022(4) N2 0.048(6) 0.048(6) 0.040(9) 0.000 0.000 0.024(3) C1 0.058(9) 0.089(11) 0.106(12) -0.045(9) -0.031(8) 0.053(9) C2 0.036(6) 0.046(7) 0.039(6) -0.001(5) -0.006(5) 0.019(5) C4 0.048(7) 0.042(7) 0.050(7) -0.003(5) -0.009(6) 0.023(6) C5 0.055(8) 0.050(7) 0.044(6) -0.012(5) -0.010(5) 0.031(6) C6 0.058(8) 0.042(6) 0.044(6) -0.006(5) -0.002(6) 0.034(6) C7 0.033(6) 0.027(5) 0.039(5) -0.001(5) 0.001(5) 0.009(5) C8 0.060(9) 0.042(7) 0.094(10) 0.007(7) -0.016(7) 0.032(7) C9 0.030(5) 0.026(5) 0.032(5) 0.007(4) 0.006(4) 0.011(4) _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 Ni1 O1 2.072(6) 8 ? Ni1 O1 2.072(6) 9 ? Ni1 O1 2.072(6) 7 ? Ni1 O1 2.072(6) . ? Ni1 O1 2.072(6) 3 ? Ni1 O1 2.072(6) 2 ? Ni2 O2 1.983(6) 9 ? Ni2 O2 1.999(6) . ? Ni2 O1 2.045(6) . ? Ni2 N1 2.080(8) 9 ? Ni2 O1 2.088(6) 9 ? Ni2 O3 2.280(7) . ? O1 Ni2 2.088(6) 8 ? O1 H1 1.0000 . ? O2 C9 1.304(11) . ? O2 Ni2 1.983(6) 8 ? O3 C8 1.403(12) . ? O3 C7 1.446(12) . ? O4 N2 1.238(9) . ? N1 C2 1.286(13) . ? N1 C1 1.526(14) . ? N1 Ni2 2.080(8) 8 ? N2 O4 1.238(9) 3_665 ? N2 O4 1.238(9) 2_655 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.439(14) . ? C2 H2 0.9500 . ? C3 C9 1.419(14) . ? C3 C4 1.427(14) . ? C4 C5 1.355(14) . ? C4 H4 0.9500 . ? C5 C6 1.386(15) . ? C5 H5 0.9500 . ? C6 C7 1.375(14) . ? C6 H6 0.9500 . ? C7 C9 1.398(14) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 O1 Ni1 O1 97.5(2) 8 9 ? O1 Ni1 O1 97.5(2) 8 7 ? O1 Ni1 O1 97.5(2) 9 7 ? O1 Ni1 O1 82.5(2) 8 . ? O1 Ni1 O1 82.5(2) 9 . ? O1 Ni1 O1 180.0(6) 7 . ? O1 Ni1 O1 82.5(2) 8 3 ? O1 Ni1 O1 180.0(4) 9 3 ? O1 Ni1 O1 82.5(2) 7 3 ? O1 Ni1 O1 97.5(2) . 3 ? O1 Ni1 O1 180.0(4) 8 2 ? O1 Ni1 O1 82.5(2) 9 2 ? O1 Ni1 O1 82.5(2) 7 2 ? O1 Ni1 O1 97.5(2) . 2 ? O1 Ni1 O1 97.5(2) 3 2 ? O2 Ni2 O2 168.54(15) 9 . ? O2 Ni2 O1 109.6(2) 9 . ? O2 Ni2 O1 79.6(2) . . ? O2 Ni2 N1 86.8(3) 9 9 ? O2 Ni2 N1 98.6(3) . 9 ? O1 Ni2 N1 100.1(3) . 9 ? O2 Ni2 O1 78.9(2) 9 9 ? O2 Ni2 O1 95.9(2) . 9 ? O1 Ni2 O1 82.8(3) . 9 ? N1 Ni2 O1 165.5(3) 9 9 ? O2 Ni2 O3 95.6(3) 9 . ? O2 Ni2 O3 74.8(2) . . ? O1 Ni2 O3 154.2(2) . . ? N1 Ni2 O3 86.6(3) 9 . ? O1 Ni2 O3 96.9(2) 9 . ? Ni2 O1 Ni1 97.7(2) . . ? Ni2 O1 Ni2 97.8(2) . 8 ? Ni1 O1 Ni2 96.3(2) . 8 ? Ni2 O1 H1 119.9 . . ? Ni1 O1 H1 119.9 . . ? Ni2 O1 H1 119.9 8 . ? C9 O2 Ni2 130.7(6) . 8 ? C9 O2 Ni2 121.1(6) . . ? Ni2 O2 Ni2 102.9(3) 8 . ? C8 O3 C7 116.1(8) . . ? C8 O3 Ni2 127.9(7) . . ? C7 O3 Ni2 109.9(5) . . ? C2 N1 C1 115.1(9) . . ? C2 N1 Ni2 127.7(7) . 8 ? C1 N1 Ni2 116.6(7) . 8 ? O4 N2 O4 119.89(10) 3_665 2_655 ? O4 N2 O4 119.89(11) 3_665 . ? O4 N2 O4 119.89(10) 2_655 . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 125.7(10) . . ? N1 C2 H2 117.2 . . ? C3 C2 H2 117.2 . . ? C9 C3 C4 120.1(9) . . ? C9 C3 C2 122.6(9) . . ? C4 C3 C2 117.2(9) . . ? C5 C4 C3 120.5(10) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.2(10) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C6 C5 120.0(10) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C9 123.0(10) . . ? C6 C7 O3 124.3(9) . . ? C9 C7 O3 112.6(8) . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C7 119.6(9) . . ? O2 C9 C3 124.2(9) . . ? C7 C9 C3 116.2(9) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.961 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.210 # Attachment '[Ni7](2)cif.cif' data_lfj54d-1 _database_code_depnum_ccdc_archive 'CCDC 741052' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ni7(OH)6(L1)6)(NO3)2.3MeNO2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H75 N11 Ni7 O24' _chemical_formula_weight 1709.25 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' _cell_length_a 13.933(2) _cell_length_b 13.933(2) _cell_length_c 22.742(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3823.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1764 _exptl_absorpt_coefficient_mu 1.762 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _exptl_absorpt_correction_T_min 0.97599 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 9773 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.0529 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0466997139 _diffrn_orient_matrix_UB_12 -0.0455575681 _diffrn_orient_matrix_UB_13 0.0131894495 _diffrn_orient_matrix_UB_21 0.0157415404 _diffrn_orient_matrix_UB_22 0.0269490050 _diffrn_orient_matrix_UB_23 0.0276872274 _diffrn_orient_matrix_UB_31 -0.0320891875 _diffrn_orient_matrix_UB_32 0.0256188138 _diffrn_orient_matrix_UB_33 -0.0056400845 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -41.00 13.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - -17.2341 -77.0000 90.0000 54 #__ type_ start__ end____ width___ exp.time_ 2 omega 7.00 81.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 37.0000 90.0000 74 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 2333 _reflns_number_gt 1835 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1104P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 10(10) _refine_ls_number_reflns 2333 _refine_ls_number_parameters 157 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1725 _refine_ls_wR_factor_gt 0.1676 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.191 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.0000 0.5000 0.0157(4) Uani 1 6 d S . . Ni2 Ni 0.10544(5) 0.25516(5) 0.50881(3) 0.0188(3) Uani 1 1 d . . . O1 O 0.1258(3) 0.1325(3) 0.54483(14) 0.0186(7) Uani 1 1 d . . . O2 O 0.2396(3) 0.2769(3) 0.46571(15) 0.0199(7) Uani 1 1 d . . . O3 O 0.1491(3) 0.3966(3) 0.44262(17) 0.0263(9) Uani 1 1 d . . . O4 O 0.4181(5) 0.6561(5) 0.2054(3) 0.0704(16) Uani 1 1 d . . . O5 O 0.156(2) 0.075(2) 0.1729(13) 0.209(11) Uiso 0.50 1 d PD . . O6 O 0.066(2) 0.178(2) 0.1837(12) 0.197(11) Uiso 0.50 1 d PD . . N1 N 0.3770(4) 0.1955(4) 0.4284(2) 0.0259(10) Uani 1 1 d . . . N2 N 0.3333 0.6667 0.2029(4) 0.039(2) Uani 1 3 d S . . N3 N 0.1255(17) 0.1389(18) 0.1949(8) 0.144(9) Uiso 0.50 1 d PD . . C1 C 0.4355(6) 0.1312(6) 0.4268(3) 0.0427(16) Uani 1 1 d . . . H1A H 0.4914 0.1601 0.3955 0.064 Uiso 1 1 calc R . . H1B H 0.3820 0.0530 0.4190 0.064 Uiso 1 1 calc R . . H1C H 0.4717 0.1378 0.4647 0.064 Uiso 1 1 calc R . . C2 C 0.4055(5) 0.2703(4) 0.3898(2) 0.0278(12) Uani 1 1 d . . . H2 H 0.4634 0.2810 0.3639 0.033 Uiso 1 1 calc R . . C3 C 0.3580(4) 0.3417(4) 0.3814(2) 0.0243(11) Uani 1 1 d . . . C4 C 0.3970(5) 0.4162(5) 0.3323(2) 0.0313(13) Uani 1 1 d . . . H4 H 0.4539 0.4198 0.3078 0.038 Uiso 1 1 calc R . . C5 C 0.3523(5) 0.4824(5) 0.3208(3) 0.0338(14) Uani 1 1 d . . . H5 H 0.3786 0.5315 0.2881 0.041 Uiso 1 1 calc R . . C6 C 0.2683(5) 0.4785(5) 0.3564(2) 0.0309(13) Uani 1 1 d . . . H6 H 0.2366 0.5234 0.3478 0.037 Uiso 1 1 calc R . . C7 C 0.2325(4) 0.4080(4) 0.4045(2) 0.0231(11) Uani 1 1 d . . . C8 C 0.1433(5) 0.4950(4) 0.4542(3) 0.0350(14) Uani 1 1 d . . . H8A H 0.2166 0.5552 0.4657 0.052 Uiso 1 1 calc R . . H8B H 0.0904 0.4804 0.4861 0.052 Uiso 1 1 calc R . . H8C H 0.1188 0.5164 0.4186 0.052 Uiso 1 1 calc R . . C9 C 0.2764(4) 0.3394(4) 0.4180(2) 0.0196(11) Uani 1 1 d . . . C10 C 0.1878(14) 0.1878(14) 0.2500 0.122(6) Uiso 1 2 d SD . . 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 Ni1 0.0138(5) 0.0138(5) 0.0196(8) 0.000 0.000 0.0069(2) Ni2 0.0164(4) 0.0156(4) 0.0239(4) -0.0011(3) 0.0030(3) 0.0077(3) O1 0.0160(17) 0.0160(17) 0.0210(17) -0.0006(14) 0.0002(14) 0.0059(14) O2 0.0207(17) 0.0160(17) 0.0242(18) 0.0066(14) 0.0082(15) 0.0101(15) O3 0.028(2) 0.0213(18) 0.035(2) 0.0042(16) 0.0059(17) 0.0163(16) O4 0.056(3) 0.073(4) 0.086(4) 0.031(3) 0.019(3) 0.035(3) N1 0.024(2) 0.027(2) 0.031(3) 0.004(2) 0.004(2) 0.016(2) N2 0.036(3) 0.036(3) 0.044(5) 0.000 0.000 0.0180(15) C1 0.045(4) 0.053(4) 0.051(4) 0.019(3) 0.020(3) 0.040(3) C2 0.028(3) 0.026(3) 0.029(3) 0.003(2) 0.006(2) 0.013(2) C3 0.022(3) 0.023(3) 0.026(3) -0.002(2) 0.002(2) 0.010(2) C4 0.041(3) 0.034(3) 0.022(3) 0.001(2) 0.005(3) 0.021(3) C5 0.046(4) 0.028(3) 0.027(3) 0.003(2) 0.007(3) 0.018(3) C6 0.044(3) 0.026(3) 0.030(3) 0.000(2) -0.002(3) 0.022(3) C7 0.023(3) 0.018(2) 0.026(3) -0.001(2) -0.002(2) 0.009(2) C8 0.035(3) 0.022(3) 0.053(4) -0.003(3) 0.003(3) 0.018(3) C9 0.021(3) 0.014(2) 0.019(2) 0.000(2) 0.000(2) 0.005(2) _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 Ni1 O1 2.070(3) . ? Ni1 O1 2.070(3) 7_556 ? Ni1 O1 2.070(3) 2 ? Ni1 O1 2.070(3) 8_556 ? Ni1 O1 2.070(3) 3 ? Ni1 O1 2.070(3) 9_556 ? Ni2 O2 1.976(3) 9_556 ? Ni2 O2 1.996(3) . ? Ni2 O1 2.038(3) . ? Ni2 N1 2.060(4) 9_556 ? Ni2 O1 2.089(3) 9_556 ? Ni2 O3 2.307(4) . ? O1 Ni2 2.089(3) 8_556 ? O2 C9 1.323(6) . ? O2 Ni2 1.976(3) 8_556 ? O3 C7 1.394(6) . ? O3 C8 1.437(6) . ? O4 N2 1.262(6) . ? O5 N3 1.258(17) . ? O5 O6 1.77(3) 3 ? O6 N3 1.224(17) . ? O6 O5 1.77(3) 2 ? N1 C2 1.265(7) . ? N1 C1 1.483(7) . ? N1 Ni2 2.060(4) 8_556 ? N2 O4 1.262(6) 2_665 ? N2 O4 1.262(6) 3_565 ? N3 C10 1.483(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.456(7) . ? C2 H2 0.9500 . ? C3 C9 1.397(7) . ? C3 C4 1.434(8) . ? C4 C5 1.371(8) . ? C4 H4 0.9500 . ? C5 C6 1.402(8) . ? C5 H5 0.9500 . ? C6 C7 1.385(7) . ? C6 H6 0.9500 . ? C7 C9 1.404(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 N3 1.483(17) 4 ? 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 O1 Ni1 O1 180.0 . 7_556 ? O1 Ni1 O1 97.82(12) . 2 ? O1 Ni1 O1 82.18(12) 7_556 2 ? O1 Ni1 O1 82.18(12) . 8_556 ? O1 Ni1 O1 97.82(12) 7_556 8_556 ? O1 Ni1 O1 180.00(16) 2 8_556 ? O1 Ni1 O1 97.82(12) . 3 ? O1 Ni1 O1 82.18(12) 7_556 3 ? O1 Ni1 O1 97.82(12) 2 3 ? O1 Ni1 O1 82.18(12) 8_556 3 ? O1 Ni1 O1 82.18(12) . 9_556 ? O1 Ni1 O1 97.82(12) 7_556 9_556 ? O1 Ni1 O1 82.18(12) 2 9_556 ? O1 Ni1 O1 97.82(12) 8_556 9_556 ? O1 Ni1 O1 180.00(16) 3 9_556 ? O2 Ni2 O2 167.34(8) 9_556 . ? O2 Ni2 O1 110.14(14) 9_556 . ? O2 Ni2 O1 79.17(13) . . ? O2 Ni2 N1 87.82(15) 9_556 9_556 ? O2 Ni2 N1 99.11(16) . 9_556 ? O1 Ni2 N1 100.51(15) . 9_556 ? O2 Ni2 O1 78.40(13) 9_556 9_556 ? O2 Ni2 O1 94.83(14) . 9_556 ? O1 Ni2 O1 82.48(17) . 9_556 ? N1 Ni2 O1 166.05(15) 9_556 9_556 ? O2 Ni2 O3 96.09(14) 9_556 . ? O2 Ni2 O3 73.93(13) . . ? O1 Ni2 O3 152.95(13) . . ? N1 Ni2 O3 86.60(16) 9_556 . ? O1 Ni2 O3 96.90(13) 9_556 . ? Ni2 O1 Ni1 98.02(14) . . ? Ni2 O1 Ni2 98.22(13) . 8_556 ? Ni1 O1 Ni2 96.41(13) . 8_556 ? C9 O2 Ni2 130.6(3) . 8_556 ? C9 O2 Ni2 121.8(3) . . ? Ni2 O2 Ni2 103.55(15) 8_556 . ? C7 O3 C8 116.5(4) . . ? C7 O3 Ni2 110.6(3) . . ? C8 O3 Ni2 125.3(4) . . ? N3 O5 O6 133(2) . 3 ? N3 O6 O5 115(2) . 2 ? C2 N1 C1 116.1(5) . . ? C2 N1 Ni2 127.3(4) . 8_556 ? C1 N1 Ni2 116.6(4) . 8_556 ? O4 N2 O4 119.79(9) 2_665 3_565 ? O4 N2 O4 119.79(9) 2_665 . ? O4 N2 O4 119.79(9) 3_565 . ? O6 N3 O5 140(3) . . ? O6 N3 C10 110(2) . . ? O5 N3 C10 110(2) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 126.3(5) . . ? N1 C2 H2 116.8 . . ? C3 C2 H2 116.8 . . ? C9 C3 C4 119.3(5) . . ? C9 C3 C2 123.2(5) . . ? C4 C3 C2 117.4(5) . . ? C5 C4 C3 120.1(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.9(5) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 118.8(5) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C6 C7 O3 123.8(5) . . ? C6 C7 C9 122.1(5) . . ? O3 C7 C9 114.1(4) . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C3 123.2(5) . . ? O2 C9 C7 118.1(5) . . ? C3 C9 C7 118.7(5) . . ? N3 C10 N3 117.0(18) . 4 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.881 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.159 # Attachment '[Ni7](3)cif.cif' data_lfj41c-4 _database_code_depnum_ccdc_archive 'CCDC 741053' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ni7(OH)6(L2)6)(NO3)2.2MeCN _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H66 Br6 N10 Ni7 O24' _chemical_formula_weight 2177.64 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.8575(14) _cell_length_b 11.1352(3) _cell_length_c 27.4079(13) _cell_angle_alpha 90.00 _cell_angle_beta 109.603(6) _cell_angle_gamma 90.00 _cell_volume 8296.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 373(2) _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4328 _exptl_absorpt_coefficient_mu 4.516 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _exptl_absorpt_correction_T_min 0.79476 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 18887 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.1312 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.6741 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 0.0205093959 _diffrn_orient_matrix_UB_12 0.0134896450 _diffrn_orient_matrix_UB_13 -0.0077844625 _diffrn_orient_matrix_UB_21 0.0160299555 _diffrn_orient_matrix_UB_22 -0.0113405526 _diffrn_orient_matrix_UB_23 0.0255346062 _diffrn_orient_matrix_UB_31 0.0015659969 _diffrn_orient_matrix_UB_32 -0.0612051726 _diffrn_orient_matrix_UB_33 -0.0064358310 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 51.00 90.00 1.0000 70.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 77.0000 -120.0000 39 #__ type_ start__ end____ width___ exp.time_ 2 omega -10.00 87.00 1.0000 70.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 77.0000 -150.0000 97 #__ type_ start__ end____ width___ exp.time_ 3 omega -21.00 80.00 1.0000 70.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 21.0000 -136.0000 101 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 373(2) _reflns_number_total 7348 _reflns_number_gt 3779 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7348 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 0.852 _refine_ls_restrained_S_all 0.852 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.30834(4) 0.32502(8) 0.61337(4) 0.0209(3) Uani 1 1 d . . . Ni2 Ni 0.36004(4) 0.32193(8) 0.53002(4) 0.0239(3) Uani 1 1 d . . . Ni3 Ni 0.30592(4) 0.19807(8) 0.42406(4) 0.0203(3) Uani 1 1 d . . . Ni4 Ni 0.2500 0.2500 0.5000 0.0192(3) Uani 1 2 d S . . Br1 Br 0.37781(5) 0.94535(8) 0.63389(5) 0.0596(4) Uani 1 1 d . . . Br2 Br 0.51546(4) -0.19234(9) 0.57124(4) 0.0530(3) Uani 1 1 d . . . Br3 Br 0.25576(4) 0.72170(7) 0.27376(4) 0.0372(3) Uani 1 1 d . . . O1 O 0.31542(19) 0.2110(4) 0.55773(19) 0.0213(13) Uani 1 1 d . . . H1 H 0.3248 0.1272 0.5665 0.026 Uiso 1 1 calc R . . O2 O 0.29627(19) 0.3396(4) 0.4694(2) 0.0225(13) Uani 1 1 d . . . H2 H 0.2867 0.4188 0.4536 0.027 Uiso 1 1 calc R . . O3 O 0.25382(19) 0.1187(4) 0.44759(19) 0.0224(13) Uani 1 1 d . . . H3A H 0.2573 0.0341 0.4581 0.027 Uiso 1 1 calc R . . O4 O 0.2452(2) 0.2345(4) 0.36281(19) 0.0201(12) Uani 1 1 d . . . O5 O 0.3318(2) 0.3317(4) 0.3763(2) 0.0270(14) Uani 1 1 d . . . O6 O 0.3694(2) 0.1985(4) 0.4815(2) 0.0245(13) Uani 1 1 d . . . O7 O 0.4323(2) 0.2281(5) 0.5743(2) 0.0373(15) Uani 1 1 d . . . O8 O 0.3567(2) 0.4177(4) 0.5890(2) 0.0258(14) Uani 1 1 d . . . O9 O 0.3215(2) 0.5037(4) 0.6582(2) 0.0306(15) Uani 1 1 d . . . O10 O 0.6073(3) 0.2984(6) 0.6121(3) 0.062(2) Uani 1 1 d . . . O11 O 0.5910(3) 0.1768(7) 0.6656(3) 0.071(2) Uani 1 1 d . . . O12 O 0.5991(3) 0.3640(7) 0.6814(4) 0.094(3) Uani 1 1 d . . . N1 N 0.3991(3) 0.4605(6) 0.5128(3) 0.0304(17) Uiso 1 1 d . . . N2 N 0.3303(3) 0.0541(5) 0.3945(3) 0.0223(15) Uiso 1 1 d . . . N3 N 0.1433(2) 0.2563(5) 0.3234(2) 0.0235(15) Uiso 1 1 d . . . N4 N 0.5995(3) 0.2794(9) 0.6532(4) 0.053(2) Uani 1 1 d . . . N5 N 0.2518(5) 0.5951(9) 0.4774(5) 0.107(4) Uani 1 1 d . . . C1 C 0.3307(4) 0.5163(7) 0.7127(3) 0.038(2) Uani 1 1 d . . . H1A H 0.3651 0.5316 0.7300 0.057 Uiso 1 1 calc R . . H1B H 0.3215 0.4436 0.7259 0.057 Uiso 1 1 calc R . . H1C H 0.3118 0.5821 0.7186 0.057 Uiso 1 1 calc R . . C2 C 0.3444(3) 0.5845(6) 0.6355(3) 0.028(2) Uani 1 1 d . . . C3 C 0.3479(4) 0.7060(7) 0.6459(4) 0.041(3) Uani 1 1 d . . . H3 H 0.3354 0.7391 0.6701 0.049 Uiso 1 1 calc R . . C4 C 0.3705(4) 0.7770(7) 0.6189(4) 0.041(3) Uani 1 1 d . . . C5 C 0.3865(4) 0.7338(7) 0.5816(4) 0.039(3) Uani 1 1 d . . . H5 H 0.4002 0.7854 0.5634 0.047 Uiso 1 1 calc R . . C6 C 0.3608(3) 0.5343(6) 0.5969(3) 0.027(2) Uani 1 1 d . . . C7 C 0.3824(3) 0.6089(7) 0.5699(3) 0.029(2) Uani 1 1 d . . . C8 C 0.4022(3) 0.5666(7) 0.5311(3) 0.033(2) Uani 1 1 d . . . H8 H 0.4190 0.6225 0.5181 0.040 Uiso 1 1 calc R . . C9 C 0.4246(4) 0.4410(9) 0.4748(4) 0.072(4) Uani 1 1 d . . . H9A H 0.4375 0.5161 0.4676 0.108 Uiso 1 1 calc R . . H9B H 0.4019 0.4092 0.4433 0.108 Uiso 1 1 calc R . . H9C H 0.4512 0.3853 0.4887 0.108 Uiso 1 1 calc R . . C10 C 0.4774(4) 0.2832(10) 0.6058(4) 0.061(3) Uani 1 1 d . . . H10A H 0.4920 0.2357 0.6364 0.092 Uiso 1 1 calc R . . H10B H 0.4707 0.3624 0.6155 0.092 Uiso 1 1 calc R . . H10C H 0.4997 0.2882 0.5866 0.092 Uiso 1 1 calc R . . C11 C 0.4362(3) 0.1205(8) 0.5490(3) 0.029(2) Uani 1 1 d . . . C12 C 0.4704(3) 0.0351(8) 0.5703(4) 0.037(2) Uani 1 1 d . . . H12 H 0.4935 0.0446 0.6032 0.044 Uiso 1 1 calc R . . C13 C 0.4698(3) -0.0668(7) 0.5411(4) 0.034(2) Uani 1 1 d . . . C14 C 0.4363(3) -0.0845(7) 0.4927(4) 0.034(2) Uani 1 1 d . . . H14 H 0.4369 -0.1547 0.4745 0.041 Uiso 1 1 calc R . . C15 C 0.4008(3) 0.1113(7) 0.5005(3) 0.0227(19) Uani 1 1 d . . . C16 C 0.4006(3) 0.0056(7) 0.4705(3) 0.025(2) Uani 1 1 d . . . C17 C 0.3674(3) -0.0124(6) 0.4188(3) 0.022(2) Uani 1 1 d . . . H17 H 0.3732 -0.0787 0.4010 0.026 Uiso 1 1 calc R . . C18 C 0.3034(4) 0.0167(8) 0.3423(4) 0.051(3) Uani 1 1 d . . . H18A H 0.3228 -0.0400 0.3310 0.077 Uiso 1 1 calc R . . H18B H 0.2966 0.0853 0.3198 0.077 Uiso 1 1 calc R . . H18C H 0.2731 -0.0202 0.3413 0.077 Uiso 1 1 calc R . . C19 C 0.0904(3) 0.2185(8) 0.3047(4) 0.042(2) Uani 1 1 d . . . H19A H 0.0730 0.2612 0.3235 0.063 Uiso 1 1 calc R . . H19B H 0.0883 0.1337 0.3101 0.063 Uiso 1 1 calc R . . H19C H 0.0761 0.2362 0.2684 0.063 Uiso 1 1 calc R . . C20 C 0.1534(3) 0.3457(6) 0.2981(3) 0.0238(19) Uani 1 1 d . . . H20 H 0.1280 0.3771 0.2704 0.029 Uiso 1 1 calc R . . C21 C 0.2022(3) 0.3997(6) 0.3105(3) 0.0169(18) Uani 1 1 d . . . C22 C 0.2451(3) 0.3406(6) 0.3410(3) 0.022(2) Uani 1 1 d . . . C23 C 0.2910(3) 0.3978(6) 0.3482(3) 0.0197(19) Uani 1 1 d . . . C24 C 0.2940(3) 0.5097(6) 0.3287(3) 0.023(2) Uani 1 1 d . . . H24 H 0.3242 0.5474 0.3348 0.027 Uiso 1 1 calc R . . C25 C 0.2507(4) 0.5642(6) 0.2995(3) 0.027(2) Uani 1 1 d . . . C26 C 0.2062(3) 0.5129(6) 0.2903(3) 0.0210(19) Uani 1 1 d . . . H26 H 0.1780 0.5533 0.2704 0.025 Uiso 1 1 calc R . . C27 C 0.3671(3) 0.3124(9) 0.3507(4) 0.053(3) Uani 1 1 d . . . H27A H 0.3511 0.2768 0.3174 0.080 Uiso 1 1 calc R . . H27B H 0.3925 0.2597 0.3712 0.080 Uiso 1 1 calc R . . H27C H 0.3814 0.3879 0.3463 0.080 Uiso 1 1 calc R . . C29 C 0.2682(5) 0.6622(11) 0.4576(5) 0.080(4) Uani 1 1 d . . . C30 C 0.2884(5) 0.7528(11) 0.4333(6) 0.095(5) Uani 1 1 d . . . H30A H 0.2922 0.7207 0.4024 0.143 Uiso 1 1 calc R . . H30B H 0.3198 0.7778 0.4567 0.143 Uiso 1 1 calc R . . H30C H 0.2665 0.8205 0.4245 0.143 Uiso 1 1 calc R . . 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 Ni1 0.0248(6) 0.0164(5) 0.0224(6) -0.0003(4) 0.0090(5) -0.0009(5) Ni2 0.0217(6) 0.0240(5) 0.0277(6) -0.0072(5) 0.0104(6) -0.0027(5) Ni3 0.0222(6) 0.0181(5) 0.0215(6) 0.0021(5) 0.0084(5) 0.0038(5) Ni4 0.0203(9) 0.0178(7) 0.0205(8) 0.0002(6) 0.0083(7) 0.0003(7) Br1 0.0878(10) 0.0219(5) 0.0929(9) -0.0093(5) 0.0618(9) -0.0096(6) Br2 0.0323(6) 0.0529(6) 0.0720(8) 0.0310(6) 0.0150(6) 0.0191(6) Br3 0.0525(7) 0.0192(4) 0.0420(6) 0.0094(4) 0.0187(5) 0.0012(4) O1 0.021(3) 0.012(2) 0.030(3) -0.001(2) 0.007(3) 0.000(2) O2 0.024(3) 0.017(3) 0.030(3) 0.001(2) 0.013(3) 0.001(3) O3 0.028(4) 0.015(3) 0.025(3) 0.001(2) 0.011(3) 0.007(3) O4 0.026(3) 0.011(2) 0.025(3) 0.005(2) 0.011(3) 0.003(3) O5 0.023(3) 0.033(3) 0.028(3) 0.007(3) 0.012(3) 0.002(3) O6 0.022(3) 0.026(3) 0.026(3) -0.004(3) 0.009(3) 0.007(3) O7 0.021(4) 0.054(4) 0.033(4) -0.015(3) 0.004(3) 0.004(3) O8 0.031(4) 0.017(3) 0.033(4) -0.006(2) 0.015(3) -0.005(3) O9 0.048(4) 0.024(3) 0.026(4) -0.004(3) 0.021(3) -0.007(3) O10 0.075(6) 0.052(4) 0.065(5) -0.011(4) 0.031(5) -0.012(4) O11 0.080(7) 0.057(5) 0.081(6) 0.003(4) 0.032(5) 0.003(5) O12 0.091(7) 0.091(6) 0.113(8) -0.069(6) 0.052(7) -0.032(6) N4 0.032(6) 0.064(6) 0.063(7) -0.031(6) 0.015(5) -0.008(5) N5 0.111(11) 0.058(7) 0.153(12) 0.038(7) 0.045(10) 0.007(7) C1 0.055(7) 0.042(5) 0.016(5) -0.002(4) 0.011(5) 0.000(5) C2 0.033(6) 0.019(4) 0.039(6) -0.006(4) 0.023(5) -0.005(4) C3 0.053(7) 0.033(5) 0.048(6) -0.014(5) 0.033(6) -0.013(5) C4 0.059(7) 0.020(4) 0.052(7) -0.004(4) 0.030(6) -0.011(5) C5 0.047(7) 0.023(4) 0.057(7) -0.002(4) 0.031(6) 0.000(5) C6 0.029(6) 0.018(4) 0.039(6) -0.005(4) 0.019(5) -0.005(4) C7 0.040(6) 0.026(4) 0.028(5) -0.006(4) 0.023(5) -0.010(4) C8 0.022(5) 0.040(5) 0.046(6) -0.011(5) 0.023(5) -0.018(4) C9 0.096(10) 0.068(7) 0.087(9) -0.044(7) 0.078(9) -0.042(7) C10 0.035(7) 0.082(8) 0.060(8) -0.030(7) 0.007(6) -0.008(6) C11 0.019(5) 0.040(5) 0.029(5) -0.001(5) 0.009(5) 0.008(5) C12 0.026(6) 0.057(6) 0.031(6) 0.002(5) 0.013(5) 0.001(5) C13 0.021(6) 0.035(5) 0.047(6) 0.018(5) 0.013(5) 0.013(5) C14 0.033(6) 0.021(4) 0.061(7) 0.012(5) 0.033(6) 0.007(4) C15 0.020(5) 0.029(4) 0.021(5) 0.001(4) 0.010(4) 0.001(4) C16 0.026(5) 0.023(4) 0.029(5) 0.013(4) 0.013(5) 0.005(4) C17 0.026(5) 0.020(4) 0.021(5) -0.007(4) 0.010(5) 0.000(4) C18 0.056(8) 0.038(5) 0.048(7) -0.018(5) 0.002(6) 0.008(6) C19 0.031(6) 0.055(6) 0.039(6) 0.000(5) 0.011(5) -0.003(5) C20 0.024(5) 0.025(4) 0.017(5) -0.008(4) -0.001(4) 0.002(4) C21 0.017(5) 0.018(4) 0.016(4) -0.003(3) 0.005(4) 0.005(4) C22 0.033(5) 0.020(4) 0.018(5) -0.003(4) 0.014(4) -0.003(4) C23 0.022(5) 0.023(4) 0.013(4) 0.004(4) 0.005(4) 0.009(4) C24 0.024(5) 0.023(4) 0.023(5) -0.001(4) 0.010(4) -0.003(4) C25 0.048(7) 0.013(4) 0.029(5) 0.002(4) 0.026(5) 0.005(4) C26 0.018(5) 0.024(4) 0.018(5) -0.003(4) 0.001(4) 0.003(4) C27 0.040(7) 0.070(7) 0.062(7) 0.021(6) 0.034(6) 0.023(6) C29 0.088(11) 0.051(7) 0.085(10) 0.021(7) 0.010(9) 0.004(8) C30 0.083(11) 0.106(11) 0.111(12) 0.021(9) 0.051(10) -0.014(9) _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 Ni1 O4 1.984(5) 7_556 ? Ni1 O8 2.020(5) . ? Ni1 N3 2.036(7) 7_556 ? Ni1 O1 2.046(5) . ? Ni1 O3 2.096(5) 7_556 ? Ni1 O9 2.302(5) . ? Ni2 O8 1.966(5) . ? Ni2 O6 1.993(5) . ? Ni2 O2 2.034(6) . ? Ni2 N1 2.056(6) . ? Ni2 O1 2.101(5) . ? Ni2 O7 2.283(6) . ? Ni3 O6 1.975(6) . ? Ni3 O4 2.019(6) . ? Ni3 N2 2.027(6) . ? Ni3 O3 2.027(5) . ? Ni3 O2 2.083(5) . ? Ni3 O5 2.266(5) . ? Ni4 O2 2.058(4) 7_556 ? Ni4 O2 2.058(4) . ? Ni4 O1 2.062(5) . ? Ni4 O1 2.062(5) 7_556 ? Ni4 O3 2.079(4) 7_556 ? Ni4 O3 2.079(4) . ? Br1 C4 1.915(8) . ? Br2 C13 1.909(8) . ? Br3 C25 1.915(7) . ? O1 H1 0.9800 . ? O2 H2 0.9800 . ? O3 Ni1 2.096(5) 7_556 ? O3 H3A 0.9800 . ? O4 C22 1.324(8) . ? O4 Ni1 1.984(5) 7_556 ? O5 C23 1.383(9) . ? O5 C27 1.437(9) . ? O6 C15 1.312(9) . ? O7 C11 1.408(9) . ? O7 C10 1.436(11) . ? O8 C6 1.316(8) . ? O9 C2 1.382(8) . ? O9 C1 1.433(9) . ? O10 N4 1.237(10) . ? O11 N4 1.239(10) . ? O12 N4 1.222(9) . ? N1 C8 1.275(9) . ? N1 C9 1.481(10) . ? N2 C17 1.287(10) . ? N2 C18 1.441(11) . ? N3 C20 1.302(9) . ? N3 C19 1.497(10) . ? N3 Ni1 2.036(7) 7_556 ? N5 C29 1.117(14) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.379(10) . ? C2 C6 1.411(10) . ? C3 C4 1.387(11) . ? C3 H3 0.9300 . ? C4 C5 1.344(11) . ? C5 C7 1.423(10) . ? C5 H5 0.9300 . ? C6 C7 1.391(10) . ? C7 C8 1.446(10) . ? C8 H8 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.354(11) . ? C11 C15 1.380(11) . ? C12 C13 1.384(12) . ? C12 H12 0.9300 . ? C13 C14 1.369(13) . ? C14 C16 1.421(11) . ? C14 H14 0.9300 . ? C15 C16 1.434(11) . ? C16 C17 1.435(11) . ? C17 H17 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.461(10) . ? C20 H20 0.9300 . ? C21 C26 1.397(10) . ? C21 C22 1.405(11) . ? C22 C23 1.420(10) . ? C23 C24 1.371(10) . ? C24 C25 1.378(11) . ? C24 H24 0.9300 . ? C25 C26 1.350(11) . ? C26 H26 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C29 C30 1.436(16) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? 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 O4 Ni1 O8 168.66(19) 7_556 . ? O4 Ni1 N3 87.7(2) 7_556 7_556 ? O8 Ni1 N3 98.9(2) . 7_556 ? O4 Ni1 O1 108.77(19) 7_556 . ? O8 Ni1 O1 79.51(19) . . ? N3 Ni1 O1 98.4(2) 7_556 . ? O4 Ni1 O3 79.0(2) 7_556 7_556 ? O8 Ni1 O3 94.9(2) . 7_556 ? N3 Ni1 O3 166.0(2) 7_556 7_556 ? O1 Ni1 O3 82.2(2) . 7_556 ? O4 Ni1 O9 96.92(18) 7_556 . ? O8 Ni1 O9 74.12(18) . . ? N3 Ni1 O9 89.3(2) 7_556 . ? O1 Ni1 O9 153.38(18) . . ? O3 Ni1 O9 96.4(2) 7_556 . ? O8 Ni2 O6 167.9(2) . . ? O8 Ni2 O2 109.8(2) . . ? O6 Ni2 O2 79.0(2) . . ? O8 Ni2 N1 87.9(2) . . ? O6 Ni2 N1 99.0(2) . . ? O2 Ni2 N1 98.9(2) . . ? O8 Ni2 O1 79.40(19) . . ? O6 Ni2 O1 94.18(19) . . ? O2 Ni2 O1 81.71(19) . . ? N1 Ni2 O1 166.7(2) . . ? O8 Ni2 O7 95.7(2) . . ? O6 Ni2 O7 74.6(2) . . ? O2 Ni2 O7 153.28(19) . . ? N1 Ni2 O7 89.6(3) . . ? O1 Ni2 O7 95.8(2) . . ? O6 Ni3 O4 167.46(19) . . ? O6 Ni3 N2 88.1(2) . . ? O4 Ni3 N2 98.5(2) . . ? O6 Ni3 O3 109.7(2) . . ? O4 Ni3 O3 79.8(2) . . ? N2 Ni3 O3 100.2(2) . . ? O6 Ni3 O2 78.3(2) . . ? O4 Ni3 O2 95.3(2) . . ? N2 Ni3 O2 166.3(3) . . ? O3 Ni3 O2 83.01(18) . . ? O6 Ni3 O5 93.5(2) . . ? O4 Ni3 O5 75.5(2) . . ? N2 Ni3 O5 93.6(2) . . ? O3 Ni3 O5 153.2(2) . . ? O2 Ni3 O5 89.03(18) . . ? O2 Ni4 O2 180.00(19) 7_556 . ? O2 Ni4 O1 97.90(19) 7_556 . ? O2 Ni4 O1 82.10(19) . . ? O2 Ni4 O1 82.10(19) 7_556 7_556 ? O2 Ni4 O1 97.90(19) . 7_556 ? O1 Ni4 O1 180.000(1) . 7_556 ? O2 Ni4 O3 82.37(18) 7_556 7_556 ? O2 Ni4 O3 97.63(18) . 7_556 ? O1 Ni4 O3 82.24(19) . 7_556 ? O1 Ni4 O3 97.76(19) 7_556 7_556 ? O2 Ni4 O3 97.63(18) 7_556 . ? O2 Ni4 O3 82.37(18) . . ? O1 Ni4 O3 97.76(19) . . ? O1 Ni4 O3 82.24(19) 7_556 . ? O3 Ni4 O3 180.000(1) 7_556 . ? Ni1 O1 Ni4 98.4(2) . . ? Ni1 O1 Ni2 97.55(19) . . ? Ni4 O1 Ni2 96.5(2) . . ? Ni1 O1 H1 119.8 . . ? Ni4 O1 H1 119.8 . . ? Ni2 O1 H1 119.8 . . ? Ni2 O2 Ni4 98.8(2) . . ? Ni2 O2 Ni3 98.6(2) . . ? Ni4 O2 Ni3 96.39(19) . . ? Ni2 O2 H2 119.4 . . ? Ni4 O2 H2 119.4 . . ? Ni3 O2 H2 119.4 . . ? Ni3 O3 Ni4 97.5(2) . . ? Ni3 O3 Ni1 98.3(2) . 7_556 ? Ni4 O3 Ni1 96.36(19) . 7_556 ? Ni3 O3 H3A 119.9 . . ? Ni4 O3 H3A 119.9 . . ? Ni1 O3 H3A 119.9 7_556 . ? C22 O4 Ni1 124.3(5) . 7_556 ? C22 O4 Ni3 115.2(5) . . ? Ni1 O4 Ni3 102.3(2) 7_556 . ? C23 O5 C27 114.8(6) . . ? C23 O5 Ni3 106.7(4) . . ? C27 O5 Ni3 127.6(5) . . ? C15 O6 Ni3 130.4(5) . . ? C15 O6 Ni2 118.4(5) . . ? Ni3 O6 Ni2 103.7(2) . . ? C11 O7 C10 116.9(7) . . ? C11 O7 Ni2 109.7(5) . . ? C10 O7 Ni2 127.3(6) . . ? C6 O8 Ni2 130.1(5) . . ? C6 O8 Ni1 119.0(4) . . ? Ni2 O8 Ni1 103.0(2) . . ? C2 O9 C1 117.1(6) . . ? C2 O9 Ni1 109.9(4) . . ? C1 O9 Ni1 125.5(4) . . ? C8 N1 C9 115.2(7) . . ? C8 N1 Ni2 125.3(5) . . ? C9 N1 Ni2 119.5(5) . . ? C17 N2 C18 115.1(7) . . ? C17 N2 Ni3 126.0(6) . . ? C18 N2 Ni3 118.8(6) . . ? C20 N3 C19 114.7(7) . . ? C20 N3 Ni1 125.4(6) . 7_556 ? C19 N3 Ni1 119.7(5) . 7_556 ? O12 N4 O10 119.2(10) . . ? O12 N4 O11 119.5(10) . . ? O10 N4 O11 121.3(8) . . ? O9 C1 H1A 109.5 . . ? O9 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O9 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O9 123.9(6) . . ? C3 C2 C6 121.6(7) . . ? O9 C2 C6 114.3(6) . . ? C2 C3 C4 117.6(7) . . ? C2 C3 H3 121.2 . . ? C4 C3 H3 121.2 . . ? C5 C4 C3 123.0(7) . . ? C5 C4 Br1 118.2(6) . . ? C3 C4 Br1 118.7(6) . . ? C4 C5 C7 119.8(7) . . ? C4 C5 H5 120.1 . . ? C7 C5 H5 120.1 . . ? O8 C6 C7 122.3(6) . . ? O8 C6 C2 118.6(6) . . ? C7 C6 C2 119.0(6) . . ? C6 C7 C5 118.9(7) . . ? C6 C7 C8 123.7(7) . . ? C5 C7 C8 117.4(7) . . ? N1 C8 C7 126.7(7) . . ? N1 C8 H8 116.6 . . ? C7 C8 H8 116.6 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O7 C10 H10A 109.5 . . ? O7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 124.0(8) . . ? C12 C11 O7 123.5(9) . . ? C15 C11 O7 112.4(7) . . ? C11 C12 C13 117.4(9) . . ? C11 C12 H12 121.3 . . ? C13 C12 H12 121.3 . . ? C14 C13 C12 123.1(8) . . ? C14 C13 Br2 118.3(7) . . ? C12 C13 Br2 118.5(8) . . ? C13 C14 C16 119.2(8) . . ? C13 C14 H14 120.4 . . ? C16 C14 H14 120.4 . . ? O6 C15 C11 121.2(7) . . ? O6 C15 C16 120.6(8) . . ? C11 C15 C16 118.2(8) . . ? C14 C16 C15 118.1(8) . . ? C14 C16 C17 118.1(7) . . ? C15 C16 C17 123.7(7) . . ? N2 C17 C16 126.4(7) . . ? N2 C17 H17 116.8 . . ? C16 C17 H17 116.8 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C21 124.3(8) . . ? N3 C20 H20 117.9 . . ? C21 C20 H20 117.9 . . ? C26 C21 C22 119.0(7) . . ? C26 C21 C20 118.8(8) . . ? C22 C21 C20 122.2(7) . . ? O4 C22 C21 123.7(7) . . ? O4 C22 C23 118.4(8) . . ? C21 C22 C23 117.9(7) . . ? C24 C23 O5 123.2(7) . . ? C24 C23 C22 122.1(8) . . ? O5 C23 C22 114.7(6) . . ? C23 C24 C25 117.5(8) . . ? C23 C24 H24 121.2 . . ? C25 C24 H24 121.2 . . ? C26 C25 C24 122.9(7) . . ? C26 C25 Br3 120.3(7) . . ? C24 C25 Br3 116.8(6) . . ? C25 C26 C21 120.5(8) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? O5 C27 H27A 109.5 . . ? O5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N5 C29 C30 177.4(15) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.892 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.142