# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sm216b-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Mn4]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H44 Mn4 N3 O16' _chemical_formula_weight 982.49 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' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.6508(4) _cell_length_b 16.9627(6) _cell_length_c 20.6910(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4089.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2012 _exptl_absorpt_coefficient_mu 1.280 _cell_measurement_theta_max 29.1182 _cell_measurement_theta_min 2.8882 _cell_measurement_reflns_used 3906 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _exptl_absorpt_correction_T_min 0.90375 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) 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 12960 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.8882 _diffrn_reflns_theta_max 29.1182 _diffrn_orient_matrix_UB_11 0.0272084000 _diffrn_orient_matrix_UB_12 -0.0363997000 _diffrn_orient_matrix_UB_13 0.0070036000 _diffrn_orient_matrix_UB_21 -0.0374407000 _diffrn_orient_matrix_UB_22 -0.0055075000 _diffrn_orient_matrix_UB_23 0.0266722000 _diffrn_orient_matrix_UB_31 -0.0395916000 _diffrn_orient_matrix_UB_32 -0.0198016000 _diffrn_orient_matrix_UB_33 -0.0203576000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 35.00 93.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 18.6403 179.0000 -90.0000 58 #__ type_ start__ end____ width___ exp.time_ 2 omega -13.00 31.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 18.6403 84.0000 51.0000 44 #__ type_ start__ end____ width___ exp.time_ 3 omega 38.00 86.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 18.6403 179.0000 30.0000 48 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 6272 _reflns_number_gt 4611 _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^)+(0.0470P)^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 -0.04(3) _chemical_absolute_configuration ; absolute configuration established by anomalous dispersion effects in diffraction measurements on the crystal. ; _refine_ls_number_reflns 6272 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Mn1 Mn 0.84379(9) 0.34287(7) 0.20363(5) 0.0183(3) Uani 1 1 d . . . Mn2 Mn 0.95061(10) 0.48443(7) 0.16843(5) 0.0179(3) Uani 1 1 d . . . Mn3 Mn 0.74896(10) 0.40807(7) 0.09180(5) 0.0179(3) Uani 1 1 d . . . Mn4 Mn 0.70503(10) 0.47266(7) 0.23478(5) 0.0216(3) Uani 1 1 d . . . O1 O 1.0195(4) 0.5202(3) 0.0920(2) 0.0224(12) Uani 1 1 d . . . O2 O 1.0595(5) 0.5462(3) -0.0313(2) 0.0321(15) Uani 1 1 d . . . O3 O 0.7261(5) 0.5614(3) 0.2884(2) 0.0359(15) Uani 1 1 d . . . O4 O 0.8111(6) 0.6740(3) 0.3590(3) 0.0407(16) Uani 1 1 d . . . O5 O 0.6000(4) 0.4265(3) 0.0633(2) 0.0287(14) Uani 1 1 d . . . O6 O 0.3882(5) 0.4691(5) 0.0665(3) 0.056(2) Uani 1 1 d . . . O7 O 0.6663(4) 0.3890(3) 0.3151(2) 0.0313(14) Uani 1 1 d . . . O8 O 0.7808(4) 0.2921(3) 0.2801(2) 0.0294(14) Uani 1 1 d . . . O9 O 1.0978(4) 0.4164(3) 0.2091(2) 0.0260(13) Uani 1 1 d . . . O10 O 0.9955(4) 0.3083(3) 0.2333(2) 0.0211(12) Uani 1 1 d . . . O11 O 0.8242(4) 0.2394(3) 0.1605(2) 0.0258(13) Uani 1 1 d . . . O12 O 0.7461(5) 0.2826(3) 0.0682(2) 0.0270(13) Uani 1 1 d . . . O13 O 0.7731(4) 0.5224(3) 0.1421(2) 0.0268(13) Uani 1 1 d . . . O14 O 0.8649(4) 0.4416(3) 0.2417(2) 0.0198(12) Uani 1 1 d . . . O15 O 0.7006(4) 0.3816(3) 0.1797(2) 0.0186(11) Uani 1 1 d . . . O16 O 0.8980(4) 0.3889(3) 0.1282(2) 0.0160(12) Uani 1 1 d . . . N1 N 1.0050(5) 0.5810(4) 0.2150(3) 0.0244(15) Uani 1 1 d . . . N2 N 0.5341(6) 0.4919(4) 0.2338(3) 0.0317(17) Uani 1 1 d . . . N3 N 0.8103(5) 0.4282(4) 0.0020(3) 0.0211(15) Uani 1 1 d . . . C1 C 1.0138(8) 0.5783(5) 0.2856(3) 0.033(2) Uani 1 1 d . . . H1A H 1.0414 0.6292 0.3017 0.050 Uiso 1 1 calc R . . H1B H 1.0679 0.5367 0.2982 0.050 Uiso 1 1 calc R . . H1C H 0.9382 0.5670 0.3041 0.050 Uiso 1 1 calc R . . C2 C 1.0353(7) 0.6445(5) 0.1863(3) 0.0251(19) Uani 1 1 d . . . H2 H 1.0574 0.6874 0.2130 0.030 Uiso 1 1 calc R . . C3 C 1.0393(7) 0.6574(5) 0.1177(3) 0.0241(18) Uani 1 1 d . . . C4 C 1.0558(8) 0.7351(5) 0.0948(4) 0.041(2) Uani 1 1 d . . . H4 H 1.0579 0.7778 0.1246 0.049 Uiso 1 1 calc R . . C5 C 1.0687(9) 0.7493(5) 0.0312(4) 0.049(3) Uani 1 1 d . . . H5 H 1.0768 0.8019 0.0162 0.059 Uiso 1 1 calc R . . C6 C 1.0703(8) 0.6871(5) -0.0130(4) 0.036(2) Uani 1 1 d . . . H6 H 1.0819 0.6976 -0.0576 0.043 Uiso 1 1 calc R . . C7 C 1.0550(7) 0.6101(5) 0.0077(3) 0.027(2) Uani 1 1 d . . . C8 C 1.0360(6) 0.5944(5) 0.0741(3) 0.0200(17) Uani 1 1 d . . . C9 C 1.0796(8) 0.5577(5) -0.0996(3) 0.038(2) Uani 1 1 d . . . H9A H 1.0161 0.5880 -0.1182 0.058 Uiso 1 1 calc R . . H9B H 1.0848 0.5063 -0.1211 0.058 Uiso 1 1 calc R . . H9C H 1.1516 0.5866 -0.1057 0.058 Uiso 1 1 calc R . . C10 C 0.4614(7) 0.4292(5) 0.2074(4) 0.041(2) Uani 1 1 d . . . H10A H 0.3805 0.4440 0.2121 0.061 Uiso 1 1 calc R . . H10B H 0.4759 0.3801 0.2309 0.061 Uiso 1 1 calc R . . H10C H 0.4792 0.4217 0.1616 0.061 Uiso 1 1 calc R . . C11 C 0.4844(8) 0.5523(5) 0.2569(4) 0.036(2) Uani 1 1 d . . . H11 H 0.4037 0.5552 0.2508 0.043 Uiso 1 1 calc R . . C12 C 0.5361(8) 0.6165(5) 0.2910(4) 0.036(2) Uani 1 1 d . . . C13 C 0.4649(9) 0.6791(6) 0.3122(5) 0.055(3) Uani 1 1 d . . . H13 H 0.3857 0.6801 0.3013 0.065 Uiso 1 1 calc R . . C14 C 0.5119(12) 0.7382(6) 0.3485(6) 0.070(4) Uani 1 1 d . . . H14 H 0.4639 0.7799 0.3630 0.083 Uiso 1 1 calc R . . C15 C 0.6279(10) 0.7393(6) 0.3652(5) 0.051(3) Uani 1 1 d . . . H15 H 0.6583 0.7810 0.3906 0.061 Uiso 1 1 calc R . . C16 C 0.6974(9) 0.6791(5) 0.3443(4) 0.033(2) Uani 1 1 d . . . C17 C 0.6539(8) 0.6161(5) 0.3065(4) 0.033(2) Uani 1 1 d . . . C18 C 0.8593(9) 0.7298(5) 0.4039(4) 0.055(3) Uani 1 1 d . . . H18A H 0.8564 0.7828 0.3850 0.083 Uiso 1 1 calc R . . H18B H 0.9393 0.7157 0.4129 0.083 Uiso 1 1 calc R . . H18C H 0.8151 0.7290 0.4441 0.083 Uiso 1 1 calc R . . C19 C 0.9229(6) 0.3952(5) -0.0132(3) 0.028(2) Uani 1 1 d . . . H19A H 0.9401 0.4040 -0.0590 0.042 Uiso 1 1 calc R . . H19B H 0.9226 0.3384 -0.0043 0.042 Uiso 1 1 calc R . . H19C H 0.9814 0.4209 0.0135 0.042 Uiso 1 1 calc R . . C20 C 0.7528(7) 0.4650(4) -0.0414(3) 0.0253(18) Uani 1 1 d . . . H20 H 0.7913 0.4747 -0.0811 0.030 Uiso 1 1 calc R . . C21 C 0.6358(7) 0.4935(5) -0.0368(4) 0.0271(19) Uani 1 1 d . . . C22 C 0.5921(8) 0.5385(4) -0.0874(4) 0.033(2) Uani 1 1 d . . . H22 H 0.6400 0.5529 -0.1227 0.039 Uiso 1 1 calc R . . C23 C 0.4794(9) 0.5621(5) -0.0860(4) 0.046(3) Uani 1 1 d . . . H23 H 0.4492 0.5932 -0.1202 0.055 Uiso 1 1 calc R . . C24 C 0.4087(8) 0.5405(5) -0.0341(4) 0.043(3) Uani 1 1 d . . . H24 H 0.3312 0.5579 -0.0335 0.052 Uiso 1 1 calc R . . C25 C 0.4478(7) 0.4959(5) 0.0148(4) 0.036(2) Uani 1 1 d . . . C26 C 0.5661(7) 0.4712(5) 0.0146(3) 0.0258(19) Uani 1 1 d . . . C27 C 0.2724(7) 0.4943(7) 0.0733(4) 0.063(3) Uani 1 1 d . . . H27A H 0.2704 0.5516 0.0798 0.095 Uiso 1 1 calc R . . H27B H 0.2376 0.4680 0.1107 0.095 Uiso 1 1 calc R . . H27C H 0.2293 0.4808 0.0342 0.095 Uiso 1 1 calc R . . C28 C 0.7055(7) 0.3202(5) 0.3170(4) 0.031(2) Uani 1 1 d . . . C29 C 0.6539(9) 0.2647(6) 0.3656(5) 0.063(3) Uani 1 1 d . . . H29A H 0.6535 0.2897 0.4083 0.095 Uiso 1 1 calc R . . H29B H 0.6994 0.2162 0.3673 0.095 Uiso 1 1 calc R . . H29C H 0.5750 0.2520 0.3528 0.095 Uiso 1 1 calc R . . C30 C 1.0867(7) 0.3511(5) 0.2342(4) 0.0245(18) Uani 1 1 d . . . C31 C 1.1862(6) 0.3135(5) 0.2681(4) 0.034(2) Uani 1 1 d . . . H31A H 1.2487 0.3049 0.2373 0.051 Uiso 1 1 calc R . . H31B H 1.1621 0.2629 0.2864 0.051 Uiso 1 1 calc R . . H31C H 1.2127 0.3483 0.3029 0.051 Uiso 1 1 calc R . . C32 C 0.7834(7) 0.2304(5) 0.1030(4) 0.028(2) Uani 1 1 d . . . C33 C 0.7848(9) 0.1472(4) 0.0782(4) 0.049(3) Uani 1 1 d . . . H33A H 0.7059 0.1288 0.0720 0.074 Uiso 1 1 calc R . . H33B H 0.8238 0.1132 0.1095 0.074 Uiso 1 1 calc R . . H33C H 0.8258 0.1455 0.0368 0.074 Uiso 1 1 calc R . . C34 C 0.7506(8) 0.5952(5) 0.1135(4) 0.039(2) Uani 1 1 d . . . H34A H 0.7618 0.5895 0.0663 0.047 Uiso 1 1 calc R . . H34B H 0.8090 0.6331 0.1291 0.047 Uiso 1 1 calc R . . C35 C 0.6407(9) 0.6291(6) 0.1239(5) 0.068(3) Uani 1 1 d . . . H35A H 0.5812 0.5895 0.1158 0.102 Uiso 1 1 calc R . . H35B H 0.6300 0.6738 0.0944 0.102 Uiso 1 1 calc R . . H35C H 0.6350 0.6476 0.1686 0.102 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 Mn1 0.0169(6) 0.0172(6) 0.0209(5) 0.0024(5) 0.0012(5) 0.0002(6) Mn2 0.0207(6) 0.0161(6) 0.0168(5) -0.0008(5) 0.0013(5) -0.0017(6) Mn3 0.0155(6) 0.0199(6) 0.0182(5) 0.0011(5) -0.0002(5) -0.0008(6) Mn4 0.0212(6) 0.0212(7) 0.0223(5) 0.0025(6) 0.0029(5) 0.0055(6) O1 0.032(3) 0.020(3) 0.016(2) 0.000(2) 0.007(2) -0.001(3) O2 0.051(4) 0.030(3) 0.015(3) 0.000(2) 0.000(3) -0.007(3) O3 0.037(4) 0.036(3) 0.035(3) -0.008(3) -0.002(3) 0.015(3) O4 0.055(4) 0.028(3) 0.040(3) -0.012(3) 0.015(3) 0.003(4) O5 0.013(3) 0.048(4) 0.025(3) 0.010(3) 0.002(2) 0.000(3) O6 0.025(3) 0.101(6) 0.043(4) 0.010(4) -0.002(3) 0.028(4) O7 0.026(3) 0.041(4) 0.027(3) 0.012(3) 0.014(3) 0.012(3) O8 0.026(3) 0.029(3) 0.033(3) 0.015(3) 0.002(3) 0.009(3) O9 0.022(3) 0.028(3) 0.028(3) 0.000(3) -0.001(3) -0.003(3) O10 0.016(3) 0.020(3) 0.027(3) 0.007(2) 0.001(3) 0.005(3) O11 0.028(3) 0.019(3) 0.031(3) 0.002(2) -0.007(3) 0.000(3) O12 0.031(3) 0.021(3) 0.029(3) -0.004(3) -0.006(3) -0.001(3) O13 0.024(3) 0.018(3) 0.039(3) 0.004(3) -0.005(2) -0.002(3) O14 0.017(3) 0.028(3) 0.015(2) 0.001(2) 0.002(2) 0.001(3) O15 0.018(3) 0.020(3) 0.018(2) 0.005(2) -0.001(2) 0.000(3) O16 0.015(3) 0.016(3) 0.017(2) -0.002(2) 0.002(2) -0.009(3) N1 0.030(4) 0.025(4) 0.018(3) -0.002(3) 0.006(3) -0.006(4) N2 0.034(4) 0.031(4) 0.030(3) 0.015(3) 0.006(3) 0.012(4) N3 0.018(3) 0.025(4) 0.020(3) -0.002(3) -0.001(3) -0.012(3) C1 0.050(5) 0.036(5) 0.014(4) -0.005(4) -0.003(4) -0.019(5) C2 0.033(5) 0.020(4) 0.023(4) -0.009(4) 0.007(4) -0.001(4) C3 0.027(4) 0.019(4) 0.027(4) -0.001(4) 0.000(4) -0.004(5) C4 0.067(7) 0.022(5) 0.033(5) 0.003(4) -0.002(5) -0.015(6) C5 0.080(8) 0.026(5) 0.042(5) 0.007(5) 0.002(6) -0.011(6) C6 0.057(6) 0.026(5) 0.025(4) 0.009(4) -0.001(5) -0.007(5) C7 0.028(5) 0.030(5) 0.024(4) 0.003(4) -0.007(4) -0.006(5) C8 0.014(4) 0.021(4) 0.026(4) 0.002(4) -0.002(3) 0.006(4) C9 0.060(6) 0.039(5) 0.017(4) 0.010(4) -0.003(4) 0.015(5) C10 0.030(5) 0.052(6) 0.040(5) 0.017(5) 0.010(5) 0.007(5) C11 0.032(5) 0.039(6) 0.038(5) 0.018(5) 0.012(4) 0.025(5) C12 0.045(6) 0.026(5) 0.037(5) 0.020(4) 0.016(5) 0.013(5) C13 0.048(6) 0.046(6) 0.069(7) 0.019(6) 0.032(6) 0.021(6) C14 0.088(10) 0.033(6) 0.088(9) 0.014(6) 0.048(8) 0.022(7) C15 0.071(8) 0.026(5) 0.055(6) 0.006(5) 0.029(6) 0.003(6) C16 0.047(6) 0.025(5) 0.027(4) 0.008(4) 0.025(5) 0.013(5) C17 0.049(6) 0.026(5) 0.024(4) 0.005(4) 0.007(4) 0.016(5) C18 0.092(9) 0.033(5) 0.040(5) -0.015(5) 0.010(6) -0.011(7) C19 0.030(5) 0.039(5) 0.016(4) -0.007(4) 0.001(4) -0.006(5) C20 0.035(4) 0.022(4) 0.019(4) -0.002(4) 0.006(4) -0.008(5) C21 0.032(5) 0.020(4) 0.029(4) 0.000(4) -0.003(4) -0.002(4) C22 0.056(6) 0.019(4) 0.023(4) 0.004(4) -0.017(4) -0.001(5) C23 0.071(7) 0.033(5) 0.035(5) 0.000(4) -0.028(5) 0.012(6) C24 0.043(6) 0.046(6) 0.042(5) -0.009(5) -0.014(5) 0.021(6) C25 0.034(5) 0.046(6) 0.029(4) -0.003(4) -0.017(4) 0.018(5) C26 0.027(4) 0.026(5) 0.024(4) 0.000(4) -0.016(4) 0.003(5) C27 0.026(5) 0.116(10) 0.047(5) -0.005(6) -0.004(4) 0.025(7) C28 0.024(4) 0.036(5) 0.034(5) 0.016(4) 0.004(4) 0.011(5) C29 0.055(7) 0.060(7) 0.074(7) 0.036(6) 0.039(6) 0.016(7) C30 0.029(5) 0.026(5) 0.019(4) -0.001(4) 0.005(4) 0.009(4) C31 0.024(4) 0.046(5) 0.031(4) 0.007(4) 0.000(4) 0.018(5) C32 0.019(4) 0.024(5) 0.040(5) -0.011(4) 0.003(4) 0.005(4) C33 0.076(8) 0.017(4) 0.055(6) -0.010(4) -0.015(6) 0.011(6) C34 0.035(5) 0.031(5) 0.050(5) -0.004(5) -0.020(5) 0.009(5) C35 0.079(9) 0.049(7) 0.075(8) 0.015(6) 0.012(7) 0.019(7) _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 Mn1 O16 1.855(4) . ? Mn1 O15 1.859(5) . ? Mn1 O14 1.867(5) . ? Mn1 O8 1.946(5) . ? Mn1 O10 1.960(5) . ? Mn1 O11 1.981(5) . ? Mn1 Mn3 2.7926(15) . ? Mn1 Mn2 2.8010(16) . ? Mn1 Mn4 2.8065(16) . ? Mn2 O1 1.875(4) . ? Mn2 O16 1.922(5) . ? Mn2 O14 1.956(5) . ? Mn2 N1 2.003(6) . ? Mn2 O9 2.232(5) . ? Mn2 O13 2.234(5) . ? Mn2 Mn3 3.1164(16) . ? Mn2 Mn4 3.1798(16) . ? Mn3 O5 1.859(5) . ? Mn3 O16 1.921(5) . ? Mn3 O15 1.957(5) . ? Mn3 N3 2.020(6) . ? Mn3 O12 2.183(5) . ? Mn3 O13 2.219(5) . ? Mn3 Mn4 3.1962(15) . ? Mn4 O3 1.886(5) . ? Mn4 O15 1.921(5) . ? Mn4 O14 1.941(5) . ? Mn4 N2 2.018(7) . ? Mn4 O7 2.232(5) . ? Mn4 O13 2.240(5) . ? O1 C8 1.325(9) . ? O2 C7 1.353(9) . ? O2 C9 1.444(8) . ? O3 C17 1.307(9) . ? O4 C16 1.361(11) . ? O4 C18 1.441(10) . ? O5 C26 1.322(8) . ? O6 C25 1.354(10) . ? O6 C27 1.423(9) . ? O7 C28 1.253(9) . ? O8 C28 1.257(9) . ? O9 C30 1.231(9) . ? O10 C30 1.287(9) . ? O11 C32 1.291(9) . ? O12 C32 1.223(9) . ? O13 C34 1.394(9) . ? N1 C2 1.279(9) . ? N1 C1 1.466(8) . ? N2 C11 1.270(9) . ? N2 C10 1.465(10) . ? N3 C20 1.282(9) . ? N3 C19 1.460(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.436(10) . ? C2 H2 0.9500 . ? C3 C8 1.399(10) . ? C3 C4 1.414(11) . ? C4 C5 1.347(11) . ? C4 H4 0.9500 . ? C5 C6 1.396(11) . ? C5 H5 0.9500 . ? C6 C7 1.385(10) . ? C6 H6 0.9500 . ? C7 C8 1.418(9) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.431(12) . ? C11 H11 0.9500 . ? C12 C17 1.409(12) . ? C12 C13 1.418(12) . ? C13 C14 1.368(15) . ? C13 H13 0.9500 . ? C14 C15 1.394(15) . ? C14 H14 0.9500 . ? C15 C16 1.374(12) . ? C15 H15 0.9500 . ? C16 C17 1.418(12) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.449(11) . ? C20 H20 0.9500 . ? C21 C26 1.391(10) . ? C21 C22 1.393(10) . ? C22 C23 1.373(12) . ? C22 H22 0.9500 . ? C23 C24 1.403(13) . ? C23 H23 0.9500 . ? C24 C25 1.342(11) . ? C24 H24 0.9500 . ? C25 C26 1.441(10) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.502(11) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.497(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.501(10) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.421(12) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 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 O16 Mn1 O15 86.2(2) . . ? O16 Mn1 O14 86.2(2) . . ? O15 Mn1 O14 85.1(2) . . ? O16 Mn1 O8 177.1(2) . . ? O15 Mn1 O8 92.0(2) . . ? O14 Mn1 O8 95.9(2) . . ? O16 Mn1 O10 94.7(2) . . ? O15 Mn1 O10 175.9(2) . . ? O14 Mn1 O10 91.0(2) . . ? O8 Mn1 O10 87.3(2) . . ? O16 Mn1 O11 91.9(2) . . ? O15 Mn1 O11 95.1(2) . . ? O14 Mn1 O11 178.0(2) . . ? O8 Mn1 O11 86.0(2) . . ? O10 Mn1 O11 88.8(2) . . ? O16 Mn1 Mn3 43.23(15) . . ? O15 Mn1 Mn3 44.35(14) . . ? O14 Mn1 Mn3 92.68(15) . . ? O8 Mn1 Mn3 134.46(16) . . ? O10 Mn1 Mn3 137.25(15) . . ? O11 Mn1 Mn3 86.12(15) . . ? O16 Mn1 Mn2 43.07(14) . . ? O15 Mn1 Mn2 91.54(15) . . ? O14 Mn1 Mn2 44.13(14) . . ? O8 Mn1 Mn2 139.34(17) . . ? O10 Mn1 Mn2 86.40(15) . . ? O11 Mn1 Mn2 133.89(15) . . ? Mn3 Mn1 Mn2 67.71(4) . . ? O16 Mn1 Mn4 93.41(15) . . ? O15 Mn1 Mn4 42.90(15) . . ? O14 Mn1 Mn4 43.56(15) . . ? O8 Mn1 Mn4 86.75(16) . . ? O10 Mn1 Mn4 133.01(16) . . ? O11 Mn1 Mn4 137.03(16) . . ? Mn3 Mn1 Mn4 69.62(4) . . ? Mn2 Mn1 Mn4 69.09(4) . . ? O1 Mn2 O16 92.5(2) . . ? O1 Mn2 O14 173.3(2) . . ? O16 Mn2 O14 81.92(19) . . ? O1 Mn2 N1 90.3(2) . . ? O16 Mn2 N1 176.9(2) . . ? O14 Mn2 N1 95.3(2) . . ? O1 Mn2 O9 99.0(2) . . ? O16 Mn2 O9 88.4(2) . . ? O14 Mn2 O9 84.71(19) . . ? N1 Mn2 O9 89.9(2) . . ? O1 Mn2 O13 95.6(2) . . ? O16 Mn2 O13 80.94(19) . . ? O14 Mn2 O13 79.82(19) . . ? N1 Mn2 O13 100.0(2) . . ? O9 Mn2 O13 162.28(19) . . ? O1 Mn2 Mn1 133.40(16) . . ? O16 Mn2 Mn1 41.23(13) . . ? O14 Mn2 Mn1 41.66(14) . . ? N1 Mn2 Mn1 135.79(17) . . ? O9 Mn2 Mn1 78.48(14) . . ? O13 Mn2 Mn1 84.21(13) . . ? O1 Mn2 Mn3 91.61(15) . . ? O16 Mn2 Mn3 35.82(15) . . ? O14 Mn2 Mn3 81.67(14) . . ? N1 Mn2 Mn3 145.37(19) . . ? O9 Mn2 Mn3 123.82(14) . . ? O13 Mn2 Mn3 45.38(13) . . ? Mn1 Mn2 Mn3 56.01(4) . . ? O1 Mn2 Mn4 140.35(16) . . ? O16 Mn2 Mn4 81.21(14) . . ? O14 Mn2 Mn4 35.16(14) . . ? N1 Mn2 Mn4 97.37(18) . . ? O9 Mn2 Mn4 119.74(13) . . ? O13 Mn2 Mn4 44.78(13) . . ? Mn1 Mn2 Mn4 55.54(4) . . ? Mn3 Mn2 Mn4 61.00(4) . . ? O5 Mn3 O16 175.4(2) . . ? O5 Mn3 O15 93.7(2) . . ? O16 Mn3 O15 81.74(19) . . ? O5 Mn3 N3 90.6(2) . . ? O16 Mn3 N3 94.0(2) . . ? O15 Mn3 N3 174.8(2) . . ? O5 Mn3 O12 94.5(2) . . ? O16 Mn3 O12 86.3(2) . . ? O15 Mn3 O12 88.9(2) . . ? N3 Mn3 O12 87.9(2) . . ? O5 Mn3 O13 96.9(2) . . ? O16 Mn3 O13 81.36(19) . . ? O15 Mn3 O13 78.52(19) . . ? N3 Mn3 O13 103.8(2) . . ? O12 Mn3 O13 163.47(19) . . ? O5 Mn3 Mn1 134.32(16) . . ? O16 Mn3 Mn1 41.41(13) . . ? O15 Mn3 Mn1 41.62(15) . . ? N3 Mn3 Mn1 133.58(19) . . ? O12 Mn3 Mn1 78.79(14) . . ? O13 Mn3 Mn1 84.68(13) . . ? O5 Mn3 Mn2 142.67(19) . . ? O16 Mn3 Mn2 35.84(14) . . ? O15 Mn3 Mn2 80.76(15) . . ? N3 Mn3 Mn2 97.54(17) . . ? O12 Mn3 Mn2 122.03(16) . . ? O13 Mn3 Mn2 45.78(13) . . ? Mn1 Mn3 Mn2 56.27(4) . . ? O5 Mn3 Mn4 94.96(16) . . ? O16 Mn3 Mn4 80.78(13) . . ? O15 Mn3 Mn4 34.12(15) . . ? N3 Mn3 Mn4 148.24(18) . . ? O12 Mn3 Mn4 122.62(14) . . ? O13 Mn3 Mn4 44.47(13) . . ? Mn1 Mn3 Mn4 55.40(4) . . ? Mn2 Mn3 Mn4 60.48(3) . . ? O3 Mn4 O15 174.1(2) . . ? O3 Mn4 O14 92.8(2) . . ? O15 Mn4 O14 81.4(2) . . ? O3 Mn4 N2 90.3(3) . . ? O15 Mn4 N2 95.6(3) . . ? O14 Mn4 N2 172.5(2) . . ? O3 Mn4 O7 95.5(2) . . ? O15 Mn4 O7 85.7(2) . . ? O14 Mn4 O7 88.1(2) . . ? N2 Mn4 O7 84.9(2) . . ? O3 Mn4 O13 99.1(2) . . ? O15 Mn4 O13 78.74(19) . . ? O14 Mn4 O13 79.98(19) . . ? N2 Mn4 O13 106.3(2) . . ? O7 Mn4 O13 161.54(19) . . ? O3 Mn4 Mn1 133.34(17) . . ? O15 Mn4 Mn1 41.23(15) . . ? O14 Mn4 Mn1 41.51(14) . . ? N2 Mn4 Mn1 133.9(2) . . ? O7 Mn4 Mn1 77.78(14) . . ? O13 Mn4 Mn1 83.97(13) . . ? O3 Mn4 Mn2 95.00(18) . . ? O15 Mn4 Mn2 79.54(15) . . ? O14 Mn4 Mn2 35.47(13) . . ? N2 Mn4 Mn2 150.87(17) . . ? O7 Mn4 Mn2 122.91(14) . . ? O13 Mn4 Mn2 44.63(13) . . ? Mn1 Mn4 Mn2 55.37(4) . . ? O3 Mn4 Mn3 142.90(18) . . ? O15 Mn4 Mn3 34.86(14) . . ? O14 Mn4 Mn3 79.73(14) . . ? N2 Mn4 Mn3 101.80(19) . . ? O7 Mn4 Mn3 120.23(15) . . ? O13 Mn4 Mn3 43.94(13) . . ? Mn1 Mn4 Mn3 54.99(4) . . ? Mn2 Mn4 Mn3 58.52(3) . . ? C8 O1 Mn2 127.2(4) . . ? C7 O2 C9 118.8(6) . . ? C17 O3 Mn4 130.6(5) . . ? C16 O4 C18 118.8(7) . . ? C26 O5 Mn3 128.1(5) . . ? C25 O6 C27 117.6(8) . . ? C28 O7 Mn4 122.8(5) . . ? C28 O8 Mn1 126.1(5) . . ? C30 O9 Mn2 122.9(5) . . ? C30 O10 Mn1 125.5(5) . . ? C32 O11 Mn1 124.3(5) . . ? C32 O12 Mn3 124.7(5) . . ? C34 O13 Mn3 123.5(5) . . ? C34 O13 Mn2 122.2(5) . . ? Mn3 O13 Mn2 88.84(19) . . ? C34 O13 Mn4 129.1(5) . . ? Mn3 O13 Mn4 91.59(19) . . ? Mn2 O13 Mn4 90.60(18) . . ? Mn1 O14 Mn4 94.9(2) . . ? Mn1 O14 Mn2 94.2(2) . . ? Mn4 O14 Mn2 109.4(2) . . ? Mn1 O15 Mn4 95.9(2) . . ? Mn1 O15 Mn3 94.0(2) . . ? Mn4 O15 Mn3 111.0(2) . . ? Mn1 O16 Mn3 95.4(2) . . ? Mn1 O16 Mn2 95.7(2) . . ? Mn3 O16 Mn2 108.3(2) . . ? C2 N1 C1 118.0(7) . . ? C2 N1 Mn2 123.6(5) . . ? C1 N1 Mn2 118.4(5) . . ? C11 N2 C10 117.5(7) . . ? C11 N2 Mn4 125.2(6) . . ? C10 N2 Mn4 117.2(5) . . ? C20 N3 C19 120.3(6) . . ? C20 N3 Mn3 122.8(5) . . ? C19 N3 Mn3 116.8(5) . . ? 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 126.5(7) . . ? N1 C2 H2 116.7 . . ? C3 C2 H2 116.7 . . ? C8 C3 C4 120.0(7) . . ? C8 C3 C2 121.3(7) . . ? C4 C3 C2 118.5(7) . . ? C5 C4 C3 120.6(8) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.5(8) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 120.5(7) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? O2 C7 C6 124.5(7) . . ? O2 C7 C8 115.7(7) . . ? C6 C7 C8 119.8(8) . . ? O1 C8 C3 123.4(6) . . ? O1 C8 C7 118.1(7) . . ? C3 C8 C7 118.5(7) . . ? O2 C9 H9A 109.5 . . ? O2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 127.4(8) . . ? N2 C11 H11 116.3 . . ? C12 C11 H11 116.3 . . ? C17 C12 C13 120.2(9) . . ? C17 C12 C11 121.2(8) . . ? C13 C12 C11 118.5(9) . . ? C14 C13 C12 119.0(10) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 122.2(11) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C16 C15 C14 118.9(11) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? O4 C16 C15 123.4(9) . . ? O4 C16 C17 115.1(8) . . ? C15 C16 C17 121.5(10) . . ? O3 C17 C12 124.4(8) . . ? O3 C17 C16 117.5(8) . . ? C12 C17 C16 118.0(9) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 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 127.4(7) . . ? N3 C20 H20 116.3 . . ? C21 C20 H20 116.3 . . ? C26 C21 C22 120.6(8) . . ? C26 C21 C20 120.7(7) . . ? C22 C21 C20 118.5(8) . . ? C23 C22 C21 119.6(9) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 120.1(9) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 121.7(9) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C24 C25 O6 127.6(9) . . ? C24 C25 C26 119.1(9) . . ? O6 C25 C26 113.3(7) . . ? O5 C26 C21 124.3(7) . . ? O5 C26 C25 116.8(7) . . ? C21 C26 C25 118.9(7) . . ? O6 C27 H27A 109.5 . . ? O6 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O6 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O7 C28 O8 126.0(7) . . ? O7 C28 C29 117.3(7) . . ? O8 C28 C29 116.6(8) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O9 C30 O10 126.1(7) . . ? O9 C30 C31 119.9(8) . . ? O10 C30 C31 114.0(7) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O12 C32 O11 126.0(7) . . ? O12 C32 C33 118.9(7) . . ? O11 C32 C33 115.1(8) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O13 C34 C35 117.7(8) . . ? O13 C34 H34A 107.9 . . ? C35 C34 H34A 107.9 . . ? O13 C34 H34B 107.9 . . ? C35 C34 H34B 107.9 . . ? H34A C34 H34B 107.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.592 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.142 _database_code_depnum_ccdc_archive 'CCDC 936642' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sm83a-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ni4(OMe)4(L2)4(MeOH)4]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H60 N4 Ni4 O16' _chemical_formula_weight 1087.76 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 Tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 22.187(3) _cell_length_b 22.187(3) _cell_length_c 9.5524(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4702.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 1.648 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.9541 _cell_measurement_reflns_used 1770 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _exptl_absorpt_correction_T_min 0.72639 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) 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 5465 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.9541 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 0.0304977000 _diffrn_orient_matrix_UB_12 -0.0077056000 _diffrn_orient_matrix_UB_13 0.0133962000 _diffrn_orient_matrix_UB_21 -0.0095895000 _diffrn_orient_matrix_UB_22 -0.0252407000 _diffrn_orient_matrix_UB_23 0.0397709000 _diffrn_orient_matrix_UB_31 0.0004264000 _diffrn_orient_matrix_UB_32 -0.0180622000 _diffrn_orient_matrix_UB_33 -0.0612195000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 63.00 89.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 179.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 2 omega -50.00 37.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 0.0000 60.0000 87 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 2060 _reflns_number_gt 1134 _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^)+(0.0096P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2060 _refine_ls_number_parameters 152 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 0.811 _refine_ls_restrained_S_all 0.811 _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 0.56644(3) 0.22884(3) 0.98698(6) 0.0330(3) Uani 1 1 d . . . N1 N 0.57274(19) 0.23319(16) 1.1961(3) 0.0268(10) Uani 1 1 d . . . H1N H 0.5635 0.2678 1.2354 0.032 Uiso 1 1 calc R . . O1 O 0.64606(18) 0.27886(19) 0.9728(4) 0.0482(11) Uani 1 1 d D . . O2 O 0.55680(16) 0.23053(16) 0.7752(3) 0.0348(9) Uani 1 1 d . . . O3 O 0.60359(15) 0.14713(16) 0.9886(3) 0.0352(9) Uani 1 1 d . . . O4 O 0.63089(17) 0.03565(17) 0.9397(4) 0.0456(10) Uani 1 1 d . . . C1 C 0.6555(4) -0.0215(3) 0.9106(7) 0.083(2) Uani 1 1 d . . . H1A H 0.6973 -0.0229 0.9434 0.124 Uiso 1 1 calc R . . H1B H 0.6544 -0.0288 0.8095 0.124 Uiso 1 1 calc R . . H1C H 0.6319 -0.0526 0.9588 0.124 Uiso 1 1 calc R . . C2 C 0.6296(2) 0.0524(2) 1.0788(6) 0.0375(14) Uani 1 1 d . . . C3 C 0.6417(3) 0.0145(2) 1.1903(6) 0.0493(16) Uani 1 1 d . . . H3 H 0.6530 -0.0261 1.1735 0.059 Uiso 1 1 calc R . . C4 C 0.6376(3) 0.0357(3) 1.3273(6) 0.0560(18) Uani 1 1 d . . . H4 H 0.6464 0.0097 1.4036 0.067 Uiso 1 1 calc R . . C5 C 0.6210(3) 0.0932(3) 1.3512(6) 0.0537(17) Uani 1 1 d . . . H5 H 0.6175 0.1070 1.4450 0.064 Uiso 1 1 calc R . . C6 C 0.6087(3) 0.1335(3) 1.2393(5) 0.0409(15) Uani 1 1 d . . . C7 C 0.6134(2) 0.1137(2) 1.0975(5) 0.0360(13) Uani 1 1 d . . . C8 C 0.5880(3) 0.1931(3) 1.2730(6) 0.0444(16) Uani 1 1 d . . . H8 H 0.5860 0.2021 1.3701 0.053 Uiso 1 1 calc R . . C9 C 0.7038(3) 0.2647(3) 1.0145(7) 0.082(2) Uani 1 1 d . . . H9A H 0.7023 0.2344 1.0890 0.122 Uiso 1 1 calc R . . H9B H 0.7239 0.3010 1.0494 0.122 Uiso 1 1 calc R . . H9C H 0.7264 0.2485 0.9346 0.122 Uiso 1 1 calc R . . C10 C 0.6078(2) 0.2144(3) 0.6911(5) 0.0503(17) Uani 1 1 d . . . H10A H 0.6028 0.1731 0.6566 0.076 Uiso 1 1 calc R . . H10B H 0.6445 0.2170 0.7476 0.076 Uiso 1 1 calc R . . H10C H 0.6108 0.2421 0.6114 0.076 Uiso 1 1 calc R . . H1 H 0.643(2) 0.311(2) 0.906(5) 0.053(18) Uiso 1 1 d 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 0.0389(5) 0.0314(5) 0.0286(4) -0.0005(3) -0.0049(3) 0.0016(3) N1 0.056(3) 0.013(2) 0.0115(19) -0.0042(17) -0.0067(19) 0.0147(19) O1 0.038(3) 0.046(3) 0.060(2) 0.019(2) -0.016(2) -0.007(2) O2 0.037(2) 0.040(2) 0.0278(19) -0.0037(17) 0.0011(16) 0.0008(17) O3 0.042(3) 0.034(2) 0.0290(19) 0.0037(17) -0.0011(16) 0.0051(18) O4 0.049(3) 0.034(2) 0.054(2) -0.010(2) 0.004(2) 0.0005(19) C1 0.124(8) 0.036(4) 0.087(5) -0.016(4) 0.020(5) 0.001(4) C2 0.033(3) 0.032(3) 0.048(3) -0.005(3) 0.000(3) -0.002(3) C3 0.055(4) 0.019(3) 0.073(4) 0.010(3) 0.002(3) 0.004(3) C4 0.073(5) 0.055(5) 0.040(4) 0.009(3) -0.007(3) 0.003(4) C5 0.073(5) 0.050(4) 0.037(3) 0.005(3) -0.008(3) 0.008(4) C6 0.054(4) 0.033(4) 0.035(3) 0.002(3) -0.008(3) 0.010(3) C7 0.032(3) 0.039(4) 0.037(3) 0.001(3) -0.004(3) -0.002(3) C8 0.055(4) 0.041(4) 0.037(3) -0.011(3) -0.006(3) 0.003(3) C9 0.038(4) 0.097(7) 0.109(6) 0.029(5) -0.023(4) 0.015(4) C10 0.032(4) 0.071(5) 0.048(4) -0.012(3) 0.007(3) 0.005(3) _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 O3 1.992(3) . ? Ni1 N1 2.005(3) . ? Ni1 O2 2.023(4) 12_657 ? Ni1 O2 2.035(3) . ? Ni1 O2 2.067(3) 11_667 ? Ni1 O1 2.091(4) . ? N1 C8 1.202(6) . ? N1 H1N 0.8800 . ? O1 C9 1.379(6) . ? O1 H1 0.96(5) . ? O2 C10 1.433(5) . ? O2 Ni1 2.023(4) 11_667 ? O2 Ni1 2.067(3) 12_657 ? O3 C7 1.296(5) . ? O4 C2 1.380(6) . ? O4 C1 1.408(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.383(7) . ? C2 C7 1.418(7) . ? C3 C4 1.393(7) . ? C3 H3 0.9500 . ? C4 C5 1.346(8) . ? C4 H4 0.9500 . ? C5 C6 1.421(7) . ? C5 H5 0.9500 . ? C6 C7 1.429(7) . ? C6 C8 1.435(7) . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 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 O3 Ni1 N1 90.41(14) . . ? O3 Ni1 O2 172.80(14) . 12_657 ? N1 Ni1 O2 92.98(14) . 12_657 ? O3 Ni1 O2 93.89(13) . . ? N1 Ni1 O2 175.68(16) . . ? O2 Ni1 O2 82.71(14) 12_657 . ? O3 Ni1 O2 91.93(14) . 11_667 ? N1 Ni1 O2 97.97(15) . 11_667 ? O2 Ni1 O2 81.31(16) 12_657 11_667 ? O2 Ni1 O2 81.62(14) . 11_667 ? O3 Ni1 O1 97.71(16) . . ? N1 Ni1 O1 88.87(16) . . ? O2 Ni1 O1 88.72(15) 12_657 . ? O2 Ni1 O1 90.83(15) . . ? O2 Ni1 O1 168.15(15) 11_667 . ? C8 N1 Ni1 126.3(4) . . ? C8 N1 H1N 116.8 . . ? Ni1 N1 H1N 116.8 . . ? C9 O1 Ni1 130.2(4) . . ? C9 O1 H1 115(3) . . ? Ni1 O1 H1 112(3) . . ? C10 O2 Ni1 120.9(3) . 11_667 ? C10 O2 Ni1 118.0(3) . . ? Ni1 O2 Ni1 97.90(14) 11_667 . ? C10 O2 Ni1 120.1(3) . 12_657 ? Ni1 O2 Ni1 98.32(16) 11_667 12_657 ? Ni1 O2 Ni1 96.49(14) . 12_657 ? C7 O3 Ni1 126.7(3) . . ? C2 O4 C1 116.1(5) . . ? O4 C1 H1A 109.5 . . ? O4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O4 C2 C3 125.1(5) . . ? O4 C2 C7 112.6(5) . . ? C3 C2 C7 122.3(5) . . ? C2 C3 C4 120.4(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.8(6) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.4(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C7 120.3(5) . . ? C5 C6 C8 118.3(5) . . ? C7 C6 C8 121.3(5) . . ? O3 C7 C2 119.4(5) . . ? O3 C7 C6 124.9(5) . . ? C2 C7 C6 115.7(5) . . ? N1 C8 C6 129.4(5) . . ? N1 C8 H8 115.3 . . ? C6 C8 H8 115.3 . . ? O1 C9 H9A 109.5 . . ? O1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 H10A 109.5 . . ? O2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.607 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 936643' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sm138b-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Mn(immp)2(Cl)]n' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 Cl Mn N2 O4' _chemical_formula_weight 418.75 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 14.731(3) _cell_length_b 12.851(3) _cell_length_c 9.6901(19) _cell_angle_alpha 90.00 _cell_angle_beta 106.66(3) _cell_angle_gamma 90.00 _cell_volume 1757.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _exptl_crystal_description Tabloid _exptl_crystal_colour Brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.930 _cell_measurement_theta_max 25.34 _cell_measurement_theta_min 2.8810 _cell_measurement_reflns_used 2493 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _exptl_absorpt_correction_T_min 0.45138 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) 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 4006 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.8810 _diffrn_reflns_theta_max 25.34 _diffrn_orient_matrix_UB_11 0.0432298000 _diffrn_orient_matrix_UB_12 -0.0272360000 _diffrn_orient_matrix_UB_13 0.0276918000 _diffrn_orient_matrix_UB_21 -0.0250902000 _diffrn_orient_matrix_UB_22 -0.0478920000 _diffrn_orient_matrix_UB_23 -0.0112821000 _diffrn_orient_matrix_UB_31 0.0053628000 _diffrn_orient_matrix_UB_32 -0.0031228000 _diffrn_orient_matrix_UB_33 -0.0703240000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -86.00 12.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - -17.2341 -77.0000 90.0000 98 #__ type_ start__ end____ width___ exp.time_ 2 omega -64.00 6.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - -17.2341 118.0000 -110.0000 70 #__ type_ start__ end____ width___ exp.time_ 3 omega 21.00 80.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 19.5778 37.0000 -180.0000 59 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 1610 _reflns_number_gt 1374 _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^)+(0.1068P)^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 1610 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1716 _refine_ls_wR_factor_gt 0.1627 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Mn1 Mn 0.0000 0.0000 0.0000 0.0151(3) Uani 1 2 d S . . Cl1 Cl 0.0000 0.08874(10) -0.2500 0.0178(4) Uani 1 2 d S . . N1 N -0.08262(18) 0.1160(2) 0.0398(3) 0.0152(7) Uani 1 1 d . . . O1 O 0.10725(15) 0.07388(19) 0.0979(3) 0.0173(6) Uani 1 1 d . . . O2 O 0.28019(15) 0.1371(2) 0.1749(3) 0.0221(6) Uani 1 1 d . . . C1 C -0.0527(2) 0.2098(3) 0.0710(3) 0.0167(8) Uani 1 1 d . . . H1 H -0.0984 0.2601 0.0783 0.020 Uiso 1 1 calc R . . C2 C 0.0441(2) 0.2461(3) 0.0960(3) 0.0176(8) Uani 1 1 d . . . C3 C 0.0632(3) 0.3537(3) 0.1170(4) 0.0226(9) Uani 1 1 d . . . H3 H 0.0124 0.4014 0.1064 0.027 Uiso 1 1 calc R . . C4 C 0.15502(18) 0.3895(2) 0.1527(3) 0.0254(9) Uani 1 1 d . . . H4 H 0.1674 0.4621 0.1637 0.031 Uiso 1 1 calc R . . C5 C 0.23072(18) 0.3188(2) 0.1728(3) 0.0226(9) Uani 1 1 d R . . H5 H 0.2941 0.3438 0.1988 0.027 Uiso 1 1 calc R . . C6 C 0.2136(2) 0.2136(3) 0.1549(3) 0.0181(8) Uani 1 1 d . . . C7 C 0.1187(2) 0.1751(3) 0.1127(4) 0.0168(8) Uani 1 1 d . . . C8 C 0.3770(2) 0.1685(3) 0.2159(4) 0.0259(9) Uani 1 1 d . . . H8A H 0.3890 0.2115 0.1395 0.039 Uiso 1 1 calc R . . H8B H 0.4177 0.1068 0.2309 0.039 Uiso 1 1 calc R . . H8C H 0.3907 0.2088 0.3053 0.039 Uiso 1 1 calc R . . C9 C -0.1808(2) 0.0921(3) 0.0360(4) 0.0202(8) Uani 1 1 d . . . H9A H -0.1810 0.0456 0.1161 0.030 Uiso 1 1 calc R . . H9B H -0.2130 0.0579 -0.0554 0.030 Uiso 1 1 calc R . . H9C H -0.2141 0.1567 0.0447 0.030 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 Mn1 0.0120(5) 0.0207(6) 0.0097(5) -0.0023(3) -0.0014(3) -0.0016(3) Cl1 0.0200(6) 0.0247(7) 0.0074(6) 0.000 0.0017(4) 0.000 N1 0.0152(13) 0.0245(18) 0.0031(13) -0.0007(13) -0.0021(11) 0.0005(13) O1 0.0129(11) 0.0225(14) 0.0128(12) -0.0011(11) -0.0023(9) -0.0027(10) O2 0.0148(11) 0.0298(16) 0.0184(14) 0.0004(12) -0.0006(10) -0.0053(12) C1 0.0216(17) 0.024(2) 0.0034(16) 0.0018(15) 0.0021(13) 0.0037(15) C2 0.0210(17) 0.026(2) 0.0042(16) 0.0024(16) 0.0018(13) -0.0030(16) C3 0.0251(18) 0.027(2) 0.0150(19) -0.0006(17) 0.0049(14) 0.0000(17) C4 0.036(2) 0.023(2) 0.0170(19) -0.0053(17) 0.0065(16) -0.0111(18) C5 0.0222(17) 0.032(2) 0.0122(17) -0.0044(17) 0.0024(14) -0.0112(17) C6 0.0230(18) 0.024(2) 0.0070(16) -0.0004(15) 0.0032(13) -0.0020(15) C7 0.0237(17) 0.021(2) 0.0036(15) -0.0003(15) 0.0007(13) -0.0035(16) C8 0.0165(16) 0.039(2) 0.0190(19) -0.0014(19) -0.0007(14) -0.0067(17) C9 0.0152(16) 0.029(2) 0.0146(17) -0.0011(16) 0.0014(13) 0.0001(15) _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 Mn1 O1 1.854(2) . ? Mn1 O1 1.854(2) 5 ? Mn1 N1 2.030(3) . ? Mn1 N1 2.030(3) 5 ? Mn1 Cl1 2.6775(7) . ? Mn1 Cl1 2.6775(7) 5 ? Cl1 Mn1 2.6775(7) 2_554 ? N1 C1 1.290(5) . ? N1 C9 1.469(4) . ? O1 C7 1.314(4) . ? O2 C6 1.363(4) . ? O2 C8 1.424(4) . ? C1 C2 1.453(5) . ? C1 H1 0.9500 . ? C2 C7 1.402(5) . ? C2 C3 1.414(5) . ? C3 C4 1.376(4) . ? C3 H3 0.9500 . ? C4 C5 1.4087 . ? C4 H4 0.9500 . ? C5 C6 1.376(5) . ? C5 H5 0.9500 . ? C6 C7 1.427(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 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 Mn1 O1 180.00(16) . 5 ? O1 Mn1 N1 89.79(11) . . ? O1 Mn1 N1 90.21(11) 5 . ? O1 Mn1 N1 90.21(11) . 5 ? O1 Mn1 N1 89.79(11) 5 5 ? N1 Mn1 N1 180.00(16) . 5 ? O1 Mn1 Cl1 91.35(8) . . ? O1 Mn1 Cl1 88.65(8) 5 . ? N1 Mn1 Cl1 90.85(8) . . ? N1 Mn1 Cl1 89.15(8) 5 . ? O1 Mn1 Cl1 88.65(8) . 5 ? O1 Mn1 Cl1 91.35(8) 5 5 ? N1 Mn1 Cl1 89.15(8) . 5 ? N1 Mn1 Cl1 90.85(8) 5 5 ? Cl1 Mn1 Cl1 180.00(5) . 5 ? Mn1 Cl1 Mn1 129.58(5) 2_554 . ? C1 N1 C9 118.0(3) . . ? C1 N1 Mn1 123.2(2) . . ? C9 N1 Mn1 118.8(2) . . ? C7 O1 Mn1 128.8(2) . . ? C6 O2 C8 117.2(3) . . ? N1 C1 C2 126.3(3) . . ? N1 C1 H1 116.8 . . ? C2 C1 H1 116.8 . . ? C7 C2 C3 120.2(3) . . ? C7 C2 C1 120.7(3) . . ? C3 C2 C1 118.9(3) . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.0(2) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.48(18) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? O2 C6 C5 126.3(3) . . ? O2 C6 C7 113.3(3) . . ? C5 C6 C7 120.4(3) . . ? O1 C7 C2 124.0(3) . . ? O1 C7 C6 117.4(3) . . ? C2 C7 C6 118.5(3) . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.299 _refine_diff_density_min -1.597 _refine_diff_density_rms 0.187 _database_code_depnum_ccdc_archive 'CCDC 936644' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sm1-40c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Na2Fe2(OMe)2(L1)4(NO3)2].2MeOH' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H52 Fe2 N6 Na2 O18' _chemical_formula_weight 1062.56 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n 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 11.6905(5) _cell_length_b 11.1560(5) _cell_length_c 19.0629(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.391(4) _cell_angle_gamma 90.00 _cell_volume 2481.82(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.677 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 3.2012 _cell_measurement_reflns_used 4431 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _exptl_absorpt_correction_T_min 0.76803 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) 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 15820 _diffrn_reflns_av_R_equivalents 0.0956 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.2012 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0150382000 _diffrn_orient_matrix_UB_12 0.0328891000 _diffrn_orient_matrix_UB_13 0.0298943000 _diffrn_orient_matrix_UB_21 -0.0419703000 _diffrn_orient_matrix_UB_22 0.0315778000 _diffrn_orient_matrix_UB_23 -0.0210094000 _diffrn_orient_matrix_UB_31 -0.0411378000 _diffrn_orient_matrix_UB_32 -0.0442818000 _diffrn_orient_matrix_UB_33 0.0071867000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -14.00 32.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -19.8687 -112.0000 168.0000 46 #__ type_ start__ end____ width___ exp.time_ 2 omega -92.00 -40.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -19.8687 -45.0000 120.0000 52 #__ type_ start__ end____ width___ exp.time_ 3 omega 3.00 55.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -19.8687 0.0000 60.0000 52 #__ type_ start__ end____ width___ exp.time_ 4 omega 1.00 53.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -19.8687 45.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 5 omega -43.00 5.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -19.8687 62.0000 293.0000 48 #__ type_ start__ end____ width___ exp.time_ 6 omega -41.00 13.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -19.8687 -77.0000 30.0000 54 #__ type_ start__ end____ width___ exp.time_ 7 omega -30.00 -3.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 22.3687 112.0000 81.0000 27 #__ type_ start__ end____ width___ exp.time_ 8 omega 6.00 47.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 22.3687 -77.0000 120.0000 41 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 4336 _reflns_number_gt 2737 _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^)+(0.1314P)^2^+15.8836P] 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 4336 _refine_ls_number_parameters 307 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1581 _refine_ls_R_factor_gt 0.0996 _refine_ls_wR_factor_ref 0.2723 _refine_ls_wR_factor_gt 0.2439 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 Fe1 Fe 0.43452(9) 0.55203(10) 0.06259(6) 0.0133(3) Uani 1 1 d . . . Na1 Na 0.6517(3) 0.3450(3) 0.10294(16) 0.0180(7) Uani 1 1 d . . . N1 N 0.2581(6) 0.5291(6) 0.0852(3) 0.0162(15) Uani 1 1 d . . . N2 N 0.4865(5) 0.6595(6) 0.1529(3) 0.0153(15) Uani 1 1 d . . . N3 N 0.8723(6) 0.4117(6) 0.1664(4) 0.0199(16) Uani 1 1 d . . . O1 O 0.5793(5) 0.2769(6) 0.2127(3) 0.0232(14) Uani 1 1 d . . . O2 O 0.4637(5) 0.4092(5) 0.1195(3) 0.0170(13) Uani 1 1 d . . . O3 O 0.3164(5) 0.8618(5) -0.0765(3) 0.0251(14) Uani 1 1 d . . . O4 O 0.3993(5) 0.7045(5) 0.0157(3) 0.0170(13) Uani 1 1 d . . . O5 O 0.5949(4) 0.5355(5) 0.0302(3) 0.0177(13) Uani 1 1 d . . . O6 O 0.8516(7) 0.3060(7) 0.1592(6) 0.077(3) Uani 1 1 d . . . O7 O 0.9639(5) 0.4476(6) 0.1949(3) 0.0302(15) Uani 1 1 d . . . O8 O 0.7982(8) 0.4808(8) 0.1418(7) 0.099(4) Uani 1 1 d . . . C1 C 0.6426(8) 0.2390(10) 0.2753(5) 0.036(3) Uani 1 1 d . . . H1A H 0.6135 0.2804 0.3160 0.047 Uiso 1 1 calc R . . H1B H 0.7239 0.2585 0.2718 0.047 Uiso 1 1 calc R . . H1C H 0.6339 0.1523 0.2811 0.047 Uiso 1 1 calc R . . C2 C 0.4616(7) 0.2769(8) 0.2148(4) 0.0177(18) Uani 1 1 d . . . C3 C 0.4031(8) 0.2082(8) 0.2616(4) 0.024(2) Uani 1 1 d . . . H3 H 0.4438 0.1562 0.2936 0.032 Uiso 1 1 calc R . . C4 C 0.2831(7) 0.2162(9) 0.2613(5) 0.028(2) Uani 1 1 d . . . H4 H 0.2422 0.1686 0.2927 0.036 Uiso 1 1 calc R . . C5 C 0.2253(7) 0.2929(8) 0.2155(5) 0.026(2) Uani 1 1 d . . . H5 H 0.1442 0.2980 0.2156 0.034 Uiso 1 1 calc R . . C6 C 0.2845(7) 0.3646(8) 0.1681(4) 0.0180(18) Uani 1 1 d . . . C7 C 0.4027(7) 0.3522(7) 0.1661(4) 0.0181(18) Uani 1 1 d . . . C8 C 0.2195(7) 0.4499(8) 0.1257(4) 0.0191(18) Uani 1 1 d . . . H8 H 0.1386 0.4468 0.1281 0.023 Uiso 1 1 calc R . . C9 C 0.1718(7) 0.6075(9) 0.0490(5) 0.027(2) Uani 1 1 d . . . H9A H 0.1764 0.5995 -0.0020 0.035 Uiso 1 1 calc R . . H9B H 0.1865 0.6910 0.0628 0.035 Uiso 1 1 calc R . . H9C H 0.0951 0.5841 0.0621 0.035 Uiso 1 1 calc R . . C10 C 0.2656(9) 0.9476(9) -0.1241(5) 0.038(3) Uani 1 1 d . . . H10A H 0.2052 0.9910 -0.1012 0.050 Uiso 1 1 calc R . . H10B H 0.2326 0.9064 -0.1660 0.050 Uiso 1 1 calc R . . H10C H 0.3242 1.0043 -0.1378 0.050 Uiso 1 1 calc R . . C11 C 0.3532(8) 0.9064(8) -0.0106(5) 0.025(2) Uani 1 1 d . . . C12 C 0.3472(10) 1.0228(8) 0.0085(5) 0.037(3) Uani 1 1 d . . . H12 H 0.3175 1.0805 -0.0244 0.049 Uiso 1 1 calc R . . C13 C 0.3846(10) 1.0590(9) 0.0763(5) 0.043(3) Uani 1 1 d . . . H13 H 0.3816 1.1411 0.0893 0.056 Uiso 1 1 calc R . . C14 C 0.4249(9) 0.9761(8) 0.1232(5) 0.030(2) Uani 1 1 d . . . H14 H 0.4484 1.0007 0.1695 0.039 Uiso 1 1 calc R . . C15 C 0.4328(8) 0.8545(8) 0.1050(5) 0.023(2) Uani 1 1 d . . . C16 C 0.3957(7) 0.8162(7) 0.0372(5) 0.0181(18) Uani 1 1 d . . . C17 C 0.4786(7) 0.7708(7) 0.1579(4) 0.0158(18) Uani 1 1 d . . . H17 H 0.5058 0.8048 0.2014 0.019 Uiso 1 1 calc R . . C18 C 0.5383(8) 0.5975(8) 0.2163(5) 0.023(2) Uani 1 1 d . . . H18A H 0.5605 0.6571 0.2524 0.030 Uiso 1 1 calc R . . H18B H 0.6062 0.5528 0.2036 0.030 Uiso 1 1 calc R . . H18C H 0.4823 0.5420 0.2346 0.030 Uiso 1 1 calc R . . C19 C 0.6722(11) 0.6387(11) 0.0359(6) 0.049(3) Uani 1 1 d . . . H19A H 0.6616 0.6881 -0.0064 0.064 Uiso 1 1 calc R . . H19B H 0.7517 0.6105 0.0409 0.064 Uiso 1 1 calc R . . H19C H 0.6551 0.6864 0.0772 0.064 Uiso 1 1 calc R . . O9 O 0.0000 1.0000 0.0000 0.080 Uiso 1 2 d SD . . C20 C 0.006(3) 0.8810(14) 0.0323(15) 0.080 Uiso 0.50 1 d PD . . H20A H -0.0684 0.8409 0.0248 0.120 Uiso 0.50 1 calc PR . . H20B H 0.0251 0.8889 0.0828 0.120 Uiso 0.50 1 calc PR . . H20C H 0.0651 0.8334 0.0109 0.120 Uiso 0.50 1 calc PR . . O9A O 0.100(2) 0.967(2) 0.1159(15) 0.122(9) Uiso 0.50 1 d PD . . C20A C 0.081(3) 1.082(2) 0.0817(16) 0.080(9) Uiso 0.50 1 d PD . . H20D H 0.0373 1.1337 0.1117 0.119 Uiso 0.50 1 calc PR . . H20E H 0.0380 1.0699 0.0365 0.119 Uiso 0.50 1 calc PR . . H20F H 0.1550 1.1192 0.0737 0.119 Uiso 0.50 1 calc PR . . 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 Fe1 0.0146(6) 0.0115(6) 0.0136(6) -0.0001(5) -0.0002(4) 0.0020(5) Na1 0.0152(15) 0.0201(18) 0.0183(17) 0.0009(14) -0.0007(13) 0.0005(14) N1 0.020(4) 0.018(4) 0.011(3) -0.003(3) 0.001(3) 0.002(3) N2 0.019(3) 0.011(4) 0.016(4) 0.002(3) 0.001(3) 0.006(3) N3 0.016(4) 0.016(4) 0.027(4) 0.005(3) -0.002(3) 0.002(3) O1 0.017(3) 0.030(4) 0.023(3) 0.009(3) 0.001(2) 0.008(3) O2 0.016(3) 0.016(3) 0.020(3) 0.001(2) 0.003(2) -0.003(2) O3 0.038(4) 0.014(3) 0.021(3) 0.002(3) -0.010(3) 0.007(3) O4 0.023(3) 0.006(3) 0.023(3) 0.000(2) 0.001(2) 0.004(2) O5 0.016(3) 0.013(3) 0.024(3) -0.002(3) 0.000(2) -0.009(2) O6 0.056(5) 0.025(5) 0.145(10) -0.007(5) -0.045(6) 0.004(4) O7 0.018(3) 0.034(4) 0.037(4) -0.001(3) -0.009(3) -0.007(3) O8 0.074(7) 0.036(6) 0.178(12) -0.034(6) -0.076(7) 0.014(5) C1 0.031(5) 0.049(7) 0.028(6) 0.018(5) -0.006(4) 0.004(5) C2 0.017(4) 0.021(5) 0.015(4) -0.003(4) 0.003(3) 0.003(4) C3 0.036(5) 0.025(5) 0.012(4) 0.004(4) 0.001(4) 0.001(4) C4 0.024(5) 0.033(6) 0.026(5) 0.009(4) 0.007(4) 0.003(4) C5 0.020(5) 0.028(5) 0.031(5) 0.011(4) 0.007(4) 0.000(4) C6 0.023(4) 0.015(4) 0.016(4) 0.002(4) 0.001(3) 0.005(4) C7 0.031(5) 0.009(4) 0.015(4) -0.002(3) 0.004(4) 0.001(4) C8 0.015(4) 0.023(5) 0.020(4) -0.004(4) 0.004(3) 0.000(4) C9 0.022(5) 0.030(5) 0.029(5) 0.008(4) 0.002(4) 0.002(4) C10 0.056(7) 0.025(5) 0.031(5) 0.005(5) -0.019(5) 0.005(5) C11 0.034(5) 0.016(5) 0.023(5) -0.001(4) -0.008(4) 0.005(4) C12 0.069(8) 0.012(5) 0.030(6) 0.000(4) -0.009(5) 0.005(5) C13 0.078(8) 0.013(5) 0.037(6) -0.009(5) -0.012(6) 0.011(5) C14 0.047(6) 0.019(5) 0.024(5) -0.006(4) -0.010(4) 0.004(4) C15 0.035(5) 0.015(5) 0.019(5) -0.005(4) 0.001(4) 0.001(4) C16 0.019(4) 0.011(4) 0.024(5) 0.000(4) 0.007(4) 0.001(3) C17 0.018(4) 0.015(5) 0.015(4) -0.007(3) 0.003(3) -0.001(3) C18 0.031(5) 0.008(4) 0.030(5) 0.002(4) -0.012(4) -0.003(4) C19 0.070(8) 0.048(7) 0.030(6) 0.002(5) 0.004(6) 0.002(6) _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 Fe1 O2 1.946(6) . ? Fe1 O4 1.953(5) . ? Fe1 O5 2.017(5) . ? Fe1 O5 2.032(6) 3_665 ? Fe1 N1 2.148(7) . ? Fe1 N2 2.156(7) . ? Fe1 Na1 3.452(3) 3_665 ? Fe1 Na1 3.485(3) . ? Na1 O2 2.351(6) . ? Na1 O4 2.371(6) 3_665 ? Na1 O8 2.372(9) . ? Na1 O3 2.395(7) 3_665 ? Na1 O1 2.425(6) . ? Na1 O6 2.550(9) . ? Na1 O5 2.602(6) . ? Na1 N3 2.880(8) . ? Na1 Fe1 3.452(3) 3_665 ? N1 C8 1.273(11) . ? N1 C9 1.476(11) . ? N2 C17 1.250(10) . ? N2 C18 1.489(10) . ? N3 O6 1.210(10) . ? N3 O8 1.231(11) . ? N3 O7 1.239(9) . ? O1 C2 1.380(9) . ? O1 C1 1.430(10) . ? O2 C7 1.333(9) . ? O3 C11 1.396(10) . ? O3 C10 1.423(11) . ? O3 Na1 2.395(7) 3_665 ? O4 C16 1.313(10) . ? O4 Na1 2.371(6) 3_665 ? O5 C19 1.463(13) . ? O5 Fe1 2.032(6) 3_665 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.386(12) . ? C2 C7 1.402(12) . ? C3 C4 1.405(12) . ? C3 H3 0.9500 . ? C4 C5 1.371(12) . ? C4 H4 0.9500 . ? C5 C6 1.418(12) . ? C5 H5 0.9500 . ? C6 C7 1.392(12) . ? C6 C8 1.437(12) . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.352(13) . ? C11 C16 1.427(12) . ? C12 C13 1.399(14) . ? C12 H12 0.9500 . ? C13 C14 1.351(14) . ? C13 H13 0.9500 . ? C14 C15 1.405(12) . ? C14 H14 0.9500 . ? C15 C16 1.406(12) . ? C15 C17 1.452(12) . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O9 C20 1.464(10) 3_575 ? O9 C20 1.464(10) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O9A C20A 1.450(10) . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 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 O2 Fe1 O4 173.1(2) . . ? O2 Fe1 O5 87.7(2) . . ? O4 Fe1 O5 96.6(2) . . ? O2 Fe1 O5 96.1(2) . 3_665 ? O4 Fe1 O5 90.0(2) . 3_665 ? O5 Fe1 O5 78.6(2) . 3_665 ? O2 Fe1 N1 86.0(2) . . ? O4 Fe1 N1 91.0(2) . . ? O5 Fe1 N1 166.4(2) . . ? O5 Fe1 N1 90.1(2) 3_665 . ? O2 Fe1 N2 88.8(2) . . ? O4 Fe1 N2 85.6(2) . . ? O5 Fe1 N2 94.1(2) . . ? O5 Fe1 N2 171.0(2) 3_665 . ? N1 Fe1 N2 97.7(2) . . ? O2 Fe1 Na1 144.49(18) . 3_665 ? O4 Fe1 Na1 41.42(17) . 3_665 ? O5 Fe1 Na1 88.69(17) . 3_665 ? O5 Fe1 Na1 48.62(17) 3_665 3_665 ? N1 Fe1 Na1 89.49(19) . 3_665 ? N2 Fe1 Na1 126.75(19) . 3_665 ? O2 Fe1 Na1 39.90(16) . . ? O4 Fe1 Na1 144.00(17) . . ? O5 Fe1 Na1 47.82(17) . . ? O5 Fe1 Na1 87.55(17) 3_665 . ? N1 Fe1 Na1 124.94(19) . . ? N2 Fe1 Na1 91.44(18) . . ? Na1 Fe1 Na1 126.30(6) 3_665 . ? O2 Na1 O4 90.8(2) . 3_665 ? O2 Na1 O8 115.2(3) . . ? O4 Na1 O8 125.7(4) 3_665 . ? O2 Na1 O3 118.7(2) . 3_665 ? O4 Na1 O3 67.0(2) 3_665 3_665 ? O8 Na1 O3 124.2(3) . 3_665 ? O2 Na1 O1 66.6(2) . . ? O4 Na1 O1 132.0(2) 3_665 . ? O8 Na1 O1 102.3(4) . . ? O3 Na1 O1 86.9(2) 3_665 . ? O2 Na1 O6 146.8(3) . . ? O4 Na1 O6 122.3(3) 3_665 . ? O8 Na1 O6 49.5(3) . . ? O3 Na1 O6 76.9(3) 3_665 . ? O1 Na1 O6 86.7(3) . . ? O2 Na1 O5 67.13(19) . . ? O4 Na1 O5 68.9(2) 3_665 . ? O8 Na1 O5 78.6(3) . . ? O3 Na1 O5 135.4(2) 3_665 . ? O1 Na1 O5 128.6(2) . . ? O6 Na1 O5 124.2(3) . . ? O2 Na1 N3 133.3(2) . . ? O4 Na1 N3 129.0(2) 3_665 . ? O8 Na1 N3 24.8(3) . . ? O3 Na1 N3 101.0(2) 3_665 . ? O1 Na1 N3 93.9(2) . . ? O6 Na1 N3 24.8(2) . . ? O5 Na1 N3 101.9(2) . . ? O2 Na1 Fe1 78.25(16) . 3_665 ? O4 Na1 Fe1 33.04(14) 3_665 3_665 ? O8 Na1 Fe1 103.9(3) . 3_665 ? O3 Na1 Fe1 99.73(17) 3_665 3_665 ? O1 Na1 Fe1 142.65(17) . 3_665 ? O6 Na1 Fe1 130.7(3) . 3_665 ? O5 Na1 Fe1 35.86(13) . 3_665 ? N3 Na1 Fe1 120.26(17) . 3_665 ? O2 Na1 Fe1 32.08(14) . . ? O4 Na1 Fe1 78.73(15) 3_665 . ? O8 Na1 Fe1 98.5(2) . . ? O3 Na1 Fe1 135.43(19) 3_665 . ? O1 Na1 Fe1 96.38(16) . . ? O6 Na1 Fe1 147.5(2) . . ? O5 Na1 Fe1 35.05(12) . . ? N3 Na1 Fe1 122.95(17) . . ? Fe1 Na1 Fe1 53.70(6) 3_665 . ? C8 N1 C9 116.0(7) . . ? C8 N1 Fe1 125.7(6) . . ? C9 N1 Fe1 118.3(5) . . ? C17 N2 C18 115.3(7) . . ? C17 N2 Fe1 126.5(6) . . ? C18 N2 Fe1 118.1(5) . . ? O6 N3 O8 115.8(8) . . ? O6 N3 O7 121.8(8) . . ? O8 N3 O7 122.4(8) . . ? O6 N3 Na1 62.1(5) . . ? O8 N3 Na1 53.8(5) . . ? O7 N3 Na1 175.8(6) . . ? C2 O1 C1 116.3(6) . . ? C2 O1 Na1 115.2(5) . . ? C1 O1 Na1 128.5(5) . . ? C7 O2 Fe1 132.7(5) . . ? C7 O2 Na1 119.0(5) . . ? Fe1 O2 Na1 108.0(2) . . ? C11 O3 C10 115.4(7) . . ? C11 O3 Na1 119.3(5) . 3_665 ? C10 O3 Na1 125.3(5) . 3_665 ? C16 O4 Fe1 133.9(5) . . ? C16 O4 Na1 120.5(5) . 3_665 ? Fe1 O4 Na1 105.5(2) . 3_665 ? C19 O5 Fe1 119.1(6) . . ? C19 O5 Fe1 121.0(5) . 3_665 ? Fe1 O5 Fe1 101.4(2) . 3_665 ? C19 O5 Na1 117.7(6) . . ? Fe1 O5 Na1 97.1(2) . . ? Fe1 O5 Na1 95.5(2) 3_665 . ? N3 O6 Na1 93.1(5) . . ? N3 O8 Na1 101.4(6) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 123.4(8) . . ? O1 C2 C7 115.6(7) . . ? C3 C2 C7 121.0(8) . . ? C2 C3 C4 119.5(8) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 119.8(8) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.1(8) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 118.9(8) . . ? C7 C6 C8 123.0(8) . . ? C5 C6 C8 118.0(7) . . ? O2 C7 C6 122.8(8) . . ? O2 C7 C2 117.8(7) . . ? C6 C7 C2 119.4(8) . . ? N1 C8 C6 127.3(8) . . ? N1 C8 H8 116.4 . . ? C6 C8 H8 116.4 . . ? 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 . . ? O3 C10 H10A 109.5 . . ? O3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 O3 124.5(8) . . ? C12 C11 C16 121.8(9) . . ? O3 C11 C16 113.6(7) . . ? C11 C12 C13 120.5(10) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 119.4(9) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 121.6(9) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C16 119.9(8) . . ? C14 C15 C17 118.5(8) . . ? C16 C15 C17 121.6(8) . . ? O4 C16 C15 124.1(8) . . ? O4 C16 C11 119.1(8) . . ? C15 C16 C11 116.7(8) . . ? N2 C17 C15 127.7(8) . . ? N2 C17 H17 116.1 . . ? C15 C17 H17 116.1 . . ? 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 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C20 O9 C20 180.0(17) 3_575 . ? O9 C20 H20A 109.5 . . ? O9 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O9 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9A C20A H20D 109.5 . . ? O9A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? O9A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 2.042 _refine_diff_density_min -2.756 _refine_diff_density_rms 0.160 _database_code_depnum_ccdc_archive 'CCDC 936645' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_lfj26c-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Na3Ni2(L)6](ClO4)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H60 Cl N6 Na3 Ni2 O16' _chemical_formula_weight 1270.92 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' Cl Cl 0.1484 0.1585 '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' Na Na 0.0362 0.0249 '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-3 _space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 13.808(2) _cell_length_b 13.808(2) _cell_length_c 17.308(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2857.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2336 _cell_measurement_theta_min 2.8963 _cell_measurement_theta_max 25.35 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Green _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.802 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.96874 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) 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 5091 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0037111000 _diffrn_orient_matrix_UB_12 -0.0053799000 _diffrn_orient_matrix_UB_21 0.0566979000 _diffrn_orient_matrix_UB_22 0.0428128000 _diffrn_orient_matrix_UB_23 0.0032754000 _diffrn_orient_matrix_UB_31 -0.0169799000 _diffrn_orient_matrix_UB_32 0.0407102000 _diffrn_orient_matrix_UB_33 0.0019881000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -89.00 -58.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - -20.0250 -62.0000 13.0000 31 #__ type_ start__ end____ width___ exp.time_ 2 omega 14.00 78.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 22.2125 77.0000 240.0000 64 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 2834 _reflns_number_gt 2239 _reflns_threshold_expression >2sigma(I) _computing_structure_solution SHELXS97 _computing_structure_refinement 'SHELXL-97/2 (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^)+(0.0000P)^2^+44.9327P] 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 2834 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1302 _refine_ls_R_factor_gt 0.1108 _refine_ls_wR_factor_ref 0.2471 _refine_ls_wR_factor_gt 0.2411 _refine_ls_goodness_of_fit_ref 1.288 _refine_ls_restrained_S_all 1.288 _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 0.3333 0.6667 0.42339(12) 0.0228(6) Uani 1 3 d S . . Ni2 Ni 0.3333 0.6667 0.07964(12) 0.0178(5) Uani 1 3 d S . . Cl1 Cl 0.3333 0.6667 -0.2398(4) 0.0619(17) Uani 1 3 d S . . Na1 Na 0.4191(3) 0.5955(4) 0.2505(2) 0.0282(10) Uani 1 1 d . . . N1 N 0.4436(10) 0.6333(9) 0.4868(5) 0.041(3) Uani 1 1 d . . . N2 N 0.4297(8) 0.8139(7) 0.0156(5) 0.025(2) Uani 1 1 d . . . O1 O 0.4650(6) 0.7618(7) 0.3505(4) 0.0304(18) Uani 1 1 d . . . O2 O 0.5923(7) 0.9475(7) 0.2772(5) 0.045(2) Uani 1 1 d . . . O3 O 0.6118(7) 0.6822(8) 0.2270(4) 0.044(2) Uani 1 1 d . . . O4 O 0.4665(6) 0.7201(6) 0.1529(4) 0.0235(16) Uani 1 1 d . . . O5 O 0.4361(9) 0.7570(9) -0.2067(7) 0.080(4) Uani 1 1 d . . . O6 O 0.3333 0.6667 -0.3138(14) 0.26(3) Uani 1 3 d S . . C1 C 0.3972(14) 0.5440(14) 0.5471(7) 0.068(5) Uani 1 1 d . . . H1A H 0.4578 0.5353 0.5691 0.102 Uiso 1 1 calc R . . H1B H 0.3413 0.4732 0.5236 0.102 Uiso 1 1 calc R . . H1C H 0.3620 0.5648 0.5880 0.102 Uiso 1 1 calc R . . C2 C 0.5501(12) 0.6856(13) 0.4789(7) 0.047(4) Uani 1 1 d . . . H2 H 0.5898 0.6608 0.5105 0.056 Uiso 1 1 calc R . . C3 C 0.6168(10) 0.7777(11) 0.4277(7) 0.036(3) Uani 1 1 d . . . C4 C 0.5701(10) 0.8135(10) 0.3691(6) 0.033(3) Uani 1 1 d . . . C5 C 0.6450(10) 0.9149(10) 0.3278(6) 0.037(3) Uani 1 1 d . . . C6 C 0.7578(12) 0.9679(14) 0.3405(7) 0.056(4) Uani 1 1 d . . . H6 H 0.8053 1.0333 0.3117 0.067 Uiso 1 1 calc R . . C7 C 0.8043(12) 0.9295(13) 0.3933(9) 0.056(4) Uani 1 1 d . . . H7 H 0.8830 0.9664 0.4005 0.067 Uiso 1 1 calc R . . C8 C 0.7331(12) 0.8346(12) 0.4366(8) 0.051(4) Uani 1 1 d . . . H8 H 0.7650 0.8078 0.4735 0.061 Uiso 1 1 calc R . . C9 C 0.6613(13) 1.0547(12) 0.2380(8) 0.063(5) Uani 1 1 d . . . H9A H 0.6956 1.1146 0.2765 0.095 Uiso 1 1 calc R . . H9B H 0.6144 1.0697 0.2031 0.095 Uiso 1 1 calc R . . H9C H 0.7200 1.0516 0.2082 0.095 Uiso 1 1 calc R . . C10 C 0.6919(12) 0.6642(12) 0.2659(8) 0.054(4) Uani 1 1 d . . . H10A H 0.7389 0.6544 0.2279 0.081 Uiso 1 1 calc R . . H10B H 0.6534 0.5970 0.2981 0.081 Uiso 1 1 calc R . . H10C H 0.7388 0.7289 0.2987 0.081 Uiso 1 1 calc R . . C11 C 0.6563(9) 0.7699(11) 0.1725(6) 0.035(3) Uani 1 1 d . . . C12 C 0.7686(9) 0.8355(12) 0.1565(7) 0.045(4) Uani 1 1 d . . . H12 H 0.8224 0.8252 0.1838 0.055 Uiso 1 1 calc R . . C13 C 0.8023(10) 0.9183(11) 0.0989(7) 0.044(3) Uani 1 1 d . . . H13 H 0.8796 0.9665 0.0889 0.053 Uiso 1 1 calc R . . C14 C 0.7260(10) 0.9293(11) 0.0581(7) 0.041(3) Uani 1 1 d . . . H14 H 0.7504 0.9842 0.0184 0.049 Uiso 1 1 calc R . . C15 C 0.6106(9) 0.8621(9) 0.0722(6) 0.031(3) Uani 1 1 d . . . C16 C 0.5742(8) 0.7813(9) 0.1328(6) 0.024(2) Uani 1 1 d . . . C17 C 0.5367(10) 0.8747(9) 0.0206(6) 0.032(3) Uani 1 1 d . . . H17 H 0.5710 0.9357 -0.0145 0.038 Uiso 1 1 calc R . . C18 C 0.3770(10) 0.8450(10) -0.0447(6) 0.031(3) Uani 1 1 d . . . H18A H 0.4339 0.9121 -0.0713 0.046 Uiso 1 1 calc R . . H18B H 0.3212 0.8603 -0.0216 0.046 Uiso 1 1 calc R . . H18C H 0.3403 0.7836 -0.0819 0.046 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 0.0259(8) 0.0259(8) 0.0166(10) 0.000 0.000 0.0129(4) Ni2 0.0177(7) 0.0177(7) 0.0181(10) 0.000 0.000 0.0088(4) Cl1 0.062(3) 0.062(3) 0.062(4) 0.000 0.000 0.0310(13) Na1 0.030(2) 0.035(2) 0.0249(19) 0.0065(18) 0.0048(18) 0.020(2) N1 0.064(8) 0.053(7) 0.017(4) 0.006(5) -0.004(5) 0.037(6) N2 0.031(5) 0.024(5) 0.023(4) 0.002(4) 0.000(4) 0.015(4) O1 0.025(4) 0.038(5) 0.022(3) 0.005(4) -0.006(3) 0.011(4) O2 0.037(5) 0.033(5) 0.036(4) 0.008(4) -0.006(4) -0.004(4) O3 0.034(5) 0.082(7) 0.031(4) 0.013(5) 0.005(4) 0.041(5) O4 0.017(4) 0.031(4) 0.020(3) 0.004(3) 0.003(3) 0.010(3) O5 0.055(7) 0.051(7) 0.126(10) 0.018(7) 0.008(7) 0.020(6) O6 0.38(4) 0.38(4) 0.032(14) 0.000 0.000 0.19(2) C1 0.085(12) 0.089(13) 0.035(7) 0.022(8) -0.003(8) 0.046(11) C2 0.055(9) 0.074(10) 0.033(7) 0.003(7) -0.014(6) 0.048(9) C3 0.029(6) 0.047(8) 0.031(6) -0.008(6) -0.013(5) 0.019(6) C4 0.029(6) 0.041(7) 0.022(5) -0.012(5) -0.016(5) 0.013(6) C5 0.037(7) 0.036(7) 0.028(6) -0.005(5) 0.000(5) 0.010(6) C6 0.032(8) 0.078(11) 0.037(7) -0.024(7) -0.008(6) 0.013(8) C7 0.034(8) 0.065(10) 0.063(9) -0.021(8) -0.004(7) 0.020(7) C8 0.051(9) 0.055(9) 0.056(8) -0.031(7) -0.036(7) 0.032(8) C9 0.058(10) 0.043(9) 0.047(8) 0.017(7) 0.007(7) -0.006(7) C10 0.058(9) 0.053(9) 0.061(9) 0.016(8) -0.008(8) 0.035(8) C11 0.021(6) 0.053(8) 0.025(5) -0.009(6) -0.003(5) 0.015(6) C12 0.015(6) 0.078(10) 0.041(7) -0.012(7) -0.006(5) 0.022(7) C13 0.019(6) 0.055(9) 0.046(7) -0.008(7) 0.010(6) 0.010(6) C14 0.036(7) 0.038(7) 0.039(6) 0.002(6) 0.015(6) 0.011(6) C15 0.023(6) 0.027(6) 0.029(5) -0.003(5) 0.002(5) 0.002(5) C16 0.012(5) 0.027(6) 0.025(5) -0.006(5) 0.001(4) 0.004(4) C17 0.041(7) 0.023(6) 0.026(6) 0.003(5) 0.004(5) 0.012(6) C18 0.048(7) 0.036(7) 0.027(5) 0.015(5) 0.011(5) 0.035(6) _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 2.058(7) 2_665 ? Ni1 O1 2.058(7) 3_565 ? Ni1 O1 2.058(7) . ? Ni1 N1 2.106(10) 2_665 ? Ni1 N1 2.106(10) 3_565 ? Ni1 N1 2.106(10) . ? Ni1 Na1 3.534(4) 2_665 ? Ni1 Na1 3.534(4) 3_565 ? Ni1 Na1 3.534(4) . ? Ni2 O4 2.043(7) 2_665 ? Ni2 O4 2.043(7) . ? Ni2 O4 2.043(7) 3_565 ? Ni2 N2 2.104(9) . ? Ni2 N2 2.104(9) 2_665 ? Ni2 N2 2.104(9) 3_565 ? Ni2 Na1 3.505(4) 2_665 ? Ni2 Na1 3.505(4) 3_565 ? Ni2 Na1 3.505(4) . ? Cl1 O6 1.28(2) . ? Cl1 O5 1.459(12) 2_665 ? Cl1 O5 1.459(12) . ? Cl1 O5 1.459(12) 3_565 ? Na1 O1 2.265(8) 3_565 ? Na1 O4 2.262(8) . ? Na1 O2 2.329(9) 3_565 ? Na1 O3 2.343(9) . ? Na1 O4 2.618(8) 3_565 ? Na1 O1 2.686(9) . ? Na1 C4 3.127(12) 3_565 ? Na1 Na1 3.257(7) 3_565 ? Na1 Na1 3.257(7) 2_665 ? N1 C2 1.281(17) . ? N1 C1 1.493(16) . ? N2 C17 1.286(14) . ? N2 C18 1.456(13) . ? O1 C4 1.298(13) . ? O1 Na1 2.265(8) 2_665 ? O2 C5 1.352(15) . ? O2 C9 1.466(14) . ? O2 Na1 2.329(9) 2_665 ? O3 C11 1.412(14) . ? O3 C10 1.419(14) . ? O4 C16 1.339(12) . ? O4 Na1 2.618(8) 2_665 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.442(18) . ? C2 H2 0.9500 . ? C3 C8 1.399(18) . ? C3 C4 1.418(15) . ? C4 C5 1.447(16) . ? C4 Na1 3.127(12) 2_665 ? C5 C6 1.368(18) . ? C6 C7 1.37(2) . ? C6 H6 0.9500 . ? C7 C8 1.40(2) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.378(16) . ? C11 C16 1.399(15) . ? C12 C13 1.409(18) . ? C12 H12 0.9500 . ? C13 C14 1.339(18) . ? C13 H13 0.9500 . ? C14 C15 1.407(16) . ? C14 H14 0.9500 . ? C15 C16 1.426(15) . ? C15 C17 1.431(16) . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 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 86.3(3) 2_665 3_565 ? O1 Ni1 O1 86.3(3) 2_665 . ? O1 Ni1 O1 86.3(3) 3_565 . ? O1 Ni1 N1 87.4(4) 2_665 2_665 ? O1 Ni1 N1 173.2(4) 3_565 2_665 ? O1 Ni1 N1 90.6(4) . 2_665 ? O1 Ni1 N1 90.6(4) 2_665 3_565 ? O1 Ni1 N1 87.4(4) 3_565 3_565 ? O1 Ni1 N1 173.2(4) . 3_565 ? N1 Ni1 N1 95.3(4) 2_665 3_565 ? O1 Ni1 N1 173.2(4) 2_665 . ? O1 Ni1 N1 90.6(4) 3_565 . ? O1 Ni1 N1 87.4(4) . . ? N1 Ni1 N1 95.3(4) 2_665 . ? N1 Ni1 N1 95.3(4) 3_565 . ? O1 Ni1 Na1 49.2(2) 2_665 2_665 ? O1 Ni1 Na1 83.8(2) 3_565 2_665 ? O1 Ni1 Na1 37.2(2) . 2_665 ? N1 Ni1 Na1 90.0(3) 2_665 2_665 ? N1 Ni1 Na1 139.2(3) 3_565 2_665 ? N1 Ni1 Na1 124.4(3) . 2_665 ? O1 Ni1 Na1 37.2(2) 2_665 3_565 ? O1 Ni1 Na1 49.2(2) 3_565 3_565 ? O1 Ni1 Na1 83.8(2) . 3_565 ? N1 Ni1 Na1 124.4(3) 2_665 3_565 ? N1 Ni1 Na1 90.0(3) 3_565 3_565 ? N1 Ni1 Na1 139.2(3) . 3_565 ? Na1 Ni1 Na1 54.87(11) 2_665 3_565 ? O1 Ni1 Na1 83.8(2) 2_665 . ? O1 Ni1 Na1 37.2(2) 3_565 . ? O1 Ni1 Na1 49.2(2) . . ? N1 Ni1 Na1 139.2(3) 2_665 . ? N1 Ni1 Na1 124.4(3) 3_565 . ? N1 Ni1 Na1 90.0(3) . . ? Na1 Ni1 Na1 54.87(11) 2_665 . ? Na1 Ni1 Na1 54.87(11) 3_565 . ? O4 Ni2 O4 85.5(3) 2_665 . ? O4 Ni2 O4 85.5(3) 2_665 3_565 ? O4 Ni2 O4 85.5(3) . 3_565 ? O4 Ni2 N2 91.8(3) 2_665 . ? O4 Ni2 N2 87.6(3) . . ? O4 Ni2 N2 172.8(3) 3_565 . ? O4 Ni2 N2 87.6(3) 2_665 2_665 ? O4 Ni2 N2 172.8(3) . 2_665 ? O4 Ni2 N2 91.8(3) 3_565 2_665 ? N2 Ni2 N2 94.8(3) . 2_665 ? O4 Ni2 N2 172.8(3) 2_665 3_565 ? O4 Ni2 N2 91.8(3) . 3_565 ? O4 Ni2 N2 87.6(3) 3_565 3_565 ? N2 Ni2 N2 94.8(3) . 3_565 ? N2 Ni2 N2 94.8(3) 2_665 3_565 ? O4 Ni2 Na1 37.6(2) 2_665 2_665 ? O4 Ni2 Na1 47.9(2) . 2_665 ? O4 Ni2 Na1 83.7(2) 3_565 2_665 ? N2 Ni2 Na1 90.0(2) . 2_665 ? N2 Ni2 Na1 125.2(2) 2_665 2_665 ? N2 Ni2 Na1 139.2(2) 3_565 2_665 ? O4 Ni2 Na1 47.9(2) 2_665 3_565 ? O4 Ni2 Na1 83.7(2) . 3_565 ? O4 Ni2 Na1 37.6(2) 3_565 3_565 ? N2 Ni2 Na1 139.2(2) . 3_565 ? N2 Ni2 Na1 90.0(2) 2_665 3_565 ? N2 Ni2 Na1 125.2(2) 3_565 3_565 ? Na1 Ni2 Na1 55.37(11) 2_665 3_565 ? O4 Ni2 Na1 83.7(2) 2_665 . ? O4 Ni2 Na1 37.6(2) . . ? O4 Ni2 Na1 47.9(2) 3_565 . ? N2 Ni2 Na1 125.2(2) . . ? N2 Ni2 Na1 139.2(2) 2_665 . ? N2 Ni2 Na1 90.0(2) 3_565 . ? Na1 Ni2 Na1 55.37(11) 2_665 . ? Na1 Ni2 Na1 55.37(11) 3_565 . ? O6 Cl1 O5 113.2(5) . 2_665 ? O6 Cl1 O5 113.2(5) . . ? O5 Cl1 O5 105.5(6) 2_665 . ? O6 Cl1 O5 113.2(5) . 3_565 ? O5 Cl1 O5 105.6(6) 2_665 3_565 ? O5 Cl1 O5 105.5(6) . 3_565 ? O1 Na1 O4 136.8(3) 3_565 . ? O1 Na1 O2 68.9(3) 3_565 3_565 ? O4 Na1 O2 143.1(3) . 3_565 ? O1 Na1 O3 140.1(3) 3_565 . ? O4 Na1 O3 70.1(3) . . ? O2 Na1 O3 107.7(4) 3_565 . ? O1 Na1 O4 90.2(3) 3_565 3_565 ? O4 Na1 O4 68.9(3) . 3_565 ? O2 Na1 O4 88.9(3) 3_565 3_565 ? O3 Na1 O4 129.6(3) . 3_565 ? O1 Na1 O1 68.7(3) 3_565 . ? O4 Na1 O1 88.6(3) . . ? O2 Na1 O1 128.3(3) 3_565 . ? O3 Na1 O1 87.3(3) . . ? O4 Na1 O1 119.3(3) 3_565 . ? O1 Na1 C4 21.0(3) 3_565 3_565 ? O4 Na1 C4 150.4(3) . 3_565 ? O2 Na1 C4 48.1(3) 3_565 3_565 ? O3 Na1 C4 139.0(3) . 3_565 ? O4 Na1 C4 87.3(3) 3_565 3_565 ? O1 Na1 C4 88.1(3) . 3_565 ? O1 Na1 Na1 54.7(2) 3_565 3_565 ? O4 Na1 Na1 86.79(19) . 3_565 ? O2 Na1 Na1 97.2(3) 3_565 3_565 ? O3 Na1 Na1 154.5(3) . 3_565 ? O4 Na1 Na1 43.62(18) 3_565 3_565 ? O1 Na1 Na1 81.26(17) . 3_565 ? C4 Na1 Na1 63.7(2) 3_565 3_565 ? O1 Na1 Na1 87.8(2) 3_565 2_665 ? O4 Na1 Na1 53.0(2) . 2_665 ? O2 Na1 Na1 154.8(3) 3_565 2_665 ? O3 Na1 Na1 96.3(3) . 2_665 ? O4 Na1 Na1 81.35(17) 3_565 2_665 ? O1 Na1 Na1 43.51(18) . 2_665 ? C4 Na1 Na1 107.9(2) 3_565 2_665 ? Na1 Na1 Na1 60.000(1) 3_565 2_665 ? O1 Na1 Ni2 117.0(2) 3_565 . ? O4 Na1 Ni2 33.49(18) . . ? O2 Na1 Ni2 119.1(3) 3_565 . ? O3 Na1 Ni2 99.6(2) . . ? O4 Na1 Ni2 35.39(16) 3_565 . ? O1 Na1 Ni2 105.8(2) . . ? C4 Na1 Ni2 120.8(2) 3_565 . ? Na1 Na1 Ni2 62.31(6) 3_565 . ? Na1 Na1 Ni2 62.31(6) 2_665 . ? O1 Na1 Ni1 33.28(19) 3_565 . ? O4 Na1 Ni1 115.5(2) . . ? O2 Na1 Ni1 98.5(2) 3_565 . ? O3 Na1 Ni1 117.2(3) . . ? O4 Na1 Ni1 106.13(19) 3_565 . ? O1 Na1 Ni1 35.44(16) . . ? C4 Na1 Ni1 53.3(2) 3_565 . ? Na1 Na1 Ni1 62.56(6) 3_565 . ? Na1 Na1 Ni1 62.56(6) 2_665 . ? Ni2 Na1 Ni1 115.41(12) . . ? C2 N1 C1 115.9(11) . . ? C2 N1 Ni1 125.0(9) . . ? C1 N1 Ni1 119.1(9) . . ? C17 N2 C18 115.8(10) . . ? C17 N2 Ni2 124.1(8) . . ? C18 N2 Ni2 119.7(7) . . ? C4 O1 Ni1 125.9(6) . . ? C4 O1 Na1 120.3(7) . 2_665 ? Ni1 O1 Na1 109.6(3) . 2_665 ? C4 O1 Na1 110.6(7) . . ? Ni1 O1 Na1 95.4(3) . . ? Na1 O1 Na1 81.8(3) 2_665 . ? C5 O2 C9 116.7(10) . . ? C5 O2 Na1 118.1(7) . 2_665 ? C9 O2 Na1 124.9(8) . 2_665 ? C11 O3 C10 115.1(9) . . ? C11 O3 Na1 116.8(6) . . ? C10 O3 Na1 127.8(8) . . ? C16 O4 Ni2 125.5(6) . . ? C16 O4 Na1 118.8(6) . . ? Ni2 O4 Na1 108.9(3) . . ? C16 O4 Na1 112.8(6) . 2_665 ? Ni2 O4 Na1 96.7(3) . 2_665 ? Na1 O4 Na1 83.4(3) . 2_665 ? 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 127.6(11) . . ? N1 C2 H2 116.2 . . ? C3 C2 H2 116.2 . . ? C8 C3 C4 118.5(12) . . ? C8 C3 C2 118.4(11) . . ? C4 C3 C2 123.1(11) . . ? O1 C4 C3 124.4(11) . . ? O1 C4 C5 118.1(10) . . ? C3 C4 C5 117.5(11) . . ? O1 C4 Na1 38.7(5) . 2_665 ? C3 C4 Na1 162.9(9) . 2_665 ? C5 C4 Na1 79.5(7) . 2_665 ? O2 C5 C6 125.8(12) . . ? O2 C5 C4 113.5(10) . . ? C6 C5 C4 120.7(12) . . ? C5 C6 C7 122.0(15) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C6 C7 C8 118.4(14) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C7 C8 C3 122.6(13) . . ? C7 C8 H8 118.7 . . ? C3 C8 H8 118.7 . . ? O2 C9 H9A 109.5 . . ? O2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O3 C10 H10A 109.5 . . ? O3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 122.4(12) . . ? C12 C11 O3 124.2(11) . . ? C16 C11 O3 113.3(9) . . ? C11 C12 C13 118.8(12) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C14 C13 C12 120.4(11) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 121.9(12) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C14 C15 C16 118.9(11) . . ? C14 C15 C17 116.8(11) . . ? C16 C15 C17 124.1(10) . . ? O4 C16 C11 120.5(10) . . ? O4 C16 C15 122.1(10) . . ? C11 C16 C15 117.4(10) . . ? N2 C17 C15 128.2(11) . . ? N2 C17 H17 115.9 . . ? C15 C17 H17 115.9 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.810 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.810 _refine_diff_density_max 1.106 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.132 _database_code_depnum_ccdc_archive 'CCDC 936646' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p21n _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Na2Ni2(N3)2(immp)4(MeCN)2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 N12 Na2 Ni2 O8' _chemical_formula_weight 986.29 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' Na Na 0.0362 0.0249 '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 P21/n 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 11.663(2) _cell_length_b 11.884(2) _cell_length_c 15.975(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.72(3) _cell_angle_gamma 90.00 _cell_volume 2188.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.946 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.8951 _cell_measurement_reflns_used 7057 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _exptl_absorpt_correction_T_min 0.96748 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) 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 10588 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.8951 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0465536000 _diffrn_orient_matrix_UB_12 -0.0065926000 _diffrn_orient_matrix_UB_13 -0.0336960000 _diffrn_orient_matrix_UB_21 -0.0401601000 _diffrn_orient_matrix_UB_22 0.0126928000 _diffrn_orient_matrix_UB_23 0.0279147000 _diffrn_orient_matrix_UB_31 0.0034445000 _diffrn_orient_matrix_UB_32 0.0579443000 _diffrn_orient_matrix_UB_33 -0.0099381000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 35.00 60.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 179.0000 30.0000 25 #__ type_ start__ end____ width___ exp.time_ 2 omega -6.00 91.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 37.0000 -180.0000 97 #__ type_ start__ end____ width___ exp.time_ 3 omega -4.00 79.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 37.0000 -90.0000 83 #__ type_ start__ end____ width___ exp.time_ 4 omega -5.00 21.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 77.0000 -180.0000 26 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 3991 _reflns_number_gt 3584 _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^)+(0.0296P)^2^+0.9361P] 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 3991 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _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 0.385740(19) 0.513930(18) 0.051412(13) 0.01344(8) Uani 1 1 d . . . Na1 Na 0.65874(6) 0.57694(6) 0.15705(4) 0.01815(16) Uani 1 1 d . . . N1 N 0.55231(13) 0.42283(12) 0.06147(9) 0.0156(3) Uani 1 1 d . . . N2 N 0.54376(13) 0.32146(13) 0.06560(9) 0.0168(3) Uani 1 1 d . . . N3 N 0.53527(16) 0.22557(13) 0.06984(10) 0.0277(4) Uani 1 1 d . . . N4 N 0.24140(12) 0.61847(13) 0.03826(9) 0.0164(3) Uani 1 1 d . . . N5 N 0.65536(13) 0.57349(13) -0.15426(9) 0.0165(3) Uani 1 1 d . . . N6 N 0.73295(16) 0.49012(14) 0.29408(11) 0.0299(4) Uani 1 1 d . . . O1 O 0.60981(11) 0.73348(11) 0.24466(8) 0.0257(3) Uani 1 1 d . . . O2 O 0.47274(10) 0.63220(10) 0.12492(8) 0.0175(3) Uani 1 1 d . . . O3 O 0.83853(11) 0.68308(11) 0.15113(8) 0.0233(3) Uani 1 1 d . . . O4 O 0.69816(10) 0.60396(10) 0.02404(7) 0.0169(3) Uani 1 1 d . . . C1 C 0.66757(18) 0.77089(18) 0.32462(12) 0.0291(5) Uani 1 1 d . . . H1A H 0.7039 0.8441 0.3179 0.044 Uiso 1 1 calc R . . H1B H 0.7273 0.7162 0.3469 0.044 Uiso 1 1 calc R . . H1C H 0.6113 0.7782 0.3641 0.044 Uiso 1 1 calc R . . C2 C 0.51215(16) 0.79217(16) 0.20960(12) 0.0203(4) Uani 1 1 d . . . C3 C 0.48640(18) 0.90015(17) 0.23186(13) 0.0264(4) Uani 1 1 d . . . H3 H 0.5364 0.9385 0.2751 0.032 Uiso 1 1 calc R . . C4 C 0.38658(18) 0.95333(17) 0.19071(13) 0.0278(5) Uani 1 1 d . . . H4 H 0.3708 1.0293 0.2035 0.033 Uiso 1 1 calc R . . C5 C 0.31206(17) 0.89541(16) 0.13218(12) 0.0234(4) Uani 1 1 d . . . H5 H 0.2437 0.9315 0.1051 0.028 Uiso 1 1 calc R . . C6 C 0.33416(16) 0.78299(15) 0.11082(11) 0.0175(4) Uani 1 1 d . . . C7 C 0.43944(15) 0.73103(15) 0.14580(11) 0.0160(4) Uani 1 1 d . . . C8 C 0.24109(16) 0.72192(16) 0.06037(11) 0.0186(4) Uani 1 1 d . . . H8 H 0.1722 0.7631 0.0416 0.022 Uiso 1 1 calc R . . C9 C 0.12905(16) 0.57099(17) 0.00094(13) 0.0234(4) Uani 1 1 d . . . H9A H 0.0704 0.6307 -0.0062 0.035 Uiso 1 1 calc R . . H9B H 0.1061 0.5126 0.0385 0.035 Uiso 1 1 calc R . . H9C H 0.1356 0.5379 -0.0543 0.035 Uiso 1 1 calc R . . C10 C 0.92269(18) 0.71612(18) 0.22094(12) 0.0291(5) Uani 1 1 d . . . H10A H 1.0007 0.7046 0.2067 0.044 Uiso 1 1 calc R . . H10B H 0.9132 0.6707 0.2706 0.044 Uiso 1 1 calc R . . H10C H 0.9121 0.7958 0.2335 0.044 Uiso 1 1 calc R . . C11 C 0.84907(16) 0.72836(15) 0.07326(11) 0.0185(4) Uani 1 1 d . . . C12 C 0.92410(16) 0.81287(15) 0.05997(12) 0.0213(4) Uani 1 1 d . . . H12 H 0.9717 0.8468 0.1067 0.026 Uiso 1 1 calc R . . C13 C 0.93074(17) 0.84939(16) -0.02273(13) 0.0250(4) Uani 1 1 d . . . H13 H 0.9821 0.9084 -0.0323 0.030 Uiso 1 1 calc R . . C14 C 0.86243(17) 0.79906(16) -0.08941(12) 0.0234(4) Uani 1 1 d . . . H14 H 0.8682 0.8229 -0.1454 0.028 Uiso 1 1 calc R . . C15 C 0.78360(16) 0.71267(15) -0.07727(11) 0.0184(4) Uani 1 1 d . . . C16 C 0.77165(15) 0.67830(14) 0.00567(11) 0.0162(4) Uani 1 1 d . . . C17 C 0.71993(16) 0.66091(15) -0.15193(11) 0.0192(4) Uani 1 1 d . . . H17 H 0.7266 0.6952 -0.2047 0.023 Uiso 1 1 calc R . . C18 C 0.60487(16) 0.53292(12) -0.23788(7) 0.0240(4) Uani 1 1 d . . . H18A H 0.6228 0.5859 -0.2811 0.036 Uiso 1 1 calc R . . H18B H 0.5206 0.5267 -0.2409 0.036 Uiso 1 1 calc R . . H18C H 0.6373 0.4589 -0.2478 0.036 Uiso 1 1 calc R . . C19 C 0.78552(12) 0.47115(11) 0.35834(7) 0.0241(4) Uani 1 1 d R . . C20 C 0.85506(13) 0.44962(10) 0.44013(7) 0.0328(5) Uani 1 1 d R . . H20A H 0.9117 0.3903 0.4343 0.049 Uiso 1 1 calc R . . H20B H 0.8045 0.4255 0.4805 0.049 Uiso 1 1 calc R . . H20C H 0.8960 0.5186 0.4608 0.049 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 0.01315(13) 0.01427(12) 0.01241(12) -0.00115(9) 0.00040(9) -0.00067(9) Na1 0.0159(4) 0.0225(4) 0.0154(3) -0.0005(3) 0.0005(3) 0.0001(3) N1 0.0158(8) 0.0150(8) 0.0156(7) 0.0005(6) 0.0007(6) 0.0003(6) N2 0.0167(8) 0.0208(9) 0.0122(7) -0.0001(6) 0.0001(6) 0.0012(7) N3 0.0402(11) 0.0163(9) 0.0252(9) 0.0015(7) 0.0003(8) -0.0002(8) N4 0.0128(7) 0.0184(8) 0.0173(8) 0.0009(6) 0.0003(6) -0.0008(6) N5 0.0164(8) 0.0190(8) 0.0140(7) -0.0012(6) 0.0015(6) 0.0022(7) N6 0.0321(10) 0.0299(9) 0.0258(10) 0.0040(8) -0.0014(8) 0.0038(8) O1 0.0218(7) 0.0285(7) 0.0239(7) -0.0121(6) -0.0056(6) 0.0034(6) O2 0.0157(6) 0.0163(6) 0.0195(6) -0.0047(5) -0.0004(5) 0.0014(5) O3 0.0232(7) 0.0302(7) 0.0155(6) -0.0030(6) -0.0006(5) -0.0087(6) O4 0.0166(6) 0.0188(6) 0.0152(6) -0.0016(5) 0.0021(5) -0.0048(5) C1 0.0315(12) 0.0304(11) 0.0227(10) -0.0095(9) -0.0044(9) -0.0038(9) C2 0.0180(9) 0.0220(9) 0.0211(10) -0.0032(8) 0.0039(8) -0.0011(8) C3 0.0252(11) 0.0250(10) 0.0294(11) -0.0120(9) 0.0053(9) -0.0047(9) C4 0.0283(11) 0.0182(9) 0.0384(12) -0.0091(9) 0.0095(9) 0.0014(9) C5 0.0228(10) 0.0210(10) 0.0278(10) 0.0003(8) 0.0084(8) 0.0046(8) C6 0.0180(9) 0.0184(9) 0.0173(9) -0.0007(7) 0.0063(7) 0.0000(8) C7 0.0175(9) 0.0167(9) 0.0149(9) -0.0009(7) 0.0060(7) -0.0017(8) C8 0.0160(9) 0.0223(10) 0.0178(9) 0.0034(8) 0.0032(7) 0.0037(8) C9 0.0140(9) 0.0245(10) 0.0302(11) 0.0012(9) -0.0018(8) -0.0006(8) C10 0.0291(11) 0.0334(11) 0.0214(10) -0.0025(9) -0.0067(8) -0.0074(10) C11 0.0168(9) 0.0186(9) 0.0198(9) -0.0020(8) 0.0019(7) 0.0019(8) C12 0.0185(10) 0.0183(9) 0.0263(10) -0.0058(8) 0.0007(8) -0.0022(8) C13 0.0254(11) 0.0159(9) 0.0341(11) -0.0001(8) 0.0056(9) -0.0054(8) C14 0.0276(11) 0.0193(9) 0.0240(10) 0.0045(8) 0.0064(8) -0.0001(8) C15 0.0201(10) 0.0148(9) 0.0200(9) 0.0001(7) 0.0022(7) 0.0007(8) C16 0.0164(9) 0.0131(8) 0.0195(9) -0.0019(7) 0.0040(7) 0.0022(7) C17 0.0204(10) 0.0209(9) 0.0166(9) 0.0037(8) 0.0041(7) 0.0038(8) C18 0.0252(10) 0.0318(11) 0.0147(9) -0.0009(8) 0.0018(8) -0.0033(9) C19 0.0240(10) 0.0205(10) 0.0280(11) -0.0001(9) 0.0047(9) -0.0013(8) C20 0.0360(12) 0.0352(12) 0.0241(11) 0.0040(10) -0.0059(9) -0.0048(10) _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 2.0038(12) 3_665 ? Ni1 O2 2.0056(13) . ? Ni1 N5 2.0609(15) 3_665 ? Ni1 N4 2.0771(15) . ? Ni1 N1 2.1758(15) 3_665 ? Ni1 N1 2.2084(15) . ? Ni1 Na1 3.4520(12) . ? Ni1 Na1 3.4642(10) 3_665 ? Na1 O2 2.2501(14) . ? Na1 O4 2.2640(14) . ? Na1 O1 2.4470(15) . ? Na1 N6 2.4558(19) . ? Na1 O3 2.4611(15) . ? Na1 N1 2.5790(17) . ? Na1 C7 3.129(2) . ? Na1 Ni1 3.4642(10) 3_665 ? N1 N2 1.211(2) . ? N1 Ni1 2.1758(15) 3_665 ? N2 N3 1.147(2) . ? N4 C8 1.279(2) . ? N4 C9 1.468(2) . ? N5 C17 1.280(2) . ? N5 C18 1.4577(18) . ? N5 Ni1 2.0609(15) 3_665 ? N6 C19 1.136(2) . ? O1 C2 1.380(2) . ? O1 C1 1.422(2) . ? O2 C7 1.296(2) . ? O3 C11 1.378(2) . ? O3 C10 1.424(2) . ? O4 C16 1.295(2) . ? O4 Ni1 2.0038(12) 3_665 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.377(3) . ? C2 C7 1.423(3) . ? C3 C4 1.398(3) . ? C3 H3 0.9500 . ? C4 C5 1.363(3) . ? C4 H4 0.9500 . ? C5 C6 1.412(3) . ? C5 H5 0.9500 . ? C6 C7 1.412(3) . ? C6 C8 1.445(3) . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.370(3) . ? C11 C16 1.428(3) . ? C12 C13 1.404(3) . ? C12 H12 0.9500 . ? C13 C14 1.367(3) . ? C13 H13 0.9500 . ? C14 C15 1.411(3) . ? C14 H14 0.9500 . ? C15 C16 1.413(3) . ? C15 C17 1.443(3) . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.4522 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 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 O4 Ni1 O2 178.54(5) 3_665 . ? O4 Ni1 N5 88.60(6) 3_665 3_665 ? O2 Ni1 N5 92.56(6) . 3_665 ? O4 Ni1 N4 92.46(6) 3_665 . ? O2 Ni1 N4 88.30(6) . . ? N5 Ni1 N4 95.69(6) 3_665 . ? O4 Ni1 N1 86.35(5) 3_665 3_665 ? O2 Ni1 N1 92.36(5) . 3_665 ? N5 Ni1 N1 168.96(6) 3_665 3_665 ? N4 Ni1 N1 94.33(6) . 3_665 ? O4 Ni1 N1 92.58(6) 3_665 . ? O2 Ni1 N1 86.54(5) . . ? N5 Ni1 N1 90.19(6) 3_665 . ? N4 Ni1 N1 172.34(6) . . ? N1 Ni1 N1 80.25(6) 3_665 . ? O4 Ni1 Na1 140.87(4) 3_665 . ? O2 Ni1 Na1 38.24(4) . . ? N5 Ni1 Na1 91.63(5) 3_665 . ? N4 Ni1 Na1 126.37(4) . . ? N1 Ni1 Na1 86.14(5) 3_665 . ? N1 Ni1 Na1 48.30(4) . . ? O4 Ni1 Na1 38.33(4) 3_665 3_665 ? O2 Ni1 Na1 140.35(4) . 3_665 ? N5 Ni1 Na1 126.17(4) 3_665 3_665 ? N4 Ni1 Na1 95.07(5) . 3_665 ? N1 Ni1 Na1 48.02(4) 3_665 3_665 ? N1 Ni1 Na1 85.35(5) . 3_665 ? Na1 Ni1 Na1 122.01(3) . 3_665 ? O2 Na1 O4 94.05(6) . . ? O2 Na1 O1 66.93(5) . . ? O4 Na1 O1 121.81(6) . . ? O2 Na1 N6 121.55(6) . . ? O4 Na1 N6 143.31(6) . . ? O1 Na1 N6 83.73(6) . . ? O2 Na1 O3 129.73(5) . . ? O4 Na1 O3 66.16(5) . . ? O1 Na1 O3 84.62(5) . . ? N6 Na1 O3 93.58(6) . . ? O2 Na1 N1 73.23(5) . . ? O4 Na1 N1 72.13(5) . . ? O1 Na1 N1 138.20(5) . . ? N6 Na1 N1 107.60(6) . . ? O3 Na1 N1 132.66(5) . . ? O2 Na1 C7 20.70(4) . . ? O4 Na1 C7 98.26(5) . . ? O1 Na1 C7 47.80(5) . . ? N6 Na1 C7 118.14(6) . . ? O3 Na1 C7 113.06(5) . . ? N1 Na1 C7 93.77(5) . . ? O2 Na1 Ni1 33.48(3) . . ? O4 Na1 Ni1 82.85(4) . . ? O1 Na1 Ni1 99.59(4) . . ? N6 Na1 Ni1 121.26(5) . . ? O3 Na1 Ni1 145.13(4) . . ? N1 Na1 Ni1 39.75(4) . . ? C7 Na1 Ni1 54.09(4) . . ? O2 Na1 Ni1 82.71(5) . 3_665 ? O4 Na1 Ni1 33.30(3) . 3_665 ? O1 Na1 Ni1 140.61(4) . 3_665 ? N6 Na1 Ni1 135.00(5) . 3_665 ? O3 Na1 Ni1 97.30(4) . 3_665 ? N1 Na1 Ni1 38.84(4) . 3_665 ? C7 Na1 Ni1 97.20(4) . 3_665 ? Ni1 Na1 Ni1 57.99(3) . 3_665 ? N2 N1 Ni1 115.40(12) . 3_665 ? N2 N1 Ni1 114.37(12) . . ? Ni1 N1 Ni1 99.75(6) 3_665 . ? N2 N1 Na1 135.25(12) . . ? Ni1 N1 Na1 93.14(6) 3_665 . ? Ni1 N1 Na1 91.95(6) . . ? N3 N2 N1 179.6(2) . . ? C8 N4 C9 116.23(16) . . ? C8 N4 Ni1 125.66(13) . . ? C9 N4 Ni1 118.11(12) . . ? C17 N5 C18 116.69(14) . . ? C17 N5 Ni1 126.35(12) . 3_665 ? C18 N5 Ni1 116.96(10) . 3_665 ? C19 N6 Na1 163.37(15) . . ? C2 O1 C1 117.13(15) . . ? C2 O1 Na1 113.70(10) . . ? C1 O1 Na1 129.17(12) . . ? C7 O2 Ni1 129.85(11) . . ? C7 O2 Na1 121.45(11) . . ? Ni1 O2 Na1 108.28(6) . . ? C11 O3 C10 117.00(15) . . ? C11 O3 Na1 115.34(11) . . ? C10 O3 Na1 126.95(12) . . ? C16 O4 Ni1 128.33(11) . 3_665 ? C16 O4 Na1 123.02(11) . . ? Ni1 O4 Na1 108.37(6) 3_665 . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 124.42(17) . . ? C3 C2 C7 122.10(18) . . ? O1 C2 C7 113.47(16) . . ? C2 C3 C4 119.91(18) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.55(18) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.53(18) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C7 C6 C5 119.85(17) . . ? C7 C6 C8 122.38(16) . . ? C5 C6 C8 117.43(17) . . ? O2 C7 C6 124.82(16) . . ? O2 C7 C2 118.54(16) . . ? C6 C7 C2 116.64(16) . . ? O2 C7 Na1 37.85(8) . . ? C6 C7 Na1 158.93(12) . . ? C2 C7 Na1 82.21(11) . . ? N4 C8 C6 127.10(17) . . ? N4 C8 H8 116.5 . . ? C6 C8 H8 116.5 . . ? N4 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O3 C10 H10A 109.5 . . ? O3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 O3 124.95(17) . . ? C12 C11 C16 122.26(17) . . ? O3 C11 C16 112.78(16) . . ? C11 C12 C13 120.03(17) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 119.28(18) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 121.73(18) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C14 C15 C16 119.88(17) . . ? C14 C15 C17 117.43(17) . . ? C16 C15 C17 122.67(17) . . ? O4 C16 C15 124.91(16) . . ? O4 C16 C11 118.49(16) . . ? C15 C16 C11 116.58(16) . . ? N5 C17 C15 126.61(17) . . ? N5 C17 H17 116.7 . . ? C15 C17 H17 116.7 . . ? N5 C18 H18A 109.5 . . ? N5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N6 C19 C20 178.29(11) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.263 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.051 _database_code_depnum_ccdc_archive 'CCDC 936647'