# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Hitoshi Miyasaka' 'Rodolphe Clerac' 'Ayumi Saitoh' 'Masahiro Yamashita' _publ_contact_author_name 'Hitoshi Miyasaka' _publ_contact_author_address ; Chemistry Tohoku University 6-3 Aramaki-Aza-Aoba Aoba-ku Sendai Miyagi 980-8578 JAPAN ; _publ_contact_author_email MIYASAKA@AGNUS.CHEM.TOHOKU.AC.JP _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Direct evidence of exchange interaction dependence of magnetization relaxation in a family of ferromagnetic-type single-chain magnets ; #============================================================================== data___Mn_saltmen_ClO4_Ni_miao_ _database_code_depnum_ccdc_archive 'CCDC 629013' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C60 H66 Cl2 Mn2 N12 Ni O14 ' _chemical_formula_moiety 'C60 H66 Cl2 Mn2 N12 Ni O14 ' _chemical_formula_weight 1418.74 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 21.761(10) _cell_length_b 15.819(7) _cell_length_c 17.876(8) _cell_angle_alpha 90.0000 _cell_angle_beta 97.911(5) _cell_angle_gamma 90.0000 _cell_volume 6095(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7768 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 31.0 _cell_measurement_temperature 93.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2936.00 _exptl_absorpt_coefficient_mu 0.878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 0.974 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 27809 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_max 31.07 _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5338 _reflns_number_gt 4179 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.1725 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5332 _refine_ls_number_parameters 451 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.51 _refine_diff_density_min -1.49 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mn Mn 0.337 0.728 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ni(1) Ni 0.5000 0.25808(6) 0.7500 0.0312(2) Uani 1.00 2 d S . . Mn(1) Mn 0.31245(3) 0.20704(4) 0.55580(4) 0.02246(19) Uani 1.00 1 d . . . Cl(1) Cl 0.39244(7) -0.23424(9) 0.65189(8) 0.0442(4) Uani 1.00 1 d . . . O(1) O 0.28556(14) 0.3206(2) 0.53706(18) 0.0257(8) Uani 1.00 1 d . . . O(2) O 0.25622(16) 0.1881(2) 0.62433(19) 0.0328(9) Uani 1.00 1 d . . . O(3) O 0.3884(2) 0.2497(2) 0.6330(3) 0.102(2) Uani 1.00 1 d . . . O(4) O 0.3869(5) -0.1582(4) 0.6187(4) 0.177(3) Uani 1.00 1 d . . . O(5) O 0.3926(3) -0.2258(4) 0.7302(2) 0.117(2) Uani 1.00 1 d . . . O(6) O 0.3464(2) -0.2913(5) 0.6263(3) 0.125(2) Uani 1.00 1 d . . . O(7) O 0.4485(2) -0.2690(4) 0.6333(3) 0.098(2) Uani 1.00 1 d . . . N(1) N 0.36754(16) 0.2139(2) 0.4765(2) 0.0231(10) Uani 1.00 1 d . . . N(2) N 0.33503(16) 0.0861(2) 0.5515(2) 0.0216(9) Uani 1.00 1 d . . . N(3) N 0.4156(3) 0.2548(3) 0.6864(4) 0.106(2) Uani 1.00 1 d . . . N(4) N 0.4491(2) 0.2605(2) 0.8369(2) 0.0421(14) Uani 1.00 1 d . . . N(5) N 0.3580(2) 0.2560(3) 0.8791(2) 0.0448(14) Uani 1.00 1 d . . . N(6) N 0.5000 0.1198(3) 0.7500 0.0302(16) Uani 1.00 2 d S . . N(7) N 0.5000 0.3929(3) 0.7500 0.0334(17) Uani 1.00 2 d S . . C(1) C 0.3244(2) 0.3822(3) 0.5200(2) 0.0288(12) Uani 1.00 1 d . . . C(2) C 0.3135(2) 0.4657(3) 0.5419(3) 0.0329(14) Uani 1.00 1 d . . . C(3) C 0.3492(2) 0.5316(3) 0.5210(3) 0.0382(15) Uani 1.00 1 d . . . C(4) C 0.3970(2) 0.5169(3) 0.4782(3) 0.0445(17) Uani 1.00 1 d . . . C(5) C 0.4088(2) 0.4358(3) 0.4571(3) 0.0420(16) Uani 1.00 1 d . . . C(6) C 0.3734(2) 0.3670(3) 0.4785(3) 0.0309(13) Uani 1.00 1 d . . . C(7) C 0.3882(2) 0.2840(3) 0.4535(3) 0.0303(13) Uani 1.00 1 d . . . C(8) C 0.3824(2) 0.1317(2) 0.4411(2) 0.0252(12) Uani 1.00 1 d . . . C(9) C 0.4443(2) 0.1366(3) 0.4086(3) 0.0332(14) Uani 1.00 1 d . . . C(10) C 0.3302(2) 0.1164(3) 0.3762(2) 0.0326(14) Uani 1.00 1 d . . . C(11) C 0.3852(2) 0.0638(2) 0.5044(2) 0.0237(12) Uani 1.00 1 d . . . C(12) C 0.4458(2) 0.0693(3) 0.5589(2) 0.0292(13) Uani 1.00 1 d . . . C(13) C 0.3770(2) -0.0252(3) 0.4711(2) 0.0301(13) Uani 1.00 1 d . . . C(14) C 0.3155(2) 0.0281(3) 0.5933(2) 0.0265(12) Uani 1.00 1 d . . . C(15) C 0.2722(2) 0.0389(3) 0.6469(2) 0.0255(12) Uani 1.00 1 d . . . C(16) C 0.2577(2) -0.0333(3) 0.6880(3) 0.0344(14) Uani 1.00 1 d . . . C(17) C 0.2171(2) -0.0281(3) 0.7389(3) 0.0373(15) Uani 1.00 1 d . . . C(18) C 0.1894(2) 0.0488(3) 0.7513(3) 0.0377(15) Uani 1.00 1 d . . . C(19) C 0.2027(2) 0.1208(3) 0.7131(3) 0.0389(15) Uani 1.00 1 d . . . C(20) C 0.2444(2) 0.1175(3) 0.6600(2) 0.0296(13) Uani 1.00 1 d . . . C(21) C 0.3591(3) 0.2552(3) 0.7386(3) 0.0464(18) Uani 1.00 1 d . . . C(22) C 0.3880(2) 0.2586(3) 0.8167(3) 0.0400(16) Uani 1.00 1 d . . . C(23) C 0.2924(3) 0.2481(4) 0.8814(4) 0.062(2) Uani 1.00 1 d . . . C(24) C 0.4035(3) 0.2583(3) 0.9405(3) 0.0500(18) Uani 1.00 1 d . . . C(25) C 0.4581(3) 0.2611(3) 0.9137(3) 0.0515(19) Uani 1.00 1 d . . . C(26) C 0.5519(2) 0.0744(3) 0.7469(2) 0.0331(14) Uani 1.00 1 d . . . C(27) C 0.5538(2) -0.0120(3) 0.7482(2) 0.0364(15) Uani 1.00 1 d . . . C(28) C 0.500000(10) -0.0580(4) 0.750000(10) 0.034(2) Uani 1.00 2 d S . . C(29) C 0.4727(2) 0.4371(3) 0.6899(3) 0.0352(14) Uani 1.00 1 d . . . C(30) C 0.4718(2) 0.5240(3) 0.6884(3) 0.0364(14) Uani 1.00 1 d . . . C(31) C 0.500000(10) 0.5686(4) 0.750000(10) 0.037(2) Uani 1.00 2 d S . . H(1) H 0.2812 0.4769 0.5714 0.038 Uiso 1.00 1 c R . . H(2) H 0.3411 0.5877 0.5361 0.045 Uiso 1.00 1 c R . . H(3) H 0.4211 0.5626 0.4637 0.053 Uiso 1.00 1 c R . . H(4) H 0.4412 0.4256 0.4277 0.051 Uiso 1.00 1 c R . . H(5) H 0.4157 0.2808 0.4167 0.036 Uiso 1.00 1 c R . . H(6) H 0.4632 0.0824 0.4111 0.040 Uiso 1.00 1 c R . . H(7) H 0.4711 0.1757 0.4372 0.040 Uiso 1.00 1 c R . . H(8) H 0.4367 0.1547 0.3575 0.040 Uiso 1.00 1 c R . . H(9) H 0.2980 0.0849 0.3942 0.039 Uiso 1.00 1 c R . . H(10) H 0.3142 0.1692 0.3570 0.039 Uiso 1.00 1 c R . . H(11) H 0.3458 0.0857 0.3373 0.039 Uiso 1.00 1 c R . . H(12) H 0.4751 0.0308 0.5435 0.035 Uiso 1.00 1 c R . . H(13) H 0.4617 0.1252 0.5585 0.035 Uiso 1.00 1 c R . . H(14) H 0.4381 0.0554 0.6084 0.035 Uiso 1.00 1 c R . . H(15) H 0.3986 -0.0646 0.5053 0.037 Uiso 1.00 1 c R . . H(16) H 0.3342 -0.0392 0.4630 0.037 Uiso 1.00 1 c R . . H(17) H 0.3932 -0.0272 0.4245 0.037 Uiso 1.00 1 c R . . H(18) H 0.3313 -0.0273 0.5883 0.031 Uiso 1.00 1 c R . . H(19) H 0.2768 -0.0859 0.6799 0.041 Uiso 1.00 1 c R . . H(20) H 0.2076 -0.0769 0.7660 0.045 Uiso 1.00 1 c R . . H(21) H 0.1608 0.0519 0.7867 0.046 Uiso 1.00 1 c R . . H(22) H 0.1835 0.1728 0.7228 0.047 Uiso 1.00 1 c R . . H(23) H 0.3159 0.2536 0.7211 0.058 Uiso 1.00 1 c R . . H(24) H 0.2740 0.2166 0.8389 0.076 Uiso 1.00 1 c R . . H(25) H 0.2742 0.3028 0.8804 0.076 Uiso 1.00 1 c R . . H(26) H 0.2857 0.2198 0.9264 0.075 Uiso 1.00 1 c R . . H(27) H 0.3975 0.2580 0.9922 0.060 Uiso 1.00 1 c R . . H(28) H 0.4974 0.2632 0.9441 0.060 Uiso 1.00 1 c R . . H(29) H 0.5894 0.1041 0.7436 0.040 Uiso 1.00 1 c R . . H(30) H 0.5922 -0.0405 0.7479 0.044 Uiso 1.00 1 c R . . H(31) H 0.5000 -0.1180 0.7500 0.042 Uiso 1.00 2 c R . . H(32) H 0.4533 0.4071 0.6470 0.041 Uiso 1.00 1 c R . . H(33) H 0.4519 0.5532 0.6453 0.043 Uiso 1.00 1 c R . . H(34) H 0.5000 0.6286 0.7500 0.045 Uiso 1.00 2 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0292(4) 0.0235(5) 0.0373(5) 0.0000 -0.0084(4) 0.0000 Mn(1) 0.0241(3) 0.0191(3) 0.0232(3) 0.0050(2) -0.0002(2) 0.0004(3) Cl(1) 0.0628(9) 0.0320(7) 0.0390(7) -0.0069(6) 0.0119(6) -0.0016(6) O(1) 0.0256(16) 0.0205(16) 0.0307(18) 0.0037(13) 0.0026(13) -0.0004(14) O(2) 0.045(2) 0.0255(19) 0.0306(19) 0.0165(15) 0.0151(15) 0.0086(15) O(3) 0.092(3) 0.034(2) 0.151(5) 0.022(2) -0.082(4) -0.029(3) O(4) 0.363(12) 0.073(4) 0.119(5) 0.121(6) 0.121(7) 0.043(4) O(5) 0.196(6) 0.121(5) 0.042(3) -0.106(5) 0.043(3) -0.027(3) O(6) 0.079(3) 0.212(8) 0.092(4) -0.082(4) 0.042(3) -0.087(4) O(7) 0.057(3) 0.129(5) 0.112(5) 0.019(3) 0.028(3) 0.047(4) N(1) 0.0200(18) 0.018(2) 0.031(2) 0.0045(15) 0.0013(16) 0.0025(16) N(2) 0.0183(18) 0.021(2) 0.025(2) 0.0031(15) -0.0008(15) 0.0013(16) N(3) 0.102(4) 0.023(2) 0.157(7) -0.017(3) -0.116(5) 0.023(3) N(4) 0.049(2) 0.023(2) 0.054(3) 0.005(2) 0.009(2) 0.002(2) N(5) 0.059(3) 0.035(2) 0.041(2) 0.006(2) 0.011(2) 0.009(2) N(6) 0.038(3) 0.031(3) 0.019(2) 0.0000 -0.005(2) 0.0000 N(7) 0.035(3) 0.022(3) 0.041(3) 0.0000 -0.002(2) 0.0000 C(1) 0.026(2) 0.018(2) 0.038(2) 0.0010(19) -0.009(2) 0.001(2) C(2) 0.034(2) 0.024(2) 0.038(3) -0.000(2) -0.003(2) -0.003(2) C(3) 0.039(2) 0.025(2) 0.048(3) -0.003(2) -0.006(2) -0.000(2) C(4) 0.044(3) 0.027(3) 0.061(3) -0.009(2) 0.002(2) 0.006(2) C(5) 0.034(2) 0.031(3) 0.061(3) -0.007(2) 0.009(2) 0.005(2) C(6) 0.027(2) 0.024(2) 0.042(3) -0.001(2) 0.002(2) 0.004(2) C(7) 0.022(2) 0.031(2) 0.038(2) 0.003(2) 0.005(2) 0.000(2) C(8) 0.027(2) 0.022(2) 0.027(2) 0.0046(19) 0.0066(19) -0.003(2) C(9) 0.031(2) 0.033(2) 0.037(3) 0.003(2) 0.007(2) -0.000(2) C(10) 0.033(2) 0.035(2) 0.029(2) 0.005(2) 0.004(2) 0.000(2) C(11) 0.022(2) 0.023(2) 0.026(2) 0.0032(18) 0.0027(19) -0.0002(19) C(12) 0.024(2) 0.033(2) 0.031(2) 0.005(2) 0.004(2) 0.002(2) C(13) 0.031(2) 0.029(2) 0.031(2) 0.005(2) 0.010(2) -0.002(2) C(14) 0.025(2) 0.022(2) 0.031(2) 0.0042(19) -0.0007(19) -0.001(2) C(15) 0.025(2) 0.025(2) 0.026(2) 0.0033(19) 0.0014(19) -0.001(2) C(16) 0.032(2) 0.030(2) 0.041(3) -0.000(2) 0.003(2) 0.002(2) C(17) 0.036(2) 0.039(3) 0.038(3) -0.006(2) 0.008(2) 0.010(2) C(18) 0.030(2) 0.052(3) 0.032(3) 0.004(2) 0.011(2) 0.009(2) C(19) 0.042(3) 0.041(3) 0.035(3) 0.014(2) 0.011(2) 0.006(2) C(20) 0.030(2) 0.034(2) 0.024(2) 0.006(2) 0.004(2) 0.004(2) C(21) 0.058(3) 0.048(3) 0.039(3) 0.024(2) 0.028(2) 0.015(2) C(22) 0.050(3) 0.026(2) 0.045(3) 0.007(2) 0.013(2) 0.008(2) C(23) 0.070(4) 0.065(4) 0.053(4) 0.008(3) 0.021(3) 0.015(3) C(24) 0.079(4) 0.032(3) 0.039(3) 0.009(3) 0.008(3) 0.001(2) C(25) 0.063(4) 0.028(3) 0.059(4) 0.011(2) -0.005(3) -0.006(2) C(26) 0.037(2) 0.030(2) 0.032(2) -0.002(2) 0.005(2) 0.000(2) C(27) 0.046(3) 0.029(2) 0.034(2) 0.006(2) 0.006(2) -0.002(2) C(28) 0.048(4) 0.030(4) 0.027(3) 0.0000 0.012(3) 0.0000 C(29) 0.033(2) 0.029(2) 0.042(3) -0.002(2) -0.002(2) 0.001(2) C(30) 0.029(2) 0.031(2) 0.048(3) -0.003(2) 0.001(2) 0.003(2) C(31) 0.032(3) 0.027(4) 0.053(5) 0.0000 0.005(3) 0.0000 #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ni(1) N(3) 2.024(7) yes . . Ni(1) N(3) 2.024(7) yes . 2_656 Ni(1) N(4) 2.029(5) yes . . Ni(1) N(4) 2.029(5) yes . 2_656 Ni(1) N(6) 2.188(6) yes . . Ni(1) N(7) 2.132(5) yes . . Mn(1) O(1) 1.905(3) yes . . Mn(1) O(1) 2.554(2) yes . 7_556 Mn(1) O(2) 1.871(3) yes . . Mn(1) O(3) 2.113(5) yes . . Mn(1) N(1) 1.981(4) yes . . Mn(1) N(2) 1.980(3) yes . . Cl(1) O(4) 1.340(7) yes . . Cl(1) O(5) 1.406(5) yes . . Cl(1) O(6) 1.378(6) yes . . Cl(1) O(7) 1.418(6) yes . . O(1) C(1) 1.351(5) yes . . O(2) C(20) 1.328(6) yes . . O(3) N(3) 1.054(10) yes . . N(1) C(7) 1.285(6) yes . . N(1) C(8) 1.500(6) yes . . N(2) C(11) 1.509(6) yes . . N(2) C(14) 1.292(6) yes . . N(3) C(21) 1.643(10) yes . . N(4) C(22) 1.328(7) yes . . N(4) C(25) 1.361(8) yes . . N(5) C(22) 1.367(8) yes . . N(5) C(23) 1.441(8) yes . . N(5) C(24) 1.375(7) yes . . N(6) C(26) 1.347(6) yes . . N(6) C(26) 1.347(6) yes . 2_656 N(7) C(29) 1.350(6) yes . . N(7) C(29) 1.350(6) yes . 2_656 C(1) C(2) 1.408(7) yes . . C(1) C(6) 1.402(7) yes . . C(2) C(3) 1.383(7) yes . . C(3) C(4) 1.392(8) yes . . C(4) C(5) 1.372(7) yes . . C(5) C(6) 1.416(7) yes . . C(6) C(7) 1.436(7) yes . . C(8) C(9) 1.540(7) yes . . C(8) C(10) 1.527(6) yes . . C(8) C(11) 1.556(6) yes . . C(11) C(12) 1.530(5) yes . . C(11) C(13) 1.529(6) yes . . C(14) C(15) 1.444(7) yes . . C(15) C(16) 1.418(7) yes . . C(15) C(20) 1.416(7) yes . . C(16) C(17) 1.356(7) yes . . C(17) C(18) 1.389(8) yes . . C(18) C(19) 1.378(8) yes . . C(19) C(20) 1.402(7) yes . . C(21) C(22) 1.451(7) yes . . C(24) C(25) 1.340(10) yes . . C(26) C(27) 1.367(7) yes . . C(27) C(28) 1.383(6) yes . . C(29) C(30) 1.375(7) yes . . C(30) C(31) 1.378(6) yes . . C(2) H(1) 0.950(7) no . . C(3) H(2) 0.950(7) no . . C(4) H(3) 0.950(8) no . . C(5) H(4) 0.950(8) no . . C(7) H(5) 0.950(7) no . . C(9) H(6) 0.950 no . . C(9) H(7) 0.950 no . . C(9) H(8) 0.950 no . . C(10) H(9) 0.950 no . . C(10) H(10) 0.950 no . . C(10) H(11) 0.950 no . . C(12) H(12) 0.950 no . . C(12) H(13) 0.950 no . . C(12) H(14) 0.950 no . . C(13) H(15) 0.950 no . . C(13) H(16) 0.950 no . . C(13) H(17) 0.950 no . . C(14) H(18) 0.950(6) no . . C(16) H(19) 0.950(7) no . . C(17) H(20) 0.950(8) no . . C(18) H(21) 0.950(7) no . . C(19) H(22) 0.950(8) no . . C(21) H(23) 0.950(8) no . . C(23) H(24) 0.950 no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(24) H(27) 0.950(9) no . . C(25) H(28) 0.950(9) no . . C(26) H(29) 0.950(7) no . . C(27) H(30) 0.950(7) no . . C(28) H(31) 0.950 no . . C(29) H(32) 0.950(7) no . . C(30) H(33) 0.950(7) no . . C(31) H(34) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(3) Ni(1) N(3) 177.1(2) yes . . 2_656 N(3) Ni(1) N(4) 83.2(2) yes . . . N(3) Ni(1) N(4) 96.9(2) yes . . 2_656 N(3) Ni(1) N(6) 88.55(15) yes . . . N(3) Ni(1) N(7) 91.45(15) yes . . . N(3) Ni(1) N(4) 96.9(2) yes 2_656 . . N(3) Ni(1) N(4) 83.2(2) yes 2_656 . 2_656 N(3) Ni(1) N(6) 88.55(15) yes 2_656 . . N(3) Ni(1) N(7) 91.45(15) yes 2_656 . . N(4) Ni(1) N(4) 177.85(17) yes . . 2_656 N(4) Ni(1) N(6) 91.08(12) yes . . . N(4) Ni(1) N(7) 88.92(12) yes . . . N(4) Ni(1) N(6) 91.08(12) yes 2_656 . . N(4) Ni(1) N(7) 88.92(12) yes 2_656 . . N(6) Ni(1) N(7) 180.0000 yes . . . O(1) Mn(1) O(1) 80.72(11) yes . . 7_556 O(1) Mn(1) O(2) 93.07(14) yes . . . O(1) Mn(1) O(3) 90.42(15) yes . . . O(1) Mn(1) N(1) 91.37(15) yes . . . O(1) Mn(1) N(2) 167.59(14) yes . . . O(1) Mn(1) O(2) 80.51(12) yes 7_556 . . O(1) Mn(1) O(3) 170.99(15) yes 7_556 . . O(1) Mn(1) N(1) 94.46(12) yes 7_556 . . O(1) Mn(1) N(2) 89.90(12) yes 7_556 . . O(2) Mn(1) O(3) 98.4(2) yes . . . O(2) Mn(1) N(1) 172.66(15) yes . . . O(2) Mn(1) N(2) 93.38(15) yes . . . O(3) Mn(1) N(1) 87.4(2) yes . . . O(3) Mn(1) N(2) 99.10(16) yes . . . N(1) Mn(1) N(2) 81.20(15) yes . . . O(4) Cl(1) O(5) 110.1(4) yes . . . O(4) Cl(1) O(6) 115.1(5) yes . . . O(4) Cl(1) O(7) 105.7(5) yes . . . O(5) Cl(1) O(6) 107.1(4) yes . . . O(5) Cl(1) O(7) 112.7(4) yes . . . O(6) Cl(1) O(7) 106.1(4) yes . . . Mn(1) O(1) Mn(1) 99.28(12) yes . . 7_556 Mn(1) O(1) C(1) 122.2(2) yes . . . Mn(1) O(1) C(1) 118.0(2) yes 7_556 . . Mn(1) O(2) C(20) 129.5(3) yes . . . Mn(1) O(3) N(3) 155.1(6) yes . . . Mn(1) N(1) C(7) 123.2(3) yes . . . Mn(1) N(1) C(8) 116.2(2) yes . . . C(7) N(1) C(8) 120.5(4) yes . . . Mn(1) N(2) C(11) 116.8(2) yes . . . Mn(1) N(2) C(14) 124.1(3) yes . . . C(11) N(2) C(14) 118.5(3) yes . . . Ni(1) N(3) O(3) 149.7(7) yes . . . Ni(1) N(3) C(21) 111.9(4) yes . . . O(3) N(3) C(21) 98.3(6) yes . . . Ni(1) N(4) C(22) 115.0(4) yes . . . Ni(1) N(4) C(25) 139.0(4) yes . . . C(22) N(4) C(25) 105.9(5) yes . . . C(22) N(5) C(23) 127.8(5) yes . . . C(22) N(5) C(24) 106.2(5) yes . . . C(23) N(5) C(24) 126.0(5) yes . . . Ni(1) N(6) C(26) 122.2(3) yes . . . Ni(1) N(6) C(26) 122.2(3) yes . . 2_656 C(26) N(6) C(26) 115.6(5) yes . . 2_656 Ni(1) N(7) C(29) 121.2(3) yes . . . Ni(1) N(7) C(29) 121.2(3) yes . . 2_656 C(29) N(7) C(29) 117.5(5) yes . . 2_656 O(1) C(1) C(2) 118.6(4) yes . . . O(1) C(1) C(6) 122.7(4) yes . . . C(2) C(1) C(6) 118.6(4) yes . . . C(1) C(2) C(3) 120.6(4) yes . . . C(2) C(3) C(4) 120.9(5) yes . . . C(3) C(4) C(5) 119.3(5) yes . . . C(4) C(5) C(6) 121.1(5) yes . . . C(1) C(6) C(5) 119.5(4) yes . . . C(1) C(6) C(7) 122.8(4) yes . . . C(5) C(6) C(7) 117.7(4) yes . . . N(1) C(7) C(6) 125.9(4) yes . . . N(1) C(8) C(9) 111.5(3) yes . . . N(1) C(8) C(10) 106.0(3) yes . . . N(1) C(8) C(11) 106.3(3) yes . . . C(9) C(8) C(10) 108.6(4) yes . . . C(9) C(8) C(11) 111.1(3) yes . . . C(10) C(8) C(11) 113.1(3) yes . . . N(2) C(11) C(8) 106.6(3) yes . . . N(2) C(11) C(12) 104.9(3) yes . . . N(2) C(11) C(13) 112.2(3) yes . . . C(8) C(11) C(12) 111.5(3) yes . . . C(8) C(11) C(13) 111.3(3) yes . . . C(12) C(11) C(13) 110.1(3) yes . . . N(2) C(14) C(15) 126.6(4) yes . . . C(14) C(15) C(16) 117.4(4) yes . . . C(14) C(15) C(20) 123.2(4) yes . . . C(16) C(15) C(20) 119.4(4) yes . . . C(15) C(16) C(17) 120.7(4) yes . . . C(16) C(17) C(18) 119.8(5) yes . . . C(17) C(18) C(19) 121.3(5) yes . . . C(18) C(19) C(20) 120.3(5) yes . . . O(2) C(20) C(15) 122.9(4) yes . . . O(2) C(20) C(19) 118.7(4) yes . . . C(15) C(20) C(19) 118.4(4) yes . . . N(3) C(21) C(22) 106.7(5) yes . . . N(4) C(22) N(5) 110.6(4) yes . . . N(4) C(22) C(21) 123.2(5) yes . . . N(5) C(22) C(21) 126.2(5) yes . . . N(5) C(24) C(25) 106.9(5) yes . . . N(4) C(25) C(24) 110.4(5) yes . . . N(6) C(26) C(27) 123.8(5) yes . . . C(26) C(27) C(28) 120.1(5) yes . . . C(27) C(28) C(27) 116.6(6) yes . . 2_656 N(7) C(29) C(30) 122.5(4) yes . . . C(29) C(30) C(31) 119.5(5) yes . . . C(30) C(31) C(30) 118.5(6) yes . . 2_656 C(1) C(2) H(1) 119.7(5) no . . . C(3) C(2) H(1) 119.7(5) no . . . C(2) C(3) H(2) 119.6(6) no . . . C(4) C(3) H(2) 119.6(6) no . . . C(3) C(4) H(3) 120.4(6) no . . . C(5) C(4) H(3) 120.4(7) no . . . C(4) C(5) H(4) 119.5(6) no . . . C(6) C(5) H(4) 119.5(6) no . . . N(1) C(7) H(5) 117.1(5) no . . . C(6) C(7) H(5) 117.1(5) no . . . C(8) C(9) H(6) 109.5 no . . . C(8) C(9) H(7) 109.5 no . . . C(8) C(9) H(8) 109.5 no . . . H(6) C(9) H(7) 109.5 no . . . H(6) C(9) H(8) 109.5 no . . . H(7) C(9) H(8) 109.5 no . . . C(8) C(10) H(9) 109.5 no . . . C(8) C(10) H(10) 109.5 no . . . C(8) C(10) H(11) 109.5 no . . . H(9) C(10) H(10) 109.5 no . . . H(9) C(10) H(11) 109.5 no . . . H(10) C(10) H(11) 109.5 no . . . C(11) C(12) H(12) 109.5 no . . . C(11) C(12) H(13) 109.5 no . . . C(11) C(12) H(14) 109.5 no . . . H(12) C(12) H(13) 109.5 no . . . H(12) C(12) H(14) 109.5 no . . . H(13) C(12) H(14) 109.5 no . . . C(11) C(13) H(15) 109.5 no . . . C(11) C(13) H(16) 109.5 no . . . C(11) C(13) H(17) 109.5 no . . . H(15) C(13) H(16) 109.5 no . . . H(15) C(13) H(17) 109.5 no . . . H(16) C(13) H(17) 109.5 no . . . N(2) C(14) H(18) 116.7(5) no . . . C(15) C(14) H(18) 116.7(5) no . . . C(15) C(16) H(19) 119.6(6) no . . . C(17) C(16) H(19) 119.6(6) no . . . C(16) C(17) H(20) 120.1(6) no . . . C(18) C(17) H(20) 120.1(6) no . . . C(17) C(18) H(21) 119.4(6) no . . . C(19) C(18) H(21) 119.3(6) no . . . C(18) C(19) H(22) 119.8(6) no . . . C(20) C(19) H(22) 119.8(6) no . . . N(3) C(21) H(23) 126.6(6) no . . . C(22) C(21) H(23) 126.6(7) no . . . N(5) C(23) H(24) 109.5 no . . . N(5) C(23) H(25) 109.5 no . . . N(5) C(23) H(26) 109.5 no . . . H(24) C(23) H(25) 109.5 no . . . H(24) C(23) H(26) 109.5 no . . . H(25) C(23) H(26) 109.5 no . . . N(5) C(24) H(27) 126.6(7) no . . . C(25) C(24) H(27) 126.5(7) no . . . N(4) C(25) H(28) 124.8(8) no . . . C(24) C(25) H(28) 124.8(8) no . . . N(6) C(26) H(29) 118.1(6) no . . . C(27) C(26) H(29) 118.1(6) no . . . C(26) C(27) H(30) 119.9(6) no . . . C(28) C(27) H(30) 119.9(6) no . . . C(27) C(28) H(31) 121.7 no . . . C(27) C(28) H(31) 121.7 no 2_656 . . N(7) C(29) H(32) 118.8(5) no . . . C(30) C(29) H(32) 118.8(6) no . . . C(29) C(30) H(33) 120.2(6) no . . . C(31) C(30) H(33) 120.3(6) no . . . C(30) C(31) H(34) 120.7 no . . . C(30) C(31) H(34) 120.7 no 2_656 . . #============================================================================== # Attachment 'CIF_comp_2_CCDC629014.cif' data___Mn_H_PF6-Nimpy _database_code_depnum_ccdc_archive 'CCDC 629014' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C60 H66 F12 Mn2 N12 Ni O6 P2 ' _chemical_formula_moiety 'C60 H66 F12 Mn2 N12 Ni O6 P2 ' _chemical_formula_weight 1509.76 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 21.848(6) _cell_length_b 16.041(4) _cell_length_c 18.444(5) _cell_angle_alpha 90.0000 _cell_angle_beta 98.856(5) _cell_angle_gamma 90.0000 _cell_volume 6387(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10046 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 31.0 _cell_measurement_temperature 93.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3096.00 _exptl_absorpt_coefficient_mu 0.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 0.921 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 28498 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_theta_max 31.11 _diffrn_measured_fraction_theta_max 0.854 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 17 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5564 _reflns_number_gt 3835 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1066 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5563 _refine_ls_number_parameters 469 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + 3.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.19 _refine_diff_density_min -1.01 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mn Mn 0.337 0.728 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ni(1) Ni 1.0000 0.26006(5) 0.2500 0.0255(2) Uani 1.00 2 d S . . Mn(1) Mn 0.81461(3) 0.20826(4) 0.05226(3) 0.01998(16) Uani 1.00 1 d . . . P(1) P 0.88779(5) -0.23357(8) 0.14923(6) 0.0318(3) Uani 1.00 1 d . . . F(1) F 0.91423(14) -0.14481(17) 0.13155(16) 0.0616(9) Uani 1.00 1 d . . . F(2) F 0.83734(12) -0.2236(2) 0.07674(14) 0.0669(10) Uani 1.00 1 d . . . F(3) F 0.93528(11) -0.27566(18) 0.10322(14) 0.0502(8) Uani 1.00 1 d . . . F(4) F 0.86007(16) -0.32208(19) 0.16216(18) 0.0733(11) Uani 1.00 1 d . . . F(5) F 0.93678(13) -0.24192(19) 0.22131(14) 0.0599(9) Uani 1.00 1 d . . . F(6) F 0.84131(12) -0.19101(19) 0.19694(13) 0.0538(9) Uani 1.00 1 d . . . O(1) O 0.78650(11) 0.31992(16) 0.03480(14) 0.0248(7) Uani 1.00 1 d . . . O(2) O 0.76277(11) 0.19017(16) 0.12302(13) 0.0223(7) Uani 1.00 1 d . . . O(3) O 0.89412(12) 0.25101(17) 0.12200(14) 0.0282(8) Uani 1.00 1 d . . . N(1) N 0.86657(13) 0.21473(19) -0.02693(15) 0.0184(8) Uani 1.00 1 d . . . N(2) N 0.83519(13) 0.0885(2) 0.04571(16) 0.0196(8) Uani 1.00 1 d . . . N(3) N 0.90949(14) 0.2575(2) 0.19440(17) 0.0273(9) Uani 1.00 1 d . . . N(4) N 0.95203(15) 0.2631(2) 0.33643(18) 0.0286(10) Uani 1.00 1 d . . . N(5) N 0.85965(15) 0.2590(2) 0.37107(18) 0.0330(10) Uani 1.00 1 d . . . N(6) N 1.0000 0.1257(3) 0.2500 0.0263(13) Uani 1.00 2 d S . . N(7) N 1.0000 0.3922(3) 0.2500 0.0286(14) Uani 1.00 2 d S . . C(1) C 0.82463(18) 0.3810(2) 0.0200(2) 0.0256(11) Uani 1.00 1 d . . . C(2) C 0.81577(19) 0.4624(2) 0.0435(2) 0.0285(11) Uani 1.00 1 d . . . C(3) C 0.8517(2) 0.5279(2) 0.0245(2) 0.0369(13) Uani 1.00 1 d . . . C(4) C 0.8975(2) 0.5140(2) -0.0183(2) 0.0415(14) Uani 1.00 1 d . . . C(5) C 0.9079(2) 0.4340(2) -0.0419(2) 0.0358(13) Uani 1.00 1 d . . . C(6) C 0.87265(18) 0.3667(2) -0.0222(2) 0.0264(11) Uani 1.00 1 d . . . C(7) C 0.88622(17) 0.2853(2) -0.0487(2) 0.0255(11) Uani 1.00 1 d . . . C(8) C 0.88100(17) 0.1343(2) -0.0614(2) 0.0230(11) Uani 1.00 1 d . . . C(9) C 0.82688(18) 0.1184(2) -0.1238(2) 0.0284(11) Uani 1.00 1 d . . . C(10) C 0.94112(18) 0.1391(2) -0.0943(2) 0.0282(11) Uani 1.00 1 d . . . C(11) C 0.88509(17) 0.0674(2) 0.0000(2) 0.0218(10) Uani 1.00 1 d . . . C(12) C 0.87744(19) -0.0211(2) -0.0316(2) 0.0277(11) Uani 1.00 1 d . . . C(13) C 0.94624(16) 0.0733(2) 0.0539(2) 0.0265(11) Uani 1.00 1 d . . . C(14) C 0.81471(17) 0.0308(2) 0.0849(2) 0.0254(11) Uani 1.00 1 d . . . C(15) C 0.77264(18) 0.0418(2) 0.1369(2) 0.0254(11) Uani 1.00 1 d . . . C(16) C 0.7550(2) -0.0300(2) 0.1725(2) 0.0419(14) Uani 1.00 1 d . . . C(17) C 0.7148(2) -0.0271(3) 0.2223(2) 0.0450(14) Uani 1.00 1 d . . . C(18) C 0.6915(2) 0.0505(2) 0.2391(2) 0.0360(13) Uani 1.00 1 d . . . C(19) C 0.70787(18) 0.1221(2) 0.2054(2) 0.0296(12) Uani 1.00 1 d . . . C(20) C 0.74838(17) 0.1196(2) 0.1538(2) 0.0213(10) Uani 1.00 1 d . . . C(21) C 0.86637(19) 0.2618(2) 0.2363(2) 0.0277(11) Uani 1.00 1 d . . . C(22) C 0.89121(18) 0.2625(2) 0.3132(2) 0.0274(11) Uani 1.00 1 d . . . C(23) C 0.7934(2) 0.2489(3) 0.3692(2) 0.0509(16) Uani 1.00 1 d . . . C(24) C 0.9030(2) 0.2588(2) 0.4343(2) 0.0361(13) Uani 1.00 1 d . . . C(25) C 0.9593(2) 0.2626(2) 0.4111(2) 0.0322(12) Uani 1.00 1 d . . . C(26) C 0.94776(19) 0.0802(2) 0.2524(2) 0.0295(12) Uani 1.00 1 d . . . C(27) C 0.9459(2) -0.0047(2) 0.2520(2) 0.0313(12) Uani 1.00 1 d . . . C(28) C 1.000000(10) -0.0493(3) 0.250000(10) 0.0307(17) Uani 1.00 2 d S . . C(29) C 1.02667(19) 0.4357(2) 0.3089(2) 0.0332(12) Uani 1.00 1 d . . . C(30) C 1.02755(19) 0.5224(2) 0.3106(2) 0.0381(13) Uani 1.00 1 d . . . C(31) C 1.000000(10) 0.5660(4) 0.250000(10) 0.040(2) Uani 1.00 2 d S . . H(1) H 0.7846 0.4731 0.0729 0.034 Uiso 1.00 1 c R . . H(2) H 0.8448 0.5826 0.0411 0.044 Uiso 1.00 1 c R . . H(3) H 0.9216 0.5592 -0.0315 0.049 Uiso 1.00 1 c R . . H(4) H 0.9391 0.4245 -0.0717 0.043 Uiso 1.00 1 c R . . H(5) H 0.9120 0.2831 -0.0857 0.031 Uiso 1.00 1 c R . . H(6) H 0.7955 0.0873 -0.1055 0.035 Uiso 1.00 1 c R . . H(7) H 0.8103 0.1702 -0.1426 0.035 Uiso 1.00 1 c R . . H(8) H 0.8414 0.0878 -0.1619 0.035 Uiso 1.00 1 c R . . H(9) H 0.9321 0.1575 -0.1438 0.035 Uiso 1.00 1 c R . . H(10) H 0.9687 0.1774 -0.0668 0.035 Uiso 1.00 1 c R . . H(11) H 0.9598 0.0856 -0.0928 0.035 Uiso 1.00 1 c R . . H(12) H 0.8999 -0.0592 0.0018 0.034 Uiso 1.00 1 c R . . H(13) H 0.8929 -0.0230 -0.0770 0.034 Uiso 1.00 1 c R . . H(14) H 0.8348 -0.0357 -0.0393 0.034 Uiso 1.00 1 c R . . H(15) H 0.9390 0.0594 0.1019 0.032 Uiso 1.00 1 c R . . H(16) H 0.9619 0.1286 0.0538 0.032 Uiso 1.00 1 c R . . H(17) H 0.9756 0.0357 0.0392 0.033 Uiso 1.00 1 c R . . H(18) H 0.8289 -0.0243 0.0787 0.031 Uiso 1.00 1 c R . . H(19) H 0.7716 -0.0824 0.1614 0.053 Uiso 1.00 1 c R . . H(20) H 0.7030 -0.0765 0.2450 0.057 Uiso 1.00 1 c R . . H(21) H 0.6641 0.0540 0.2742 0.045 Uiso 1.00 1 c R . . H(22) H 0.6912 0.1741 0.2175 0.037 Uiso 1.00 1 c R . . H(23) H 0.8233 0.2641 0.2180 0.034 Uiso 1.00 1 c R . . H(24) H 0.7768 0.2174 0.3272 0.064 Uiso 1.00 1 c R . . H(25) H 0.7860 0.2205 0.4122 0.064 Uiso 1.00 1 c R . . H(26) H 0.7742 0.3021 0.3671 0.064 Uiso 1.00 1 c R . . H(27) H 0.8952 0.2565 0.4835 0.044 Uiso 1.00 1 c R . . H(28) H 0.9981 0.2647 0.4425 0.038 Uiso 1.00 1 c R . . H(29) H 0.9103 0.1095 0.2544 0.035 Uiso 1.00 1 c R . . H(30) H 0.9079 -0.0330 0.2531 0.038 Uiso 1.00 1 c R . . H(31) H 1.0000 -0.1085 0.2500 0.037 Uiso 1.00 2 c R . . H(32) H 1.0456 0.4061 0.3510 0.040 Uiso 1.00 1 c R . . H(33) H 1.0469 0.5512 0.3530 0.045 Uiso 1.00 1 c R . . H(34) H 1.0000 0.6252 0.2500 0.048 Uiso 1.00 2 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0204(3) 0.0222(4) 0.0340(4) 0.0000 0.0047(3) 0.0000 Mn(1) 0.0213(3) 0.0166(3) 0.0236(3) 0.0047(2) 0.0083(2) 0.0023(2) P(1) 0.0325(6) 0.0298(6) 0.0349(6) -0.0009(5) 0.0109(5) 0.0012(5) F(1) 0.070(2) 0.0349(17) 0.079(2) -0.0063(15) 0.0072(16) 0.0140(15) F(2) 0.0342(14) 0.127(3) 0.0400(16) 0.0010(17) 0.0081(12) -0.0080(17) F(3) 0.0434(15) 0.057(2) 0.0564(17) 0.0088(13) 0.0262(13) 0.0063(14) F(4) 0.101(2) 0.0441(19) 0.089(2) -0.0372(17) 0.0575(19) -0.0188(16) F(5) 0.0687(19) 0.061(2) 0.0434(16) 0.0222(16) -0.0127(14) 0.0012(14) F(6) 0.0595(17) 0.065(2) 0.0391(15) 0.0212(15) 0.0148(13) -0.0084(13) O(1) 0.0258(14) 0.0182(15) 0.0323(15) 0.0037(11) 0.0113(11) 0.0023(12) O(2) 0.0247(13) 0.0183(15) 0.0257(14) 0.0041(11) 0.0094(11) 0.0020(11) O(3) 0.0297(15) 0.0299(17) 0.0246(15) 0.0006(13) 0.0024(11) -0.0045(12) N(1) 0.0167(15) 0.0191(18) 0.0189(16) 0.0018(14) 0.0008(12) 0.0003(13) N(2) 0.0192(16) 0.0191(18) 0.0214(17) 0.0056(14) 0.0057(13) -0.0028(14) N(3) 0.0272(18) 0.026(2) 0.028(2) -0.0007(15) 0.0025(15) -0.0035(15) N(4) 0.0326(19) 0.023(2) 0.032(2) 0.0029(15) 0.0088(15) -0.0037(15) N(5) 0.0355(19) 0.033(2) 0.032(2) 0.0066(17) 0.0108(16) -0.0010(16) N(6) 0.022(2) 0.030(3) 0.028(2) 0.0000 0.005(2) 0.0000 N(7) 0.023(2) 0.026(2) 0.037(3) 0.0000 0.005(2) 0.0000 C(1) 0.024(2) 0.020(2) 0.031(2) 0.0019(18) -0.0015(17) 0.0003(18) C(2) 0.027(2) 0.026(2) 0.032(2) 0.0012(19) 0.0015(17) -0.0016(19) C(3) 0.038(2) 0.023(2) 0.048(2) 0.001(2) 0.001(2) -0.004(2) C(4) 0.040(2) 0.023(2) 0.061(3) -0.009(2) 0.003(2) 0.006(2) C(5) 0.036(2) 0.030(2) 0.043(2) -0.005(2) 0.010(2) 0.005(2) C(6) 0.028(2) 0.020(2) 0.032(2) -0.0016(18) 0.0065(18) 0.0026(18) C(7) 0.020(2) 0.031(2) 0.025(2) -0.0011(18) 0.0035(16) -0.0008(18) C(8) 0.023(2) 0.019(2) 0.029(2) 0.0013(17) 0.0128(17) -0.0041(17) C(9) 0.030(2) 0.030(2) 0.027(2) 0.0026(19) 0.0086(17) -0.0013(18) C(10) 0.028(2) 0.030(2) 0.029(2) 0.0035(19) 0.0109(17) -0.0028(19) C(11) 0.020(2) 0.022(2) 0.025(2) 0.0050(16) 0.0064(16) -0.0025(17) C(12) 0.033(2) 0.022(2) 0.031(2) 0.0055(19) 0.0103(18) -0.0011(18) C(13) 0.022(2) 0.028(2) 0.029(2) 0.0075(18) 0.0060(17) -0.0009(18) C(14) 0.027(2) 0.017(2) 0.034(2) 0.0033(18) 0.0082(18) -0.0007(18) C(15) 0.030(2) 0.018(2) 0.031(2) 0.0040(18) 0.0129(17) 0.0013(18) C(16) 0.055(2) 0.021(2) 0.057(3) 0.005(2) 0.028(2) 0.003(2) C(17) 0.055(3) 0.028(2) 0.060(3) -0.004(2) 0.033(2) 0.011(2) C(18) 0.040(2) 0.035(2) 0.037(2) -0.004(2) 0.020(2) 0.002(2) C(19) 0.033(2) 0.026(2) 0.032(2) 0.0023(19) 0.0149(19) -0.0014(18) C(20) 0.022(2) 0.018(2) 0.024(2) -0.0001(17) 0.0059(16) 0.0029(17) C(21) 0.031(2) 0.023(2) 0.031(2) 0.0019(18) 0.0102(18) 0.0010(18) C(22) 0.024(2) 0.023(2) 0.036(2) 0.0028(18) 0.0078(18) -0.0023(19) C(23) 0.038(2) 0.065(3) 0.055(3) 0.009(2) 0.024(2) 0.006(2) C(24) 0.044(2) 0.038(2) 0.027(2) 0.007(2) 0.010(2) 0.001(2) C(25) 0.044(2) 0.025(2) 0.026(2) 0.006(2) 0.0007(19) -0.0049(18) C(26) 0.027(2) 0.028(2) 0.034(2) 0.0004(19) 0.0049(18) 0.0019(19) C(27) 0.036(2) 0.027(2) 0.032(2) -0.008(2) 0.0092(19) 0.0012(19) C(28) 0.043(3) 0.025(3) 0.025(3) 0.0000 0.007(2) 0.0000 C(29) 0.032(2) 0.026(2) 0.042(2) 0.0041(19) 0.007(2) -0.001(2) C(30) 0.031(2) 0.029(2) 0.053(3) 0.001(2) 0.003(2) -0.004(2) C(31) 0.029(3) 0.032(4) 0.059(4) 0.0000 0.008(3) 0.0000 #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ni(1) N(3) 2.083(2) yes . . Ni(1) N(3) 2.083(2) yes . 2_755 Ni(1) N(4) 2.039(3) yes . . Ni(1) N(4) 2.039(3) yes . 2_755 Ni(1) N(6) 2.155(4) yes . . Ni(1) N(7) 2.119(5) yes . . Mn(1) O(1) 1.905(2) yes . . Mn(1) O(2) 1.878(2) yes . . Mn(1) O(3) 2.111(2) yes . . Mn(1) N(1) 1.986(3) yes . . Mn(1) N(2) 1.981(3) yes . . P(1) F(1) 1.589(3) yes . . P(1) F(2) 1.604(2) yes . . P(1) F(3) 1.589(2) yes . . P(1) F(4) 1.576(3) yes . . P(1) F(5) 1.579(2) yes . . P(1) F(6) 1.596(3) yes . . O(1) C(1) 1.340(4) yes . . O(2) C(20) 1.325(4) yes . . O(3) N(3) 1.330(3) yes . . N(1) C(7) 1.296(5) yes . . N(1) C(8) 1.494(4) yes . . N(2) C(11) 1.515(5) yes . . N(2) C(14) 1.295(5) yes . . N(3) C(21) 1.310(5) yes . . N(4) C(22) 1.332(4) yes . . N(4) C(25) 1.362(5) yes . . N(5) C(22) 1.358(5) yes . . N(5) C(23) 1.451(5) yes . . N(5) C(24) 1.385(4) yes . . N(6) C(26) 1.361(4) yes . . N(6) C(26) 1.361(4) yes . 2_755 N(7) C(29) 1.347(4) yes . . N(7) C(29) 1.347(4) yes . 2_755 C(1) C(2) 1.399(5) yes . . C(1) C(6) 1.419(6) yes . . C(2) C(3) 1.387(6) yes . . C(3) C(4) 1.385(6) yes . . C(4) C(5) 1.386(6) yes . . C(5) C(6) 1.406(6) yes . . C(6) C(7) 1.441(5) yes . . C(8) C(9) 1.539(5) yes . . C(8) C(10) 1.531(5) yes . . C(8) C(11) 1.553(5) yes . . C(11) C(12) 1.533(5) yes . . C(11) C(13) 1.540(4) yes . . C(14) C(15) 1.438(5) yes . . C(15) C(16) 1.408(6) yes . . C(15) C(20) 1.410(5) yes . . C(16) C(17) 1.365(7) yes . . C(17) C(18) 1.397(6) yes . . C(18) C(19) 1.379(6) yes . . C(19) C(20) 1.396(5) yes . . C(21) C(22) 1.438(5) yes . . C(24) C(25) 1.365(6) yes . . C(26) C(27) 1.362(6) yes . . C(27) C(28) 1.388(5) yes . . C(29) C(30) 1.391(6) yes . . C(30) C(31) 1.375(5) yes . . C(2) H(1) 0.950(6) no . . C(3) H(2) 0.950(6) no . . C(4) H(3) 0.950(6) no . . C(5) H(4) 0.950(6) no . . C(7) H(5) 0.950(5) no . . C(9) H(6) 0.950 no . . C(9) H(7) 0.950 no . . C(9) H(8) 0.950 no . . C(10) H(9) 0.950 no . . C(10) H(10) 0.950 no . . C(10) H(11) 0.950 no . . C(12) H(12) 0.950 no . . C(12) H(13) 0.950 no . . C(12) H(14) 0.950 no . . C(13) H(15) 0.950 no . . C(13) H(16) 0.950 no . . C(13) H(17) 0.950 no . . C(14) H(18) 0.950(5) no . . C(16) H(19) 0.950(6) no . . C(17) H(20) 0.950(6) no . . C(18) H(21) 0.950(6) no . . C(19) H(22) 0.950(6) no . . C(21) H(23) 0.950 no . . C(23) H(24) 0.950 no . . C(23) H(25) 0.950 no . . C(23) H(26) 0.950 no . . C(24) H(27) 0.950(6) no . . C(25) H(28) 0.950(5) no . . C(26) H(29) 0.950 no . . C(27) H(30) 0.950 no . . C(28) H(31) 0.950 no . . C(29) H(32) 0.950 no . . C(30) H(33) 0.950 no . . C(31) H(34) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(3) Ni(1) N(3) 177.74(13) yes . . 2_755 N(3) Ni(1) N(4) 79.75(12) yes . . . N(3) Ni(1) N(4) 100.30(12) yes . . 2_755 N(3) Ni(1) N(6) 88.87(9) yes . . . N(3) Ni(1) N(7) 91.13(9) yes . . . N(3) Ni(1) N(4) 100.30(12) yes 2_755 . . N(3) Ni(1) N(4) 79.75(12) yes 2_755 . 2_755 N(3) Ni(1) N(6) 88.87(9) yes 2_755 . . N(3) Ni(1) N(7) 91.13(9) yes 2_755 . . N(4) Ni(1) N(4) 177.29(14) yes . . 2_755 N(4) Ni(1) N(6) 91.35(9) yes . . . N(4) Ni(1) N(7) 88.65(9) yes . . . N(4) Ni(1) N(6) 91.35(9) yes 2_755 . . N(4) Ni(1) N(7) 88.65(9) yes 2_755 . . N(6) Ni(1) N(7) 180(254) yes . . . O(1) Mn(1) O(2) 92.84(11) yes . . . O(1) Mn(1) O(3) 90.64(10) yes . . . O(1) Mn(1) N(1) 91.86(12) yes . . . O(1) Mn(1) N(2) 166.39(11) yes . . . O(2) Mn(1) O(3) 98.89(10) yes . . . O(2) Mn(1) N(1) 173.54(12) yes . . . O(2) Mn(1) N(2) 93.40(12) yes . . . O(3) Mn(1) N(1) 85.48(11) yes . . . O(3) Mn(1) N(2) 100.31(10) yes . . . N(1) Mn(1) N(2) 81.09(12) yes . . . F(1) P(1) F(2) 87.98(17) yes . . . F(1) P(1) F(3) 89.04(16) yes . . . F(1) P(1) F(4) 176.85(17) yes . . . F(1) P(1) F(5) 91.61(15) yes . . . F(1) P(1) F(6) 90.70(16) yes . . . F(2) P(1) F(3) 91.06(14) yes . . . F(2) P(1) F(4) 89.14(17) yes . . . F(2) P(1) F(5) 178.86(18) yes . . . F(2) P(1) F(6) 90.18(14) yes . . . F(3) P(1) F(4) 89.76(17) yes . . . F(3) P(1) F(5) 89.99(14) yes . . . F(3) P(1) F(6) 178.72(13) yes . . . F(4) P(1) F(5) 91.30(16) yes . . . F(4) P(1) F(6) 90.57(17) yes . . . F(5) P(1) F(6) 88.76(14) yes . . . Mn(1) O(1) C(1) 121.8(2) yes . . . Mn(1) O(2) C(20) 129.7(2) yes . . . Mn(1) O(3) N(3) 134.0(2) yes . . . Mn(1) N(1) C(7) 121.9(2) yes . . . Mn(1) N(1) C(8) 116.7(2) yes . . . C(7) N(1) C(8) 121.4(3) yes . . . Mn(1) N(2) C(11) 116.1(2) yes . . . Mn(1) N(2) C(14) 123.8(2) yes . . . C(11) N(2) C(14) 119.4(3) yes . . . Ni(1) N(3) O(3) 124.7(2) yes . . . Ni(1) N(3) C(21) 115.0(2) yes . . . O(3) N(3) C(21) 120.3(2) yes . . . Ni(1) N(4) C(22) 110.9(2) yes . . . Ni(1) N(4) C(25) 142.8(2) yes . . . C(22) N(4) C(25) 106.3(3) yes . . . C(22) N(5) C(23) 127.7(3) yes . . . C(22) N(5) C(24) 107.3(3) yes . . . C(23) N(5) C(24) 124.7(3) yes . . . Ni(1) N(6) C(26) 122.4(2) yes . . . Ni(1) N(6) C(26) 122.4(2) yes . . 2_755 C(26) N(6) C(26) 115.2(4) yes . . 2_755 Ni(1) N(7) C(29) 121.3(2) yes . . . Ni(1) N(7) C(29) 121.3(2) yes . . 2_755 C(29) N(7) C(29) 117.5(4) yes . . 2_755 O(1) C(1) C(2) 120.0(3) yes . . . O(1) C(1) C(6) 121.9(3) yes . . . C(2) C(1) C(6) 118.0(3) yes . . . C(1) C(2) C(3) 121.3(4) yes . . . C(2) C(3) C(4) 120.6(4) yes . . . C(3) C(4) C(5) 119.7(4) yes . . . C(4) C(5) C(6) 120.5(4) yes . . . C(1) C(6) C(5) 119.9(3) yes . . . C(1) C(6) C(7) 122.8(3) yes . . . C(5) C(6) C(7) 117.3(3) yes . . . N(1) C(7) C(6) 126.2(3) yes . . . N(1) C(8) C(9) 105.8(2) yes . . . N(1) C(8) C(10) 112.0(3) yes . . . N(1) C(8) C(11) 106.2(3) yes . . . C(9) C(8) C(10) 108.6(3) yes . . . C(9) C(8) C(11) 112.5(3) yes . . . C(10) C(8) C(11) 111.6(3) yes . . . N(2) C(11) C(8) 106.6(2) yes . . . N(2) C(11) C(12) 111.9(3) yes . . . N(2) C(11) C(13) 104.8(2) yes . . . C(8) C(11) C(12) 111.7(3) yes . . . C(8) C(11) C(13) 112.0(3) yes . . . C(12) C(11) C(13) 109.6(3) yes . . . N(2) C(14) C(15) 126.6(3) yes . . . C(14) C(15) C(16) 117.4(3) yes . . . C(14) C(15) C(20) 123.8(3) yes . . . C(16) C(15) C(20) 118.8(3) yes . . . C(15) C(16) C(17) 122.4(4) yes . . . C(16) C(17) C(18) 118.3(4) yes . . . C(17) C(18) C(19) 120.9(4) yes . . . C(18) C(19) C(20) 121.3(3) yes . . . O(2) C(20) C(15) 122.6(3) yes . . . O(2) C(20) C(19) 119.0(3) yes . . . C(15) C(20) C(19) 118.4(3) yes . . . N(3) C(21) C(22) 112.7(3) yes . . . N(4) C(22) N(5) 110.5(3) yes . . . N(4) C(22) C(21) 121.5(3) yes . . . N(5) C(22) C(21) 127.9(3) yes . . . N(5) C(24) C(25) 105.6(3) yes . . . N(4) C(25) C(24) 110.3(3) yes . . . N(6) C(26) C(27) 124.1(4) yes . . . C(26) C(27) C(28) 119.4(4) yes . . . C(27) C(28) C(27) 117.9(5) yes . . 2_755 N(7) C(29) C(30) 122.6(3) yes . . . C(29) C(30) C(31) 119.1(4) yes . . . C(30) C(31) C(30) 119.0(5) yes . . 2_755 C(1) C(2) H(1) 119.4(4) no . . . C(3) C(2) H(1) 119.4(4) no . . . C(2) C(3) H(2) 119.7(5) no . . . C(4) C(3) H(2) 119.7(5) no . . . C(3) C(4) H(3) 120.1(5) no . . . C(5) C(4) H(3) 120.2(5) no . . . C(4) C(5) H(4) 119.8(5) no . . . C(6) C(5) H(4) 119.8(5) no . . . N(1) C(7) H(5) 116.9(4) no . . . C(6) C(7) H(5) 116.9(4) no . . . C(8) C(9) H(6) 109.5 no . . . C(8) C(9) H(7) 109.5 no . . . C(8) C(9) H(8) 109.5 no . . . H(6) C(9) H(7) 109.5 no . . . H(6) C(9) H(8) 109.5 no . . . H(7) C(9) H(8) 109.5 no . . . C(8) C(10) H(9) 109.5 no . . . C(8) C(10) H(10) 109.5 no . . . C(8) C(10) H(11) 109.5 no . . . H(9) C(10) H(10) 109.5 no . . . H(9) C(10) H(11) 109.5 no . . . H(10) C(10) H(11) 109.5 no . . . C(11) C(12) H(12) 109.5 no . . . C(11) C(12) H(13) 109.5 no . . . C(11) C(12) H(14) 109.5 no . . . H(12) C(12) H(13) 109.5 no . . . H(12) C(12) H(14) 109.5 no . . . H(13) C(12) H(14) 109.5 no . . . C(11) C(13) H(15) 109.5 no . . . C(11) C(13) H(16) 109.5 no . . . C(11) C(13) H(17) 109.5 no . . . H(15) C(13) H(16) 109.5 no . . . H(15) C(13) H(17) 109.5 no . . . H(16) C(13) H(17) 109.5 no . . . N(2) C(14) H(18) 116.7(4) no . . . C(15) C(14) H(18) 116.7(4) no . . . C(15) C(16) H(19) 118.8(5) no . . . C(17) C(16) H(19) 118.8(5) no . . . C(16) C(17) H(20) 120.8(5) no . . . C(18) C(17) H(20) 120.8(5) no . . . C(17) C(18) H(21) 119.6(5) no . . . C(19) C(18) H(21) 119.6(5) no . . . C(18) C(19) H(22) 119.4(4) no . . . C(20) C(19) H(22) 119.4(4) no . . . N(3) C(21) H(23) 123.6 no . . . C(22) C(21) H(23) 123.6 no . . . N(5) C(23) H(24) 109.5 no . . . N(5) C(23) H(25) 109.5 no . . . N(5) C(23) H(26) 109.5 no . . . H(24) C(23) H(25) 109.5 no . . . H(24) C(23) H(26) 109.5 no . . . H(25) C(23) H(26) 109.5 no . . . N(5) C(24) H(27) 127.2(5) no . . . C(25) C(24) H(27) 127.2(4) no . . . N(4) C(25) H(28) 124.9(5) no . . . C(24) C(25) H(28) 124.9(4) no . . . N(6) C(26) H(29) 118.0 no . . . C(27) C(26) H(29) 118.0 no . . . C(26) C(27) H(30) 120.3 no . . . C(28) C(27) H(30) 120.3 no . . . C(27) C(28) H(31) 121.0 no . . . C(27) C(28) H(31) 121.0 no 2_755 . . N(7) C(29) H(32) 118.7 no . . . C(30) C(29) H(32) 118.7 no . . . C(29) C(30) H(33) 120.4 no . . . C(31) C(30) H(33) 120.4 no . . . C(30) C(31) H(34) 120.5 no . . . C(30) C(31) H(34) 120.5 no 2_755 . . # Attachment 'CIF_comp_3_CCDC629015.cif' data___Mn_H_ClO4-Ni_eiao_py _database_code_depnum_ccdc_archive 'CCDC 629015' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C62 H70 Cl2 Mn2 N12 Ni O14 ' _chemical_formula_moiety 'C62 H70 Cl2 Mn2 N12 Ni O14 ' _chemical_formula_weight 1446.79 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 21.992(10) _cell_length_b 16.141(7) _cell_length_c 17.831(8) _cell_angle_alpha 90.0000 _cell_angle_beta 98.103(5) _cell_angle_gamma 90.0000 _cell_volume 6266(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8736 _cell_measurement_theta_min 6.3 _cell_measurement_theta_max 31.0 _cell_measurement_temperature 93.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3000.00 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.910 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 27994 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_max 31.06 _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5427 _reflns_number_gt 3532 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1296 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5424 _refine_ls_number_parameters 462 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + 2.5000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0015 _refine_diff_density_max 1.71 _refine_diff_density_min -1.07 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mn Mn 0.337 0.728 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ni(1) Ni 1.0000 0.23199(6) 0.2500 0.0291(2) Uani 1.00 2 d S . . Mn(1) Mn 1.18599(3) 0.28806(4) 0.44395(4) 0.02104(19) Uani 1.00 1 d . . . Cl(1) Cl 1.10961(7) 0.71731(9) 0.34243(8) 0.0429(4) Uani 1.00 1 d . . . O(1) O 1.21538(14) 0.17849(18) 0.46779(16) 0.0238(8) Uani 1.00 1 d . . . O(2) O 1.23691(14) 0.30196(19) 0.36915(16) 0.0255(8) Uani 1.00 1 d . . . O(3) O 1.10750(15) 0.2401(2) 0.37529(18) 0.0334(10) Uani 1.00 1 d . . . O(4) O 1.1646(3) 0.6781(4) 0.3666(10) 0.280(6) Uani 1.00 1 d . . . O(5) O 1.0746(3) 0.6660(4) 0.3752(3) 0.131(2) Uani 1.00 1 d . . . O(6) O 1.1063(6) 0.7156(5) 0.2688(3) 0.237(5) Uani 1.00 1 d . . . O(7) O 1.1195(2) 0.7971(2) 0.3724(2) 0.0642(14) Uani 1.00 1 d . . . N(1) N 1.13456(16) 0.2853(2) 0.52699(19) 0.0195(10) Uani 1.00 1 d . . . N(2) N 1.16363(17) 0.4077(2) 0.4439(2) 0.0210(10) Uani 1.00 1 d . . . N(3) N 1.0908(2) 0.2335(2) 0.3024(2) 0.0333(12) Uani 1.00 1 d . . . N(4) N 1.04518(19) 0.2286(2) 0.1577(2) 0.0320(12) Uani 1.00 1 d . . . N(5) N 1.1353(2) 0.2238(2) 0.1155(2) 0.0339(12) Uani 1.00 1 d . . . N(6) N 1.0000 0.0993(3) 0.2500 0.0361(18) Uani 1.00 2 d S . . N(7) N 1.0000 0.3653(3) 0.2500 0.0256(16) Uani 1.00 2 d S . . C(1) C 1.1772(2) 0.1192(2) 0.4865(2) 0.0259(13) Uani 1.00 1 d . . . C(2) C 1.1861(2) 0.0370(2) 0.4638(2) 0.0288(14) Uani 1.00 1 d . . . C(3) C 1.1492(2) -0.0263(3) 0.4851(3) 0.0365(15) Uani 1.00 1 d . . . C(4) C 1.1035(2) -0.0104(3) 0.5301(3) 0.0423(17) Uani 1.00 1 d . . . C(5) C 1.0949(2) 0.0698(3) 0.5518(3) 0.0364(15) Uani 1.00 1 d . . . C(6) C 1.1300(2) 0.1351(2) 0.5296(2) 0.0266(13) Uani 1.00 1 d . . . C(7) C 1.1161(2) 0.2178(3) 0.5537(2) 0.0269(13) Uani 1.00 1 d . . . C(8) C 1.1190(2) 0.3679(2) 0.5587(2) 0.0231(12) Uani 1.00 1 d . . . C(9) C 1.0596(2) 0.3642(3) 0.5931(2) 0.0293(14) Uani 1.00 1 d . . . C(10) C 1.1728(2) 0.3874(3) 0.6212(2) 0.0298(14) Uani 1.00 1 d . . . C(11) C 1.1144(2) 0.4302(2) 0.4913(2) 0.0223(12) Uani 1.00 1 d . . . C(12) C 1.0532(2) 0.4215(3) 0.4388(2) 0.0280(13) Uani 1.00 1 d . . . C(13) C 1.1212(2) 0.5192(2) 0.5200(2) 0.0309(14) Uani 1.00 1 d . . . C(14) C 1.1835(2) 0.4621(3) 0.4005(2) 0.0250(13) Uani 1.00 1 d . . . C(15) C 1.2261(2) 0.4490(2) 0.3473(2) 0.0229(12) Uani 1.00 1 d . . . C(16) C 1.2432(2) 0.5183(3) 0.3069(2) 0.0321(14) Uani 1.00 1 d . . . C(17) C 1.2841(2) 0.5110(3) 0.2557(2) 0.0326(15) Uani 1.00 1 d . . . C(18) C 1.3083(2) 0.4339(3) 0.2428(2) 0.0372(16) Uani 1.00 1 d . . . C(19) C 1.2923(2) 0.3646(3) 0.2813(2) 0.0320(14) Uani 1.00 1 d . . . C(20) C 1.2507(2) 0.3704(2) 0.3341(2) 0.0246(13) Uani 1.00 1 d . . . C(21) C 1.1325(2) 0.2266(3) 0.2568(2) 0.0323(14) Uani 1.00 1 d . . . C(22) C 1.1064(2) 0.2250(2) 0.1779(2) 0.0287(14) Uani 1.00 1 d . . . C(23) C 1.2017(2) 0.2258(3) 0.1136(2) 0.0350(15) Uani 1.00 1 d . . . C(24) C 1.2213(2) 0.3072(3) 0.0833(3) 0.0512(19) Uani 1.00 1 d . . . C(25) C 1.0901(2) 0.2261(3) 0.0530(2) 0.0368(15) Uani 1.00 1 d . . . C(26) C 1.0358(2) 0.2271(3) 0.0804(2) 0.0363(15) Uani 1.00 1 d . . . C(27) C 0.9714(2) 0.0563(3) 0.1907(3) 0.0386(16) Uani 1.00 1 d . . . C(28) C 0.9707(2) -0.0291(3) 0.1891(3) 0.0421(17) Uani 1.00 1 d . . . C(29) C 1.000000(10) -0.0732(5) 0.250000(10) 0.043(2) Uani 1.00 2 d S . . C(30) C 0.9489(2) 0.4104(3) 0.2585(2) 0.0323(14) Uani 1.00 1 d . . . C(31) C 0.9477(2) 0.4967(3) 0.2577(2) 0.0334(15) Uani 1.00 1 d . . . C(32) C 1.000000(10) 0.5410(4) 0.250000(10) 0.032(2) Uani 1.00 2 d S . . H(1) H 1.2174 0.0247 0.4338 0.034 Uiso 1.00 1 c R . . H(2) H 1.1553 -0.0814 0.4688 0.043 Uiso 1.00 1 c R . . H(3) H 1.0789 -0.0540 0.5452 0.051 Uiso 1.00 1 c R . . H(4) H 1.0641 0.0812 0.5829 0.045 Uiso 1.00 1 c R . . H(5) H 1.0910 0.2222 0.5927 0.033 Uiso 1.00 1 c R . . H(6) H 1.0286 0.3392 0.5579 0.035 Uiso 1.00 1 c R . . H(7) H 1.0473 0.4187 0.6043 0.036 Uiso 1.00 1 c R . . H(8) H 1.0658 0.3323 0.6383 0.036 Uiso 1.00 1 c R . . H(9) H 1.1641 0.3657 0.6681 0.036 Uiso 1.00 1 c R . . H(10) H 1.1780 0.4457 0.6254 0.036 Uiso 1.00 1 c R . . H(11) H 1.2093 0.3629 0.6087 0.036 Uiso 1.00 1 c R . . H(12) H 1.0430 0.4728 0.4142 0.034 Uiso 1.00 1 c R . . H(13) H 1.0218 0.4064 0.4678 0.034 Uiso 1.00 1 c R . . H(14) H 1.0568 0.3799 0.4020 0.034 Uiso 1.00 1 c R . . H(15) H 1.1623 0.5283 0.5432 0.037 Uiso 1.00 1 c R . . H(16) H 1.0939 0.5287 0.5559 0.038 Uiso 1.00 1 c R . . H(17) H 1.1117 0.5562 0.4785 0.038 Uiso 1.00 1 c R . . H(18) H 1.1685 0.5169 0.4041 0.030 Uiso 1.00 1 c R . . H(19) H 1.2262 0.5711 0.3153 0.038 Uiso 1.00 1 c R . . H(20) H 1.2956 0.5583 0.2293 0.039 Uiso 1.00 1 c R . . H(21) H 1.3363 0.4286 0.2072 0.045 Uiso 1.00 1 c R . . H(22) H 1.3096 0.3124 0.2718 0.039 Uiso 1.00 1 c R . . H(23) H 1.1753 0.2230 0.2740 0.040 Uiso 1.00 1 c R . . H(24) H 1.2225 0.2177 0.1635 0.043 Uiso 1.00 1 c R . . H(25) H 1.2122 0.1824 0.0817 0.043 Uiso 1.00 1 c R . . H(27) H 1.2196 0.3040 0.0299 0.062 Uiso 1.00 1 c R . . H(28) H 1.1948 0.3500 0.0956 0.062 Uiso 1.00 1 c R . . H(29) H 1.0960 0.2269 0.0013 0.044 Uiso 1.00 1 c R . . H(30) H 0.9967 0.2268 0.0501 0.042 Uiso 1.00 1 c R . . H(31) H 0.9509 0.0859 0.1484 0.046 Uiso 1.00 1 c R . . H(32) H 0.9502 -0.0575 0.1462 0.051 Uiso 1.00 1 c R . . H(33) H 0.9125 0.3815 0.2652 0.039 Uiso 1.00 1 c R . . H(34) H 0.9106 0.5251 0.2626 0.040 Uiso 1.00 1 c R . . H(41) H 1.0000 -0.1404 0.2500 0.051 Uiso 1.00 2 c R . . H(42) H 1.0000 0.5884 0.2500 0.038 Uiso 1.00 2 c R . . H(44) H 1.2622 0.3190 0.1057 0.062 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0237(5) 0.0302(5) 0.0331(5) 0.0000 0.0027(4) 0.0000 Mn(1) 0.0208(3) 0.0217(4) 0.0213(3) 0.0051(3) 0.0052(3) 0.0022(3) Cl(1) 0.0471(8) 0.0398(8) 0.0464(8) -0.0131(7) 0.0225(6) -0.0091(6) O(1) 0.0254(18) 0.0207(17) 0.0264(17) 0.0037(14) 0.0075(14) 0.0018(14) O(2) 0.0297(18) 0.0220(17) 0.0260(17) 0.0044(14) 0.0078(14) 0.0062(14) O(3) 0.035(2) 0.038(2) 0.0256(19) 0.0022(16) 0.0002(15) -0.0075(15) O(4) 0.076(5) 0.087(5) 0.66(2) 0.010(4) 0.013(9) -0.122(9) O(5) 0.199(7) 0.121(4) 0.092(4) -0.095(5) 0.084(4) -0.024(3) O(6) 0.519(19) 0.160(6) 0.046(3) -0.206(10) 0.092(6) -0.045(4) O(7) 0.094(3) 0.036(2) 0.063(2) 0.000(2) 0.013(2) -0.013(2) N(1) 0.0155(19) 0.024(2) 0.0182(19) 0.0012(17) 0.0010(15) -0.0016(17) N(2) 0.020(2) 0.021(2) 0.021(2) 0.0054(16) 0.0015(17) -0.0008(17) N(3) 0.038(2) 0.022(2) 0.039(2) 0.0003(19) 0.001(2) 0.0007(19) N(4) 0.030(2) 0.027(2) 0.039(2) 0.0034(19) 0.004(2) -0.0036(19) N(5) 0.038(2) 0.035(2) 0.031(2) 0.008(2) 0.011(2) 0.0005(19) N(6) 0.025(3) 0.039(3) 0.045(3) 0.0000 0.004(3) 0.0000 N(7) 0.023(3) 0.030(3) 0.024(3) 0.0000 0.003(2) 0.0000 C(1) 0.027(2) 0.023(2) 0.026(2) -0.000(2) -0.004(2) 0.002(2) C(2) 0.034(3) 0.022(2) 0.030(2) 0.001(2) 0.005(2) -0.001(2) C(3) 0.042(3) 0.023(2) 0.044(3) 0.000(2) 0.000(2) -0.001(2) C(4) 0.040(3) 0.031(3) 0.057(3) -0.008(2) 0.010(2) 0.003(2) C(5) 0.036(3) 0.032(3) 0.044(3) -0.001(2) 0.014(2) 0.005(2) C(6) 0.025(2) 0.024(2) 0.032(2) -0.001(2) 0.007(2) 0.004(2) C(7) 0.022(2) 0.034(2) 0.026(2) 0.001(2) 0.007(2) -0.000(2) C(8) 0.026(2) 0.020(2) 0.023(2) 0.003(2) 0.005(2) -0.002(2) C(9) 0.027(2) 0.033(2) 0.029(2) 0.003(2) 0.008(2) -0.006(2) C(10) 0.030(2) 0.037(3) 0.023(2) 0.002(2) 0.005(2) -0.005(2) C(11) 0.021(2) 0.021(2) 0.026(2) 0.002(2) 0.005(2) -0.005(2) C(12) 0.022(2) 0.032(2) 0.030(2) 0.008(2) 0.006(2) -0.000(2) C(13) 0.033(3) 0.028(2) 0.033(2) 0.003(2) 0.009(2) -0.005(2) C(14) 0.030(2) 0.021(2) 0.023(2) 0.003(2) 0.000(2) -0.000(2) C(15) 0.024(2) 0.023(2) 0.022(2) -0.002(2) 0.003(2) 0.002(2) C(16) 0.036(3) 0.028(2) 0.030(2) -0.002(2) -0.001(2) 0.003(2) C(17) 0.037(3) 0.035(3) 0.026(2) -0.010(2) 0.005(2) 0.005(2) C(18) 0.033(3) 0.052(3) 0.029(2) -0.004(2) 0.010(2) 0.007(2) C(19) 0.032(3) 0.033(3) 0.034(2) 0.004(2) 0.012(2) 0.003(2) C(20) 0.023(2) 0.028(2) 0.022(2) -0.001(2) 0.001(2) 0.001(2) C(21) 0.034(3) 0.030(2) 0.036(2) 0.007(2) 0.016(2) 0.000(2) C(22) 0.029(2) 0.025(2) 0.031(2) 0.005(2) 0.003(2) 0.000(2) C(23) 0.040(3) 0.032(3) 0.035(2) 0.007(2) 0.013(2) 0.001(2) C(24) 0.050(3) 0.048(3) 0.057(3) 0.005(3) 0.012(3) 0.013(3) C(25) 0.045(3) 0.037(3) 0.028(2) 0.012(2) 0.001(2) -0.001(2) C(26) 0.040(3) 0.033(3) 0.032(3) 0.011(2) -0.006(2) -0.007(2) C(27) 0.036(3) 0.037(3) 0.043(3) -0.002(2) 0.005(2) -0.003(2) C(28) 0.034(3) 0.036(3) 0.058(3) 0.002(2) 0.011(2) -0.010(2) C(29) 0.035(4) 0.033(4) 0.061(5) 0.0000 0.009(4) 0.0000 C(30) 0.029(2) 0.034(3) 0.034(2) -0.001(2) 0.003(2) -0.001(2) C(31) 0.034(3) 0.033(3) 0.033(2) 0.008(2) 0.005(2) -0.003(2) C(32) 0.039(4) 0.030(4) 0.028(3) 0.0000 0.009(3) 0.0000 #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ni(1) N(3) 2.083(4) yes . . Ni(1) N(3) 2.083(4) yes . 2_755 Ni(1) N(4) 2.040(4) yes . . Ni(1) N(4) 2.040(4) yes . 2_755 Ni(1) N(6) 2.141(6) yes . . Ni(1) N(7) 2.152(5) yes . . Mn(1) O(1) 1.910(2) yes . . Mn(1) O(1) 2.552(2) yes . 7_756 Mn(1) O(2) 1.872(3) yes . . Mn(1) O(3) 2.117(3) yes . . Mn(1) N(1) 1.986(3) yes . . Mn(1) N(2) 1.992(3) yes . . Cl(1) O(4) 1.378(8) yes . . Cl(1) O(5) 1.322(7) yes . . Cl(1) O(6) 1.305(6) yes . . Cl(1) O(7) 1.399(4) yes . . O(1) C(1) 1.345(5) yes . . O(2) C(20) 1.326(5) yes . . O(3) N(3) 1.305(5) yes . . N(1) C(7) 1.278(6) yes . . N(1) C(8) 1.507(5) yes . . N(2) C(11) 1.509(6) yes . . N(2) C(14) 1.287(6) yes . . N(3) C(21) 1.312(7) yes . . N(4) C(22) 1.344(6) yes . . N(4) C(26) 1.363(6) yes . . N(5) C(22) 1.358(6) yes . . N(5) C(23) 1.465(6) yes . . N(5) C(25) 1.385(6) yes . . N(6) C(27) 1.344(6) yes . . N(6) C(27) 1.344(6) yes . 2_755 N(7) C(30) 1.364(6) yes . . N(7) C(30) 1.364(6) yes . 2_755 C(1) C(2) 1.408(6) yes . . C(1) C(6) 1.401(7) yes . . C(2) C(3) 1.390(7) yes . . C(3) C(4) 1.396(8) yes . . C(4) C(5) 1.372(7) yes . . C(5) C(6) 1.397(7) yes . . C(6) C(7) 1.447(6) yes . . C(8) C(9) 1.521(7) yes . . C(8) C(10) 1.538(6) yes . . C(8) C(11) 1.559(6) yes . . C(11) C(12) 1.534(6) yes . . C(11) C(13) 1.526(6) yes . . C(14) C(15) 1.440(7) yes . . C(15) C(16) 1.411(6) yes . . C(15) C(20) 1.412(6) yes . . C(16) C(17) 1.374(7) yes . . C(17) C(18) 1.384(7) yes . . C(18) C(19) 1.383(7) yes . . C(19) C(20) 1.405(7) yes . . C(21) C(22) 1.444(6) yes . . C(23) C(24) 1.506(7) yes . . C(25) C(26) 1.352(8) yes . . C(27) C(28) 1.380(7) yes . . C(28) C(29) 1.380(7) yes . . C(30) C(31) 1.394(7) yes . . C(31) C(32) 1.377(6) yes . . C(2) H(1) 0.950 no . . C(3) H(2) 0.950 no . . C(4) H(3) 0.950 no . . C(5) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(9) H(6) 0.950 no . . C(9) H(7) 0.950 no . . C(9) H(8) 0.950 no . . C(10) H(9) 0.950 no . . C(10) H(10) 0.950 no . . C(10) H(11) 0.950 no . . C(12) H(12) 0.950 no . . C(12) H(13) 0.950 no . . C(12) H(14) 0.950 no . . C(13) H(15) 0.950 no . . C(13) H(16) 0.950 no . . C(13) H(17) 0.950 no . . C(14) H(18) 0.950 no . . C(16) H(19) 0.950 no . . C(17) H(20) 0.950 no . . C(18) H(21) 0.950 no . . C(19) H(22) 0.950 no . . C(21) H(23) 0.950 no . . C(23) H(24) 0.950 no . . C(23) H(25) 0.950 no . . C(24) H(27) 0.950 no . . C(24) H(28) 0.950 no . . C(24) H(44) 0.950 no . . C(25) H(29) 0.950 no . . C(26) H(30) 0.950 no . . C(27) H(31) 0.950 no . . C(28) H(32) 0.950 no . . C(29) H(41) 1.084 no . . C(30) H(33) 0.950 no . . C(31) H(34) 0.950 no . . C(32) H(42) 0.765 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(3) Ni(1) N(3) 178.69(15) yes . . 2_755 N(3) Ni(1) N(4) 79.44(16) yes . . . N(3) Ni(1) N(4) 100.60(16) yes . . 2_755 N(3) Ni(1) N(6) 90.66(10) yes . . . N(3) Ni(1) N(7) 89.34(10) yes . . . N(3) Ni(1) N(4) 100.60(16) yes 2_755 . . N(3) Ni(1) N(4) 79.44(16) yes 2_755 . 2_755 N(3) Ni(1) N(6) 90.66(10) yes 2_755 . . N(3) Ni(1) N(7) 89.34(10) yes 2_755 . . N(4) Ni(1) N(4) 176.94(16) yes . . 2_755 N(4) Ni(1) N(6) 88.47(11) yes . . . N(4) Ni(1) N(7) 91.53(11) yes . . . N(4) Ni(1) N(6) 88.47(11) yes 2_755 . . N(4) Ni(1) N(7) 91.53(11) yes 2_755 . . N(6) Ni(1) N(7) 0(311) yes . . . O(1) Mn(1) O(1) 80.04(10) yes . . 7_756 O(1) Mn(1) O(2) 92.97(13) yes . . . O(1) Mn(1) O(3) 90.75(12) yes . . . O(1) Mn(1) N(1) 91.34(14) yes . . . O(1) Mn(1) N(2) 166.68(13) yes . . . O(1) Mn(1) O(2) 82.66(11) yes 7_756 . . O(1) Mn(1) O(3) 170.75(11) yes 7_756 . . O(1) Mn(1) N(1) 93.95(11) yes 7_756 . . O(1) Mn(1) N(2) 89.06(12) yes 7_756 . . O(2) Mn(1) O(3) 98.78(13) yes . . . O(2) Mn(1) N(1) 173.97(14) yes . . . O(2) Mn(1) N(2) 93.20(14) yes . . . O(3) Mn(1) N(1) 85.37(13) yes . . . O(3) Mn(1) N(2) 99.95(13) yes . . . N(1) Mn(1) N(2) 81.73(15) yes . . . O(4) Cl(1) O(5) 96.5(5) yes . . . O(4) Cl(1) O(6) 103.2(9) yes . . . O(4) Cl(1) O(7) 102.8(4) yes . . . O(5) Cl(1) O(6) 118.6(5) yes . . . O(5) Cl(1) O(7) 118.4(3) yes . . . O(6) Cl(1) O(7) 112.8(4) yes . . . Mn(1) O(1) Mn(1) 99.96(11) yes . . 7_756 Mn(1) O(1) C(1) 120.7(2) yes . . . Mn(1) O(1) C(1) 120.2(2) yes 7_756 . . Mn(1) O(2) C(20) 129.5(2) yes . . . Mn(1) O(3) N(3) 134.3(2) yes . . . Mn(1) N(1) C(7) 122.8(3) yes . . . Mn(1) N(1) C(8) 116.3(2) yes . . . C(7) N(1) C(8) 120.9(3) yes . . . Mn(1) N(2) C(11) 115.4(2) yes . . . Mn(1) N(2) C(14) 123.9(3) yes . . . C(11) N(2) C(14) 120.3(3) yes . . . Ni(1) N(3) O(3) 124.4(3) yes . . . Ni(1) N(3) C(21) 115.5(3) yes . . . O(3) N(3) C(21) 120.1(4) yes . . . Ni(1) N(4) C(22) 111.6(3) yes . . . Ni(1) N(4) C(26) 142.6(3) yes . . . C(22) N(4) C(26) 105.8(4) yes . . . C(22) N(5) C(23) 127.0(3) yes . . . C(22) N(5) C(25) 107.0(4) yes . . . C(23) N(5) C(25) 125.8(4) yes . . . Ni(1) N(6) C(27) 121.1(3) yes . . . Ni(1) N(6) C(27) 121.1(3) yes . . 2_755 C(27) N(6) C(27) 117.9(5) yes . . 2_755 Ni(1) N(7) C(30) 122.3(2) yes . . . Ni(1) N(7) C(30) 122.3(2) yes . . 2_755 C(30) N(7) C(30) 115.5(4) yes . . 2_755 O(1) C(1) C(2) 118.9(4) yes . . . O(1) C(1) C(6) 122.8(4) yes . . . C(2) C(1) C(6) 118.3(4) yes . . . C(1) C(2) C(3) 120.4(4) yes . . . C(2) C(3) C(4) 121.1(4) yes . . . C(3) C(4) C(5) 118.4(5) yes . . . C(4) C(5) C(6) 121.9(5) yes . . . C(1) C(6) C(5) 120.0(4) yes . . . C(1) C(6) C(7) 122.5(4) yes . . . C(5) C(6) C(7) 117.6(4) yes . . . N(1) C(7) C(6) 125.7(4) yes . . . N(1) C(8) C(9) 111.7(3) yes . . . N(1) C(8) C(10) 105.2(3) yes . . . N(1) C(8) C(11) 106.0(3) yes . . . C(9) C(8) C(10) 109.4(3) yes . . . C(9) C(8) C(11) 111.7(3) yes . . . C(10) C(8) C(11) 112.7(3) yes . . . N(2) C(11) C(8) 107.6(3) yes . . . N(2) C(11) C(12) 105.9(3) yes . . . N(2) C(11) C(13) 111.7(3) yes . . . C(8) C(11) C(12) 111.6(3) yes . . . C(8) C(11) C(13) 110.9(3) yes . . . C(12) C(11) C(13) 109.1(3) yes . . . N(2) C(14) C(15) 127.1(4) yes . . . C(14) C(15) C(16) 117.7(4) yes . . . C(14) C(15) C(20) 122.9(4) yes . . . C(16) C(15) C(20) 119.4(4) yes . . . C(15) C(16) C(17) 121.2(4) yes . . . C(16) C(17) C(18) 119.3(4) yes . . . C(17) C(18) C(19) 121.0(5) yes . . . C(18) C(19) C(20) 120.9(4) yes . . . O(2) C(20) C(15) 123.5(4) yes . . . O(2) C(20) C(19) 118.3(4) yes . . . C(15) C(20) C(19) 118.2(4) yes . . . N(3) C(21) C(22) 112.9(4) yes . . . N(4) C(22) N(5) 110.4(4) yes . . . N(4) C(22) C(21) 120.4(4) yes . . . N(5) C(22) C(21) 129.2(4) yes . . . N(5) C(23) C(24) 111.4(4) yes . . . N(5) C(25) C(26) 106.3(4) yes . . . N(4) C(26) C(25) 110.5(4) yes . . . N(6) C(27) C(28) 122.4(5) yes . . . C(27) C(28) C(29) 119.7(5) yes . . . C(28) C(29) C(28) 118.0(6) yes . . 2_755 N(7) C(30) C(31) 123.2(4) yes . . . C(30) C(31) C(32) 120.2(5) yes . . . C(31) C(32) C(31) 117.5(6) yes . . 2_755 C(1) C(2) H(1) 119.9 no . . . C(3) C(2) H(1) 119.8 no . . . C(2) C(3) H(2) 119.4 no . . . C(4) C(3) H(2) 119.5 no . . . C(3) C(4) H(3) 120.7 no . . . C(5) C(4) H(3) 120.8 no . . . C(4) C(5) H(4) 119.0 no . . . C(6) C(5) H(4) 119.1 no . . . N(1) C(7) H(5) 117.2 no . . . C(6) C(7) H(5) 117.2 no . . . C(8) C(9) H(6) 109.1 no . . . C(8) C(9) H(7) 109.6 no . . . C(8) C(9) H(8) 109.6 no . . . H(6) C(9) H(7) 109.5 no . . . H(6) C(9) H(8) 109.5 no . . . H(7) C(9) H(8) 109.5 no . . . C(8) C(10) H(9) 109.5 no . . . C(8) C(10) H(10) 109.4 no . . . C(8) C(10) H(11) 109.5 no . . . H(9) C(10) H(10) 109.5 no . . . H(9) C(10) H(11) 109.5 no . . . H(10) C(10) H(11) 109.5 no . . . C(11) C(12) H(12) 109.5 no . . . C(11) C(12) H(13) 109.5 no . . . C(11) C(12) H(14) 109.5 no . . . H(12) C(12) H(13) 109.5 no . . . H(12) C(12) H(14) 109.5 no . . . H(13) C(12) H(14) 109.5 no . . . C(11) C(13) H(15) 109.5 no . . . C(11) C(13) H(16) 109.6 no . . . C(11) C(13) H(17) 109.3 no . . . H(15) C(13) H(16) 109.5 no . . . H(15) C(13) H(17) 109.5 no . . . H(16) C(13) H(17) 109.5 no . . . N(2) C(14) H(18) 116.4 no . . . C(15) C(14) H(18) 116.4 no . . . C(15) C(16) H(19) 119.4 no . . . C(17) C(16) H(19) 119.4 no . . . C(16) C(17) H(20) 120.3 no . . . C(18) C(17) H(20) 120.4 no . . . C(17) C(18) H(21) 119.5 no . . . C(19) C(18) H(21) 119.5 no . . . C(18) C(19) H(22) 119.6 no . . . C(20) C(19) H(22) 119.6 no . . . N(3) C(21) H(23) 123.5 no . . . C(22) C(21) H(23) 123.6 no . . . N(5) C(23) H(24) 108.9 no . . . N(5) C(23) H(25) 108.9 no . . . C(24) C(23) H(24) 109.3 no . . . C(24) C(23) H(25) 108.8 no . . . H(24) C(23) H(25) 109.5 no . . . C(23) C(24) H(27) 109.8 no . . . C(23) C(24) H(28) 109.6 no . . . C(23) C(24) H(44) 109.1 no . . . H(27) C(24) H(28) 109.5 no . . . H(27) C(24) H(44) 109.5 no . . . H(28) C(24) H(44) 109.5 no . . . N(5) C(25) H(29) 126.9 no . . . C(26) C(25) H(29) 126.9 no . . . N(4) C(26) H(30) 124.7 no . . . C(25) C(26) H(30) 124.7 no . . . N(6) C(27) H(31) 118.8 no . . . C(28) C(27) H(31) 118.8 no . . . C(27) C(28) H(32) 120.1 no . . . C(29) C(28) H(32) 120.1 no . . . C(28) C(29) H(41) 121.0 no . . . C(28) C(29) H(41) 121.0 no 2_755 . . N(7) C(30) H(33) 118.3 no . . . C(31) C(30) H(33) 118.4 no . . . C(30) C(31) H(34) 119.8 no . . . C(32) C(31) H(34) 119.9 no . . . C(31) C(32) H(42) 121.2 no . . . C(31) C(32) H(42) 121.2 no 2_755 . . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data___Ni_eiao_phen _database_code_depnum_ccdc_archive 'CCDC 629016' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24.64 H28.64 Cl1.92 N8 O4 Ni ' _chemical_formula_moiety 'C24.64 H28.64 Cl1.92 N8 O4 Ni ' _chemical_formula_weight 627.64 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 16.960(17) _cell_length_b 10.715(11) _cell_length_c 16.298(17) _cell_angle_alpha 90.0000 _cell_angle_beta 107.737(13) _cell_angle_gamma 90.0000 _cell_volume 2821(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3168 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 93.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300.48 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.982 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 10814 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2446 _reflns_number_gt 1634 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1210 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2446 _refine_ls_number_parameters 261 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0004Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.21 _refine_diff_density_min -0.57 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ni(1) Ni 0.5000 0.17393(9) 0.2500 0.0293(2) Uani 1.00 2 d S . . Cl(1) Cl 0.2674(2) 0.6363(4) 0.1513(2) 0.0578(16) Uani 0.33 1 d P . . Cl(2) Cl 0.17866(12) 0.3265(2) 0.45861(17) 0.0798(9) Uani 0.64 1 d P . . O(1) O 0.35123(14) 0.1463(3) 0.08616(17) 0.0358(9) Uani 1.00 1 d . . . O(2) O 0.1810(2) 0.1378(4) 0.0147(2) 0.0454(11) Uani 1.00 1 d . . . N(1) N 0.38006(18) 0.1950(3) 0.1643(2) 0.0280(10) Uani 1.00 1 d . . . N(2) N 0.45284(18) 0.3046(3) 0.3170(2) 0.0277(9) Uani 1.00 1 d . . . N(3) N 0.3416(2) 0.4047(3) 0.3205(2) 0.0413(12) Uani 1.00 1 d . . . N(4) N 0.53027(17) 0.0238(3) 0.1829(2) 0.0277(10) Uani 1.00 1 d . . . C(1) C 0.3348(2) 0.2757(4) 0.1899(2) 0.0329(13) Uani 1.00 1 d . . . C(2) C 0.3741(2) 0.3286(4) 0.2738(2) 0.0268(11) Uani 1.00 1 d . . . C(3) C 0.2611(6) 0.4769(12) 0.2768(7) 0.045(3) Uani 0.64 1 d P . . C(4) C 0.2668(4) 0.5729(7) 0.2166(5) 0.043(2) Uani 0.64 1 d P . . C(5) C 0.2537(12) 0.436(2) 0.3206(14) 0.056(6) Uani 0.37 1 d P . . C(6) C 0.2214(8) 0.352(2) 0.3883(9) 0.110(7) Uani 0.37 1 d P . . C(7) C 0.4026(2) 0.4294(4) 0.3973(3) 0.0366(14) Uani 1.00 1 d . . . C(8) C 0.4702(2) 0.3659(4) 0.3938(2) 0.0288(12) Uani 1.00 1 d . . . C(9) C 0.5597(2) 0.0237(5) 0.1162(2) 0.0352(14) Uani 1.00 1 d . . . C(10) C 0.5799(2) -0.0857(5) 0.0795(3) 0.0379(14) Uani 1.00 1 d . . . C(11) C 0.5670(2) -0.1977(5) 0.1112(3) 0.0415(15) Uani 1.00 1 d . . . C(12) C 0.5332(2) -0.2046(4) 0.1796(2) 0.0356(13) Uani 1.00 1 d . . . C(13) C 0.5165(2) -0.0898(4) 0.2140(2) 0.0301(12) Uani 1.00 1 d . . . C(14) C 0.5160(2) -0.3196(5) 0.2172(3) 0.0404(14) Uani 1.00 1 d . . . C(15) C 0.2878(11) 0.6579(19) 0.0427(9) 0.172(7) Uani 0.59 1 d P . . H(1) H 0.282(2) 0.296(4) 0.156(3) 0.058(15) Uiso 1.00 1 c . . . H(2) H 0.222(3) 0.407(4) 0.254(3) 0.053(15) Uiso 1.00 1 c . . . H(3) H 0.247(2) 0.520(4) 0.330(2) 0.027(12) Uiso 1.00 1 c . . . H(4) H 0.391(2) 0.482(3) 0.439(2) 0.027(11) Uiso 1.00 1 c . . . H(5) H 0.525(2) 0.359(3) 0.438(2) 0.022(10) Uiso 1.00 1 c . . . H(6) H 0.565(2) 0.105(3) 0.092(2) 0.014(10) Uiso 1.00 1 c . . . H(7) H 0.597(2) -0.074(4) 0.028(3) 0.051(14) Uiso 1.00 1 c . . . H(8) H 0.577(2) -0.277(4) 0.083(2) 0.039(12) Uiso 1.00 1 c . . . H(9) H 0.525(2) -0.387(4) 0.190(2) 0.035(13) Uiso 1.00 1 c . . . H(10) H 0.173(3) 0.211(5) -0.011(3) 0.07(2) Uiso 1.00 1 c . . . H(11) H 0.229(3) 0.132(4) 0.033(3) 0.044(15) Uiso 1.00 1 c . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0155(3) 0.0507(6) 0.0221(4) 0.0000 0.0064(2) 0.0000 Cl(1) 0.039(2) 0.071(4) 0.063(3) -0.006(2) 0.015(2) -0.008(2) Cl(2) 0.0466(13) 0.083(2) 0.094(2) 0.0236(12) -0.0028(11) -0.0030(16) O(1) 0.0209(14) 0.067(2) 0.0176(15) -0.0005(14) 0.0024(11) -0.0026(15) O(2) 0.0212(18) 0.068(3) 0.041(2) -0.0145(18) 0.0003(14) 0.015(2) N(1) 0.0167(15) 0.046(2) 0.0218(18) -0.0015(16) 0.0067(14) 0.0037(17) N(2) 0.0146(15) 0.046(2) 0.0209(18) 0.0011(15) 0.0033(13) 0.0024(18) N(3) 0.0191(17) 0.042(2) 0.058(2) 0.0028(17) 0.0044(17) -0.015(2) N(4) 0.0150(15) 0.045(2) 0.0213(19) -0.0029(16) 0.0028(14) -0.0024(18) C(1) 0.016(2) 0.045(3) 0.035(2) 0.000(2) 0.0033(19) 0.006(2) C(2) 0.0169(19) 0.031(2) 0.033(2) -0.0026(18) 0.0082(17) -0.000(2) C(3) 0.017(3) 0.064(8) 0.047(6) 0.014(4) 0.000(4) -0.024(6) C(4) 0.038(4) 0.033(5) 0.051(5) 0.010(3) 0.004(3) 0.006(4) C(5) 0.031(8) 0.051(15) 0.069(15) 0.017(8) -0.012(10) -0.031(12) C(6) 0.029(7) 0.26(2) 0.042(8) -0.055(12) 0.017(6) 0.014(13) C(7) 0.027(2) 0.032(3) 0.052(3) -0.001(2) 0.015(2) -0.017(2) C(8) 0.024(2) 0.040(3) 0.023(2) 0.002(2) 0.0081(18) 0.003(2) C(9) 0.028(2) 0.052(3) 0.024(2) -0.004(2) 0.0069(19) 0.001(2) C(10) 0.032(2) 0.053(3) 0.032(2) -0.004(2) 0.013(2) -0.015(2) C(11) 0.030(2) 0.054(4) 0.039(2) -0.011(2) 0.009(2) -0.021(2) C(12) 0.023(2) 0.046(3) 0.035(2) -0.004(2) 0.0039(19) -0.010(2) C(13) 0.0113(18) 0.047(3) 0.027(2) -0.0032(19) -0.0013(16) 0.002(2) C(14) 0.026(2) 0.045(3) 0.048(3) -0.003(2) 0.007(2) -0.006(2) C(15) 0.201(17) 0.21(2) 0.074(9) -0.101(15) -0.005(10) 0.059(11) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.7.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ni(1) N(1) 2.100(2) ? . . Ni(1) N(1) 2.100(2) ? . 65502 Ni(1) N(2) 2.080(3) ? . . Ni(1) N(2) 2.080(3) ? . 65502 Ni(1) N(4) 2.095(3) ? . . Ni(1) N(4) 2.095(3) ? . 65502 Cl(1) C(4) 1.265(10) ? . . Cl(1) C(15) 1.919(17) ? . . Cl(2) C(6) 1.555(17) ? . . Cl(2) C(15) 1.947(15) ? . 56504 Cl(2) C(15) 1.90(2) ? . 54506 O(1) N(1) 1.324(4) ? . . N(1) C(1) 1.306(6) ? . . N(2) C(2) 1.331(4) ? . . N(2) C(8) 1.363(5) ? . . N(3) C(2) 1.343(6) ? . . N(3) C(3) 1.542(11) ? . . N(3) C(5) 1.53(2) ? . . N(3) C(7) 1.386(5) ? . . N(4) C(9) 1.327(6) ? . . N(4) C(13) 1.366(6) ? . . C(1) C(2) 1.443(5) ? . . C(3) C(4) 1.445(15) ? . . C(3) C(5) 0.88(2) ? . . C(5) C(6) 1.64(3) ? . . C(7) C(8) 1.348(6) ? . . C(9) C(10) 1.405(8) ? . . C(10) C(11) 1.350(8) ? . . C(11) C(12) 1.404(7) ? . . C(12) C(13) 1.415(7) ? . . C(12) C(14) 1.446(7) ? . . C(13) C(13) 1.444(6) ? . 65502 C(14) C(14) 1.337(8) ? . 65502 C(1) H(1) 0.92(4) ? . . C(7) H(4) 0.95(4) ? . . C(8) H(5) 0.99(3) ? . . C(9) H(6) 0.98(4) ? . . C(10) H(7) 0.97(5) ? . . C(11) H(8) 1.01(4) ? . . C(14) H(9) 0.88(4) ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) Ni(1) N(1) 167.67(15) ? . . 65502 N(1) Ni(1) N(2) 80.07(12) ? . . . N(1) Ni(1) N(2) 91.59(12) ? . . 65502 N(1) Ni(1) N(4) 94.41(12) ? . . . N(1) Ni(1) N(4) 95.05(12) ? . . 65502 N(1) Ni(1) N(2) 91.59(12) ? 65502 . . N(1) Ni(1) N(2) 80.07(12) ? 65502 . 65502 N(1) Ni(1) N(4) 95.05(12) ? 65502 . . N(1) Ni(1) N(4) 94.41(12) ? 65502 . 65502 N(2) Ni(1) N(2) 95.35(14) ? . . 65502 N(2) Ni(1) N(4) 170.28(13) ? . . . N(2) Ni(1) N(4) 92.79(14) ? . . 65502 N(2) Ni(1) N(4) 92.79(14) ? 65502 . . N(2) Ni(1) N(4) 170.28(13) ? 65502 . 65502 N(4) Ni(1) N(4) 79.64(14) ? . . 65502 C(4) Cl(1) C(15) 152.9(8) ? . . . C(6) Cl(2) C(15) 86.9(7) ? . . 56504 C(6) Cl(2) C(15) 87.2(11) ? . . 54506 C(15) Cl(2) C(15) 82.3(7) ? 56504 . 54506 Ni(1) N(1) O(1) 126.6(2) ? . . . Ni(1) N(1) C(1) 113.8(2) ? . . . O(1) N(1) C(1) 119.1(2) ? . . . Ni(1) N(2) C(2) 109.7(2) ? . . . Ni(1) N(2) C(8) 142.8(2) ? . . . C(2) N(2) C(8) 107.1(3) ? . . . C(2) N(3) C(3) 120.1(5) ? . . . C(2) N(3) C(5) 134.8(8) ? . . . C(2) N(3) C(7) 107.8(3) ? . . . C(3) N(3) C(5) 33.2(10) ? . . . C(3) N(3) C(7) 129.4(5) ? . . . C(5) N(3) C(7) 114.6(9) ? . . . Ni(1) N(4) C(9) 129.8(3) ? . . . Ni(1) N(4) C(13) 113.2(2) ? . . . C(9) N(4) C(13) 117.0(4) ? . . . N(1) C(1) C(2) 114.6(3) ? . . . N(2) C(2) N(3) 109.7(3) ? . . . N(2) C(2) C(1) 121.7(4) ? . . . N(3) C(2) C(1) 128.7(3) ? . . . N(3) C(3) C(4) 116.0(8) ? . . . N(3) C(3) C(5) 72.6(15) ? . . . C(4) C(3) C(5) 164(2) ? . . . Cl(1) C(4) C(3) 166.7(8) ? . . . N(3) C(5) C(3) 74.2(17) ? . . . N(3) C(5) C(6) 113.7(14) ? . . . C(3) C(5) C(6) 168(2) ? . . . Cl(2) C(6) C(5) 156.4(19) ? . . . N(3) C(7) C(8) 106.0(4) ? . . . N(2) C(8) C(7) 109.5(3) ? . . . N(4) C(9) C(10) 123.4(5) ? . . . C(9) C(10) C(11) 119.4(5) ? . . . C(10) C(11) C(12) 120.2(5) ? . . . C(11) C(12) C(13) 116.7(4) ? . . . C(11) C(12) C(14) 124.5(4) ? . . . C(13) C(12) C(14) 118.8(4) ? . . . N(4) C(13) C(12) 123.3(4) ? . . . N(4) C(13) C(13) 117.0(4) ? . . 65502 C(12) C(13) C(13) 119.7(4) ? . . 65502 C(12) C(14) C(14) 121.5(5) ? . . 65502 Cl(1) C(15) Cl(2) 105.0(9) ? . . 56404 Cl(1) C(15) Cl(2) 105.3(8) ? . . 55506 Cl(2) C(15) Cl(2) 97.7(8) ? 56404 . 55506 H(10) O(2) H(11) 104(5) ? . . . N(1) C(1) H(1) 121(3) ? . . . C(2) C(1) H(1) 124(3) ? . . . N(3) C(3) H(2) 101(3) ? . . . N(3) C(3) H(3) 103(2) ? . . . C(4) C(3) H(2) 118(3) ? . . . C(4) C(3) H(3) 109(2) ? . . . C(5) C(3) H(2) 71(3) ? . . . C(5) C(3) H(3) 55(3) ? . . . H(2) C(3) H(3) 109(4) ? . . . N(3) C(5) H(2) 97(3) ? . . . N(3) C(5) H(3) 113(3) ? . . . C(3) C(5) H(2) 59(3) ? . . . C(3) C(5) H(3) 74(3) ? . . . C(6) C(5) H(2) 110(3) ? . . . C(6) C(5) H(3) 109(3) ? . . . H(2) C(5) H(3) 113(4) ? . . . N(3) C(7) H(4) 120(2) ? . . . C(8) C(7) H(4) 134(2) ? . . . N(2) C(8) H(5) 122(2) ? . . . C(7) C(8) H(5) 128(2) ? . . . N(4) C(9) H(6) 116(2) ? . . . C(10) C(9) H(6) 120(2) ? . . . C(9) C(10) H(7) 116(2) ? . . . C(11) C(10) H(7) 125(2) ? . . . C(10) C(11) H(8) 120(2) ? . . . C(12) C(11) H(8) 120(2) ? . . . C(12) C(14) H(9) 114(3) ? . . . C(14) C(14) H(9) 125(3) ? 65502 . . C(3) H(2) C(5) 49(2) ? . . . C(3) H(3) C(5) 51(2) ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(2) Cl(2) 2.893(3) ? . 55607 Cl(2) C(6) 3.190(19) ? . 55607 O(1) O(2) 2.766(4) ? . . O(1) O(2) 2.794(5) ? . 55507 O(1) C(10) 3.317(6) ? . 65503 O(2) O(1) 2.766(4) ? . . O(2) O(1) 2.794(5) ? . 55507 O(2) O(2) 3.488(5) ? . 55507 O(2) N(1) 3.564(4) ? . . O(2) N(1) 3.309(5) ? . 55507 O(2) C(1) 3.550(5) ? . . O(2) C(1) 3.391(6) ? . 55507 O(2) C(5) 3.36(2) ? . 54506 O(2) C(7) 3.209(6) ? . 54506 O(2) C(8) 3.519(4) ? . 45408 O(2) C(11) 3.343(7) ? . 45505 O(2) C(15) 3.39(2) ? . 55507 N(1) O(2) 3.564(4) ? . . N(1) O(2) 3.309(5) ? . 55507 C(1) O(2) 3.550(5) ? . . C(1) O(2) 3.391(6) ? . 55507 C(4) C(9) 3.433(7) ? . 45505 C(5) O(2) 3.36(2) ? . 55506 C(6) Cl(2) 3.190(19) ? . 55607 C(7) O(2) 3.209(6) ? . 55506 C(8) O(2) 3.519(4) ? . 55508 C(9) C(4) 3.433(7) ? . 54505 C(9) C(10) 3.409(5) ? . 65503 C(10) O(1) 3.317(6) ? . 65503 C(10) C(9) 3.409(5) ? . 65503 C(11) O(2) 3.343(7) ? . 54505 C(15) O(2) 3.39(2) ? . 55507 C(15) C(15) 2.53(2) ? . 56507 Cl(1) H(2) 3.20(5) ? . . Cl(1) H(2) 3.26(5) ? . 55506 Cl(1) H(3) 3.29(4) ? . . Cl(1) H(6) 3.28(3) ? . 45505 Cl(2) H(3) 3.38(4) ? . . Cl(2) H(6) 3.39(4) ? . 45508 Cl(2) H(7) 3.35(5) ? . 45508 O(1) H(3) 2.80(4) ? . 54506 O(1) H(7) 2.42(5) ? . 65503 O(1) H(10) 3.03(5) ? . . O(1) H(10) 1.93(6) ? . 55507 O(1) H(11) 2.00(4) ? . . O(1) H(11) 3.11(4) ? . 55507 O(2) H(1) 2.95(4) ? . . O(2) H(1) 3.11(5) ? . 55507 O(2) H(3) 2.76(4) ? . 54506 O(2) H(4) 2.32(4) ? . 54506 O(2) H(5) 2.56(3) ? . 45408 O(2) H(7) 3.44(4) ? . 45505 O(2) H(8) 2.52(4) ? . 45505 O(2) H(10) 0.87(6) ? . . O(2) H(10) 2.97(6) ? . 55507 O(2) H(11) 0.78(4) ? . . O(2) H(11) 3.13(5) ? . 55507 N(1) H(3) 2.88(4) ? . 54506 N(1) H(7) 3.53(5) ? . 65503 N(1) H(10) 2.59(5) ? . 55507 N(1) H(11) 2.87(4) ? . . N(2) H(9) 3.33(4) ? . 66502 N(3) H(2) 1.99(4) ? . . N(3) H(3) 2.07(4) ? . . N(3) H(9) 3.22(4) ? . 66502 N(4) H(2) 3.34(4) ? . 54505 N(4) H(7) 3.50(4) ? . 65503 C(1) H(2) 2.83(5) ? . . C(1) H(3) 3.04(4) ? . 54506 C(1) H(10) 2.89(6) ? . 55507 C(1) H(11) 3.05(4) ? . . C(2) H(2) 2.64(5) ? . . C(2) H(3) 3.30(4) ? . . C(2) H(9) 3.46(4) ? . 66502 C(3) H(2) 0.99(4) ? . . C(3) H(3) 1.08(4) ? . . C(3) H(11) 3.47(5) ? . 55506 C(4) H(2) 2.10(5) ? . . C(4) H(3) 2.07(4) ? . . C(4) H(6) 3.42(3) ? . 45505 C(4) H(9) 3.43(3) ? . 66502 C(5) H(2) 1.10(5) ? . . C(5) H(3) 0.92(5) ? . . C(5) H(11) 3.11(5) ? . 55506 C(6) H(2) 2.26(5) ? . . C(6) H(3) 2.13(5) ? . . C(6) H(11) 3.27(5) ? . 55506 C(7) H(2) 3.25(4) ? . . C(7) H(3) 2.71(3) ? . . C(7) H(5) 3.44(3) ? . 66603 C(7) H(8) 3.17(4) ? . 66502 C(7) H(9) 2.91(4) ? . 66502 C(7) H(11) 3.53(5) ? . 55506 C(8) H(4) 3.42(3) ? . 66603 C(8) H(8) 3.21(3) ? . 55504 C(8) H(9) 2.99(4) ? . 66502 C(8) H(10) 3.42(5) ? . 55508 C(9) H(2) 3.23(4) ? . 54505 C(9) H(7) 3.01(3) ? . 65503 C(10) H(1) 3.51(4) ? . 54505 C(10) H(2) 3.12(4) ? . 54505 C(10) H(6) 3.12(3) ? . 65503 C(10) H(7) 3.43(4) ? . 65503 C(10) H(10) 3.30(6) ? . 54505 C(11) H(1) 3.49(5) ? . 54505 C(11) H(2) 3.14(4) ? . 54505 C(11) H(5) 3.19(3) ? . 55404 C(11) H(6) 3.53(3) ? . 65503 C(11) H(10) 3.22(6) ? . 54505 C(12) H(2) 3.28(4) ? . 54505 C(13) H(2) 3.34(5) ? . 54505 C(15) H(11) 3.32(5) ? . 55507 H(1) O(2) 2.95(4) ? . . H(1) O(2) 3.11(5) ? . 55507 H(1) C(10) 3.51(4) ? . 45505 H(1) C(11) 3.49(5) ? . 45505 H(1) H(2) 2.46(8) ? . . H(1) H(3) 3.02(6) ? . 54506 H(1) H(7) 3.49(6) ? . 45505 H(1) H(8) 3.40(6) ? . 45505 H(1) H(10) 2.92(6) ? . . H(1) H(10) 2.70(8) ? . 55507 H(1) H(11) 2.60(6) ? . . H(1) H(11) 3.13(7) ? . 55507 H(2) Cl(1) 3.20(5) ? . . H(2) Cl(1) 3.26(5) ? . 54506 H(2) N(3) 1.99(4) ? . . H(2) N(4) 3.34(4) ? . 45505 H(2) C(1) 2.83(5) ? . . H(2) C(2) 2.64(5) ? . . H(2) C(3) 0.99(4) ? . . H(2) C(4) 2.10(5) ? . . H(2) C(5) 1.10(5) ? . . H(2) C(6) 2.26(5) ? . . H(2) C(7) 3.25(4) ? . . H(2) C(9) 3.23(4) ? . 45505 H(2) C(10) 3.12(4) ? . 45505 H(2) C(11) 3.14(4) ? . 45505 H(2) C(12) 3.28(4) ? . 45505 H(2) C(13) 3.34(5) ? . 45505 H(2) H(1) 2.46(8) ? . . H(2) H(3) 1.69(6) ? . . H(2) H(4) 3.56(5) ? . . H(3) Cl(1) 3.29(4) ? . . H(3) Cl(2) 3.38(4) ? . . H(3) O(1) 2.80(4) ? . 55506 H(3) O(2) 2.76(4) ? . 55506 H(3) N(1) 2.88(4) ? . 55506 H(3) N(3) 2.07(4) ? . . H(3) C(1) 3.04(4) ? . 55506 H(3) C(2) 3.30(4) ? . . H(3) C(3) 1.08(4) ? . . H(3) C(4) 2.07(4) ? . . H(3) C(5) 0.92(5) ? . . H(3) C(6) 2.13(5) ? . . H(3) C(7) 2.71(3) ? . . H(3) H(1) 3.02(6) ? . 55506 H(3) H(2) 1.69(6) ? . . H(3) H(4) 2.58(4) ? . . H(3) H(10) 3.50(7) ? . 55506 H(3) H(11) 2.45(6) ? . 55506 H(4) O(2) 2.32(4) ? . 55506 H(4) C(8) 3.42(3) ? . 66603 H(4) H(2) 3.56(5) ? . . H(4) H(3) 2.58(4) ? . . H(4) H(5) 2.68(5) ? . 66603 H(4) H(8) 2.68(6) ? . 66502 H(4) H(9) 3.21(6) ? . 66502 H(4) H(10) 3.05(7) ? . 55506 H(4) H(11) 2.73(6) ? . 55506 H(5) O(2) 2.56(3) ? . 55508 H(5) C(7) 3.44(3) ? . 66603 H(5) C(11) 3.19(3) ? . 55504 H(5) H(4) 2.68(5) ? . 66603 H(5) H(7) 3.44(6) ? . 55504 H(5) H(8) 2.41(5) ? . 55504 H(5) H(9) 3.38(5) ? . 66502 H(5) H(10) 2.52(6) ? . 55508 H(5) H(11) 3.34(5) ? . 55508 H(6) Cl(1) 3.28(3) ? . 54505 H(6) Cl(2) 3.39(4) ? . 55408 H(6) C(4) 3.42(3) ? . 54505 H(6) C(10) 3.12(3) ? . 65503 H(6) C(11) 3.53(3) ? . 65503 H(6) H(7) 2.86(4) ? . 65503 H(7) Cl(2) 3.35(5) ? . 55408 H(7) O(1) 2.42(5) ? . 65503 H(7) O(2) 3.44(4) ? . 54505 H(7) N(1) 3.53(5) ? . 65503 H(7) N(4) 3.50(4) ? . 65503 H(7) C(9) 3.01(4) ? . 65503 H(7) C(10) 3.43(4) ? . 65503 H(7) H(1) 3.49(6) ? . 54505 H(7) H(5) 3.44(6) ? . 55404 H(7) H(6) 2.86(5) ? . 65503 H(7) H(7) 3.50(6) ? . 65503 H(7) H(10) 2.82(8) ? . 54505 H(7) H(11) 3.46(7) ? . 65503 H(8) O(2) 2.52(4) ? . 54505 H(8) C(7) 3.17(4) ? . 64502 H(8) C(8) 3.21(3) ? . 55404 H(8) H(1) 3.40(6) ? . 54505 H(8) H(4) 2.68(6) ? . 64502 H(8) H(5) 2.41(5) ? . 55404 H(8) H(10) 2.55(8) ? . 54505 H(8) H(11) 3.07(7) ? . 54505 H(9) N(2) 3.33(4) ? . 64502 H(9) N(3) 3.22(4) ? . 64502 H(9) C(2) 3.46(4) ? . 64502 H(9) C(4) 3.43(3) ? . 64502 H(9) C(7) 2.91(4) ? . 64502 H(9) C(8) 2.99(4) ? . 64502 H(9) H(4) 3.21(6) ? . 64502 H(9) H(5) 3.38(5) ? . 64502 H(10) O(1) 3.03(5) ? . . H(10) O(1) 1.93(6) ? . 55507 H(10) O(2) 0.87(6) ? . . H(10) O(2) 2.97(6) ? . 55507 H(10) N(1) 2.59(5) ? . 55507 H(10) C(1) 2.89(6) ? . 55507 H(10) C(8) 3.42(5) ? . 45408 H(10) C(10) 3.30(6) ? . 45505 H(10) C(11) 3.22(6) ? . 45505 H(10) H(1) 2.92(6) ? . . H(10) H(1) 2.70(8) ? . 55507 H(10) H(3) 3.50(7) ? . 54506 H(10) H(4) 3.05(7) ? . 54506 H(10) H(5) 2.52(6) ? . 45408 H(10) H(7) 2.82(8) ? . 45505 H(10) H(8) 2.55(8) ? . 45505 H(10) H(10) 2.66(8) ? . 55507 H(10) H(11) 1.30(7) ? . . H(10) H(11) 2.47(8) ? . 55507 H(11) O(1) 2.00(4) ? . . H(11) O(1) 3.11(4) ? . 55507 H(11) O(2) 0.78(4) ? . . H(11) O(2) 3.13(5) ? . 55507 H(11) N(1) 2.87(4) ? . . H(11) C(1) 3.05(4) ? . . H(11) C(3) 3.47(5) ? . 54506 H(11) C(5) 3.11(5) ? . 54506 H(11) C(6) 3.27(5) ? . 54506 H(11) C(7) 3.53(5) ? . 54506 H(11) C(15) 3.32(5) ? . 55507 H(11) H(1) 2.60(6) ? . . H(11) H(1) 3.13(7) ? . 55507 H(11) H(3) 2.45(6) ? . 54506 H(11) H(4) 2.73(6) ? . 54506 H(11) H(5) 3.34(5) ? . 45408 H(11) H(7) 3.46(7) ? . 65503 H(11) H(8) 3.07(7) ? . 45505 H(11) H(10) 1.30(7) ? . . H(11) H(10) 2.47(8) ? . 55507 H(11) H(11) 2.93(7) ? . 55507