Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_General _journal_coden_Cambridge 1145 #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Tomoyuki Akutagawa' _publ_contact_author_address ; Dr T Akutagawa Research Institute for Electronic Science Hokkaido University Sapporo 060-0812 JAPAN ; _publ_contact_author_email 'takuta@imd.es.hokudai.ac.jp' _publ_contact_author_fax '+81-11-706-4972' _publ_contact_author_phone '+81-11-706-2884' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'Jounal of Material Chemsitry' _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Diversity in 1/2 spin arrangement of [Ni(dmit)2]- anions in divalent Ca2+(crown ethers) supramolecular cation salts ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name #_publ_author_footnote #_publ_author_address 'Akutagawa, T.' 'Awaga, Kunio' 'Fujita, Wataru' 'Hasegawa, Tatsuo' 'Inabe, Tamotsu' 'Nakamura, Takayoshi' 'Shitagami, Kozo' 'Takamatsu, Nobuhiro' _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). CrystalStructure. Single Crystal Structure Analysis Software. Version 1.00. MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W., CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data__Ca(12C4)2[Ni(dmit)2]2 _database_code_CSD 158716 _audit_creation_date '2001-04-11' _audit_creation_method 'by CrystalStructure v1.00' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C28 H32 Ca Ni2 O8 S20 ' _chemical_formula_moiety 'C28 H32 Ca Ni2 O8 S20 ' _chemical_formula_weight 1295.24 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _cell_length_a 19.872(1) _cell_length_b 19.7547(8) _cell_length_c 12.6242(6) _cell_angle_alpha 90 _cell_angle_beta 95.442(1) _cell_angle_gamma 90 _cell_volume 4933.5(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 32151 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 297 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.756 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_number 10878 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). 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_obs 4662 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0410 _refine_ls_wR_factor_obs 0.0500 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 4662 _refine_ls_number_parameters 564 _refine_ls_goodness_of_fit_obs 1.776 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/\s^2^(Fo^2^)' _refine_ls_shift/esd_max 0.0340 _refine_diff_density_max 0.55 _refine_diff_density_min -0.67 _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' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Ca' 'Ca' 0.252 0.372 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Ni' 'Ni' 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.148 0.159 ; 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) ; #============================================================================== # 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_thermal_displace_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N(I1) Ni 0.41360(3) 0.23710(4) 0.71705(5) 0.0532(2) Uani 1.00 1 d . . . S(1) S 0.35250(7) 0.20723(8) 0.5741(1) 0.0630(5) Uani 1.00 1 d . . . S(2) S 0.26813(8) 0.2924(1) 0.4093(1) 0.0831(6) Uani 1.00 1 d . . . S(3) S 0.21305(9) 0.4227(1) 0.3216(2) 0.1073(8) Uani 1.00 1 d . . . S(4) S 0.30663(8) 0.41697(9) 0.5174(1) 0.0836(6) Uani 1.00 1 d . . . S(5) S 0.39450(7) 0.34368(8) 0.6899(1) 0.0658(5) Uani 1.00 1 d . . . S(6) S 0.47312(7) 0.26797(8) 0.8605(1) 0.0646(5) Uani 1.00 1 d . . . S(7) S 0.56498(8) 0.18777(9) 1.0200(1) 0.0754(6) Uani 1.00 1 d . . . S(8) S 0.62934(8) 0.0609(1) 1.1046(1) 0.0824(6) Uani 1.00 1 d . . . S(9) S 0.53153(7) 0.06100(8) 0.9124(1) 0.0686(6) Uani 1.00 1 d . . . S(10) S 0.43686(7) 0.13076(8) 0.7430(1) 0.0613(5) Uani 1.00 1 d . . . C(1) C 0.3234(2) 0.2839(3) 0.5238(4) 0.058(2) Uani 1.00 1 d . . . C(2) C 0.2608(3) 0.3805(3) 0.4104(5) 0.077(2) Uani 1.00 1 d . . . C(3) C 0.3411(2) 0.3431(3) 0.5735(5) 0.059(2) Uani 1.00 1 d . . . C(4) C 0.5081(3) 0.1930(3) 0.9067(4) 0.057(2) Uani 1.00 1 d . . . C(5) C 0.5781(3) 0.1007(3) 1.0172(4) 0.061(2) Uani 1.00 1 d . . . C(6) C 0.4918(2) 0.1334(3) 0.8566(4) 0.052(2) Uani 1.00 1 d . . . N(I2) Ni 0.19336(3) 0.04702(4) 0.50544(6) 0.0543(2) Uani 1.00 1 d . . . S(11) S 0.15225(7) -0.01085(7) 0.6295(1) 0.0593(5) Uani 1.00 1 d . . . S(12) S 0.01562(7) -0.00269(8) 0.7180(1) 0.0662(5) Uani 1.00 1 d . . . S(13) S -0.11982(8) 0.05854(9) 0.7333(1) 0.0826(6) Uani 1.00 1 d . . . S(14) S -0.02908(7) 0.10597(8) 0.5758(1) 0.0631(5) Uani 1.00 1 d . . . S(15) S 0.10280(7) 0.10670(9) 0.4730(1) 0.0661(5) Uani 1.00 1 d . . . S(16) S 0.23112(8) 0.1015(1) 0.3784(2) 0.138(1) Uani 1.00 1 d . . . S(17) S 0.3667(1) 0.1050(1) 0.2908(1) 0.141(1) Uani 1.00 1 d . . . S(18) S 0.5090(1) 0.0644(1) 0.2853(2) 0.146(1) Uani 1.00 1 d . . . S(19) S 0.4218(1) 0.0119(1) 0.4453(3) 0.158(1) Uani 1.00 1 d . . . S(20) S 0.28899(8) -0.0004(1) 0.5456(2) 0.1098(8) Uani 1.00 1 d . . . C(7) C 0.0730(2) 0.0242(3) 0.6313(4) 0.048(2) Uani 1.00 1 d . . . C(8) C -0.0481(2) 0.0547(3) 0.6797(4) 0.058(2) Uani 1.00 1 d . . . C(9) C 0.0522(2) 0.0745(3) 0.5649(4) 0.049(2) Uani 1.00 1 d . . . C(10) C 0.3124(3) 0.0752(4) 0.3800(5) 0.079(2) Uani 1.00 1 d . . . C(11) C 0.4360(3) 0.0605(4) 0.3362(6) 0.100(3) Uani 1.00 1 d . . . C(12) C 0.3367(3) 0.0304(3) 0.4513(6) 0.073(2) Uani 1.00 1 d . . . Ca(1) Ca 0.66454(5) 0.28741(6) 0.46743(9) 0.0484(3) Uani 1.00 1 d . . . O(1) O 0.5577(2) 0.3443(2) 0.3933(4) 0.080(2) Uani 1.00 1 d . . . O(2) O 0.6266(2) 0.3720(2) 0.5850(4) 0.086(2) Uani 1.00 1 d . . . O(3) O 0.6417(2) 0.2351(3) 0.6298(3) 0.078(2) Uani 1.00 1 d . . . O(4) O 0.5704(2) 0.2116(2) 0.4416(3) 0.066(1) Uani 1.00 1 d . . . O(5) O 0.6771(2) 0.2750(2) 0.2812(3) 0.063(1) Uani 1.00 1 d . . . O(6) O 0.7302(2) 0.3802(2) 0.4067(4) 0.073(2) Uani 1.00 1 d . . . O(7) O 0.7793(2) 0.2894(2) 0.5582(3) 0.062(1) Uani 1.00 1 d . . . O(8) O 0.7269(2) 0.1867(2) 0.4341(3) 0.052(1) Uani 1.00 1 d . . . C(13) C 0.5276(4) 0.3876(5) 0.4606(6) 0.119(4) Uani 1.00 1 d . . . C(14) C 0.5804(4) 0.4213(4) 0.5299(7) 0.102(3) Uani 1.00 1 d . . . C(15) C 0.6023(4) 0.3497(4) 0.6773(5) 0.109(3) Uani 1.00 1 d . . . C(16) C 0.6415(3) 0.2870(4) 0.7133(5) 0.103(3) Uani 1.00 1 d . . . C(17) C 0.5881(4) 0.1902(5) 0.6283(7) 0.144(4) Uani 1.00 1 d . . . C(18) C 0.5703(4) 0.1639(4) 0.5287(6) 0.113(3) Uani 1.00 1 d . . . C(19) C 0.5065(4) 0.2359(4) 0.4045(7) 0.119(4) Uani 1.00 1 d . . . C(20) C 0.5105(4) 0.2932(5) 0.3482(7) 0.136(4) Uani 1.00 1 d . . . C(26) C 0.7865(3) 0.3973(3) 0.4814(6) 0.089(3) Uani 1.00 1 d . . . C(25) C 0.8255(3) 0.3354(3) 0.5155(5) 0.073(2) Uani 1.00 1 d . . . C(24) C 0.8043(3) 0.2212(3) 0.5736(5) 0.075(2) Uani 1.00 1 d . . . C(23) C 0.7963(3) 0.1810(3) 0.4753(5) 0.069(2) Uani 1.00 1 d . . . C(22) C 0.7135(3) 0.1644(3) 0.3270(4) 0.062(2) Uani 1.00 1 d . . . C(21) C 0.7194(3) 0.2209(3) 0.2512(4) 0.064(2) Uani 1.00 1 d . . . C(28) C 0.6907(3) 0.3393(3) 0.2338(5) 0.087(3) Uani 1.00 1 d . . . C(27) C 0.7469(3) 0.3750(3) 0.3002(6) 0.090(3) Uani 1.00 1 d . . . H(1) H 0.5007(4) 0.4199(5) 0.4200(6) 0.144(4) Uiso 1.00 1 d . . . H(2) H 0.5000(4) 0.3627(5) 0.5042(6) 0.144(4) Uiso 1.00 1 d . . . H(3) H 0.5616(4) 0.4498(4) 0.5800(7) 0.124(3) Uiso 1.00 1 d . . . H(4) H 0.6056(4) 0.4478(4) 0.4849(7) 0.124(3) Uiso 1.00 1 d . . . H(5) H 0.6062(4) 0.3844(4) 0.7296(5) 0.131(3) Uiso 1.00 1 d . . . H(6) H 0.5562(4) 0.3369(4) 0.6634(5) 0.131(3) Uiso 1.00 1 d . . . H(7) H 0.6242(3) 0.2684(4) 0.7746(5) 0.124(3) Uiso 1.00 1 d . . . H(8) H 0.6869(3) 0.3010(4) 0.7308(5) 0.124(3) Uiso 1.00 1 d . . . H(9) H 0.6001(4) 0.1545(5) 0.6769(7) 0.172(4) Uiso 1.00 1 d . . . H(10) H 0.5498(4) 0.2134(5) 0.6497(7) 0.172(4) Uiso 1.00 1 d . . . H(11) H 0.5265(4) 0.1444(4) 0.5269(6) 0.139(4) Uiso 1.00 1 d . . . H(12) H 0.6023(4) 0.1297(4) 0.5171(6) 0.139(4) Uiso 1.00 1 d . . . H(13) H 0.4815(4) 0.2020(4) 0.3645(7) 0.141(4) Uiso 1.00 1 d . . . H(14) H 0.4838(4) 0.2475(4) 0.4649(7) 0.141(4) Uiso 1.00 1 d . . . H(15) H 0.4671(4) 0.3135(5) 0.3355(7) 0.160(4) Uiso 1.00 1 d . . . H(16) H 0.5258(4) 0.2795(5) 0.2824(7) 0.160(4) Uiso 1.00 1 d . . . H(17) H 0.7058(3) 0.2072(3) 0.1802(4) 0.078(2) Uiso 1.00 1 d . . . H(18) H 0.7652(3) 0.2355(3) 0.2562(4) 0.078(2) Uiso 1.00 1 d . . . H(19) H 0.7441(3) 0.1292(3) 0.3136(4) 0.075(2) Uiso 1.00 1 d . . . H(20) H 0.6685(3) 0.1477(3) 0.3173(4) 0.075(2) Uiso 1.00 1 d . . . H(21) H 0.8083(3) 0.1349(3) 0.4881(5) 0.082(2) Uiso 1.00 1 d . . . H(22) H 0.8245(3) 0.1999(3) 0.4263(5) 0.082(2) Uiso 1.00 1 d . . . H(23) H 0.8505(3) 0.2226(3) 0.6010(5) 0.089(2) Uiso 1.00 1 d . . . H(24) H 0.7786(3) 0.1996(3) 0.6235(5) 0.089(2) Uiso 1.00 1 d . . . H(25) H 0.8618(3) 0.3459(3) 0.5674(5) 0.088(2) Uiso 1.00 1 d . . . H(26) H 0.8429(3) 0.3156(3) 0.4551(5) 0.088(2) Uiso 1.00 1 d . . . H(27) H 0.8150(3) 0.4287(3) 0.4502(6) 0.107(3) Uiso 1.00 1 d . . . H(28) H 0.7700(3) 0.4171(3) 0.5425(6) 0.107(3) Uiso 1.00 1 d . . . H(29) H 0.7538(3) 0.4187(3) 0.2719(6) 0.111(3) Uiso 1.00 1 d . . . H(30) H 0.7870(3) 0.3490(3) 0.2986(6) 0.111(3) Uiso 1.00 1 d . . . H(31) H 0.7021(3) 0.3323(3) 0.1632(5) 0.105(3) Uiso 1.00 1 d . . . H(32) H 0.6516(3) 0.3670(3) 0.2323(5) 0.105(3) Uiso 1.00 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N(I1) 0.0443(4) 0.0607(5) 0.0562(5) -0.0073(4) 0.0135(3) -0.0103(4) S(1) 0.065(1) 0.065(1) 0.059(1) -0.0021(9) 0.0051(8) -0.0109(9) S(2) 0.083(1) 0.092(1) 0.072(1) 0.002(1) -0.0057(9) 0.003(1) S(3) 0.091(1) 0.122(2) 0.109(2) 0.020(1) 0.010(1) 0.036(1) S(4) 0.073(1) 0.068(1) 0.109(2) 0.000(1) 0.008(1) 0.015(1) S(5) 0.0580(9) 0.058(1) 0.082(1) -0.0087(8) 0.0081(8) -0.0083(9) S(6) 0.0608(9) 0.065(1) 0.068(1) -0.0050(9) 0.0064(8) -0.0167(9) S(7) 0.074(1) 0.081(1) 0.068(1) 0.001(1) -0.0062(9) -0.020(1) S(8) 0.075(1) 0.101(2) 0.069(1) 0.022(1) -0.0016(9) -0.009(1) S(9) 0.071(1) 0.067(1) 0.068(1) -0.0030(9) 0.0025(9) -0.007(1) S(10) 0.0593(9) 0.061(1) 0.063(1) -0.0085(8) 0.0031(8) -0.0121(9) C(1) 0.053(4) 0.062(4) 0.059(4) -0.004(3) 0.011(3) -0.008(3) C(2) 0.064(4) 0.091(5) 0.078(5) 0.000(4) 0.021(3) 0.023(4) C(3) 0.043(3) 0.068(5) 0.067(4) 0.002(3) 0.014(3) 0.009(4) C(4) 0.049(3) 0.069(4) 0.053(4) -0.006(3) 0.010(3) -0.014(3) C(5) 0.048(3) 0.077(5) 0.060(4) -0.005(3) 0.018(3) -0.016(3) C(6) 0.043(3) 0.057(4) 0.058(4) -0.007(3) 0.009(3) -0.006(3) N(I2) 0.0455(4) 0.0573(5) 0.0606(5) -0.0030(4) 0.0070(3) -0.0000(4) S(11) 0.0473(8) 0.0452(9) 0.087(1) 0.0069(7) 0.0126(8) 0.0137(9) S(12) 0.0523(9) 0.063(1) 0.085(1) 0.0071(9) 0.0171(8) 0.020(1) S(13) 0.056(1) 0.095(1) 0.101(1) 0.014(1) 0.0273(9) 0.014(1) S(14) 0.0491(9) 0.071(1) 0.068(1) 0.0143(8) 0.0040(8) 0.0115(9) S(15) 0.0567(9) 0.086(1) 0.056(1) 0.0080(9) 0.0057(8) 0.0186(9) S(16) 0.057(1) 0.248(3) 0.107(2) 0.001(1) 0.004(1) 0.100(2) S(17) 0.086(1) 0.278(3) 0.061(1) -0.061(2) 0.012(1) 0.021(2) S(18) 0.115(2) 0.151(2) 0.188(2) -0.069(2) 0.102(2) -0.099(2) S(19) 0.086(1) 0.079(2) 0.328(4) 0.019(1) 0.112(2) 0.057(2) S(20) 0.062(1) 0.080(1) 0.196(2) 0.022(1) 0.055(1) 0.071(1) C(7) 0.045(3) 0.044(4) 0.055(4) -0.002(3) 0.010(3) -0.004(3) C(8) 0.055(3) 0.053(4) 0.067(4) 0.010(3) 0.008(3) -0.009(3) C(9) 0.041(3) 0.057(4) 0.047(3) -0.003(3) -0.000(3) -0.007(3) C(10) 0.063(4) 0.123(6) 0.053(4) -0.044(4) 0.011(3) -0.014(4) C(11) 0.089(5) 0.089(6) 0.129(6) -0.043(4) 0.052(5) -0.058(5) C(12) 0.061(4) 0.047(4) 0.116(6) -0.005(3) 0.034(4) -0.003(4) Ca(1) 0.0422(6) 0.0460(7) 0.0595(7) 0.0016(6) 0.0179(5) -0.0053(6) O(1) 0.074(3) 0.065(3) 0.104(4) 0.022(3) 0.029(3) 0.009(3) O(2) 0.068(3) 0.096(4) 0.102(4) -0.009(3) 0.039(3) -0.038(3) O(3) 0.062(3) 0.117(4) 0.057(3) -0.015(3) 0.016(2) 0.001(3) O(4) 0.047(2) 0.069(3) 0.083(3) -0.009(2) 0.006(2) -0.011(2) O(5) 0.057(2) 0.068(3) 0.067(3) 0.020(2) 0.020(2) 0.019(2) O(6) 0.069(3) 0.057(3) 0.098(3) 0.003(2) 0.031(3) 0.006(3) O(7) 0.056(2) 0.060(3) 0.070(3) -0.008(2) 0.014(2) -0.012(2) O(8) 0.057(2) 0.051(2) 0.049(2) 0.008(2) 0.009(2) -0.008(2) C(13) 0.123(7) 0.150(9) 0.087(6) 0.056(7) 0.026(5) 0.025(6) C(14) 0.091(6) 0.077(6) 0.141(7) 0.032(5) 0.022(5) -0.025(5) C(15) 0.101(6) 0.167(9) 0.059(5) -0.009(6) 0.013(5) -0.049(5) C(16) 0.071(5) 0.181(8) 0.057(5) 0.041(5) 0.001(4) -0.018(6) C(17) 0.132(7) 0.17(1) 0.126(8) -0.081(7) -0.005(6) 0.065(7) C(18) 0.179(9) 0.079(6) 0.090(6) -0.069(6) 0.062(6) -0.018(5) C(19) 0.075(5) 0.091(7) 0.19(1) -0.014(5) -0.011(6) -0.035(6) C(20) 0.093(6) 0.112(7) 0.20(1) -0.032(6) -0.037(6) 0.030(8) C(26) 0.084(5) 0.069(5) 0.114(6) -0.027(4) 0.020(5) -0.016(5) C(25) 0.053(4) 0.093(5) 0.074(5) -0.020(4) 0.004(3) -0.020(4) C(24) 0.070(4) 0.075(5) 0.076(5) 0.010(4) -0.009(3) -0.000(4) C(23) 0.064(4) 0.054(4) 0.088(5) 0.014(3) 0.002(4) -0.017(4) C(22) 0.069(4) 0.061(4) 0.059(4) 0.008(3) 0.019(3) -0.016(4) C(21) 0.070(4) 0.074(4) 0.050(4) 0.013(4) 0.013(3) -0.006(4) C(28) 0.079(5) 0.089(6) 0.095(6) 0.019(4) 0.018(4) 0.048(5) C(27) 0.082(5) 0.076(5) 0.119(6) 0.008(4) 0.040(5) 0.037(5) #============================================================================== _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR92' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 1.00' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 . S1 . 2.1593(16) yes Ni1 . S5 . 2.1608(17) yes Ni1 . S6 . 2.1550(15) yes Ni1 . S10 . 2.1691(17) yes S1 . C1 . 1.721(6) yes S2 . C1 . 1.738(5) yes S2 . C2 . 1.745(7) yes S3 . C2 . 1.629(6) yes S4 . C2 . 1.714(6) yes S4 . C3 . 1.735(6) yes S5 . C3 . 1.729(6) yes S6 . C4 . 1.714(6) yes S7 . C4 . 1.741(5) yes S7 . C5 . 1.742(6) yes S8 . C5 . 1.630(6) yes S9 . C5 . 1.729(5) yes S9 . C6 . 1.748(6) yes S10 . C6 . 1.720(5) yes C1 . C3 . 1.358(7) yes C4 . C6 . 1.361(7) yes Ni2 . S11 . 2.1614(16) yes Ni2 . S15 . 2.1578(16) yes Ni2 . S16 . 2.1263(19) yes Ni2 . S20 . 2.1360(18) yes S11 . C7 . 1.722(5) yes S12 . C7 . 1.738(5) yes S12 . C8 . 1.734(5) yes S13 . C8 . 1.636(5) yes S14 . C8 . 1.728(5) yes S14 . C9 . 1.749(5) yes S15 . C9 . 1.726(5) yes S16 . C10 . 1.695(7) yes S17 . C10 . 1.734(6) yes S17 . C11 . 1.688(8) yes S18 . C11 . 1.643(6) yes S19 . C11 . 1.724(7) yes S19 . C12 . 1.738(6) yes S20 . C12 . 1.704(6) yes C7 . C9 . 1.341(6) yes C10 . C12 . 1.320(8) yes Ca1 . O2 . 2.403(4) yes Ca1 . O3 . 2.377(4) yes Ca1 . O4 . 2.395(4) yes Ca1 . O5 . 2.401(4) yes Ca1 . O6 . 2.416(4) yes Ca1 . O7 . 2.453(4) yes Ca1 . O8 . 2.403(3) yes O1 . C13 . 1.381(7) yes O1 . C14 . 2.311(8) yes O1 . C19 . 2.380(8) yes O1 . C20 . 1.457(8) yes O1 . H1 . 1.923(8) no O1 . H2 . 1.927(7) no O1 . H4 . 2.493(9) no O1 . H15 . 1.973(8) no O1 . H16 . 1.957(9) no O2 . C13 . 2.417(9) yes O2 . C14 . 1.468(7) yes O2 . C15 . 1.376(7) yes O2 . C16 . 2.333(9) yes O2 . H3 . 2.005(7) no O2 . H4 . 1.978(9) no O2 . H5 . 1.923(7) no O2 . H6 . 1.918(7) no O3 . C15 . 2.488(9) yes O3 . C16 . 1.471(7) yes O3 . C17 . 1.385(7) yes O3 . C18 . 2.297(8) yes O3 . H7 . 2.004(6) no O3 . H8 . 1.979(8) no O3 . H9 . 1.915(8) no O3 . H10 . 1.915(8) no O4 . C17 . 2.387(8) yes O4 . C18 . 1.447(7) yes O4 . C19 . 1.396(7) yes O4 . C20 . 2.267(9) yes O4 . H11 . 1.964(7) no O4 . H12 . 1.952(8) no O4 . H13 . 1.942(7) no O4 . H14 . 1.910(8) no O5 . C22 . 2.357(6) yes O5 . C21 . 1.434(5) yes O5 . C28 . 1.441(6) yes O5 . C27 . 2.413(7) yes O5 . H17 . 1.970(6) no O5 . H18 . 1.970(5) no O5 . H31 . 1.972(6) no O5 . H32 . 1.971(6) no O6 . C26 . 1.434(7) yes O6 . C25 . 2.400(7) yes O6 . C28 . 2.389(8) yes O6 . C27 . 1.419(6) yes O6 . H27 . 1.971(6) no O6 . H28 . 1.959(7) no O6 . H29 . 1.961(6) no O6 . H30 . 1.952(6) no O7 . C26 . 2.352(8) yes O7 . C25 . 1.434(6) yes O7 . C24 . 1.443(6) yes O7 . C23 . 2.423(6) yes O7 . H23 . 1.973(6) no O7 . H24 . 1.958(7) no O7 . H25 . 1.977(6) no O7 . H26 . 1.967(6) no O8 . C24 . 2.327(6) yes O8 . C23 . 1.430(6) yes O8 . C22 . 1.423(5) yes O8 . C21 . 2.397(6) yes O8 . H19 . 1.955(5) no O8 . H20 . 1.947(6) no O8 . H21 . 1.979(6) no O8 . H22 . 1.968(6) no C13 . C14 . 1.460(9) yes C13 . C20 . 2.349(12) yes C13 . H3 . 2.01(1) no C13 . H4 . 1.95(1) no C13 . H15 . 2.392(12) no C14 . C15 . 2.345(11) yes C14 . H1 . 2.003(9) no C14 . H2 . 1.97(1) no C14 . H6 . 2.450(11) no C15 . C16 . 1.511(9) yes C15 . H3 . 2.426(11) no C15 . H7 . 2.04(1) no C15 . H8 . 1.998(8) no C16 . C17 . 2.392(11) yes C16 . H5 . 2.066(9) no C16 . H6 . 2.010(8) no C16 . H10 . 2.41(1) no C17 . C18 . 1.375(9) yes C17 . H7 . 2.463(11) no C17 . H11 . 1.913(9) no C17 . H12 . 1.885(11) no C18 . C19 . 2.389(11) yes C18 . H9 . 1.917(9) no C18 . H10 . 1.89(1) no C18 . H14 . 2.463(11) no C19 . C20 . 1.342(9) yes C19 . H11 . 2.387(11) no C19 . H15 . 1.89(1) no C19 . H16 . 1.837(11) no C20 . H2 . 2.427(12) no C20 . H13 . 1.907(9) no C20 . H14 . 1.847(11) no C26 . C25 . 1.489(8) yes C26 . C27 . 2.39(1) yes C26 . H25 . 2.035(8) no C26 . H26 . 2.010(8) no C26 . H30 . 2.50(1) no C25 . C24 . 2.422(9) yes C25 . H27 . 2.022(8) no C25 . H28 . 2.002(8) no C24 . C23 . 1.470(7) yes C24 . H21 . 2.023(7) no C24 . H22 . 1.984(7) no C23 . C22 . 2.394(8) yes C23 . H19 . 2.425(8) no C23 . H23 . 2.008(7) no C23 . H24 . 1.971(7) no C22 . C21 . 1.482(7) yes C22 . H17 . 2.029(7) no C22 . H18 . 2.000(7) no C21 . C28 . 2.413(8) yes C21 . H19 . 2.018(7) no C21 . H20 . 1.993(7) no C21 . H31 . 2.476(8) no C28 . C27 . 1.506(8) yes C28 . H29 . 2.037(8) no C28 . H30 . 2.017(8) no C27 . H27 . 2.46(1) no C27 . H31 . 2.049(9) no C27 . H32 . 2.010(8) no H1 . H2 . 1.551 no H1 . H3 . 2.330(9) no H1 . H4 . 2.234(9) no H1 . H15 . 2.422(12) no H2 . H3 . 2.27(1) no H2 . H6 . 2.26(1) no H2 . H14 . 2.345(12) no H2 . H15 . 2.376(12) no H3 . H4 . 1.551 no H3 . H5 . 2.388(11) no H3 . H6 . 2.473(11) no H5 . H6 . 1.551 no H5 . H7 . 2.38(1) no H5 . H8 . 2.299(9) no H6 . H7 . 2.296(9) no H6 . H10 . 2.449(12) no H7 . H8 . 1.551 no H7 . H10 . 2.33(1) no H9 . H10 . 1.551 no H9 . H11 . 2.29(1) no H9 . H12 . 2.081(9) no H10 . H11 . 2.084(9) no H11 . H12 . 1.551 no H11 . H13 . 2.438(11) no H11 . H14 . 2.315(11) no H13 . H14 . 1.551 no H13 . H15 . 2.246(9) no H13 . H16 . 2.089(9) no H14 . H15 . 2.09(1) no H15 . H16 . 1.551 no H17 . H18 . 1.551 no H17 . H19 . 2.356(7) no H17 . H20 . 2.274(7) no H17 . H31 . 2.481(8) no H18 . H19 . 2.274(7) no H18 . H22 . 2.452(8) no H18 . H30 . 2.335(9) no H19 . H20 . 1.551 no H19 . H21 . 2.440(8) no H19 . H22 . 2.468(8) no H21 . H22 . 1.551 no H21 . H23 . 2.346(7) no H21 . H24 . 2.256(7) no H22 . H23 . 2.262(7) no H22 . H26 . 2.339(9) no H23 . H24 . 1.551 no H23 . H25 . 2.487(9) no H25 . H26 . 1.551 no H25 . H27 . 2.339(8) no H25 . H28 . 2.302(8) no H26 . H27 . 2.302(8) no H26 . H30 . 2.270(9) no H27 . H28 . 1.551 no H27 . H29 . 2.46(1) no H29 . H30 . 1.551 no H29 . H31 . 2.363(9) no H29 . H32 . 2.286(8) no H30 . H31 . 2.308(8) no H31 . H32 . 1.551 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S16 . C10 . C12 . 120.0(5) yes S17 . C11 . S18 . 124.4(5) yes C13 . O1 . C20 . 111.7(6) yes C14 . O2 . C15 . 111.1(5) yes C16 . O3 . C17 . 113.7(6) yes C18 . O4 . C19 . 114.3(5) yes C21 . O5 . C28 . 114.2(4) yes C26 . O6 . C27 . 113.7(5) yes C25 . O7 . C24 . 114.7(4) yes C23 . O8 . C22 . 114.1(4) yes O1 . C13 . C14 . 108.8(6) yes O1 . C13 . H1 . 109.8(4) no C14 . C13 . H1 . 110.7(5) no O1 . C13 . H2 . 110.1(4) no C14 . C13 . H2 . 108.0(5) no H1 . C13 . H2 . 109.458 no O2 . C14 . C13 . 111.3(6) yes O2 . C14 . H3 . 110.2(3) no C13 . C14 . H3 . 111.4(4) no O2 . C14 . H4 . 107.9(3) no C13 . C14 . H4 . 106.4(5) no H3 . C14 . H4 . 109.458 no O2 . C15 . C16 . 107.7(6) yes O2 . C15 . H5 . 110.3(4) no C16 . C15 . H5 . 112.2(4) no O2 . C15 . H6 . 109.8(4) no C16 . C15 . H6 . 107.3(4) no H5 . C15 . H6 . 109.457 no O3 . C16 . C15 . 113.1(5) yes O3 . C16 . H7 . 109.9(3) no C15 . C16 . H7 . 110.3(4) no O3 . C16 . H8 . 107.7(3) no C15 . C16 . H8 . 106.3(4) no H7 . C16 . H8 . 109.463 no O3 . C17 . C18 . 112.6(7) yes O3 . C17 . H9 . 108.8(4) no C18 . C17 . H9 . 109.8(6) no O3 . C17 . H10 . 108.8(5) no C18 . C17 . H10 . 107.4(6) no H9 . C17 . H10 . 109.469 no O4 . C18 . C17 . 115.5(6) yes O4 . C18 . H11 . 108.2(4) no C17 . C18 . H11 . 109.4(5) no O4 . C18 . H12 . 107.2(3) no C17 . C18 . H12 . 106.9(6) no H11 . C18 . H12 . 109.465 no O4 . C19 . C20 . 111.8(7) yes O4 . C19 . H13 . 110.3(3) no C20 . C19 . H13 . 111.5(5) no O4 . C19 . H14 . 107.4(4) no C20 . C19 . H14 . 106.1(6) no H13 . C19 . H14 . 109.460 no O1 . C20 . C19 . 116.4(7) yes O1 . C20 . H15 . 108.3(4) no C19 . C20 . H15 . 110.3(5) no O1 . C20 . H16 . 106.9(4) no C19 . C20 . H16 . 105.3(6) no H15 . C20 . H16 . 109.466 no O6 . C26 . C25 . 110.4(5) yes O6 . C26 . H27 . 109.9(3) no C25 . C26 . H27 . 110.0(3) no O6 . C26 . H28 . 108.8(3) no C25 . C26 . H28 . 108.3(4) no H27 . C26 . H28 . 109.468 no O7 . C25 . C26 . 107.1(5) yes O7 . C25 . H25 . 110.5(3) no C26 . C25 . H25 . 111.2(3) no O7 . C25 . H26 . 109.6(3) no C26 . C25 . H26 . 109.0(4) no H25 . C25 . H26 . 109.453 no O7 . C24 . C23 . 112.6(5) yes O7 . C24 . H23 . 109.3(3) no C23 . C24 . H23 . 110.3(3) no O7 . C24 . H24 . 108.0(3) no C23 . C24 . H24 . 107.1(3) no H23 . C24 . H24 . 109.460 no O8 . C23 . C24 . 106.7(4) yes O8 . C23 . H21 . 110.8(3) no C24 . C23 . H21 . 111.6(3) no O8 . C23 . H22 . 109.9(3) no C24 . C23 . H22 . 108.3(3) no H21 . C23 . H22 . 109.458 no O8 . C22 . C21 . 111.2(5) yes O8 . C22 . H19 . 109.3(3) no C21 . C22 . H19 . 110.2(3) no O8 . C22 . H20 . 108.6(3) no C21 . C22 . H20 . 108.0(3) no H19 . C22 . H20 . 109.469 no O5 . C21 . C22 . 107.9(4) yes O5 . C21 . H17 . 109.8(3) no C22 . C21 . H17 . 111.2(3) no O5 . C21 . H18 . 109.8(3) no C22 . C21 . H18 . 108.7(3) no H17 . C21 . H18 . 109.465 no O5 . C28 . C27 . 109.9(5) yes O5 . C28 . H31 . 109.4(3) no C27 . C28 . H31 . 111.1(4) no O5 . C28 . H32 . 109.2(3) no C27 . C28 . H32 . 107.7(4) no H31 . C28 . H32 . 109.466 no O6 . C27 . C28 . 109.5(5) yes O6 . C27 . H29 . 110.2(3) no C28 . C27 . H29 . 110.0(3) no O6 . C27 . H30 . 109.3(3) no C28 . C27 . H30 . 108.3(4) no H29 . C27 . H30 . 109.466 no C13 . H1 . H2 . 35.273 no C13 . H2 . H1 . 35.269 no C14 . H3 . H4 . 35.271 no C14 . H4 . H3 . 35.271 no C15 . H5 . H6 . 35.273 no C15 . H6 . H5 . 35.270 no C16 . H7 . H8 . 35.268 no C16 . H8 . H7 . 35.269 no C17 . H9 . H10 . 35.264 no C17 . H10 . H9 . 35.267 no C18 . H11 . H12 . 35.268 no C18 . H12 . H11 . 35.267 no C19 . H13 . H14 . 35.268 no C19 . H14 . H13 . 35.272 no C20 . H15 . H16 . 35.267 no C20 . H16 . H15 . 35.268 no C21 . H17 . H18 . 35.268 no C21 . H18 . H17 . 35.267 no C22 . H19 . H20 . 35.266 no C22 . H20 . H19 . 35.265 no C23 . H21 . H22 . 35.271 no C23 . H22 . H21 . 35.271 no C24 . H23 . H24 . 35.273 no C24 . H24 . H23 . 35.267 no C25 . H25 . H26 . 35.274 no C25 . H26 . H25 . 35.273 no C26 . H27 . H28 . 35.266 no C26 . H28 . H27 . 35.266 no C27 . H29 . H30 . 35.268 no C27 . H30 . H29 . 35.265 no C28 . H31 . H32 . 35.268 no C28 . H32 . H31 . 35.267 no loop_ _geom_contact_atom_site_label_1 _geom_contact_site_symmetry_1 _geom_contact_atom_site_label_2 _geom_contact_site_symmetry_2 _geom_contact_distance _geom_contact_publ_flag Ni1 . H18 4_455 3.084(5) no Ni1 . H22 4_455 3.543(6) no Ni1 . H26 4_455 3.591(6) no Ni1 . H30 4_455 3.282(6) no S1 . C21 4_455 3.889(5) yes S1 . H17 4_455 3.726(6) no S1 . H18 4_455 3.214(5) no S1 . H30 4_455 3.414(7) no S1 . H31 4_455 3.383(6) no S2 . C16 4_454 3.706(7) yes S2 . H7 4_454 3.404(7) no S2 . H8 4_454 3.226(7) no S2 . H17 4_455 3.746(5) no S2 . H24 4_454 3.638(6) no S3 . S9 4_454 3.900(2) yes S3 . C5 4_454 3.842(5) yes S3 . S13 4_554 3.621(2) yes S3 . C10 3_555 3.944(7) yes S3 . C17 4_454 3.992(9) yes S3 . H9 4_454 3.150(9) no S3 . H24 4_454 3.795(7) no S3 . H28 2_666 3.601(7) no S4 . S8 4_454 3.815(2) yes S4 . C14 2_666 3.983(8) yes S4 . H3 2_666 3.988(8) no S4 . H4 2_666 3.192(8) no S4 . H17 4_455 3.878(5) no S4 . H27 2_666 3.935(7) no S4 . H28 2_666 3.663(7) no S5 . S11 3_556 3.836(2) yes S5 . S12 3_556 3.655(2) yes S5 . C21 4_455 3.852(5) yes S5 . H17 4_455 3.872(6) no S5 . H18 4_455 3.187(5) no S5 . H19 4_455 3.541(5) no S5 . H22 4_455 3.516(6) no S6 . S14 4_555 3.689(2) yes S6 . S15 4_555 3.754(2) yes S6 . H22 4_455 3.207(6) no S6 . H26 4_455 3.382(6) no S7 . H16 1_556 3.92(1) no S7 . H17 1_556 3.317(6) no S8 . S9 2_657 3.991(2) yes S8 . C2 4_555 3.923(6) yes S8 . S18 1_556 3.459(2) yes S8 . C26 3_646 3.841(7) yes S8 . C22 1_556 3.738(6) yes S8 . C21 1_556 4.000(6) yes S8 . H17 1_556 3.363(6) no S8 . H19 1_556 3.585(6) no S8 . H20 1_556 3.219(6) no S8 . H29 3_646 3.875(8) no S9 . S9 2_657 3.578(3) yes S9 . S18 2_656 3.553(2) yes S10 . C27 4_455 3.912(6) yes S10 . H26 4_455 3.568(6) no S10 . H27 4_455 3.911(7) no S10 . H29 4_455 3.818(6) no S10 . H30 4_455 3.149(6) no C1 . C21 4_455 3.693(7) yes C1 . H17 4_455 3.203(7) no C1 . H18 4_455 3.276(7) no C1 . H31 4_455 3.870(9) no C2 . S13 4_554 3.618(6) yes C2 . H24 4_454 3.999(8) no C3 . C21 4_455 3.676(7) yes C3 . H17 4_455 3.274(7) no C3 . H18 4_455 3.266(7) no C3 . H19 4_455 3.783(7) no C4 . H25 4_455 3.777(7) no C4 . H26 4_455 3.399(7) no C5 . S18 1_556 3.839(5) yes C5 . H17 1_556 3.758(8) no C6 . H25 4_455 3.902(7) no C6 . H26 4_455 3.467(7) no Ni2 . S13 2_556 3.838(2) yes Ni2 . C28 4_455 3.658(6) yes Ni2 . H5 4_454 3.977(6) no Ni2 . H21 2_656 3.596(6) no Ni2 . H29 4_455 3.529(7) no Ni2 . H31 4_455 3.100(6) no Ni2 . H32 4_455 3.497(6) no S11 . S14 2_556 3.878(2) yes S11 . C23 2_656 3.787(6) yes S11 . C28 4_455 3.689(6) yes S11 . C27 4_455 3.823(7) yes S11 . H19 2_656 3.152(6) no S11 . H21 2_656 3.008(6) no S11 . H22 2_656 3.836(6) no S11 . H29 4_455 3.151(7) no S11 . H31 4_455 3.677(6) no S11 . H32 4_455 3.124(6) no S12 . S15 2_556 3.808(2) yes S12 . C9 2_556 3.959(5) yes S12 . O1 4_455 3.878(4) yes S12 . C13 4_455 3.803(7) yes S12 . H1 4_455 3.067(7) no S12 . H3 3_546 3.237(7) no S12 . H4 4_455 3.818(9) no S12 . H5 3_546 3.401(8) no S12 . H6 3_546 3.837(8) no S12 . H32 4_455 3.797(6) no S13 . H1 4_455 3.226(8) no S13 . H3 3_546 3.315(8) no S13 . H5 3_546 3.478(8) no S13 . H15 4_455 3.259(9) no S13 . H21 1_455 3.614(6) no S13 . H23 1_455 3.668(6) no S13 . H24 1_455 3.637(6) no S14 . C7 2_556 3.711(5) yes S14 . C9 2_556 3.990(5) yes S14 . C20 4_455 3.988(9) yes S14 . C23 1_455 3.875(6) yes S14 . H15 4_455 3.652(9) no S14 . H16 4_455 3.546(8) no S14 . H21 1_455 3.364(6) no S14 . H22 1_455 3.799(6) no S14 . H23 1_455 3.358(6) no S14 . H32 4_455 3.966(6) no S15 . C8 2_556 3.830(5) yes S15 . C15 4_454 3.831(7) yes S15 . C28 4_455 3.733(6) yes S15 . H5 4_454 3.085(7) no S15 . H7 4_454 3.570(8) no S15 . H31 4_455 3.195(6) no S15 . H32 4_455 3.365(7) no S16 . C15 4_454 3.563(7) yes S16 . C16 4_454 3.415(8) yes S16 . H7 4_454 3.509(8) no S16 . H31 4_455 3.920(7) no S17 . O7 4_454 3.876(4) yes S17 . C25 4_454 3.688(6) yes S17 . H28 4_454 3.545(8) no S18 . S19 2_656 3.852(4) yes S19 . S19 2_656 3.314(5) yes S19 . C18 2_656 3.491(8) yes S19 . H9 2_656 3.64(1) no S19 . H11 2_656 3.262(8) no S20 . O8 2_656 3.705(4) yes S20 . C23 2_656 3.947(6) yes S20 . C22 2_656 3.620(6) yes S20 . H12 2_656 3.485(8) no S20 . H19 2_656 3.207(6) no S20 . H20 2_656 3.449(6) no S20 . H21 2_656 3.290(6) no S20 . H29 4_455 3.411(7) no C7 . C9 2_556 3.868(7) yes C7 . C28 4_455 3.720(8) yes C7 . H31 4_455 3.819(8) no C8 . O1 4_455 3.822(7) yes C8 . C13 4_455 3.889(9) yes C8 . C20 4_455 3.80(1) yes C8 . H1 4_455 3.137(9) no C8 . H3 3_546 3.704(9) no C8 . H5 3_546 3.77(1) no C8 . H15 4_455 3.26(1) no C8 . H16 4_455 3.77(1) no C8 . H21 1_455 3.898(8) no C8 . H23 1_455 3.958(8) no C9 . C9 2_556 3.88(1) yes C9 . C28 4_455 3.729(7) yes C9 . H31 4_455 3.619(7) no C10 . H8 4_454 3.854(11) no C12 . H12 2_656 3.40(1) no C13 . H3 2_666 3.681(9) no C14 . H1 2_666 3.61(1) no C14 . H3 2_666 3.954(15) no H1 . H1 2_666 3.758(18) no H1 . H4 2_666 3.637(9) no H3 . H3 2_666 3.615(15) no H3 . H4 2_666 3.910(14) no H15 . H23 4_454 3.65(1) no H16 . H23 4_454 3.984(9) no #============================================================================== #============================================================================== # End of CIF #============================================================================== #============================================================================== data__densi01 _database_code_CSD 158717 _audit_creation_date '2001-05-01' _audit_creation_method 'by CrystalStructure v1.00' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C28 H32 Ca O8 Ni2 S20 ' _chemical_formula_moiety 'C28 H32 Ca O8 Ni2 S20 ' _chemical_formula_weight 1295.24 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _cell_length_a 19.8366(2) _cell_length_b 19.5053(3) _cell_length_c 12.5358(4) _cell_angle_alpha 90 _cell_angle_beta 94.7610(2) _cell_angle_gamma 90 _cell_volume 4833.6(-12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 67140 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.793 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.637 _exptl_absorpt_correction_T_max 0.836 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11401 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9562 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9562 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). 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_gt 8538 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0370 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 8538 _refine_ls_number_parameters 564 _refine_ls_goodness_of_fit_ref 1.790 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/\s^2^(Fo^2^)' _refine_ls_shift/su_max 0.0530 _refine_diff_density_max 0.33 _refine_diff_density_min -0.49 _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' 0.006 0.003 ; 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) ; 'O' 'O' 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Ca' 'Ca' 0.252 0.372 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Ni' 'Ni' 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.148 0.159 ; 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 1.09089(1) -0.26431(1) -0.21055(2) 0.02266(6) Uani 1.00 1 d . . . Ni(2) Ni 1.30851(1) -0.45278(1) -0.00175(2) 0.02154(6) Uani 1.00 1 d . . . Ca(1) Ca 0.83988(2) -0.21229(2) 0.03968(3) 0.01979(9) Uani 1.00 1 d . . . S(1) S 1.06795(2) -0.37176(3) -0.23941(4) 0.0265(1) Uani 1.00 1 d . . . S(2) S 0.97159(3) -0.44012(3) -0.40887(4) 0.0293(1) Uani 1.00 1 d . . . S(3) S 0.87123(3) -0.43800(3) -0.59845(4) 0.0350(1) Uani 1.00 1 d . . . S(4) S 0.93711(3) -0.31024(3) -0.51250(4) 0.0326(1) Uani 1.00 1 d . . . S(5) S 1.03065(2) -0.23108(3) -0.35278(4) 0.0276(1) Uani 1.00 1 d . . . S(6) S 1.10937(2) -0.15649(3) -0.17975(4) 0.0285(1) Uani 1.00 1 d . . . S(7) S 1.19787(3) -0.08463(3) -0.00513(4) 0.0350(1) Uani 1.00 1 d . . . S(8) S 1.29381(3) -0.08165(3) 0.19020(5) 0.0459(2) Uani 1.00 1 d . . . S(9) S 1.23804(3) -0.21276(3) 0.09795(4) 0.0354(1) Uani 1.00 1 d . . . S(10) S 1.15285(2) -0.29656(3) -0.06898(4) 0.0269(1) Uani 1.00 1 d . . . S(11) S 1.21128(2) -0.49945(3) -0.04540(4) 0.0357(1) Uani 1.00 1 d . . . S(12) S 1.07778(3) -0.48657(3) 0.05584(5) 0.0455(2) Uani 1.00 1 d . . . S(13) S 0.98978(3) -0.43284(3) 0.21872(5) 0.0457(2) Uani 1.00 1 d . . . S(14) S 1.13521(3) -0.39627(4) 0.22019(4) 0.0450(2) Uani 1.00 1 d . . . S(15) S 1.27227(3) -0.40043(4) 0.13229(4) 0.0448(2) Uani 1.00 1 d . . . S(16) S 1.39975(2) -0.39298(3) 0.03085(4) 0.0257(1) Uani 1.00 1 d . . . S(17) S 1.53266(2) -0.39466(3) -0.07349(4) 0.0263(1) Uani 1.00 1 d . . . S(18) S 1.62387(2) -0.44359(3) -0.23396(4) 0.0354(1) Uani 1.00 1 d . . . S(19) S 1.48686(2) -0.50388(3) -0.21842(4) 0.0265(1) Uani 1.00 1 d . . . S(20) S 1.34946(2) -0.51092(3) -0.12829(4) 0.0239(1) Uani 1.00 1 d . . . O(1) O 0.87671(6) -0.12506(7) -0.07824(9) 0.0258(4) Uani 1.00 1 d . . . O(2) O 0.86413(6) -0.26255(7) -0.12752(9) 0.0255(3) Uani 1.00 1 d . . . O(3) O 0.93412(6) -0.28994(6) 0.06355(9) 0.0241(3) Uani 1.00 1 d . . . O(4) O 0.94599(6) -0.15447(7) 0.11494(9) 0.0256(4) Uani 1.00 1 d . . . O(5) O 0.77822(6) -0.31575(7) 0.07073(9) 0.0226(3) Uani 1.00 1 d . . . O(6) O 0.72562(6) -0.21109(7) -0.05472(9) 0.0248(3) Uani 1.00 1 d . . . O(7) O 0.77311(6) -0.11925(7) 0.1014(1) 0.0277(4) Uani 1.00 1 d . . . O(8) O 0.82638(6) -0.22655(7) 0.22648(9) 0.0242(3) Uani 1.00 1 d . . . C(1) C 1.01173(9) -0.3678(1) -0.3515(1) 0.0248(5) Uani 1.00 1 d . . . C(2) C 0.92373(9) -0.3983(1) -0.5110(1) 0.0252(5) Uani 1.00 1 d . . . C(3) C 0.99549(9) -0.3066(1) -0.4002(1) 0.0252(5) Uani 1.00 1 d . . . C(4) C 1.16325(9) -0.1588(1) -0.0648(1) 0.0271(5) Uani 1.00 1 d . . . C(5) C 1.2459(1) -0.1239(1) 0.0999(1) 0.0330(6) Uani 1.00 1 d . . . C(6) C 1.18165(9) -0.2191(1) -0.0167(1) 0.0265(5) Uani 1.00 1 d . . . C(7) C 1.16322(9) -0.4680(1) 0.0517(1) 0.0271(5) Uani 1.00 1 d . . . C(8) C 1.0636(1) -0.4388(1) 0.1684(2) 0.0338(6) Uani 1.00 1 d . . . C(9) C 1.18997(9) -0.4251(1) 0.1286(1) 0.0283(5) Uani 1.00 1 d . . . C(10) C 1.45065(8) -0.4254(1) -0.0610(1) 0.0222(5) Uani 1.00 1 d . . . C(11) C 1.55166(9) -0.4471(1) -0.1787(1) 0.0259(5) Uani 1.00 1 d . . . C(12) C 1.42905(9) -0.4762(1) -0.1299(1) 0.0217(5) Uani 1.00 1 d . . . C(13) C 0.90207(9) -0.1494(1) -0.1759(1) 0.0285(5) Uani 1.00 1 d . . . C(14) C 0.86089(9) -0.2112(1) -0.2106(1) 0.0287(5) Uani 1.00 1 d . . . C(15) C 0.92156(9) -0.3068(1) -0.1283(1) 0.0317(6) Uani 1.00 1 d . . . C(16) C 0.9305(1) -0.3405(1) -0.0204(1) 0.0307(6) Uani 1.00 1 d . . . C(17) C 1.00041(9) -0.2634(1) 0.0920(2) 0.0341(6) Uani 1.00 1 d . . . C(18) C 0.9923(1) -0.2043(1) 0.1649(2) 0.0344(6) Uani 1.00 1 d . . . C(19) C 0.97624(9) -0.1086(1) 0.0431(1) 0.0308(5) Uani 1.00 1 d . . . C(20) C 0.9194(1) -0.0750(1) -0.0226(2) 0.0325(6) Uani 1.00 1 d . . . C(21) C 0.70873(9) -0.3220(1) 0.0279(1) 0.0290(5) Uani 1.00 1 d . . . C(22) C 0.7015(1) -0.2801(1) -0.0734(1) 0.0298(5) Uani 1.00 1 d . . . C(23) C 0.67819(9) -0.1666(1) -0.0083(2) 0.0312(6) Uani 1.00 1 d . . . C(24) C 0.7165(1) -0.1027(1) 0.0254(2) 0.0352(6) Uani 1.00 1 d . . . C(25) C 0.7550(1) -0.1255(1) 0.2102(1) 0.0322(6) Uani 1.00 1 d . . . C(26) C 0.8122(1) -0.1610(1) 0.2734(1) 0.0306(6) Uani 1.00 1 d . . . C(27) C 0.78344(9) -0.2814(1) 0.2561(1) 0.0271(5) Uani 1.00 1 d . . . C(28) C 0.79175(9) -0.3392(1) 0.1794(1) 0.0256(5) Uani 1.00 1 d . . . H(1) H 0.89845(9) -0.1148(1) -0.2294(1) 0.034(1) Uiso 1.00 1 d . . . H(2) H 0.94810(9) -0.1626(1) -0.1624(1) 0.034(1) Uiso 1.00 1 d . . . H(3) H 0.87671(9) -0.2303(1) -0.2736(1) 0.034(1) Uiso 1.00 1 d . . . H(4) H 0.81530(9) -0.1967(1) -0.2250(1) 0.034(1) Uiso 1.00 1 d . . . H(5) H 0.91455(9) -0.3401(1) -0.1833(1) 0.038(1) Uiso 1.00 1 d . . . H(6) H 0.96055(9) -0.2804(1) -0.1397(1) 0.038(1) Uiso 1.00 1 d . . . H(7) H 0.9714(1) -0.3661(1) -0.0145(1) 0.037(1) Uiso 1.00 1 d . . . H(8) H 0.8934(1) -0.3704(1) -0.0128(1) 0.037(1) Uiso 1.00 1 d . . . H(9) H 1.02826(9) -0.2978(1) 0.1263(2) 0.041(1) Uiso 1.00 1 d . . . H(10) H 1.01996(9) -0.2481(1) 0.0295(2) 0.041(1) Uiso 1.00 1 d . . . H(11) H 1.0350(1) -0.1829(1) 0.1814(2) 0.040(1) Uiso 1.00 1 d . . . H(12) H 0.9755(1) -0.2208(1) 0.2289(2) 0.040(1) Uiso 1.00 1 d . . . H(13) H 1.00345(9) -0.0755(1) 0.0821(1) 0.038(1) Uiso 1.00 1 d . . . H(14) H 1.00332(9) -0.1338(1) -0.0022(1) 0.037(1) Uiso 1.00 1 d . . . H(15) H 0.9367(1) -0.0452(1) -0.0737(2) 0.040(1) Uiso 1.00 1 d . . . H(16) H 0.8936(1) -0.0493(1) 0.0239(2) 0.040(1) Uiso 1.00 1 d . . . H(17) H 0.69790(9) -0.3687(1) 0.0138(1) 0.035(1) Uiso 1.00 1 d . . . H(18) H 0.67951(9) -0.3041(1) 0.0774(1) 0.034(1) Uiso 1.00 1 d . . . H(19) H 0.6554(1) -0.2789(1) -0.1009(1) 0.035(1) Uiso 1.00 1 d . . . H(20) H 0.7279(1) -0.3011(1) -0.1243(1) 0.035(1) Uiso 1.00 1 d . . . H(21) H 0.64164(9) -0.1561(1) -0.0595(2) 0.037(1) Uiso 1.00 1 d . . . H(22) H 0.66125(9) -0.1879(1) 0.0522(2) 0.037(1) Uiso 1.00 1 d . . . H(23) H 0.6873(1) -0.0720(1) 0.0581(2) 0.043(1) Uiso 1.00 1 d . . . H(24) H 0.7327(1) -0.0816(1) -0.0358(2) 0.042(1) Uiso 1.00 1 d . . . H(25) H 0.7475(1) -0.0814(1) 0.2392(1) 0.039(1) Uiso 1.00 1 d . . . H(26) H 0.7150(1) -0.1523(1) 0.2116(1) 0.039(1) Uiso 1.00 1 d . . . H(27) H 0.8005(1) -0.1684(1) 0.3445(1) 0.037(1) Uiso 1.00 1 d . . . H(28) H 0.8510(1) -0.1325(1) 0.2747(1) 0.037(1) Uiso 1.00 1 d . . . H(29) H 0.79526(9) -0.2954(1) 0.3278(1) 0.033(1) Uiso 1.00 1 d . . . H(30) H 0.73777(9) -0.2663(1) 0.2492(1) 0.033(1) Uiso 1.00 1 d . . . H(31) H 0.76112(9) -0.3752(1) 0.1921(1) 0.031(1) Uiso 1.00 1 d . . . H(32) H 0.83684(9) -0.3558(1) 0.1901(1) 0.031(1) Uiso 1.00 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0194(1) 0.0256(1) 0.0233(1) 0.0030(1) 0.0035(1) 0.0034(1) Ni(2) 0.0187(1) 0.0222(1) 0.0236(1) -0.0005(1) 0.0011(1) -0.0014(1) Ca(1) 0.0179(2) 0.0194(2) 0.0229(2) -0.0008(2) 0.0063(1) 0.0012(1) S(1) 0.0246(2) 0.0269(3) 0.0275(2) 0.0042(2) -0.0008(2) 0.0032(2) S(2) 0.0297(3) 0.0289(3) 0.0286(3) 0.0014(2) -0.0013(2) 0.0029(2) S(3) 0.0312(3) 0.0427(4) 0.0303(3) -0.0097(3) -0.0023(2) 0.0059(2) S(4) 0.0329(3) 0.0339(3) 0.0297(3) -0.0011(3) -0.0060(2) 0.0082(2) S(5) 0.0277(3) 0.0269(3) 0.0280(3) 0.0013(2) 0.0005(2) 0.0071(2) S(6) 0.0259(2) 0.0263(3) 0.0331(3) 0.0044(2) 0.0011(2) 0.0037(2) S(7) 0.0310(3) 0.0294(3) 0.0443(3) 0.0011(3) 0.0010(3) -0.0041(2) S(8) 0.0375(3) 0.0526(4) 0.0468(3) -0.0069(3) -0.0015(3) -0.0160(3) S(9) 0.0357(3) 0.0382(3) 0.0308(3) 0.0012(3) -0.0056(2) -0.0007(2) S(10) 0.0278(3) 0.0265(3) 0.0261(2) 0.0020(2) 0.0003(2) 0.0044(2) S(11) 0.0227(3) 0.0346(3) 0.0510(3) -0.0066(3) 0.0108(2) -0.0219(3) S(12) 0.0264(3) 0.0347(3) 0.0781(4) -0.0059(3) 0.0210(3) -0.0195(3) S(13) 0.0382(3) 0.0517(4) 0.0508(3) 0.0170(3) 0.0248(3) 0.0217(3) S(14) 0.0328(3) 0.0759(5) 0.0263(3) 0.0153(3) 0.0026(2) -0.0107(3) S(15) 0.0238(3) 0.0701(5) 0.0398(3) -0.0007(3) -0.0010(2) -0.0290(3) S(16) 0.0228(2) 0.0309(3) 0.0230(2) -0.0045(2) 0.0005(2) -0.0051(2) S(17) 0.0215(2) 0.0297(3) 0.0275(2) -0.0055(2) 0.0007(2) 0.0001(2) S(18) 0.0233(3) 0.0407(3) 0.0436(3) -0.0034(3) 0.0109(2) -0.0006(3) S(19) 0.0223(2) 0.0259(3) 0.0318(3) -0.0010(2) 0.0057(2) -0.0029(2) S(20) 0.0201(2) 0.0211(3) 0.0307(2) -0.0026(2) 0.0036(2) -0.0037(2) O(1) 0.0243(7) 0.0250(8) 0.0285(7) -0.0016(6) 0.0054(6) 0.0050(6) O(2) 0.0217(6) 0.0313(8) 0.0239(7) 0.0044(6) 0.0038(6) 0.0030(6) O(3) 0.0225(6) 0.0215(7) 0.0279(7) 0.0016(6) 0.0002(6) -0.0026(6) O(4) 0.0255(7) 0.0221(8) 0.0297(7) -0.0029(6) 0.0058(6) 0.0000(6) O(5) 0.0237(7) 0.0240(7) 0.0202(6) -0.0038(6) 0.0021(5) 0.0036(5) O(6) 0.0230(7) 0.0229(8) 0.0290(7) -0.0012(6) 0.0046(6) 0.0016(6) O(7) 0.0256(7) 0.0232(8) 0.0355(7) 0.0010(6) 0.0095(6) -0.0025(6) O(8) 0.0250(7) 0.0243(8) 0.0241(7) -0.0055(6) 0.0074(6) -0.0050(6) C(1) 0.0212(9) 0.032(1) 0.0216(9) 0.0031(9) 0.0042(8) 0.0023(8) C(2) 0.0221(9) 0.032(1) 0.0222(9) -0.0009(9) 0.0050(8) 0.0045(8) C(3) 0.022(1) 0.031(1) 0.023(1) 0.0035(9) 0.0022(8) 0.0045(8) C(4) 0.0189(9) 0.033(1) 0.030(1) 0.002(1) 0.0057(8) -0.0022(9) C(5) 0.025(1) 0.040(1) 0.035(1) -0.001(1) 0.0069(9) -0.005(1) C(6) 0.0215(9) 0.033(1) 0.025(1) 0.0026(9) 0.0032(8) 0.0012(9) C(7) 0.0214(9) 0.021(1) 0.039(1) 0.0015(9) 0.0081(9) -0.0004(9) C(8) 0.035(1) 0.032(1) 0.036(1) 0.012(1) 0.012(1) 0.0142(9) C(9) 0.0238(9) 0.035(1) 0.026(1) 0.009(1) 0.0004(8) 0.0014(9) C(10) 0.0175(9) 0.024(1) 0.0241(9) -0.0009(9) -0.0010(8) 0.0046(8) C(11) 0.0241(9) 0.025(1) 0.028(1) -0.0001(9) 0.0002(8) 0.0031(8) C(12) 0.0194(9) 0.019(1) 0.0265(9) 0.0024(9) 0.0024(8) 0.0039(8) C(13) 0.025(1) 0.040(1) 0.0209(9) -0.002(1) 0.0037(8) 0.0086(9) C(14) 0.026(1) 0.040(1) 0.0196(9) -0.002(1) -0.0001(8) 0.0043(9) C(15) 0.026(1) 0.036(1) 0.033(1) 0.009(1) 0.0050(9) -0.0058(9) C(16) 0.029(1) 0.024(1) 0.039(1) 0.006(1) 0.0044(9) -0.0023(9) C(17) 0.025(1) 0.031(1) 0.045(1) 0.004(1) -0.006(1) 0.004(1) C(18) 0.031(1) 0.035(1) 0.036(1) -0.003(1) -0.007(1) 0.003(1) C(19) 0.030(1) 0.031(1) 0.032(1) -0.013(1) 0.0074(9) -0.0029(9) C(20) 0.040(1) 0.022(1) 0.038(1) -0.006(1) 0.013(1) 0.0024(9) C(21) 0.024(1) 0.027(1) 0.035(1) -0.007(1) -0.0003(9) 0.0045(9) C(22) 0.028(1) 0.031(1) 0.029(1) -0.005(1) -0.0036(9) 0.0009(9) C(23) 0.022(1) 0.040(1) 0.032(1) 0.007(1) 0.0043(9) 0.0053(9) C(24) 0.034(1) 0.028(1) 0.045(1) 0.010(1) 0.008(1) 0.004(1) C(25) 0.031(1) 0.032(1) 0.035(1) -0.003(1) 0.0092(9) -0.0127(9) C(26) 0.030(1) 0.032(1) 0.031(1) -0.009(1) 0.0063(9) -0.0127(9) C(27) 0.030(1) 0.027(1) 0.025(1) -0.009(1) 0.0084(9) 0.0021(8) C(28) 0.028(1) 0.025(1) 0.0234(9) -0.0037(9) 0.0033(8) 0.0061(8) #============================================================================== _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR92' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 1.00' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 . S1 . 2.169(12) yes Ni1 . S5 . 2.162(19) yes Ni1 . S6 . 2.164(13) yes Ni1 . S10 . 2.167(18) yes Ni2 . S11 . 2.162(8) yes Ni2 . S15 . 2.14(3) yes Ni2 . S16 . 2.163(8) yes Ni2 . S20 . 2.16(3) yes Ca1 . O1 . 2.41(4) yes Ca1 . O2 . 2.40(3) yes Ca1 . O3 . 2.405(7) yes Ca1 . O5 . 2.408(11) yes Ca1 . O6 . 2.4684(13) yes Ca1 . O7 . 2.41(2) yes Ca1 . O8 . 2.40(1) yes S1 . C1 . 1.722(3) yes S2 . C1 . 1.74(2) yes S2 . C2 . 1.73(2) yes S3 . C2 . 1.642(18) yes S4 . C2 . 1.739(2) yes S4 . C3 . 1.748(3) yes S5 . C3 . 1.715(18) yes S6 . C4 . 1.722(2) yes S7 . C4 . 1.74(2) yes S7 . C5 . 1.74(2) yes S8 . C5 . 1.64(2) yes S9 . C5 . 1.740(2) yes S9 . C6 . 1.751(4) yes S10 . C6 . 1.72(2) yes S11 . C7 . 1.720(15) yes S12 . C7 . 1.7380(18) yes S12 . C8 . 1.73(3) yes S13 . C8 . 1.647(2) yes S14 . C8 . 1.724(11) yes S14 . C9 . 1.738(13) yes S15 . C9 . 1.699(2) yes S16 . C10 . 1.714(15) yes S17 . C10 . 1.753(3) yes S17 . C11 . 1.73(3) yes S18 . C11 . 1.644(2) yes S19 . C11 . 1.739(11) yes S19 . C12 . 1.747(12) yes S20 . C12 . 1.7199(18) yes O1 . C13 . 1.442(14) yes O1 . C14 . 2.36(4) yes O1 . C19 . 2.411(7) yes O1 . C20 . 1.434(17) yes O1 . H1 . 1.988(7) no O1 . H2 . 1.975(14) no O1 . H15 . 1.959(3) no O1 . H16 . 1.96(3) no O2 . C13 . 2.425(19) yes O2 . C14 . 1.44(3) yes O2 . C15 . 1.430(2) yes O2 . C16 . 2.36(3) yes O2 . H3 . 1.97(2) no O2 . H4 . 1.97(3) no O2 . H5 . 1.973(19) no O2 . H6 . 1.963(2) no O3 . C15 . 2.419(12) yes O3 . C16 . 1.44(3) yes O3 . C17 . 1.431(5) yes O3 . C18 . 2.34(3) yes O3 . H7 . 1.96(3) no O3 . H8 . 1.98(3) no O3 . H9 . 1.971(3) no O3 . H10 . 1.966(7) no O4 . C17 . 2.411(9) yes O4 . C18 . 1.445(15) yes O4 . C19 . 1.44(2) yes O4 . C20 . 2.35(4) yes O4 . H11 . 1.968(8) no O4 . H12 . 1.98(3) no O4 . H13 . 1.979(11) no O4 . H14 . 1.972(11) no O5 . C21 . 1.442(3) yes O5 . C22 . 2.368(19) yes O5 . C27 . 2.41(2) yes O5 . C28 . 1.441(15) yes O5 . H17 . 1.982(13) no O5 . H18 . 1.980(2) no O5 . H31 . 1.96(3) no O5 . H32 . 1.98(2) no O6 . C21 . 2.43(3) yes O6 . C22 . 1.441(8) yes O6 . C23 . 1.438(12) yes O6 . C24 . 2.35(3) yes O6 . H19 . 1.972(14) no O6 . H20 . 1.96(3) no O6 . H21 . 1.978(2) no O6 . H22 . 1.979(11) no O7 . C23 . 2.420(18) yes O7 . C24 . 1.446(8) yes O7 . C25 . 1.446(5) yes O7 . C26 . 2.37(3) yes O7 . H23 . 1.971(9) no O7 . H24 . 1.98(2) no O7 . H25 . 1.98(2) no O7 . H26 . 1.980(16) no O8 . C25 . 2.426(6) yes O8 . C26 . 1.445(18) yes O8 . C27 . 1.44(1) yes O8 . C28 . 2.363(19) yes O8 . H27 . 1.97(3) no O8 . H28 . 1.98(2) no O8 . H29 . 1.98(3) no O8 . H30 . 1.963(4) no C1 . C3 . 1.367(19) yes C4 . C6 . 1.359(18) yes C7 . C9 . 1.35(2) yes C10 . C12 . 1.36(2) yes C13 . C14 . 1.499(12) yes C13 . C20 . 2.41(4) yes C13 . H3 . 2.03(3) no C13 . H4 . 2.00(1) no C13 . H15 . 2.47(4) no C14 . C15 . 2.41(3) yes C14 . H1 . 2.043(8) no C14 . H2 . 2.02(1) no C14 . H6 . 2.496(17) no C15 . C16 . 1.50(2) yes C15 . H3 . 2.46(4) no C15 . H7 . 2.03(3) no C15 . H8 . 2.02(3) no C16 . C17 . 2.42(3) yes C16 . H5 . 2.041(3) no C16 . H6 . 2.03(3) no C17 . C18 . 1.49(2) yes C17 . H7 . 2.45(4) no C17 . H11 . 2.02(3) no C17 . H12 . 2.01(2) no C18 . C19 . 2.42(4) yes C18 . H9 . 2.031(15) no C18 . H10 . 2.02(3) no C19 . C20 . 1.491(13) yes C19 . H11 . 2.48(4) no C19 . H15 . 2.02(3) no C19 . H16 . 2.004(6) no C20 . H13 . 2.035(3) no C20 . H14 . 2.020(6) no C21 . C22 . 1.51(2) yes C21 . C28 . 2.43(1) yes C21 . H19 . 2.04(2) no C21 . H20 . 2.017(14) no C21 . H31 . 2.46(3) no C22 . C23 . 2.42(3) yes C22 . H17 . 2.05(3) no C22 . H18 . 2.031(15) no C23 . C24 . 1.501(13) yes C23 . H23 . 2.03(3) no C23 . H24 . 2.02(1) no C24 . C25 . 2.419(15) yes C24 . H21 . 2.039(19) no C24 . H22 . 2.03(1) no C25 . C26 . 1.499(13) yes C25 . H23 . 2.47(3) no C25 . H27 . 2.02(2) no C25 . H28 . 2.013(3) no C26 . C27 . 2.423(8) yes C26 . H25 . 2.037(12) no C26 . H26 . 2.024(4) no C27 . C28 . 1.50(3) yes C27 . H27 . 2.48(3) no C27 . H31 . 2.03(3) no C27 . H32 . 2.01(2) no C28 . H29 . 2.04(3) no C28 . H30 . 2.02(2) no H1 . H2 . 1.551(18) no H1 . H3 . 2.352(19) no H1 . H4 . 2.301(3) no H1 . H15 . 2.45(4) no H2 . H3 . 2.32(3) no H2 . H6 . 2.33(1) no H2 . H14 . 2.277(17) no H3 . H4 . 1.551(9) no H3 . H6 . 2.46(2) no H5 . H6 . 1.551(14) no H5 . H7 . 2.369(16) no H5 . H8 . 2.290(19) no H6 . H7 . 2.29(4) no H6 . H10 . 2.422(19) no H7 . H8 . 1.551 no H7 . H9 . 2.41(3) no H9 . H10 . 1.55(3) no H9 . H11 . 2.35(2) no H9 . H12 . 2.29(3) no H10 . H11 . 2.29(4) no H10 . H14 . 2.285(14) no H11 . H12 . 1.55(1) no H11 . H13 . 2.49(4) no H13 . H14 . 1.55(3) no H13 . H15 . 2.343(17) no H13 . H16 . 2.297(6) no H14 . H15 . 2.31(2) no H15 . H16 . 1.551(2) no H17 . H18 . 1.55(2) no H17 . H19 . 2.38(4) no H17 . H20 . 2.29(3) no H17 . H31 . 2.474(5) no H18 . H19 . 2.300(17) no H18 . H22 . 2.314(11) no H18 . H30 . 2.47(2) no H18 . H31 . 2.49(3) no H19 . H20 . 1.551(3) no H19 . H21 . 2.472(18) no H21 . H22 . 1.55(2) no H21 . H23 . 2.34(4) no H21 . H24 . 2.318(7) no H22 . H23 . 2.318(4) no H22 . H26 . 2.29(2) no H23 . H24 . 1.551(5) no H23 . H25 . 2.482(7) no H25 . H26 . 1.551(11) no H25 . H27 . 2.34(3) no H25 . H28 . 2.293(7) no H26 . H27 . 2.299(8) no H26 . H30 . 2.310(16) no H27 . H28 . 1.551(14) no H27 . H29 . 2.487(8) no H29 . H30 . 1.551(13) no H29 . H31 . 2.36(4) no H29 . H32 . 2.30(3) no H30 . H31 . 2.30(2) no H31 . H32 . 1.5512(2) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C13 . O1 . C20 . 113.8(11) yes C14 . O2 . C15 . 113.7(2) yes C16 . O3 . C17 . 114.74(18) yes C18 . O4 . C19 . 114.0(10) yes C21 . O5 . C28 . 115.0(3) yes C22 . O6 . C23 . 114.2(8) yes C24 . O7 . C25 . 113.6(3) yes C26 . O8 . C27 . 114.5(7) yes S15 . C9 . C7 . 121.0(5) yes O1 . C13 . C14 . 106.9(13) yes O1 . C13 . H1 . 110.7(17) no C14 . C13 . H1 . 111.1(16) no O1 . C13 . H2 . 109.6(3) no C14 . C13 . H2 . 109.1(4) no H1 . C13 . H2 . 109.5(4) no O2 . C14 . C13 . 111.0(4) yes O2 . C14 . H3 . 109.2(7) no C13 . C14 . H3 . 110.3(14) no O2 . C14 . H4 . 109.1(3) no C13 . C14 . H4 . 107.7(4) no H3 . C14 . H4 . 109.5(4) no O2 . C15 . C16 . 107.1(15) yes O2 . C15 . H5 . 110.4(13) no C16 . C15 . H5 . 110.7(18) no O2 . C15 . H6 . 109.46(16) no C16 . C15 . H6 . 109.7(4) no H5 . C15 . H6 . 109.5(5) no O3 . C16 . C15 . 110.7(7) yes O3 . C16 . H7 . 108.3(4) no C15 . C16 . H7 . 109.7(3) no O3 . C16 . H8 . 109.8(3) no C15 . C16 . H8 . 108.9(5) no H7 . C16 . H8 . 109.5(3) no O3 . C17 . C18 . 106.9(11) yes O3 . C17 . H9 . 110.2(4) no C18 . C17 . H9 . 110.9(10) no O3 . C17 . H10 . 109.7(8) no C18 . C17 . H10 . 109.7(3) no H9 . C17 . H10 . 109.5(10) no O4 . C18 . C17 . 110.6(11) yes O4 . C18 . H11 . 108.7(8) no C17 . C18 . H11 . 109.58(11) no O4 . C18 . H12 . 109.7(11) no C17 . C18 . H12 . 108.7(3) no H11 . C18 . H12 . 109.5(10) no O4 . C19 . C20 . 106.5(7) yes O4 . C19 . H13 . 110.4(8) no C20 . C19 . H13 . 110.9(11) no O4 . C19 . H14 . 109.8(9) no C20 . C19 . H14 . 109.7(7) no H13 . C19 . H14 . 109.5(9) no O1 . C20 . C19 . 111.0(5) yes O1 . C20 . H15 . 108.8(14) no C19 . C20 . H15 . 110.0(11) no O1 . C20 . H16 . 109.3(10) no C19 . C20 . H16 . 108.3(7) no H15 . C20 . H16 . 109.5(11) no O5 . C21 . C22 . 106.8(8) yes O5 . C21 . H17 . 110.2(9) no C22 . C21 . H17 . 111.1(4) no O5 . C21 . H18 . 110.0(3) no C22 . C21 . H18 . 109.4(11) no H17 . C21 . H18 . 109.5(13) no O6 . C22 . C21 . 111.2(21) yes O6 . C22 . H19 . 109.4(4) no C21 . C22 . H19 . 109.9(5) no O6 . C22 . H20 . 108.6(14) no C21 . C22 . H20 . 108.2(12) no H19 . C22 . H20 . 109.46(7) no O6 . C23 . C24 . 106.3(8) yes O6 . C23 . H21 . 110.2(13) no C24 . C23 . H21 . 110.5(5) no O6 . C23 . H22 . 110.26(14) no C24 . C23 . H22 . 110.0(19) no H21 . C23 . H22 . 109.5(9) no O7 . C24 . C23 . 110.3(15) yes O7 . C24 . H23 . 108.91(19) no C23 . C24 . H23 . 109.4(8) no O7 . C24 . H24 . 109.4(9) no C23 . C24 . H24 . 109.3(19) no H23 . C24 . H24 . 109.46(14) no O7 . C25 . C26 . 107.5(11) yes O7 . C25 . H25 . 110.1(22) no C26 . C25 . H25 . 110.57(14) no O7 . C25 . H26 . 109.7(9) no C26 . C25 . H26 . 109.5(11) no H25 . C25 . H26 . 109.5(3) no O8 . C26 . C25 . 111.0(15) yes O8 . C26 . H27 . 108.5(8) no C25 . C26 . H27 . 109.5(7) no O8 . C26 . H28 . 109.9(2) no C25 . C26 . H28 . 108.5(12) no H27 . C26 . H28 . 109.5(8) no O8 . C27 . C28 . 107.2(14) yes O8 . C27 . H29 . 110.7(14) no C28 . C27 . H29 . 111.06(12) no O8 . C27 . H30 . 109.1(7) no C28 . C27 . H30 . 109.3(8) no H29 . C27 . H30 . 109.47(12) no O5 . C28 . C27 . 110.2(20) yes O5 . C28 . H31 . 108.8(10) no C27 . C28 . H31 . 110.0(4) no O5 . C28 . H32 . 109.90(19) no C27 . C28 . H32 . 108.5(8) no H31 . C28 . H32 . 109.5(6) no C13 . H1 . H2 . 35.3(4) no C13 . H2 . H1 . 35.271 no C14 . H3 . H4 . 35.3(3) no C14 . H4 . H3 . 35.27(4) no C15 . H5 . H6 . 35.3(4) no C15 . H6 . H5 . 35.27(3) no C16 . H7 . H8 . 35.27(18) no C16 . H8 . H7 . 35.27(17) no C17 . H9 . H10 . 35.3(7) no C17 . H10 . H9 . 35.3(7) no C18 . H11 . H12 . 35.27(16) no C18 . H12 . H11 . 35.3(5) no C19 . H13 . H14 . 35.3(6) no C19 . H14 . H13 . 35.3(6) no C20 . H15 . H16 . 35.3(3) no C20 . H16 . H15 . 35.3(3) no C21 . H17 . H18 . 35.3(7) no C21 . H18 . H17 . 35.3(7) no C22 . H19 . H20 . 35.3(4) no C22 . H20 . H19 . 35.27(19) no C23 . H21 . H22 . 35.3(3) no C23 . H22 . H21 . 35.3(5) no C24 . H23 . H24 . 35.3(7) no C24 . H24 . H23 . 35.3(2) no C25 . H25 . H26 . 35.3(2) no C25 . H26 . H25 . 35.27(3) no C26 . H27 . H28 . 35.3(7) no C26 . H28 . H27 . 35.3(6) no C27 . H29 . H30 . 35.3(4) no C27 . H30 . H29 . 35.27(19) no C28 . H31 . H32 . 35.3(3) no C28 . H32 . H31 . 35.3(3) no loop_ _geom_contact_atom_site_label_1 _geom_contact_site_symmetry_1 _geom_contact_atom_site_label_2 _geom_contact_site_symmetry_2 _geom_contact_distance _geom_contact_publ_flag Ni1 . C27 4_544 3.978(4) yes Ni1 . H18 4_544 3.57(3) no Ni1 . H22 4_544 3.51(3) no Ni2 . S18 2_845 3.74(6) yes Ni2 . C11 2_845 3.95(4) yes Ni2 . C25 4_544 3.98(5) yes Ni2 . C26 4_544 3.59(6) yes Ni2 . H1 4_545 3.95(4) no Ni2 . H17 2_745 3.486(6) no Ni2 . H25 4_544 3.44(2) no Ni2 . H28 4_544 3.42(5) no S1 . S13 2_745 3.994(9) yes S1 . C25 4_544 3.814(2) yes S1 . H22 4_544 3.52(3) no S1 . H23 4_544 3.78(3) no S1 . H25 4_544 3.708(3) no S2 . S2 2_744 3.52(5) yes S2 . S3 2_744 3.916(2) yes S2 . S8 4_444 3.858(5) yes S2 . S13 2_745 3.48(6) yes S2 . C2 2_744 3.95(3) yes S2 . C8 2_745 3.94(6) yes S3 . S7 4_444 3.749(5) yes S3 . S13 1_554 3.419(2) yes S3 . C5 4_444 3.85(3) yes S3 . C24 3_644 3.80(3) yes S3 . C27 1_554 3.89(5) yes S3 . C28 1_554 3.64(5) yes S3 . H24 3_644 3.94(4) no S3 . H25 3_644 3.97(4) no S3 . H29 1_554 3.26(3) no S3 . H31 1_554 3.49(3) no S4 . H12 1_554 3.81(5) no S4 . H29 1_554 3.328(6) no S5 . S16 4_444 3.75(3) yes S5 . S17 4_444 3.70(6) yes S5 . H18 4_544 3.223(7) no S5 . H22 4_544 3.34(2) no S6 . S19 3_754 3.71(4) yes S6 . S20 3_754 3.85(6) yes S6 . C27 4_544 3.808(9) yes S6 . H18 4_544 3.53(2) no S6 . H29 4_544 3.798(2) no S6 . H31 4_544 3.58(1) no S7 . S18 4_445 3.852(17) yes S7 . C20 2_755 3.92(1) yes S7 . H15 2_755 3.87(2) no S7 . H23 2_755 3.900(18) no S7 . H24 2_755 3.543(17) no S7 . H29 4_544 3.78(5) no S8 . S18 4_445 3.611(5) yes S8 . O2 4_545 3.98(6) yes S8 . C2 4_545 3.773(9) yes S8 . C7 3_755 3.96(6) yes S8 . C9 3_755 3.80(6) yes S8 . C15 4_545 3.92(4) yes S8 . H20 4_545 3.59(5) no S8 . H24 2_755 3.74(6) no S9 . C14 4_545 3.60(3) yes S9 . H3 4_545 3.265(19) no S9 . H20 4_545 3.51(1) no S9 . H29 4_544 3.664(5) no S10 . C25 4_544 3.87(4) yes S10 . C26 4_544 3.952(15) yes S10 . C27 4_544 3.84(3) yes S10 . H25 4_544 3.96(5) no S10 . H26 4_544 3.26(3) no S10 . H27 4_544 3.279(8) no S10 . H29 4_544 3.67(2) no S11 . O5 2_745 3.626(11) yes S11 . C21 2_745 3.826(7) yes S11 . C28 2_745 3.57(5) yes S11 . H8 2_745 3.398(19) no S11 . H25 4_544 3.26(5) no S11 . H32 2_745 3.45(5) no S12 . S12 2_745 3.322(8) yes S12 . S13 2_745 3.92(5) yes S12 . C16 2_745 3.404(16) yes S12 . H5 2_745 3.74(5) no S13 . C2 1_556 3.79(2) yes S14 . O6 4_545 3.84(5) yes S14 . C23 4_545 3.65(4) yes S14 . H24 4_545 3.508(13) no S15 . S18 2_845 3.83(4) yes S15 . C13 4_545 3.51(2) yes S15 . C14 4_545 3.34(4) yes S15 . H3 4_545 3.43(3) no S15 . H27 4_544 3.93(4) no S16 . S19 2_845 3.71(4) yes S16 . C11 2_845 3.72(5) yes S16 . C13 4_545 3.76(3) yes S16 . C14 4_545 3.95(6) yes S16 . C26 4_544 3.69(3) yes S16 . H3 4_545 3.49(6) no S16 . H28 4_544 3.312(17) no S17 . S20 2_845 3.78(4) yes S17 . C10 2_845 3.90(5) yes S17 . C12 2_845 3.62(6) yes S17 . C18 4_544 3.83(6) yes S17 . C21 1_655 3.884(16) yes S17 . H11 4_544 3.43(5) no S17 . H12 4_544 3.47(6) no S17 . H17 1_655 3.406(6) no S17 . H18 1_655 3.78(3) no S17 . H19 1_655 3.360(8) no S17 . H28 4_544 3.967(9) no S18 . C5 4_544 3.57(3) yes S18 . H1 3_744 3.394(16) no S18 . H13 4_544 3.20(1) no S18 . H15 3_744 3.27(5) no S18 . H17 1_655 3.63(4) no S18 . H19 1_655 3.65(5) no S18 . H20 1_655 3.66(4) no S19 . O4 4_544 3.78(6) yes S19 . C10 2_845 3.87(4) yes S19 . C13 3_744 3.89(3) yes S19 . C19 4_544 3.70(6) yes S19 . H1 3_744 3.245(15) no S19 . H2 3_744 3.71(4) no S19 . H11 4_544 4.00(4) no S19 . H15 3_744 3.22(2) no S19 . H16 4_544 3.73(3) no S19 . H28 4_544 3.781(3) no S20 . C21 2_745 3.71(4) yes S20 . C25 4_544 3.75(5) yes S20 . C26 4_544 3.63(4) yes S20 . H18 2_745 3.72(2) no S20 . H27 4_544 3.639(12) no O4 . C11 4_445 3.76(5) yes C1 . H21 4_544 3.843(11) no C1 . H22 4_544 3.468(13) no C1 . H23 4_544 3.931(12) no C2 . C5 4_444 3.920(6) yes C2 . H29 1_554 3.71(4) no C3 . H21 4_544 3.725(14) no C3 . H22 4_544 3.392(3) no C4 . C27 4_544 3.60(3) yes C4 . H30 4_544 3.21(4) no C4 . H31 4_544 3.804(19) no C5 . H20 4_545 3.80(5) no C5 . H29 4_544 3.95(5) no C6 . C27 4_544 3.626(2) yes C6 . H27 4_544 3.75(4) no C6 . H30 4_544 3.236(9) no C7 . H8 2_745 3.368(16) no C9 . H4 4_545 3.80(4) no C10 . C10 2_845 3.76(4) yes C10 . C11 2_845 3.90(7) yes C10 . C12 2_845 3.76(4) yes C10 . C26 4_544 3.71(3) yes C10 . H12 4_544 3.94(7) no C10 . H27 4_544 3.61(2) no C11 . C18 4_544 3.68(5) yes C11 . C19 4_544 3.84(3) yes C11 . H1 3_744 3.63(4) no C11 . H12 4_544 3.75(4) no C11 . H15 3_744 3.67(6) no C11 . H17 1_655 3.93(3) no C11 . H19 1_655 3.95(3) no C12 . C26 4_544 3.68(3) yes C12 . H25 4_544 3.993(16) no C12 . H27 4_544 3.797(9) no C19 . H13 2_755 3.95(5) no C19 . H15 2_755 3.466(12) no C20 . H13 2_755 3.42(2) no C20 . H15 2_755 3.81(3) no H11 . H19 4_545 3.55(2) no H13 . H13 2_755 3.59(6) no H13 . H16 2_755 3.51(3) no H14 . H15 2_755 3.78(3) no H15 . H15 2_755 3.47(3) no H15 . H16 2_755 3.844(11) no #============================================================================== #============================================================================== # End of CIF #============================================================================== #------------------------------------------------------------------------------ data_ca15c5ni _database_code_CSD 158718 _audit_creation_date 'Thu Apr 12 13:48:26 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C100 H126 Ca3 N2 Ni6 O15 S60' _chemical_formula_moiety 'C100 H126 Ca3 N2 Ni6 O15 S60' _chemical_formula_weight 3992.14 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.4442(4) _cell_length_b 12.5299(4) _cell_length_c 26.872(1) _cell_angle_alpha 97.0670(7) _cell_angle_beta 91.7234(8) _cell_angle_gamma 97.214(1) _cell_volume 4120.8(2) _cell_formula_units_Z 1 _cell_measurement_reflns_used 30205 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.593 _exptl_absorpt_correction_T_max 0.854 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_reflns_number 56890 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.5 sigma(F^2^). 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 18781 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0493 _refine_ls_wR_factor_obs 0.1260 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 10905 _refine_ls_number_parameters 907 _refine_ls_goodness_of_fit_obs 1.596 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/\s^2^(Fo^2^)' _refine_ls_shift/esd_max 0.6478 _refine_diff_density_max 0.54 _refine_diff_density_min -0.37 _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 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Ca' 'Ca' 0.226 0.306 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni(1) Ni 1.42322(5) 0.61810(4) 0.57773(2) 0.0435(1) Uani 1.00 d . . . Ni(2) Ni 0.82638(6) -0.07563(5) 0.87676(2) 0.0579(2) Uani 1.00 d . . . Ni(3) Ni 1.26556(5) 0.25187(5) 0.75223(2) 0.0463(1) Uani 1.00 d . . . Ca(1) Ca 0.69264(8) 0.09075(7) 0.66830(3) 0.0441(2) Uani 1.00 d . . . Ca(2) Ca 1.0000 0.5000 1.0000 0.0532(4) Uani 1.00 d S . . S(1) S 1.2691(1) 0.66528(10) 0.55485(5) 0.0517(3) Uani 1.00 d . . . S(2) S 1.05275(10) 0.65123(9) 0.60438(5) 0.0526(3) Uani 1.00 d . . . S(3) S 0.9085(1) 0.6030(1) 0.68762(6) 0.0684(4) Uani 1.00 d . . . S(4) S 1.1382(1) 0.56048(10) 0.68861(5) 0.0552(3) Uani 1.00 d . . . S(5) S 1.36258(10) 0.56546(10) 0.64647(4) 0.0510(3) Uani 1.00 d . . . S(6) S 1.5779(1) 0.57294(10) 0.60109(4) 0.0517(3) Uani 1.00 d . . . S(7) S 1.7913(1) 0.57412(10) 0.54885(5) 0.0532(3) Uani 1.00 d . . . S(8) S 1.9349(1) 0.6223(1) 0.46541(6) 0.0688(4) Uani 1.00 d . . . S(9) S 1.7057(1) 0.6640(1) 0.46423(5) 0.0570(3) Uani 1.00 d . . . S(10) S 1.4847(1) 0.6696(1) 0.50887(5) 0.0547(3) Uani 1.00 d . . . S(11) S 0.8692(1) -0.2171(1) 0.83188(6) 0.0674(4) Uani 1.00 d . . . S(12) S 1.0840(1) -0.2717(1) 0.79344(6) 0.0794(5) Uani 1.00 d . . . S(13) S 1.3210(2) -0.2288(2) 0.78292(8) 0.1051(7) Uani 1.00 d . . . S(14) S 1.2002(1) -0.0704(1) 0.84251(6) 0.0737(4) Uani 1.00 d . . . S(15) S 0.9925(1) 0.0050(1) 0.88351(6) 0.0705(4) Uani 1.00 d . . . S(16) S 0.7744(1) 0.0741(1) 0.91028(7) 0.0795(5) Uani 1.00 d . . . S(17) S 0.5530(2) 0.1238(1) 0.94359(7) 0.0878(5) Uani 1.00 d . . . S(18) S 0.3207(2) 0.0630(2) 0.96192(8) 0.1124(7) Uani 1.00 d . . . S(19) S 0.4552(1) -0.0973(1) 0.91469(6) 0.0779(5) Uani 1.00 d . . . S(20) S 0.6678(1) -0.1669(1) 0.87922(6) 0.0657(4) Uani 1.00 d . . . S(21) S 1.2005(1) 0.27356(9) 0.67874(5) 0.0510(3) Uani 1.00 d . . . S(22) S 1.1105(1) 0.10728(9) 0.59003(5) 0.0531(3) Uani 1.00 d . . . S(23) S 1.0486(1) -0.1196(1) 0.54034(5) 0.0627(4) Uani 1.00 d . . . S(24) S 1.1530(1) -0.07235(9) 0.64310(5) 0.0580(3) Uani 1.00 d . . . S(25) S 1.2419(1) 0.0768(1) 0.73625(5) 0.0608(4) Uani 1.00 d . . . S(26) S 1.3354(1) 0.22989(10) 0.82486(5) 0.0539(3) Uani 1.00 d . . . S(27) S 1.4504(1) 0.3944(1) 0.90805(5) 0.0585(3) Uani 1.00 d . . . S(28) S 1.5313(1) 0.6211(1) 0.95454(6) 0.0713(4) Uani 1.00 d . . . S(29) S 1.4085(1) 0.5755(1) 0.85648(5) 0.0650(4) Uani 1.00 d . . . S(30) S 1.2948(1) 0.4268(1) 0.76762(5) 0.0624(4) Uani 1.00 d . . . O(1) O 0.7072(3) 0.0657(3) 0.5701(1) 0.070(1) Uani 1.00 d . . . O(2) O 0.8104(3) 0.2414(3) 0.6270(1) 0.069(1) Uani 1.00 d . . . O(3) O 0.8521(3) 0.2152(3) 0.7242(2) 0.087(1) Uani 1.00 d . . . O(4) O 0.8332(4) -0.0008(3) 0.7191(2) 0.094(2) Uani 1.00 d . . . O(5) O 0.7692(4) -0.0754(3) 0.6263(2) 0.099(2) Uani 1.00 d . . . O(6) O 0.6437(4) 0.1205(3) 0.7634(1) 0.078(1) Uani 1.00 d . . . O(7) O 0.6292(3) 0.2737(3) 0.7007(1) 0.072(1) Uani 1.00 d . . . O(8) O 0.5243(3) 0.1765(3) 0.6166(2) 0.086(1) Uani 1.00 d . . . O(9) O 0.5159(4) -0.0365(4) 0.6195(2) 0.096(2) Uani 1.00 d . . . O(10) O 0.5931(4) -0.0721(3) 0.7085(2) 0.087(1) Uani 1.00 d . . . O(11) O 1.0478(6) 0.3072(5) 1.0212(3) 0.158(3) Uani 1.00 d . . . O(12) O 1.1225(5) 0.3757(5) 0.9397(3) 0.167(3) Uani 1.00 d . . . O(13) O 0.9767(6) 0.4807(7) 0.8986(3) 0.186(3) Uani 1.00 d . . . O(14) O 0.8140(5) 0.4693(6) 0.9574(3) 0.159(3) Uani 1.00 d . . . O(15) O 0.8526(6) 0.3646(7) 1.0325(4) 0.196(4) Uani 1.00 d . . . N(1) N 0.6810(8) -0.4968(7) 0.8016(4) 0.191(4) Uani 1.00 d . . . C(1) C 1.1898(4) 0.6331(3) 0.6029(2) 0.043(1) Uani 1.00 d . . . C(2) C 1.0269(4) 0.6040(3) 0.6613(2) 0.048(1) Uani 1.00 d . . . C(3) C 1.2292(4) 0.5893(3) 0.6429(2) 0.045(1) Uani 1.00 d . . . C(4) C 1.6562(4) 0.5979(3) 0.5513(2) 0.045(1) Uani 1.00 d . . . C(5) C 1.8171(4) 0.6202(3) 0.4919(2) 0.051(1) Uani 1.00 d . . . C(6) C 1.6161(4) 0.6409(3) 0.5115(2) 0.046(1) Uani 1.00 d . . . C(7) C 1.0064(4) -0.1836(4) 0.8271(2) 0.061(1) Uani 1.00 d . . . C(8) C 1.2078(5) -0.1914(5) 0.8048(2) 0.074(2) Uani 1.00 d . . . C(9) C 1.0606(4) -0.0886(4) 0.8497(2) 0.059(1) Uani 1.00 d . . . C(10) C 0.6404(5) 0.0350(4) 0.9185(2) 0.067(2) Uani 1.00 d . . . C(11) C 0.4376(5) 0.0334(5) 0.9409(2) 0.081(2) Uani 1.00 d . . . C(12) C 0.5924(5) -0.0704(4) 0.9049(2) 0.063(2) Uani 1.00 d . . . C(13) C 1.1688(4) 0.1410(3) 0.6512(2) 0.047(1) Uani 1.00 d . . . C(14) C 1.1013(4) -0.0335(4) 0.5884(2) 0.049(1) Uani 1.00 d . . . C(15) C 1.1869(4) 0.0581(4) 0.6759(2) 0.049(1) Uani 1.00 d . . . C(16) C 1.3806(4) 0.3612(4) 0.8502(2) 0.046(1) Uani 1.00 d . . . C(17) C 1.4685(4) 0.5338(4) 0.9088(2) 0.054(1) Uani 1.00 d . . . C(18) C 1.3615(4) 0.4465(4) 0.8255(2) 0.050(1) Uani 1.00 d . . . C(19) C 0.7256(5) 0.1637(5) 0.5494(2) 0.076(2) Uani 1.00 d . . . C(20) C 0.8215(5) 0.2336(5) 0.5735(2) 0.072(2) Uani 1.00 d . . . C(21) C 0.9026(5) 0.3037(5) 0.6526(3) 0.080(2) Uani 1.00 d . . . C(22) C 0.8853(5) 0.3165(5) 0.7072(2) 0.079(2) Uani 1.00 d . . . C(23) C 0.9347(6) 0.1706(6) 0.7458(3) 0.101(2) Uani 1.00 d . . . C(24) C 0.9006(7) 0.0646(7) 0.7557(3) 0.119(3) Uani 1.00 d . . . C(25) C 0.8696(8) -0.0922(7) 0.6991(3) 0.137(3) Uani 1.00 d . . . C(26) C 0.8212(6) -0.1417(5) 0.6511(3) 0.099(2) Uani 1.00 d . . . C(27) C 0.7466(6) -0.1109(4) 0.5757(2) 0.083(2) Uani 1.00 d . . . C(28) C 0.7667(5) -0.0149(5) 0.5472(2) 0.077(2) Uani 1.00 d . . . C(29) C 0.6275(5) 0.2289(5) 0.7820(2) 0.077(2) Uani 1.00 d . . . C(30) C 0.5624(5) 0.2730(5) 0.7434(2) 0.074(2) Uani 1.00 d . . . C(31) C 0.5928(6) 0.3373(5) 0.6649(3) 0.086(2) Uani 1.00 d . . . C(32) C 0.4985(6) 0.2796(5) 0.6342(3) 0.088(2) Uani 1.00 d . . . C(33) C 0.4326(6) 0.1115(7) 0.5933(3) 0.111(3) Uani 1.00 d . . . C(34) C 0.4601(6) 0.0007(6) 0.5801(3) 0.109(3) Uani 1.00 d . . . C(35) C 0.4515(6) -0.1023(5) 0.6470(3) 0.096(2) Uani 1.00 d . . . C(36) C 0.5152(7) -0.1489(5) 0.6820(3) 0.105(3) Uani 1.00 d . . . C(37) C 0.5929(7) -0.0637(6) 0.7609(3) 0.106(3) Uani 1.00 d . . . C(38) C 0.5755(7) 0.0414(6) 0.7829(3) 0.095(2) Uani 1.00 d . . . C(39) C 1.131(1) 0.264(1) 0.9979(6) 0.267(6) Uani 1.00 d . . . C(40) C 1.1601(10) 0.2927(9) 0.9509(5) 0.192(5) Uani 1.00 d . . . C(41) C 1.0942(10) 0.3636(10) 0.8846(4) 0.189(4) Uani 1.00 d . . . C(42) C 1.047(1) 0.436(1) 0.8762(7) 0.280(7) Uani 1.00 d . . . C(43) C 0.8716(9) 0.471(1) 0.8778(4) 0.181(5) Uani 1.00 d . . . C(44) C 0.795(1) 0.481(2) 0.9129(4) 0.280(9) Uani 1.00 d . . . C(45) C 0.7285(6) 0.4059(9) 0.9751(5) 0.154(4) Uani 1.00 d . . . C(46) C 0.7609(7) 0.364(1) 1.0166(4) 0.167(5) Uani 1.00 d . . . C(47) C 0.889(1) 0.2827(8) 1.0547(5) 0.190(5) Uani 1.00 d . . . C(48) C 0.972(1) 0.2252(7) 1.0330(4) 0.166(4) Uani 1.00 d . . . C(49) C 0.6181(8) -0.3595(7) 0.7497(3) 0.127(3) Uani 1.00 d . . . C(50) C 0.6540(6) -0.4345(5) 0.7789(3) 0.099(2) Uani 1.00 d . . . H(1) H 0.7337 0.1504 0.5140 0.0903 Uiso 1.00 calc . . . H(2) H 0.6628 0.2030 0.5542 0.0903 Uiso 1.00 calc . . . H(3) H 0.8270 0.3043 0.5627 0.0879 Uiso 1.00 calc . . . H(4) H 0.8849 0.2020 0.5642 0.0879 Uiso 1.00 calc . . . H(5) H 0.9653 0.2675 0.6462 0.0951 Uiso 1.00 calc . . . H(6) H 0.9154 0.3731 0.6406 0.0951 Uiso 1.00 calc . . . H(7) H 0.8298 0.3640 0.7144 0.0956 Uiso 1.00 calc . . . H(8) H 0.9502 0.3515 0.7259 0.0956 Uiso 1.00 calc . . . H(9) H 0.9933 0.1676 0.7217 0.1226 Uiso 1.00 calc . . . H(10) H 0.9654 0.2161 0.7749 0.1226 Uiso 1.00 calc . . . H(11) H 0.8614 0.0698 0.7865 0.1419 Uiso 1.00 calc . . . H(12) H 0.9622 0.0279 0.7622 0.1419 Uiso 1.00 calc . . . H(13) H 0.9470 -0.0793 0.6963 0.1517 Uiso 1.00 calc . . . H(14) H 0.8575 -0.1461 0.7227 0.1517 Uiso 1.00 calc . . . H(15) H 0.7722 -0.2046 0.6561 0.1173 Uiso 1.00 calc . . . H(16) H 0.8783 -0.1668 0.6308 0.1173 Uiso 1.00 calc . . . H(17) H 0.7871 -0.1668 0.5633 0.0987 Uiso 1.00 calc . . . H(18) H 0.6693 -0.1408 0.5699 0.0987 Uiso 1.00 calc . . . H(19) H 0.7449 -0.0342 0.5119 0.0934 Uiso 1.00 calc . . . H(20) H 0.8433 0.0101 0.5487 0.0934 Uiso 1.00 calc . . . H(21) H 0.5937 0.2327 0.8135 0.0935 Uiso 1.00 calc . . . H(22) H 0.6980 0.2750 0.7880 0.0935 Uiso 1.00 calc . . . H(23) H 0.5444 0.3440 0.7547 0.0916 Uiso 1.00 calc . . . H(24) H 0.4949 0.2259 0.7351 0.0916 Uiso 1.00 calc . . . H(25) H 0.5766 0.4056 0.6819 0.1059 Uiso 1.00 calc . . . H(26) H 0.6526 0.3560 0.6432 0.1059 Uiso 1.00 calc . . . H(27) H 0.4839 0.3187 0.6062 0.1047 Uiso 1.00 calc . . . H(28) H 0.4365 0.2760 0.6538 0.1047 Uiso 1.00 calc . . . H(29) H 0.3735 0.1092 0.6174 0.1354 Uiso 1.00 calc . . . H(30) H 0.4055 0.1412 0.5653 0.1354 Uiso 1.00 calc . . . H(31) H 0.5058 0.0007 0.5514 0.1292 Uiso 1.00 calc . . . H(32) H 0.3959 -0.0499 0.5695 0.1292 Uiso 1.00 calc . . . H(33) H 0.4016 -0.0621 0.6653 0.1144 Uiso 1.00 calc . . . H(34) H 0.4085 -0.1596 0.6245 0.1144 Uiso 1.00 calc . . . H(35) H 0.5533 -0.2053 0.6636 0.1226 Uiso 1.00 calc . . . H(36) H 0.4711 -0.1859 0.7050 0.1226 Uiso 1.00 calc . . . H(37) H 0.5424 -0.1212 0.7719 0.1240 Uiso 1.00 calc . . . H(38) H 0.6653 -0.0791 0.7741 0.1240 Uiso 1.00 calc . . . H(39) H 0.5842 0.0490 0.8190 0.1142 Uiso 1.00 calc . . . H(40) H 0.4998 0.0486 0.7753 0.1142 Uiso 1.00 calc . . . H(41) H 1.1940 0.2791 1.0209 0.2971 Uiso 1.00 calc . . . H(42) H 1.1119 0.1842 0.9944 0.2971 Uiso 1.00 calc . . . H(43) H 1.1393 0.2284 0.9273 0.2173 Uiso 1.00 calc . . . H(44) H 1.2396 0.3032 0.9529 0.2173 Uiso 1.00 calc . . . H(45) H 1.1586 0.3527 0.8677 0.2176 Uiso 1.00 calc . . . H(46) H 1.0455 0.2941 0.8779 0.2176 Uiso 1.00 calc . . . H(47) H 1.0135 0.4167 0.8385 0.2725 Uiso 1.00 calc . . . H(48) H 1.1036 0.4990 0.8681 0.2725 Uiso 1.00 calc . . . H(49) H 0.8700 0.5228 0.8536 0.2048 Uiso 1.00 calc . . . H(50) H 0.8542 0.3998 0.8583 0.2048 Uiso 1.00 calc . . . H(51) H 0.7327 0.4422 0.9001 0.3052 Uiso 1.00 calc . . . H(52) H 0.7871 0.5609 0.9139 0.3052 Uiso 1.00 calc . . . H(53) H 0.6689 0.4460 0.9805 0.1792 Uiso 1.00 calc . . . H(54) H 0.7022 0.3458 0.9476 0.1792 Uiso 1.00 calc . . . H(55) H 0.7281 0.2845 1.0116 0.1919 Uiso 1.00 calc . . . H(56) H 0.7172 0.3940 1.0438 0.1919 Uiso 1.00 calc . . . H(57) H 0.9173 0.3127 1.0897 0.2196 Uiso 1.00 calc . . . H(58) H 0.8281 0.2289 1.0604 0.2196 Uiso 1.00 calc . . . H(59) H 0.9454 0.1774 1.0031 0.1822 Uiso 1.00 calc . . . H(60) H 1.0050 0.1804 1.0549 0.1822 Uiso 1.00 calc . . . H(61) H 0.6334 -0.2861 0.7665 0.1486 Uiso 1.00 calc . . . H(62) H 0.6519 -0.3608 0.7179 0.1486 Uiso 1.00 calc . . . H(63) H 0.5408 -0.3735 0.7426 0.1486 Uiso 1.00 calc . . . 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) 0.0475(3) 0.0433(3) 0.0393(3) 0.0026(2) -0.0022(2) 0.0084(2) Ni(2) 0.0698(4) 0.0560(3) 0.0474(3) 0.0080(3) -0.0006(3) 0.0055(3) Ni(3) 0.0437(3) 0.0532(3) 0.0427(3) 0.0109(2) -0.0013(2) 0.0056(2) Ca(1) 0.0491(5) 0.0417(4) 0.0413(5) 0.0025(4) 0.0029(4) 0.0076(4) Ca(2) 0.0360(7) 0.0710(8) 0.0536(8) 0.0099(6) -0.0015(6) 0.0097(6) S(1) 0.0504(7) 0.0596(6) 0.0467(6) 0.0044(5) -0.0048(5) 0.0181(5) S(2) 0.0458(6) 0.0518(6) 0.0609(7) 0.0055(5) -0.0066(5) 0.0134(5) S(3) 0.0571(8) 0.0637(7) 0.0905(10) 0.0188(6) 0.0182(7) 0.0194(7) S(4) 0.0559(7) 0.0603(6) 0.0559(7) 0.0183(5) 0.0093(6) 0.0208(5) S(5) 0.0490(7) 0.0626(6) 0.0459(6) 0.0124(5) 0.0015(5) 0.0196(5) S(6) 0.0533(7) 0.0602(6) 0.0454(6) 0.0108(5) 0.0011(5) 0.0185(5) S(7) 0.0496(7) 0.0566(6) 0.0544(7) 0.0097(5) 0.0009(5) 0.0085(5) S(8) 0.0605(8) 0.0660(7) 0.0772(9) 0.0017(6) 0.0205(7) 0.0013(7) S(9) 0.0613(8) 0.0641(7) 0.0472(6) 0.0052(6) 0.0061(6) 0.0152(5) S(10) 0.0540(7) 0.0686(7) 0.0450(6) 0.0104(6) -0.0014(5) 0.0198(5) S(11) 0.0606(8) 0.0668(7) 0.0681(8) 0.0005(6) 0.0052(7) -0.0108(6) S(12) 0.0641(9) 0.096(1) 0.0723(9) 0.0055(8) 0.0119(7) -0.0117(8) S(13) 0.065(1) 0.140(2) 0.114(1) 0.016(1) 0.025(1) 0.024(1) S(14) 0.0659(9) 0.0807(9) 0.0736(9) -0.0079(7) 0.0012(7) 0.0245(7) S(15) 0.0788(10) 0.0576(7) 0.0709(9) 0.0004(7) -0.0076(8) 0.0022(6) S(16) 0.089(1) 0.0603(7) 0.085(1) 0.0100(7) -0.0028(9) -0.0084(7) S(17) 0.109(1) 0.0773(9) 0.078(1) 0.0367(8) -0.0010(9) -0.0095(8) S(18) 0.107(1) 0.154(2) 0.088(1) 0.074(1) 0.012(1) 0.001(1) S(19) 0.0788(10) 0.0829(9) 0.0746(9) 0.0225(8) 0.0152(8) 0.0052(8) S(20) 0.0739(9) 0.0552(6) 0.0685(8) 0.0118(6) 0.0132(7) 0.0038(6) S(21) 0.0555(7) 0.0475(5) 0.0503(6) 0.0102(5) -0.0069(5) 0.0057(5) S(22) 0.0644(8) 0.0497(6) 0.0457(6) 0.0103(5) -0.0039(6) 0.0063(5) S(23) 0.0825(9) 0.0551(6) 0.0477(7) 0.0041(6) 0.0008(7) 0.0006(5) S(24) 0.0710(8) 0.0468(6) 0.0561(7) 0.0080(6) -0.0049(6) 0.0075(5) S(25) 0.0795(9) 0.0540(6) 0.0498(7) 0.0105(6) -0.0107(6) 0.0121(5) S(26) 0.0619(7) 0.0557(6) 0.0457(6) 0.0133(5) -0.0035(6) 0.0083(5) S(27) 0.0585(7) 0.0674(7) 0.0491(7) 0.0073(6) -0.0133(6) 0.0101(6) S(28) 0.0653(9) 0.0813(9) 0.0599(8) -0.0054(7) -0.0106(7) -0.0017(7) S(29) 0.0783(9) 0.0573(7) 0.0572(7) 0.0035(6) -0.0128(7) 0.0075(6) S(30) 0.0802(9) 0.0568(6) 0.0508(7) 0.0140(6) -0.0187(6) 0.0091(5) O(1) 0.077(3) 0.069(2) 0.067(2) 0.017(2) 0.006(2) 0.012(2) O(2) 0.065(2) 0.072(2) 0.066(2) -0.011(2) 0.008(2) 0.009(2) O(3) 0.066(3) 0.088(3) 0.104(3) -0.007(2) -0.015(2) 0.030(2) O(4) 0.077(3) 0.082(3) 0.124(4) 0.023(2) -0.023(3) 0.009(3) O(5) 0.160(4) 0.085(2) 0.067(3) 0.065(2) 0.016(3) 0.013(2) O(6) 0.100(3) 0.069(2) 0.071(2) 0.019(2) 0.027(2) 0.018(2) O(7) 0.080(3) 0.073(2) 0.071(2) 0.026(2) 0.015(2) 0.021(2) O(8) 0.071(3) 0.087(3) 0.099(3) 0.020(2) 0.004(2) 0.005(2) O(9) 0.080(3) 0.090(3) 0.113(3) -0.014(2) -0.025(3) 0.032(3) O(10) 0.087(3) 0.090(3) 0.074(3) -0.022(2) 0.003(2) 0.007(2) O(11) 0.193(7) 0.109(4) 0.182(7) 0.043(4) 0.022(6) 0.026(4) O(12) 0.114(4) 0.112(4) 0.269(9) 0.057(3) -0.007(5) -0.042(5) O(13) 0.143(6) 0.279(9) 0.130(5) 0.084(5) -0.023(4) -0.048(5) O(14) 0.105(4) 0.213(6) 0.154(5) -0.020(4) -0.070(4) 0.067(5) O(15) 0.111(5) 0.205(7) 0.283(10) -0.008(5) -0.028(6) 0.119(6) N(1) 0.221(9) 0.113(5) 0.230(8) -0.009(6) -0.130(7) 0.054(5) C(1) 0.045(2) 0.037(2) 0.048(2) 0.002(2) -0.004(2) 0.010(2) C(2) 0.050(3) 0.035(2) 0.060(3) 0.007(2) 0.006(2) 0.008(2) C(3) 0.051(3) 0.038(2) 0.045(2) 0.007(2) 0.003(2) 0.005(2) C(4) 0.052(3) 0.042(2) 0.039(2) 0.004(2) 0.000(2) 0.002(2) C(5) 0.055(3) 0.043(2) 0.052(3) 0.002(2) 0.003(2) -0.003(2) C(6) 0.056(3) 0.044(2) 0.038(2) 0.003(2) 0.001(2) 0.010(2) C(7) 0.067(3) 0.067(3) 0.046(3) 0.006(3) 0.004(2) 0.004(2) C(8) 0.077(4) 0.094(4) 0.055(3) 0.005(3) 0.006(3) 0.024(3) C(9) 0.061(3) 0.062(3) 0.053(3) 0.000(2) -0.001(2) 0.016(2) C(10) 0.087(4) 0.069(3) 0.047(3) 0.027(3) 0.001(3) 0.003(2) C(11) 0.099(4) 0.102(4) 0.051(3) 0.046(3) 0.005(3) 0.009(3) C(12) 0.079(4) 0.068(3) 0.046(3) 0.023(3) 0.011(3) 0.012(2) C(13) 0.044(2) 0.049(2) 0.048(2) 0.008(2) 0.001(2) 0.008(2) C(14) 0.044(2) 0.052(2) 0.050(3) 0.004(2) 0.010(2) 0.002(2) C(15) 0.051(3) 0.050(2) 0.048(3) 0.010(2) 0.001(2) 0.006(2) C(16) 0.043(2) 0.057(2) 0.039(2) 0.011(2) 0.000(2) 0.005(2) C(17) 0.047(3) 0.067(3) 0.047(3) 0.006(2) -0.004(2) 0.006(2) C(18) 0.053(3) 0.058(2) 0.039(2) 0.010(2) 0.001(2) 0.005(2) C(19) 0.072(4) 0.081(3) 0.081(4) 0.013(3) 0.008(3) 0.036(3) C(20) 0.076(4) 0.079(3) 0.065(3) 0.001(3) 0.017(3) 0.031(3) C(21) 0.081(4) 0.060(3) 0.091(4) -0.013(3) 0.018(3) -0.002(3) C(22) 0.077(4) 0.062(3) 0.088(4) -0.022(3) 0.004(3) 0.004(3) C(23) 0.088(5) 0.108(5) 0.101(5) 0.017(4) -0.037(4) -0.003(4) C(24) 0.105(5) 0.131(6) 0.125(5) -0.002(4) -0.057(4) 0.065(4) C(25) 0.191(7) 0.150(5) 0.100(5) 0.125(4) 0.013(5) 0.032(4) C(26) 0.111(5) 0.072(3) 0.124(6) 0.044(3) 0.001(5) 0.015(4) C(27) 0.097(5) 0.062(3) 0.086(4) 0.014(3) 0.015(4) -0.013(3) C(28) 0.099(4) 0.076(3) 0.059(3) 0.029(3) 0.016(3) 0.003(3) C(29) 0.089(4) 0.081(4) 0.061(3) 0.020(3) 0.011(3) -0.005(3) C(30) 0.074(4) 0.074(3) 0.081(4) 0.026(3) 0.017(3) 0.012(3) C(31) 0.099(5) 0.075(3) 0.095(4) 0.031(3) -0.005(4) 0.033(3) C(32) 0.089(4) 0.088(4) 0.096(5) 0.038(3) -0.001(4) 0.026(3) C(33) 0.085(5) 0.111(5) 0.136(6) 0.018(4) -0.041(4) 0.012(5) C(34) 0.096(5) 0.112(5) 0.114(5) -0.006(4) -0.056(4) 0.022(4) C(35) 0.072(4) 0.074(4) 0.137(6) -0.016(3) -0.021(4) 0.023(4) C(36) 0.127(6) 0.076(4) 0.101(5) -0.036(4) -0.012(5) 0.020(4) C(37) 0.144(7) 0.092(5) 0.076(4) -0.025(5) 0.010(4) 0.026(4) C(38) 0.126(6) 0.088(4) 0.076(4) 0.009(4) 0.030(4) 0.032(3) C(39) 0.34(1) 0.276(9) 0.28(1) 0.248(7) 0.187(10) 0.126(10) C(40) 0.206(9) 0.142(7) 0.25(1) 0.087(6) 0.114(8) 0.007(8) C(41) 0.22(1) 0.23(1) 0.109(6) 0.064(8) 0.077(6) -0.063(6) C(42) 0.190(8) 0.24(1) 0.43(2) 0.148(7) 0.12(1) -0.02(1) C(43) 0.127(7) 0.33(1) 0.097(6) 0.086(8) -0.052(5) 0.008(8) C(44) 0.21(1) 0.56(3) 0.080(7) 0.11(2) -0.021(8) 0.02(1) C(45) 0.042(4) 0.171(8) 0.24(1) -0.027(5) -0.026(6) 0.056(8) C(46) 0.074(5) 0.29(1) 0.129(8) 0.046(7) -0.032(5) -0.004(9) C(47) 0.26(1) 0.143(6) 0.201(10) 0.095(7) -0.025(8) 0.088(6) C(48) 0.23(1) 0.089(5) 0.176(9) -0.017(7) -0.061(8) 0.066(5) C(49) 0.171(8) 0.104(5) 0.104(6) 0.025(5) -0.047(5) 0.006(4) C(50) 0.111(5) 0.069(4) 0.111(5) -0.004(4) -0.041(4) 0.013(4) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) S(1) 2.170(1) . . yes Ni(1) S(5) 2.162(1) . . yes Ni(1) S(6) 2.170(1) . . yes Ni(1) S(10) 2.164(1) . . yes Ni(2) S(11) 2.152(1) . . yes Ni(2) S(15) 2.176(2) . . yes Ni(2) S(16) 2.162(2) . . yes Ni(2) S(20) 2.161(2) . . yes Ni(3) S(21) 2.173(1) . . yes Ni(3) S(25) 2.164(1) . . yes Ni(3) S(26) 2.174(1) . . yes Ni(3) S(30) 2.163(1) . . yes Ca(1) O(1) 2.634(4) . . yes Ca(1) O(2) 2.618(4) . . yes Ca(1) O(3) 2.663(4) . . yes Ca(1) O(4) 2.642(4) . . yes Ca(1) O(5) 2.549(4) . . yes Ca(1) O(6) 2.637(4) . . yes Ca(1) O(7) 2.577(4) . . yes Ca(1) O(8) 2.869(4) . . yes Ca(1) O(9) 2.744(4) . . yes Ca(1) O(10) 2.618(4) . . yes Ca(2) O(11) 2.682(6) . . yes Ca(2) O(11) 2.682(6) . 2_767 yes Ca(2) O(12) 2.739(6) . . yes Ca(2) O(12) 2.739(6) . 2_767 yes Ca(2) O(13) 2.709(7) . . yes Ca(2) O(13) 2.709(7) . 2_767 yes Ca(2) O(14) 2.514(5) . . yes Ca(2) O(14) 2.514(5) . 2_767 yes Ca(2) O(15) 2.585(8) . . yes Ca(2) O(15) 2.585(8) . 2_767 yes S(1) C(1) 1.705(5) . . yes S(2) C(1) 1.750(4) . . yes S(2) C(2) 1.730(5) . . yes S(3) C(2) 1.653(5) . . yes S(4) C(2) 1.727(5) . . yes S(4) C(3) 1.735(5) . . yes S(5) C(3) 1.725(5) . . yes S(6) C(4) 1.715(5) . . yes S(7) C(4) 1.747(5) . . yes S(7) C(5) 1.726(5) . . yes S(8) C(5) 1.647(5) . . yes S(9) C(5) 1.734(5) . . yes S(9) C(6) 1.743(5) . . yes S(10) C(6) 1.718(5) . . yes S(11) C(7) 1.720(6) . . yes S(12) C(7) 1.745(5) . . yes S(12) C(8) 1.727(6) . . yes S(13) C(8) 1.642(7) . . yes S(14) C(8) 1.732(6) . . yes S(14) C(9) 1.743(6) . . yes S(15) C(9) 1.719(5) . . yes S(16) C(10) 1.706(6) . . yes S(17) C(10) 1.744(5) . . yes S(17) C(11) 1.707(7) . . yes S(18) C(11) 1.644(7) . . yes S(19) C(11) 1.744(6) . . yes S(19) C(12) 1.734(6) . . yes S(20) C(12) 1.713(5) . . yes S(21) C(13) 1.726(4) . . yes S(22) C(13) 1.758(4) . . yes S(22) C(14) 1.748(5) . . yes S(23) C(14) 1.641(4) . . yes S(24) C(14) 1.735(5) . . yes S(24) C(15) 1.754(4) . . yes S(25) C(15) 1.718(5) . . yes S(26) C(16) 1.719(4) . . yes S(27) C(16) 1.736(4) . . yes S(27) C(17) 1.731(5) . . yes S(28) C(17) 1.648(5) . . yes S(29) C(17) 1.738(5) . . yes S(29) C(18) 1.747(4) . . yes S(30) C(18) 1.717(5) . . yes O(1) C(19) 1.404(7) . . yes O(1) C(28) 1.418(6) . . yes O(2) C(20) 1.443(7) . . yes O(2) C(21) 1.413(7) . . yes O(3) C(22) 1.418(7) . . yes O(3) C(23) 1.377(8) . . yes O(4) C(24) 1.387(8) . . yes O(4) C(25) 1.340(8) . . yes O(5) C(26) 1.342(8) . . yes O(5) C(27) 1.386(7) . . yes O(6) C(29) 1.430(7) . . yes O(6) C(38) 1.385(8) . . yes O(7) C(30) 1.438(7) . . yes O(7) C(31) 1.420(7) . . yes O(8) C(32) 1.400(7) . . yes O(8) C(33) 1.399(8) . . yes O(9) C(34) 1.407(8) . . yes O(9) C(35) 1.373(9) . . yes O(10) C(36) 1.388(8) . . yes O(10) C(37) 1.397(8) . . yes O(11) C(39) 1.36(1) . . yes O(11) C(48) 1.38(1) . . yes O(12) C(40) 1.26(1) . . yes O(12) C(41) 1.50(1) . . yes O(13) C(42) 1.23(1) . . yes O(13) C(43) 1.39(1) . . yes O(14) C(44) 1.24(1) . . yes O(14) C(45) 1.38(1) . . yes O(15) C(46) 1.21(1) . . yes O(15) C(47) 1.36(1) . . yes N(1) C(50) 1.126(10) . . yes C(1) C(3) 1.371(6) . . yes C(4) C(6) 1.364(6) . . yes C(7) C(9) 1.354(7) . . yes C(10) C(12) 1.380(8) . . yes C(13) C(15) 1.337(6) . . yes C(16) C(18) 1.366(6) . . yes C(19) C(20) 1.470(8) . . yes C(21) C(22) 1.481(9) . . yes C(23) C(24) 1.40(1) . . yes C(25) C(26) 1.44(1) . . yes C(27) C(28) 1.505(9) . . yes C(29) C(30) 1.496(9) . . yes C(31) C(32) 1.470(9) . . yes C(33) C(34) 1.47(1) . . yes C(35) C(36) 1.44(1) . . yes C(37) C(38) 1.422(10) . . yes C(39) C(40) 1.40(2) . . yes C(41) C(42) 1.18(2) . . yes C(43) C(44) 1.36(2) . . yes C(45) C(46) 1.36(2) . . yes C(47) C(48) 1.43(2) . . yes C(49) C(50) 1.40(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ni(1) S(5) 93.33(5) . 1_555 1_555 yes S(1) Ni(1) S(6) 179.29(5) . 1_555 1_555 yes S(1) Ni(1) S(10) 87.05(5) . 1_555 1_555 yes S(5) Ni(1) S(6) 86.67(5) . 1_555 1_555 yes S(5) Ni(1) S(10) 179.51(5) . 1_555 1_555 yes S(6) Ni(1) S(10) 92.94(5) . 1_555 1_555 yes S(11) Ni(2) S(15) 93.14(6) . 1_555 1_555 yes S(11) Ni(2) S(16) 170.58(7) . 1_555 1_555 yes S(11) Ni(2) S(20) 86.22(6) . 1_555 1_555 yes S(15) Ni(2) S(16) 88.64(6) . 1_555 1_555 yes S(15) Ni(2) S(20) 171.75(7) . 1_555 1_555 yes S(16) Ni(2) S(20) 93.33(6) . 1_555 1_555 yes S(21) Ni(3) S(25) 93.28(5) . 1_555 1_555 yes S(21) Ni(3) S(26) 178.29(6) . 1_555 1_555 yes S(21) Ni(3) S(30) 87.00(5) . 1_555 1_555 yes S(25) Ni(3) S(26) 86.59(5) . 1_555 1_555 yes S(25) Ni(3) S(30) 178.09(7) . 1_555 1_555 yes S(26) Ni(3) S(30) 93.07(5) . 1_555 1_555 yes O(1) Ca(1) O(2) 61.3(1) . 1_555 1_555 yes O(1) Ca(1) O(3) 118.4(1) . 1_555 1_555 yes O(1) Ca(1) O(4) 115.7(1) . 1_555 1_555 yes O(1) Ca(1) O(5) 61.0(1) . 1_555 1_555 yes O(1) Ca(1) O(6) 170.3(1) . 1_555 1_555 yes O(1) Ca(1) O(7) 111.9(1) . 1_555 1_555 yes O(1) Ca(1) O(8) 66.8(1) . 1_555 1_555 yes O(1) Ca(1) O(9) 67.4(1) . 1_555 1_555 yes O(1) Ca(1) O(10) 117.3(1) . 1_555 1_555 yes O(2) Ca(1) O(3) 61.8(1) . 1_555 1_555 yes O(2) Ca(1) O(4) 105.0(1) . 1_555 1_555 yes O(2) Ca(1) O(5) 99.2(1) . 1_555 1_555 yes O(2) Ca(1) O(6) 121.6(1) . 1_555 1_555 yes O(2) Ca(1) O(7) 72.6(1) . 1_555 1_555 yes O(2) Ca(1) O(8) 80.3(1) . 1_555 1_555 yes O(2) Ca(1) O(9) 122.8(1) . 1_555 1_555 yes O(2) Ca(1) O(10) 173.7(1) . 1_555 1_555 yes O(3) Ca(1) O(4) 60.5(1) . 1_555 1_555 yes O(3) Ca(1) O(5) 108.0(2) . 1_555 1_555 yes O(3) Ca(1) O(6) 68.7(1) . 1_555 1_555 yes O(3) Ca(1) O(7) 70.5(1) . 1_555 1_555 yes O(3) Ca(1) O(8) 123.2(1) . 1_555 1_555 yes O(3) Ca(1) O(9) 174.0(2) . 1_555 1_555 yes O(3) Ca(1) O(10) 116.5(1) . 1_555 1_555 yes O(4) Ca(1) O(5) 60.5(1) . 1_555 1_555 yes O(4) Ca(1) O(6) 73.2(1) . 1_555 1_555 yes O(4) Ca(1) O(7) 123.1(1) . 1_555 1_555 yes O(4) Ca(1) O(8) 174.6(1) . 1_555 1_555 yes O(4) Ca(1) O(9) 119.1(1) . 1_555 1_555 yes O(4) Ca(1) O(10) 69.6(1) . 1_555 1_555 yes O(5) Ca(1) O(6) 124.7(1) . 1_555 1_555 yes O(5) Ca(1) O(7) 171.5(1) . 1_555 1_555 yes O(5) Ca(1) O(8) 119.3(1) . 1_555 1_555 yes O(5) Ca(1) O(9) 75.7(2) . 1_555 1_555 yes O(5) Ca(1) O(10) 75.4(2) . 1_555 1_555 yes O(6) Ca(1) O(7) 63.0(1) . 1_555 1_555 yes O(6) Ca(1) O(8) 104.0(1) . 1_555 1_555 yes O(6) Ca(1) O(9) 105.4(1) . 1_555 1_555 yes O(6) Ca(1) O(10) 60.8(1) . 1_555 1_555 yes O(7) Ca(1) O(8) 58.0(1) . 1_555 1_555 yes O(7) Ca(1) O(9) 106.6(1) . 1_555 1_555 yes O(7) Ca(1) O(10) 113.0(1) . 1_555 1_555 yes O(8) Ca(1) O(9) 56.7(1) . 1_555 1_555 yes O(8) Ca(1) O(10) 105.0(1) . 1_555 1_555 yes O(9) Ca(1) O(10) 59.4(1) . 1_555 1_555 yes O(11) Ca(2) O(11) 180.0 . 1_555 2_767 yes O(11) Ca(2) O(12) 57.4(2) . 1_555 1_555 yes O(11) Ca(2) O(12) 122.6(2) . 1_555 2_767 yes O(11) Ca(2) O(13) 105.5(2) . 1_555 1_555 yes O(11) Ca(2) O(13) 74.5(2) . 1_555 2_767 yes O(11) Ca(2) O(14) 107.5(2) . 1_555 1_555 yes O(11) Ca(2) O(14) 72.5(2) . 1_555 2_767 yes O(11) Ca(2) O(15) 60.0(2) . 1_555 1_555 yes O(11) Ca(2) O(15) 120.0(2) . 1_555 2_767 yes O(11) Ca(2) O(12) 122.6(2) . 2_767 1_555 yes O(11) Ca(2) O(12) 57.4(2) . 2_767 2_767 yes O(11) Ca(2) O(13) 74.5(2) . 2_767 1_555 yes O(11) Ca(2) O(13) 105.5(2) . 2_767 2_767 yes O(11) Ca(2) O(14) 72.5(2) . 2_767 1_555 yes O(11) Ca(2) O(14) 107.5(2) . 2_767 2_767 yes O(11) Ca(2) O(15) 120.0(2) . 2_767 1_555 yes O(11) Ca(2) O(15) 60.0(2) . 2_767 2_767 yes O(12) Ca(2) O(12) 180.0 . 1_555 2_767 yes O(12) Ca(2) O(13) 58.5(2) . 1_555 1_555 yes O(12) Ca(2) O(13) 121.5(2) . 1_555 2_767 yes O(12) Ca(2) O(14) 105.3(2) . 1_555 1_555 yes O(12) Ca(2) O(14) 74.7(2) . 1_555 2_767 yes O(12) Ca(2) O(15) 105.6(3) . 1_555 1_555 yes O(12) Ca(2) O(15) 74.4(3) . 1_555 2_767 yes O(12) Ca(2) O(13) 121.5(2) . 2_767 1_555 yes O(12) Ca(2) O(13) 58.5(2) . 2_767 2_767 yes O(12) Ca(2) O(14) 74.7(2) . 2_767 1_555 yes O(12) Ca(2) O(14) 105.3(2) . 2_767 2_767 yes O(12) Ca(2) O(15) 74.4(3) . 2_767 1_555 yes O(12) Ca(2) O(15) 105.6(3) . 2_767 2_767 yes O(13) Ca(2) O(13) 180.0000(1) . 1_555 2_767 yes O(13) Ca(2) O(14) 59.7(2) . 1_555 1_555 yes O(13) Ca(2) O(14) 120.3(2) . 1_555 2_767 yes O(13) Ca(2) O(15) 108.7(3) . 1_555 1_555 yes O(13) Ca(2) O(15) 71.3(3) . 1_555 2_767 yes O(13) Ca(2) O(14) 120.3(2) . 2_767 1_555 yes O(13) Ca(2) O(14) 59.7(2) . 2_767 2_767 yes O(13) Ca(2) O(15) 71.3(3) . 2_767 1_555 yes O(13) Ca(2) O(15) 108.7(3) . 2_767 2_767 yes O(14) Ca(2) O(14) 180.0 . 1_555 2_767 yes O(14) Ca(2) O(15) 61.4(2) . 1_555 1_555 yes O(14) Ca(2) O(15) 118.6(2) . 1_555 2_767 yes O(14) Ca(2) O(15) 118.6(2) . 2_767 1_555 yes O(14) Ca(2) O(15) 61.4(2) . 2_767 2_767 yes O(15) Ca(2) O(15) 180.0 . 1_555 2_767 yes Ni(1) S(1) C(1) 102.0(2) . 1_555 1_555 yes C(1) S(2) C(2) 97.5(2) . 1_555 1_555 yes C(2) S(4) C(3) 97.5(2) . 1_555 1_555 yes Ni(1) S(5) C(3) 102.1(2) . 1_555 1_555 yes Ni(1) S(6) C(4) 102.3(2) . 1_555 1_555 yes C(4) S(7) C(5) 97.3(2) . 1_555 1_555 yes C(5) S(9) C(6) 97.3(2) . 1_555 1_555 yes Ni(1) S(10) C(6) 102.3(2) . 1_555 1_555 yes Ni(2) S(11) C(7) 102.0(2) . 1_555 1_555 yes C(7) S(12) C(8) 97.2(3) . 1_555 1_555 yes C(8) S(14) C(9) 97.4(3) . 1_555 1_555 yes Ni(2) S(15) C(9) 102.2(2) . 1_555 1_555 yes Ni(2) S(16) C(10) 102.0(2) . 1_555 1_555 yes C(10) S(17) C(11) 98.3(3) . 1_555 1_555 yes C(11) S(19) C(12) 96.9(3) . 1_555 1_555 yes Ni(2) S(20) C(12) 102.6(2) . 1_555 1_555 yes Ni(3) S(21) C(13) 101.6(2) . 1_555 1_555 yes C(13) S(22) C(14) 96.9(2) . 1_555 1_555 yes C(14) S(24) C(15) 97.3(2) . 1_555 1_555 yes Ni(3) S(25) C(15) 101.5(2) . 1_555 1_555 yes Ni(3) S(26) C(16) 102.1(2) . 1_555 1_555 yes C(16) S(27) C(17) 97.7(2) . 1_555 1_555 yes C(17) S(29) C(18) 97.2(2) . 1_555 1_555 yes Ni(3) S(30) C(18) 102.2(2) . 1_555 1_555 yes Ca(1) O(1) C(19) 113.9(3) . 1_555 1_555 yes Ca(1) O(1) C(28) 119.5(3) . 1_555 1_555 yes C(19) O(1) C(28) 112.9(5) . 1_555 1_555 yes Ca(1) O(2) C(20) 121.8(3) . 1_555 1_555 yes Ca(1) O(2) C(21) 121.5(4) . 1_555 1_555 yes C(20) O(2) C(21) 110.5(4) . 1_555 1_555 yes Ca(1) O(3) C(22) 114.8(4) . 1_555 1_555 yes Ca(1) O(3) C(23) 121.0(4) . 1_555 1_555 yes C(22) O(3) C(23) 114.1(5) . 1_555 1_555 yes Ca(1) O(4) C(24) 118.1(4) . 1_555 1_555 yes Ca(1) O(4) C(25) 120.9(4) . 1_555 1_555 yes C(24) O(4) C(25) 116.1(6) . 1_555 1_555 yes Ca(1) O(5) C(26) 124.1(4) . 1_555 1_555 yes Ca(1) O(5) C(27) 120.5(3) . 1_555 1_555 yes C(26) O(5) C(27) 114.9(5) . 1_555 1_555 yes Ca(1) O(6) C(29) 115.0(3) . 1_555 1_555 yes Ca(1) O(6) C(38) 119.7(4) . 1_555 1_555 yes C(29) O(6) C(38) 114.0(5) . 1_555 1_555 yes Ca(1) O(7) C(30) 115.6(3) . 1_555 1_555 yes Ca(1) O(7) C(31) 118.2(3) . 1_555 1_555 yes C(30) O(7) C(31) 112.3(4) . 1_555 1_555 yes Ca(1) O(8) C(32) 119.2(4) . 1_555 1_555 yes Ca(1) O(8) C(33) 122.9(4) . 1_555 1_555 yes C(32) O(8) C(33) 110.1(5) . 1_555 1_555 yes Ca(1) O(9) C(34) 120.0(4) . 1_555 1_555 yes Ca(1) O(9) C(35) 117.7(4) . 1_555 1_555 yes C(34) O(9) C(35) 114.3(6) . 1_555 1_555 yes Ca(1) O(10) C(36) 122.5(4) . 1_555 1_555 yes Ca(1) O(10) C(37) 118.0(4) . 1_555 1_555 yes C(36) O(10) C(37) 116.7(5) . 1_555 1_555 yes Ca(2) O(11) C(39) 119.1(7) . 1_555 1_555 yes Ca(2) O(11) C(48) 124.1(7) . 1_555 1_555 yes C(39) O(11) C(48) 109.5(9) . 1_555 1_555 yes Ca(2) O(12) C(40) 125.3(8) . 1_555 1_555 yes Ca(2) O(12) C(41) 116.0(5) . 1_555 1_555 yes C(40) O(12) C(41) 110.3(9) . 1_555 1_555 yes Ca(2) O(13) C(42) 114.5(10) . 1_555 1_555 yes Ca(2) O(13) C(43) 117.1(6) . 1_555 1_555 yes C(42) O(13) C(43) 120(1) . 1_555 1_555 yes Ca(2) O(14) C(44) 124.1(9) . 1_555 1_555 yes Ca(2) O(14) C(45) 122.3(6) . 1_555 1_555 yes C(44) O(14) C(45) 110(1) . 1_555 1_555 yes Ca(2) O(15) C(46) 116.7(8) . 1_555 1_555 yes Ca(2) O(15) C(47) 116.1(7) . 1_555 1_555 yes C(46) O(15) C(47) 124(1) . 1_555 1_555 yes S(1) C(1) S(2) 122.9(3) . 1_555 1_555 yes S(1) C(1) C(3) 121.9(3) . 1_555 1_555 yes S(2) C(1) C(3) 115.2(3) . 1_555 1_555 yes S(2) C(2) S(3) 123.6(3) . 1_555 1_555 yes S(2) C(2) S(4) 113.3(3) . 1_555 1_555 yes S(3) C(2) S(4) 123.1(3) . 1_555 1_555 yes S(4) C(3) S(5) 123.0(3) . 1_555 1_555 yes S(4) C(3) C(1) 116.4(3) . 1_555 1_555 yes S(5) C(3) C(1) 120.6(4) . 1_555 1_555 yes S(6) C(4) S(7) 122.9(3) . 1_555 1_555 yes S(6) C(4) C(6) 121.1(4) . 1_555 1_555 yes S(7) C(4) C(6) 116.0(4) . 1_555 1_555 yes S(7) C(5) S(8) 124.2(3) . 1_555 1_555 yes S(7) C(5) S(9) 113.4(3) . 1_555 1_555 yes S(8) C(5) S(9) 122.4(3) . 1_555 1_555 yes S(9) C(6) S(10) 122.8(3) . 1_555 1_555 yes S(9) C(6) C(4) 115.9(4) . 1_555 1_555 yes S(10) C(6) C(4) 121.3(4) . 1_555 1_555 yes S(11) C(7) S(12) 121.5(3) . 1_555 1_555 yes S(11) C(7) C(9) 122.2(4) . 1_555 1_555 yes S(12) C(7) C(9) 116.3(4) . 1_555 1_555 yes S(12) C(8) S(13) 122.8(4) . 1_555 1_555 yes S(12) C(8) S(14) 113.2(4) . 1_555 1_555 yes S(13) C(8) S(14) 124.0(4) . 1_555 1_555 yes S(14) C(9) S(15) 123.7(3) . 1_555 1_555 yes S(14) C(9) C(7) 115.9(4) . 1_555 1_555 yes S(15) C(9) C(7) 120.5(4) . 1_555 1_555 yes S(16) C(10) S(17) 123.3(3) . 1_555 1_555 yes S(16) C(10) C(12) 122.0(4) . 1_555 1_555 yes S(17) C(10) C(12) 114.6(5) . 1_555 1_555 yes S(17) C(11) S(18) 124.5(4) . 1_555 1_555 yes S(17) C(11) S(19) 113.4(4) . 1_555 1_555 yes S(18) C(11) S(19) 122.0(4) . 1_555 1_555 yes S(19) C(12) S(20) 123.2(3) . 1_555 1_555 yes S(19) C(12) C(10) 116.7(4) . 1_555 1_555 yes S(20) C(12) C(10) 120.1(5) . 1_555 1_555 yes S(21) C(13) S(22) 122.3(3) . 1_555 1_555 yes S(21) C(13) C(15) 121.2(3) . 1_555 1_555 yes S(22) C(13) C(15) 116.5(3) . 1_555 1_555 yes S(22) C(14) S(23) 123.5(3) . 1_555 1_555 yes S(22) C(14) S(24) 112.9(2) . 1_555 1_555 yes S(23) C(14) S(24) 123.6(3) . 1_555 1_555 yes S(24) C(15) S(25) 121.1(3) . 1_555 1_555 yes S(24) C(15) C(13) 116.4(3) . 1_555 1_555 yes S(25) C(15) C(13) 122.5(3) . 1_555 1_555 yes S(26) C(16) S(27) 123.1(3) . 1_555 1_555 yes S(26) C(16) C(18) 120.9(3) . 1_555 1_555 yes S(27) C(16) C(18) 116.0(3) . 1_555 1_555 yes S(27) C(17) S(28) 124.9(3) . 1_555 1_555 yes S(27) C(17) S(29) 113.0(3) . 1_555 1_555 yes S(28) C(17) S(29) 122.0(3) . 1_555 1_555 yes S(29) C(18) S(30) 122.4(3) . 1_555 1_555 yes S(29) C(18) C(16) 116.0(3) . 1_555 1_555 yes S(30) C(18) C(16) 121.5(3) . 1_555 1_555 yes O(1) C(19) C(20) 111.6(5) . 1_555 1_555 yes O(2) C(20) C(19) 107.5(5) . 1_555 1_555 yes O(2) C(21) C(22) 109.1(5) . 1_555 1_555 yes O(3) C(22) C(21) 111.5(5) . 1_555 1_555 yes O(3) C(23) C(24) 111.7(6) . 1_555 1_555 yes O(4) C(24) C(23) 116.1(6) . 1_555 1_555 yes O(4) C(25) C(26) 116.5(6) . 1_555 1_555 yes O(5) C(26) C(25) 114.2(5) . 1_555 1_555 yes O(5) C(27) C(28) 108.3(4) . 1_555 1_555 yes O(1) C(28) C(27) 106.9(5) . 1_555 1_555 yes O(6) C(29) C(30) 108.9(5) . 1_555 1_555 yes O(7) C(30) C(29) 104.6(5) . 1_555 1_555 yes O(7) C(31) C(32) 111.8(5) . 1_555 1_555 yes O(8) C(32) C(31) 107.1(5) . 1_555 1_555 yes O(8) C(33) C(34) 108.3(6) . 1_555 1_555 yes O(9) C(34) C(33) 112.9(6) . 1_555 1_555 yes O(9) C(35) C(36) 111.4(6) . 1_555 1_555 yes O(10) C(36) C(35) 112.1(6) . 1_555 1_555 yes O(10) C(37) C(38) 112.1(6) . 1_555 1_555 yes O(6) C(38) C(37) 110.6(6) . 1_555 1_555 yes O(11) C(39) C(40) 119(1) . 1_555 1_555 yes O(12) C(40) C(39) 114.2(9) . 1_555 1_555 yes O(12) C(41) C(42) 108(1) . 1_555 1_555 yes O(13) C(42) C(41) 132(1) . 1_555 1_555 yes O(13) C(43) C(44) 113.2(9) . 1_555 1_555 yes O(14) C(44) C(43) 122(1) . 1_555 1_555 yes O(14) C(45) C(46) 110.5(8) . 1_555 1_555 yes O(15) C(46) C(45) 127(1) . 1_555 1_555 yes O(15) C(47) C(48) 120(1) . 1_555 1_555 yes O(11) C(48) C(47) 103.0(8) . 1_555 1_555 yes N(1) C(50) C(49) 178.2(8) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ca(1) O(1) 2.634(4) . . ? Ca(1) O(2) 2.618(4) . . ? Ca(1) O(3) 2.663(4) . . ? Ca(1) O(4) 2.642(4) . . ? Ca(1) O(5) 2.549(4) . . ? Ca(1) O(6) 2.637(4) . . ? Ca(1) O(7) 2.577(4) . . ? Ca(1) O(8) 2.869(4) . . ? Ca(1) O(9) 2.744(4) . . ? Ca(1) O(10) 2.618(4) . . ? Ca(2) O(11) 2.682(6) . . ? Ca(2) O(11) 2.682(6) . 2_767 ? Ca(2) O(12) 2.739(6) . . ? Ca(2) O(12) 2.739(6) . 2_767 ? Ca(2) O(13) 2.709(7) . . ? Ca(2) O(13) 2.709(7) . 2_767 ? Ca(2) O(14) 2.514(5) . . ? Ca(2) O(14) 2.514(5) . 2_767 ? Ca(2) O(15) 2.585(8) . . ? Ca(2) O(15) 2.585(8) . 2_767 ? Ca(1) O(5) 2.549(4) . . ? Ca(1) O(7) 2.577(4) . . ? Ca(1) O(10) 2.618(4) . . ? Ca(1) O(2) 2.618(4) . . ? Ca(1) O(1) 2.634(4) . . ? Ca(1) O(6) 2.637(4) . . ? Ca(1) O(4) 2.642(4) . . ? Ca(1) O(3) 2.663(4) . . ? Ca(1) O(9) 2.744(4) . . ? Ca(1) O(8) 2.869(4) . . ? Ca(1) C(19) 3.451(6) . . ? Ca(1) C(30) 3.451(6) . . ? Ca(1) C(27) 3.465(5) . . ? Ca(1) C(31) 3.482(6) . . ? Ca(1) C(26) 3.484(6) . . ? Ca(1) C(29) 3.491(6) . . ? Ca(1) C(37) 3.499(7) . . ? Ca(1) C(22) 3.502(5) . . ? Ca(1) C(24) 3.516(7) . . ? Ca(1) C(25) 3.523(7) . . ? Ca(1) C(38) 3.535(7) . . ? Ca(1) C(28) 3.553(6) . . ? Ca(1) C(36) 3.561(7) . . ? Ca(1) C(21) 3.566(6) . . ? Ca(1) C(23) 3.572(7) . . ? Ca(1) C(35) 3.594(6) . . ? Ca(1) C(20) 3.594(6) . . ? Ca(2) O(14) 2.514(5) . . ? Ca(2) O(14) 2.514(5) . 2_767 ? Ca(2) O(15) 2.585(8) . . ? Ca(2) O(15) 2.585(8) . 2_767 ? Ca(2) O(11) 2.682(6) . . ? Ca(2) O(11) 2.682(6) . 2_767 ? Ca(2) O(13) 2.709(7) . . ? Ca(2) O(13) 2.709(7) . 2_767 ? Ca(2) O(12) 2.739(6) . . ? Ca(2) O(12) 2.739(6) . 2_767 ? Ca(2) C(46) 3.31(1) . . ? Ca(2) C(46) 3.31(1) . 2_767 ? Ca(2) C(44) 3.37(1) . . ? Ca(2) C(44) 3.37(1) . 2_767 ? Ca(2) C(42) 3.41(2) . . ? Ca(2) C(42) 3.41(2) . 2_767 ? Ca(2) C(47) 3.41(1) . . ? Ca(2) C(47) 3.41(1) . 2_767 ? Ca(2) C(45) 3.453(7) . . ? Ca(2) C(45) 3.453(7) . 2_767 ? Ca(2) C(39) 3.55(1) . . ? Ca(2) C(39) 3.55(1) . 2_767 ? Ca(2) C(43) 3.565(9) . . ? Ca(2) C(43) 3.565(9) . 2_767 ? S(2) S(7) 3.508(2) . 1_455 ? S(2) S(23) 3.529(2) . 1_565 ? S(2) S(24) 3.547(2) . 1_565 ? S(4) S(12) 3.439(2) . 1_565 ? S(4) S(30) 3.543(2) . . ? S(8) C(20) 3.580(6) . 2_866 ? S(13) S(29) 3.583(3) . 1_545 ? O(1) O(9) 2.986(6) . . ? O(1) O(8) 3.034(5) . . ? O(1) C(34) 3.109(9) . . ? O(1) C(33) 3.596(9) . . ? O(2) O(7) 3.076(5) . . ? O(2) C(31) 3.239(8) . . ? O(2) O(8) 3.545(6) . . ? O(3) O(6) 2.991(6) . . ? O(3) O(7) 3.025(6) . . ? O(3) C(29) 3.251(8) . . ? O(4) O(10) 3.003(6) . . ? O(4) O(6) 3.148(6) . . ? O(4) C(37) 3.263(10) . . ? O(5) O(10) 3.159(6) . . ? O(5) O(9) 3.252(7) . . ? O(6) C(24) 3.364(9) . . ? O(7) C(22) 3.161(7) . . ? O(8) C(19) 3.139(8) . . ? O(9) C(27) 3.332(8) . . ? O(10) C(26) 3.428(9) . . ? O(10) C(25) 3.496(10) . . ? O(11) O(14) 3.076(10) . 2_767 ? O(11) O(13) 3.261(10) . 2_767 ? O(11) C(44) 3.37(2) . 2_767 ? O(12) O(14) 3.19(1) . 2_767 ? O(12) O(15) 3.22(1) . 2_767 ? O(12) C(46) 3.45(1) . 2_767 ? O(13) O(15) 3.09(1) . 2_767 ? O(13) C(47) 3.30(1) . 2_767 ? O(14) C(39) 3.39(2) . 2_767 ? O(15) C(42) 3.37(2) . 2_767 ? N(1) C(43) 3.18(1) . 1_545 ? N(1) C(30) 3.26(1) . 1_545 ? N(1) C(44) 3.33(2) . 1_545 ? N(1) C(29) 3.39(1) . 1_545 ? C(6) C(27) 3.539(7) . 1_665 ? #------------------------------------------------------------------------------ #============================================================================== data__master_file_afc7*.xtl _database_code_CSD 158719 _audit_creation_date '2001-04-12' _audit_creation_method 'by CrystalStructure v1.00' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum ' C28 H31 Ca N3 Ni2 O5 S20 ' _chemical_formula_moiety ' C28 H31 Ca N3 Ni2 O5 S20 ' _chemical_formula_weight 1288.25 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/m n m ' _symmetry_Int_Tables_number 136 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, +z' '1/2+x,1/2-y,1/2+z' '1/2-x,1/2+y,1/2+z' ' +y, +x, +z' ' -y, -x, +z' '1/2+y,1/2-x,1/2+z' '1/2-y,1/2+x,1/2+z' ' -x, -y, -z' ' +x, +y, -z' '1/2-x,1/2+y,1/2-z' '1/2+x,1/2-y,1/2-z' ' -y, -x, -z' ' +y, +x, -z' '1/2-y,1/2+x,1/2-z' '1/2+y,1/2-x,1/2-z' #------------------------------------------------------------------------------ _cell_length_a 15.598(3) _cell_length_b 15.5975 _cell_length_c 10.222(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2486.9(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.6 _cell_measurement_theta_max 14.9 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_meas 1.800 _exptl_crystal_density_method ? _exptl_absorpt_coefficient_mu 1.739 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 0.840 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 1706 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.37 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). 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 947 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0500 _refine_ls_wR_factor_obs 0.0810 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 947 _refine_ls_number_parameters 87 _refine_ls_goodness_of_fit_obs 3.470 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/\s^2^(Fo^2^)' _refine_ls_shift/esd_max 0.2600 _refine_diff_density_max 0.96 _refine_diff_density_min -1.00 _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' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Ni' 'Ni' 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.017 0.010 ; 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) ; 'Ca' 'Ca' 0.252 0.372 ; 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_thermal_displace_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 0.81885(9) -0.18115(9) 0.5000 0.0486(4) Uani 1.00 4 d S . . Ca(1) Ca 1.0000 0.0000 0.0000 0.071(1) Uani 1.00 8 d S . . S(1) S 0.8871(1) -0.2476(1) 0.3467(2) 0.0656(6) Uani 1.00 1 d . . . S(2) S 1.0346(1) -0.3744(1) 0.3591(2) 0.0576(6) Uani 1.00 1 d . . . S(3) S 1.1576(2) -0.4855(2) 0.5000 0.0633(9) Uani 1.00 2 d S . . O(1) O 1.060(1) -0.060(1) -0.217(2) 0.238(7) Uani 1.00 2 d S . . N(1) N 1.1143(8) -0.1143(8) 0.0000 0.22(1) Uani 1.00 4 d S . . N(2) N 0.8885(6) -0.1115(6) 0.0000 0.079(4) Uani 1.00 4 d S . . C(1) C 0.9591(4) -0.3093(4) 0.4324(5) 0.044(2) Uani 1.00 1 d . . . C(2) C 1.0796(6) -0.4155(6) 0.5000 0.047(3) Uani 1.00 2 d S . . C(3) C 1.145(1) -0.145(1) -0.114(4) 0.29(2) Uani 1.00 2 d S . . C(4) C 1.0929 -0.1582 -0.2093 0.18(2) Uani 0.50 1 d P . . C(5) C 1.038(2) -0.038(2) -0.321(2) 0.30(2) Uani 1.00 2 d S . . C(6) C 0.8338(9) -0.1662(9) 0.0000 0.074(4) Uani 1.00 4 d S . . C(7) C 0.7689(6) -0.2311(6) 0.0000 0.079(5) Uani 1.00 4 d S . . 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) 0.0487(7) 0.0487(7) 0.049(1) 0.010(1) 0.0000 0.0000 Ca(1) 0.058(2) 0.058(2) 0.098(4) -0.009(2) 0.0000 0.0000 S(1) 0.075(1) 0.074(1) 0.048(1) 0.033(1) -0.004(1) -0.004(1) S(2) 0.058(1) 0.063(1) 0.052(1) 0.019(1) 0.002(1) -0.004(1) S(3) 0.052(2) 0.060(2) 0.078(2) 0.013(1) 0.0000 0.0000 O(1) 0.30(2) 0.30(2) 0.12(1) -0.00(2) 0.07(1) -0.07(1) N(1) 0.17(2) 0.17(2) 0.31(4) 0.14(2) 0.0000 0.0000 N(2) 0.067(6) 0.067(6) 0.10(1) 0.001(8) 0.0000 0.0000 C(1) 0.047(4) 0.042(4) 0.042(3) 0.005(3) -0.001(3) -0.001(3) C(2) 0.037(6) 0.035(6) 0.070(7) -0.001(4) 0.0000 0.0000 C(3) 0.21(2) 0.21(2) 0.46(7) 0.09(2) 0.09(2) -0.09(2) C(4) 0.13(3) 0.13(2) 0.27(5) -0.04(2) 0.04(3) -0.11(3) C(5) 0.40(6) 0.40(6) 0.11(1) -0.11(6) 0.09(2) -0.09(2) C(6) 0.083(8) 0.083(8) 0.05(1) 0.04(1) 0.0000 0.0000 C(7) 0.053(7) 0.053(7) 0.13(2) -0.037(8) 0.0000 0.0000 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR92' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 1.00' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 . S1 . 2.1587(18) yes S1 . C1 . 1.719(6) yes S2 . C1 . 1.726(6) yes S2 . C2 . 1.726(5) yes S3 . C2 . 1.635(9) yes O1 . C4 . 1.61(2) yes O1 . C5 . 1.18(3) yes N1 . C3 . 1.35(3) yes N2 . C6 . 1.21(2) yes C3 . C4 . 1.29(3) yes C6 . C7 . 1.43(2) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Ni1 . S1 . C1 . 102.8(2) yes C1 . S2 . C2 . 97.7(3) yes C4 . O1 . C5 . 114.8(21) yes S1 . C1 . S2 . 123.7(3) yes S2 . C2 . S3 . 123.4(3) yes N1 . C3 . C4 . 118.9(15) yes O1 . C4 . C3 . 95.0(10) yes N2 . C6 . C7 . 179.992 yes loop_ _geom_contact_atom_site_label_1 _geom_contact_site_symmetry_1 _geom_contact_atom_site_label_2 _geom_contact_site_symmetry_2 _geom_contact_distance _geom_contact_publ_flag Ni1 . S1 6_556 2.1587(18) yes Ni1 . S1 11_645 2.1587(18) yes Ni1 . S1 16_646 2.1587(18) yes Ni1 . C1 6_556 3.043(6) yes Ni1 . C1 11_645 3.043(6) yes Ni1 . C1 16_646 3.043(6) yes Ca1 . O1 2_755 2.586(14) yes Ca1 . O1 5_755 2.586(14) yes Ca1 . O1 6_555 2.586(14) yes Ca1 . N1 2_755 2.521(18) yes Ca1 . N2 2_755 2.460(13) yes Ca1 . C3 2_755 3.41(2) yes Ca1 . C3 5_755 3.41(2) yes Ca1 . C3 6_555 3.41(2) yes Ca1 . C4 2_755 3.5732(5) yes Ca1 . C4 5_755 3.5732(5) yes Ca1 . C4 6_555 3.5732(5) yes Ca1 . C4 11_645 3.5732(5) yes Ca1 . C4 12_665 3.5732(5) yes Ca1 . C4 15_665 3.5732(5) yes Ca1 . C4 16_645 3.5732(5) yes Ca1 . C5 2_755 3.39(2) yes Ca1 . C5 5_755 3.39(2) yes Ca1 . C5 6_555 3.39(2) yes S1 . S1 6_556 3.133(4) yes S1 . S1 11_645 2.970(3) yes S1 . C1 6_556 2.700(6) yes S2 . S2 6_556 2.881(4) yes S2 . C1 6_556 2.639(6) yes O1 . O1 5_755 2.67(5) yes O1 . N2 2_755 3.569(14) yes O1 . C4 15_665 1.61(2) yes O1 . C5 5_755 2.42(3) yes N1 . N2 2_755 3.522(16) yes N1 . C3 6_555 1.35(3) yes N1 . C4 6_555 2.271(2) yes N1 . C4 12_665 2.271(2) yes N1 . C4 15_665 2.271(2) yes C1 . C1 6_556 1.383(11) yes C3 . C3 6_555 2.33(8) yes C3 . C4 6_555 3.41(4) yes C3 . C4 12_665 3.41(4) yes C3 . C4 15_665 1.29(3) yes C4 . C4 15_665 1.43996(12) yes C5 . C5 5_755 1.68(8) yes #============================================================================== #============================================================================== # End of CIF #==============================================================================