Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Dr. Zhen-Feng Chen' _publ_contact_author_address ; The Key Laboratory of Medicinal Chemical Resources and Molecular Engineering (Ministry of Education) School of Chemistry and Chemical Guangxi Normal University Guilin 541004 China ; _publ_contact_author_email chenzfubc@yahoo.com _publ_contact_author_fax '86 773 5812383' _publ_contact_author_phone '86 773 5837207' #========================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Ni~2~(R*COO)~4~(H~2~O)(4,4'-bipy)~2~- a robust homochiral quartz-like network with large chiral channels ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Zhen-Feng Chen.' ? ; The Key Laboratory of Medicinal Chemical Resources and Molecular Engineering (Ministry of Education) School of Chemistry and Chemical Guangxi Normal University Guilin 541004 China ; 'Shu-Feng Zhang.' ? ; The Key Laboratory of Medicinal Chemical Resources and Molecular Engineering (Ministry of Education) School of Chemistry and Chemical Guangxi Normal University Guilin 541004 China ; 'Hai-Sheng Luo.' ? ; The Key Laboratory of Medicinal Chemical Resources and Molecular Engineering (Ministry of Education) School of Chemistry and Chemical Guangxi Normal University Guilin 541004 China ; 'Brendan F. Abrahams' ? ; School of Chemistry University of Melbourne Parkville, Victoria, 3010 Australia ; ; Hong Liang ; ? ; The Key Laboratory of Medicinal Chemical Resources and Molecular Engineering (Ministry of Education) School of Chemistry and Chemical Guangxi Normal University Guilin 541004 China ; #========================================================================== data_chenp3121 _database_code_depnum_ccdc_archive 'CCDC 619677' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H126 N4 Ni2 O9' _chemical_formula_weight 1645.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' 'y, x, -z' _cell_length_a 25.531(5) _cell_length_b 25.531(5) _cell_length_c 14.907(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 8415(4) _cell_formula_units_Z 3 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 19807 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour yellow-green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2646 _exptl_absorpt_coefficient_mu 0.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 0.909 _exptl_absorpt_process_details ; 'Jacobson, R. (1998) Private communication' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58691 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.34 _reflns_number_total 10246 _reflns_number_gt 8843 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+4.0622P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(2) _refine_ls_number_reflns 10246 _refine_ls_number_parameters 546 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.1892 _refine_ls_wR_factor_gt 0.1818 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.51642(3) 0.07144(2) 0.88273(4) 0.03379(16) Uani 1 1 d . . . O2 O 0.47055(15) 0.08181(14) 0.9908(2) 0.0400(8) Uani 1 1 d . . . O5 O 0.43701(19) 0.0000 0.8333 0.0373(11) Uani 1 2 d S . . H5A H 0.4111 -0.0129 0.8745 0.045 Uiso 0.50 1 calc PR . . H5B H 0.4240 0.0129 0.7921 0.045 Uiso 0.50 1 calc PR . . O3 O 0.52965(18) 0.01479(15) 0.9599(2) 0.0495(10) Uani 1 1 d . . . O1 O 0.38403(18) -0.00475(17) 0.9801(2) 0.0593(11) Uani 1 1 d . . . O4 O 0.49386(17) -0.07419(15) 0.8905(2) 0.0448(9) Uani 1 1 d . . . N1 N 0.5054(2) 0.13783(17) 0.8161(3) 0.0415(10) Uani 1 1 d . . . N2 N 0.5973(2) 0.13799(17) 0.9406(3) 0.0404(10) Uani 1 1 d . . . C37 C 0.6160(2) -0.0104(3) 1.0383(3) 0.0452(13) Uani 1 1 d . C . H37 H 0.6170 0.0293 1.0371 0.054 Uiso 1 1 calc R . . C3 C 0.5095(2) 0.2384(2) 0.7323(3) 0.0434(12) Uani 1 1 d . . . C32 C 0.5476(2) -0.0577(2) 1.0321(3) 0.0413(12) Uani 1 1 d . . . C17 C 0.4422(3) 0.0951(2) 1.1684(3) 0.0426(12) Uani 1 1 d . B . H17 H 0.4777 0.1256 1.1331 0.051 Uiso 1 1 calc R . . C12 C 0.3915(3) 0.0625(3) 1.0988(4) 0.0473(13) Uani 1 1 d . . . C16 C 0.4327(3) 0.1324(2) 1.2428(4) 0.0511(14) Uani 1 1 d . . . C21 C 0.4926(3) 0.1685(3) 1.2929(4) 0.0493(13) Uani 1 1 d . B . C31 C 0.5218(2) -0.0377(2) 0.9531(3) 0.0372(11) Uani 1 1 d . . . C2 C 0.5039(3) 0.1896(2) 0.6846(4) 0.0527(15) Uani 1 1 d . . . H2 H 0.5015 0.1897 0.6210 0.063 Uiso 1 1 calc R . . C4 C 0.5117(3) 0.2342(3) 0.8262(4) 0.0562(15) Uani 1 1 d . . . H4 H 0.5148 0.2660 0.8631 0.067 Uiso 1 1 calc R . . C1 C 0.5017(3) 0.1406(2) 0.7274(4) 0.0502(14) Uani 1 1 d . . . H1 H 0.4973 0.1077 0.6922 0.060 Uiso 1 1 calc R . . C5 C 0.5095(3) 0.1842(2) 0.8643(4) 0.0541(15) Uani 1 1 d . . . H5 H 0.5110 0.1823 0.9278 0.065 Uiso 1 1 calc R . . C7 C 0.7012(3) 0.2150(3) 0.9325(4) 0.075(2) Uani 1 1 d . . . H7 H 0.7353 0.2384 0.8953 0.090 Uiso 1 1 calc R . . C24 C 0.6013(4) 0.2353(3) 1.3933(4) 0.0715(18) Uani 1 1 d . . . C36 C 0.6516(3) -0.0068(3) 1.1242(4) 0.0604(16) Uani 1 1 d . . . C15 C 0.4142(3) 0.1750(3) 1.1972(4) 0.0677(18) Uani 1 1 d . . . H15A H 0.4037 0.1958 1.2439 0.081 Uiso 1 1 calc R . . H15B H 0.4490 0.2062 1.1628 0.081 Uiso 1 1 calc R . . C11 C 0.4182(2) 0.0445(2) 1.0179(3) 0.0420(12) Uani 1 1 d . . . C20 C 0.5338(3) 0.1484(3) 1.3015(4) 0.0558(15) Uani 1 1 d . . . C25 C 0.5864(3) 0.1816(3) 1.3507(4) 0.0685(18) Uani 1 1 d . B . H25 H 0.6136 0.1665 1.3554 0.082 Uiso 1 1 calc R . . C38 C 0.6510(3) -0.0087(4) 0.9545(4) 0.0701(19) Uani 1 1 d . . . H38A H 0.6603 -0.0420 0.9567 0.084 Uiso 1 1 calc R C . H38B H 0.6261 -0.0144 0.9005 0.084 Uiso 1 1 calc R . . C18 C 0.4631(3) 0.0545(3) 1.2100(4) 0.0617(17) Uani 1 1 d . . . H18A H 0.4326 0.0273 1.2541 0.074 Uiso 1 1 calc R B . H18B H 0.4662 0.0291 1.1626 0.074 Uiso 1 1 calc R . . C6 C 0.6463(3) 0.1733(3) 0.8938(4) 0.073(2) Uani 1 1 d . . . H6 H 0.6440 0.1702 0.8303 0.087 Uiso 1 1 calc R . . C13 C 0.3745(3) 0.1075(3) 1.0599(4) 0.0640(17) Uani 1 1 d . . . H13A H 0.3387 0.0855 1.0206 0.077 Uiso 1 1 calc R . . H13B H 0.4083 0.1374 1.0226 0.077 Uiso 1 1 calc R . . C35 C 0.6151(4) -0.0049(4) 1.2025(4) 0.086(2) Uani 1 1 d . C . H35A H 0.6345 -0.0071 1.2588 0.104 Uiso 1 1 calc R . . H35B H 0.6161 0.0343 1.2019 0.104 Uiso 1 1 calc R . . C9 C 0.6561(3) 0.1843(4) 1.0715(4) 0.083(3) Uani 1 1 d . . . H9 H 0.6574 0.1861 1.1351 0.100 Uiso 1 1 calc R . . C14 C 0.3602(4) 0.1410(4) 1.1340(5) 0.081(2) Uani 1 1 d . . . H14A H 0.3501 0.1701 1.1059 0.097 Uiso 1 1 calc R . . H14B H 0.3245 0.1115 1.1689 0.097 Uiso 1 1 calc R . . C19 C 0.5235(4) 0.0900(3) 1.2562(4) 0.0700(19) Uani 1 1 d . B . H19A H 0.5559 0.1004 1.2115 0.084 Uiso 1 1 calc R . . H19B H 0.5270 0.0639 1.3022 0.084 Uiso 1 1 calc R . . C27 C 0.3839(3) 0.0939(3) 1.3149(4) 0.075(2) Uani 1 1 d . . . H27A H 0.3445 0.0699 1.2858 0.112 Uiso 1 1 calc R . . H27B H 0.3815 0.1208 1.3594 0.112 Uiso 1 1 calc R . . H27C H 0.3952 0.0667 1.3448 0.112 Uiso 1 1 calc R . . C46 C 0.5346(3) -0.1228(3) 1.0159(5) 0.0671(18) Uani 1 1 d . . . H46A H 0.5550 -0.1240 0.9609 0.101 Uiso 1 1 calc R . . H46B H 0.4909 -0.1499 1.0097 0.101 Uiso 1 1 calc R . . H46C H 0.5496 -0.1358 1.0668 0.101 Uiso 1 1 calc R . . C26 C 0.3359(3) 0.0060(3) 1.1337(4) 0.075(2) Uani 1 1 d . . . H26A H 0.3058 -0.0118 1.0857 0.112 Uiso 1 1 calc R . . H26B H 0.3187 0.0167 1.1843 0.112 Uiso 1 1 calc R . . H26C H 0.3476 -0.0234 1.1534 0.112 Uiso 1 1 calc R . . C33 C 0.5166(3) -0.0538(3) 1.1186(4) 0.0687(19) Uani 1 1 d . C . H33A H 0.5147 -0.0160 1.1179 0.082 Uiso 1 1 calc R . . H33B H 0.4746 -0.0883 1.1206 0.082 Uiso 1 1 calc R . . C22 C 0.5073(3) 0.2228(3) 1.3367(4) 0.0673(18) Uani 1 1 d . . . H22 H 0.4799 0.2377 1.3329 0.081 Uiso 1 1 calc R B . C34 C 0.5505(4) -0.0550(5) 1.2024(4) 0.100(3) Uani 1 1 d . . . H34A H 0.5299 -0.0513 1.2562 0.119 Uiso 1 1 calc R C . H34B H 0.5492 -0.0943 1.2057 0.119 Uiso 1 1 calc R . . C23 C 0.5594(3) 0.2550(3) 1.3847(4) 0.0731(19) Uani 1 1 d . B . H23 H 0.5674 0.2916 1.4128 0.088 Uiso 1 1 calc R . . C49 C 0.6616(5) -0.0613(4) 1.1360(6) 0.111(3) Uani 1 1 d . C . H49A H 0.6848 -0.0633 1.0850 0.166 Uiso 1 1 calc R . . H49B H 0.6224 -0.0987 1.1389 0.166 Uiso 1 1 calc R . . H49C H 0.6840 -0.0565 1.1916 0.166 Uiso 1 1 calc R . . C39 C 0.7089(3) 0.0512(5) 0.9492(5) 0.101(3) Uani 1 1 d . C . H39A H 0.7004 0.0825 0.9262 0.121 Uiso 1 1 calc R A 1 H39B H 0.7374 0.0481 0.9075 0.121 Uiso 1 1 calc R A 1 C10 C 0.6034(3) 0.1430(3) 1.0285(4) 0.078(2) Uani 1 1 d . . . H10 H 0.5696 0.1168 1.0644 0.094 Uiso 1 1 calc R . . C28A C 0.6593(4) 0.2694(4) 1.4467(6) 0.100(3) Uani 0.50 1 d PD B 3 H28A H 0.6656 0.2388 1.4794 0.120 Uiso 0.50 1 calc PR B 3 C29A C 0.7141(7) 0.3056(9) 1.3869(10) 0.120(6) Uiso 0.61(2) 1 d PD B 3 H29A H 0.7165 0.2788 1.3422 0.180 Uiso 0.61(2) 1 calc PR B 3 H29B H 0.7509 0.3239 1.4236 0.180 Uiso 0.61(2) 1 calc PR B 3 H29C H 0.7103 0.3375 1.3564 0.180 Uiso 0.61(2) 1 calc PR B 3 C30A C 0.6595(7) 0.3133(7) 1.5161(9) 0.101(6) Uiso 0.61(2) 1 d PD B 3 H30A H 0.6238 0.2922 1.5546 0.151 Uiso 0.61(2) 1 calc PR B 3 H30B H 0.6587 0.3469 1.4856 0.151 Uiso 0.61(2) 1 calc PR B 3 H30C H 0.6961 0.3290 1.5529 0.151 Uiso 0.61(2) 1 calc PR B 3 C28B C 0.6593(4) 0.2694(4) 1.4467(6) 0.100(3) Uani 0.50 1 d PD B 4 H28B H 0.6672 0.3116 1.4387 0.120 Uiso 0.50 1 calc PR B 4 C29B C 0.7141(9) 0.2751(13) 1.4017(13) 0.087(7) Uiso 0.39(2) 1 d PD B 4 H29D H 0.7098 0.2765 1.3365 0.131 Uiso 0.39(2) 1 calc PR B 4 H29E H 0.7185 0.2402 1.4172 0.131 Uiso 0.39(2) 1 calc PR B 4 H29F H 0.7499 0.3123 1.4217 0.131 Uiso 0.39(2) 1 calc PR B 4 C30B C 0.6534(13) 0.2645(16) 1.5431(12) 0.132(13) Uiso 0.39(2) 1 d PD B 4 H30D H 0.6155 0.2624 1.5610 0.197 Uiso 0.39(2) 1 calc PR B 4 H30E H 0.6875 0.2999 1.5708 0.197 Uiso 0.39(2) 1 calc PR B 4 H30F H 0.6531 0.2277 1.5629 0.197 Uiso 0.39(2) 1 calc PR B 4 C8 C 0.7064(2) 0.2226(2) 1.0229(3) 0.0450(13) Uani 1 1 d . . . C40A C 0.7399(7) 0.0707(8) 1.0511(10) 0.067(7) Uani 0.498(17) 1 d PG C 1 C41A C 0.7099(6) 0.0442(8) 1.1306(12) 0.054(5) Uani 0.498(17) 1 d PG C 1 C42A C 0.7389(8) 0.0659(8) 1.2124(10) 0.104(8) Uani 0.498(17) 1 d PG C 1 H42A H 0.7184 0.0478 1.2668 0.125 Uiso 0.498(17) 1 calc PR C 1 C43A C 0.7980(7) 0.1140(7) 1.2146(10) 0.103(8) Uani 0.498(17) 1 d PG C 1 H43A H 0.8178 0.1289 1.2705 0.124 Uiso 0.498(17) 1 calc PR C 1 C44A C 0.8280(5) 0.1405(7) 1.1351(11) 0.077(6) Uani 0.498(17) 1 d PGD C 1 C45A C 0.7990(6) 0.1188(7) 1.0533(10) 0.079(6) Uani 0.498(17) 1 d PG C 1 H45A H 0.8195 0.1369 0.9989 0.095 Uiso 0.498(17) 1 calc PR C 1 C46A C 0.8965(7) 0.1906(7) 1.1357(13) 0.098(7) Uiso 0.498(17) 1 d PD C 1 H46D H 0.9106 0.1945 1.1992 0.117 Uiso 0.498(17) 1 calc PR C 1 C47A C 0.9407(12) 0.1819(14) 1.0789(18) 0.139(9) Uiso 0.498(17) 1 d PD C 1 H47A H 0.9376 0.1430 1.0938 0.208 Uiso 0.498(17) 1 calc PR C 1 H47B H 0.9820 0.2147 1.0908 0.208 Uiso 0.498(17) 1 calc PR C 1 H47C H 0.9312 0.1822 1.0153 0.208 Uiso 0.498(17) 1 calc PR C 1 C48A C 0.9041(11) 0.2515(9) 1.1095(16) 0.117(8) Uiso 0.498(17) 1 d PD C 1 H48A H 0.8756 0.2588 1.1437 0.175 Uiso 0.498(17) 1 calc PR C 1 H48B H 0.8961 0.2516 1.0452 0.175 Uiso 0.498(17) 1 calc PR C 1 H48C H 0.9456 0.2835 1.1226 0.175 Uiso 0.498(17) 1 calc PR C 1 C40B C 0.7405(7) 0.0791(8) 1.0211(10) 0.064(6) Uani 0.502(17) 1 d PG C 2 C41B C 0.7180(5) 0.0553(7) 1.1055(11) 0.053(5) Uani 0.502(17) 1 d PG C 2 C42B C 0.7522(5) 0.0828(8) 1.1817(9) 0.072(5) Uani 0.502(17) 1 d PG C 2 H42B H 0.7368 0.0665 1.2393 0.087 Uiso 0.502(17) 1 calc PR C 2 C43B C 0.8089(5) 0.1342(7) 1.1735(10) 0.079(7) Uani 0.502(17) 1 d PG C 2 H43B H 0.8322 0.1531 1.2255 0.095 Uiso 0.502(17) 1 calc PR C 2 C44B C 0.8314(5) 0.1581(7) 1.0891(12) 0.089(6) Uani 0.502(17) 1 d PGD C 2 C45B C 0.7972(7) 0.1305(8) 1.0129(9) 0.093(8) Uani 0.502(17) 1 d PG C 2 H45B H 0.8125 0.1468 0.9553 0.112 Uiso 0.502(17) 1 calc PR C 2 C46B C 0.8954(7) 0.2165(7) 1.0732(11) 0.089(6) Uiso 0.502(17) 1 d PD C 2 H46E H 0.8907 0.2411 1.0250 0.107 Uiso 0.502(17) 1 calc PR C 2 C47B C 0.9399(10) 0.1988(11) 1.0408(16) 0.114(8) Uiso 0.502(17) 1 d PD C 2 H47D H 0.9236 0.1730 0.9877 0.172 Uiso 0.502(17) 1 calc PR C 2 H47E H 0.9471 0.1765 1.0882 0.172 Uiso 0.502(17) 1 calc PR C 2 H47F H 0.9780 0.2352 1.0253 0.172 Uiso 0.502(17) 1 calc PR C 2 C48B C 0.9187(9) 0.2555(9) 1.1560(13) 0.102(7) Uiso 0.502(17) 1 d PD C 2 H48D H 0.8905 0.2693 1.1731 0.153 Uiso 0.502(17) 1 calc PR C 2 H48E H 0.9585 0.2906 1.1434 0.153 Uiso 0.502(17) 1 calc PR C 2 H48F H 0.9221 0.2319 1.2051 0.153 Uiso 0.502(17) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0378(4) 0.0206(3) 0.0365(3) -0.0013(3) -0.0038(3) 0.0098(3) O2 0.042(2) 0.0291(17) 0.0403(18) -0.0042(15) 0.0024(16) 0.0112(15) O5 0.038(2) 0.028(2) 0.042(3) 0.000(2) 0.0001(10) 0.0138(12) O3 0.060(2) 0.0255(18) 0.058(2) -0.0048(16) -0.0214(19) 0.0185(17) O1 0.055(2) 0.042(2) 0.057(2) -0.0151(19) 0.013(2) 0.0059(18) O4 0.055(2) 0.0326(18) 0.048(2) -0.0060(16) -0.0082(18) 0.0229(17) N1 0.051(3) 0.022(2) 0.048(3) -0.0011(18) -0.005(2) 0.0156(19) N2 0.048(3) 0.028(2) 0.040(2) -0.0009(18) -0.006(2) 0.015(2) C37 0.056(3) 0.050(3) 0.033(3) 0.000(2) -0.006(2) 0.029(3) C3 0.050(3) 0.034(3) 0.047(3) 0.006(2) 0.002(2) 0.021(2) C32 0.053(3) 0.035(3) 0.037(3) 0.009(2) 0.002(2) 0.023(2) C17 0.056(3) 0.034(3) 0.040(3) 0.004(2) 0.009(2) 0.024(3) C12 0.046(3) 0.046(3) 0.046(3) -0.009(3) 0.003(2) 0.020(3) C16 0.061(4) 0.049(3) 0.041(3) -0.010(2) 0.003(3) 0.026(3) C21 0.062(4) 0.048(3) 0.043(3) -0.005(3) -0.001(3) 0.031(3) C31 0.033(2) 0.029(2) 0.043(3) 0.004(2) 0.000(2) 0.010(2) C2 0.079(4) 0.040(3) 0.044(3) -0.004(3) -0.011(3) 0.033(3) C4 0.090(4) 0.038(3) 0.047(3) 0.000(3) -0.003(3) 0.037(3) C1 0.078(4) 0.027(3) 0.042(3) -0.004(2) -0.011(3) 0.023(3) C5 0.091(5) 0.036(3) 0.041(3) 0.005(2) 0.004(3) 0.035(3) C7 0.043(3) 0.083(5) 0.045(3) -0.010(3) 0.000(3) -0.008(3) C24 0.076(5) 0.079(5) 0.056(4) -0.021(3) -0.008(4) 0.036(4) C36 0.075(5) 0.061(4) 0.048(3) -0.002(3) -0.015(3) 0.036(4) C15 0.085(5) 0.070(4) 0.073(4) -0.031(3) -0.021(4) 0.058(4) C11 0.044(3) 0.035(3) 0.041(3) -0.004(2) -0.003(2) 0.015(2) C20 0.074(4) 0.058(4) 0.044(3) -0.007(3) -0.011(3) 0.040(3) C25 0.077(5) 0.081(5) 0.060(4) -0.012(4) -0.012(3) 0.049(4) C38 0.058(4) 0.096(5) 0.050(4) -0.015(4) 0.001(3) 0.034(4) C18 0.099(5) 0.053(4) 0.050(3) -0.005(3) -0.005(3) 0.050(4) C6 0.061(4) 0.070(4) 0.044(3) -0.011(3) -0.005(3) 0.000(4) C13 0.060(4) 0.087(5) 0.062(4) -0.023(3) -0.012(3) 0.049(4) C35 0.103(6) 0.101(6) 0.039(3) 0.001(4) -0.017(4) 0.039(5) C9 0.055(4) 0.090(5) 0.042(3) -0.008(3) -0.007(3) -0.012(4) C14 0.097(5) 0.104(6) 0.077(5) -0.038(4) -0.029(4) 0.078(5) C19 0.109(6) 0.068(4) 0.056(3) -0.006(3) -0.020(4) 0.061(5) C27 0.080(5) 0.079(5) 0.055(4) -0.016(4) 0.013(4) 0.033(4) C46 0.082(5) 0.042(3) 0.080(4) 0.001(3) -0.016(4) 0.033(3) C26 0.073(5) 0.066(4) 0.056(4) -0.016(3) 0.019(3) 0.012(4) C33 0.081(5) 0.071(4) 0.043(3) 0.020(3) 0.020(3) 0.029(4) C22 0.073(4) 0.062(4) 0.072(4) -0.025(3) -0.020(4) 0.038(4) C34 0.129(8) 0.133(8) 0.036(4) 0.022(4) 0.013(4) 0.065(7) C23 0.085(5) 0.050(4) 0.077(4) -0.015(3) -0.007(4) 0.029(4) C49 0.148(9) 0.100(6) 0.114(6) -0.006(5) -0.065(6) 0.085(6) C39 0.057(4) 0.124(8) 0.084(6) -0.007(5) 0.003(4) 0.017(5) C10 0.051(4) 0.070(4) 0.049(4) -0.011(3) -0.001(3) -0.018(3) C28A 0.083(6) 0.104(7) 0.098(6) -0.030(5) -0.022(5) 0.036(5) C28B 0.083(6) 0.104(7) 0.098(6) -0.030(5) -0.022(5) 0.036(5) C8 0.035(3) 0.039(3) 0.046(3) -0.001(2) -0.002(2) 0.007(2) C40A 0.082(14) 0.076(12) 0.037(12) 0.016(10) -0.016(10) 0.034(11) C41A 0.083(12) 0.046(8) 0.032(9) -0.003(7) -0.008(7) 0.032(8) C42A 0.095(14) 0.082(12) 0.058(12) 0.004(10) -0.033(10) -0.015(11) C43A 0.092(15) 0.106(15) 0.054(12) 0.008(10) -0.034(11) 0.006(12) C44A 0.063(11) 0.062(11) 0.071(17) 0.015(10) -0.007(12) 0.005(9) C45A 0.045(8) 0.084(12) 0.063(12) 0.006(11) -0.019(9) -0.002(8) C40B 0.051(10) 0.087(13) 0.039(10) -0.002(9) 0.013(7) 0.023(9) C41B 0.054(9) 0.060(11) 0.044(13) 0.007(9) -0.021(8) 0.028(8) C42B 0.057(10) 0.104(15) 0.040(9) 0.004(9) -0.002(7) 0.028(11) C43B 0.052(10) 0.099(15) 0.036(12) -0.008(10) -0.004(9) 0.000(10) C44B 0.049(9) 0.080(13) 0.104(17) 0.025(12) 0.021(10) 0.008(9) C45B 0.066(11) 0.132(19) 0.044(10) 0.002(10) 0.005(9) 0.021(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O3 2.004(3) . ? Ni1 O4 2.043(4) 4_556 ? Ni1 O5 2.069(3) . ? Ni1 O2 2.086(3) . ? Ni1 N2 2.095(4) . ? Ni1 N1 2.101(4) . ? O2 C11 1.258(6) . ? O5 Ni1 2.069(3) 4_556 ? O3 C31 1.256(6) . ? O1 C11 1.251(6) . ? O4 C31 1.258(6) . ? O4 Ni1 2.043(4) 4_556 ? N1 C1 1.331(6) . ? N1 C5 1.343(7) . ? N2 C6 1.317(7) . ? N2 C10 1.317(7) . ? C37 C38 1.525(8) . ? C37 C36 1.545(7) . ? C37 C32 1.552(8) . ? C3 C2 1.378(7) . ? C3 C4 1.406(7) . ? C3 C8 1.477(7) 3_664 ? C32 C46 1.540(8) . ? C32 C33 1.543(8) . ? C32 C31 1.556(7) . ? C17 C18 1.516(7) . ? C17 C12 1.539(8) . ? C17 C16 1.558(7) . ? C12 C26 1.522(8) . ? C12 C13 1.529(8) . ? C12 C11 1.564(7) . ? C16 C21 1.529(8) . ? C16 C15 1.544(8) . ? C16 C27 1.564(8) . ? C21 C20 1.388(8) . ? C21 C22 1.403(8) . ? C2 C1 1.378(7) . ? C4 C5 1.373(8) . ? C7 C8 1.358(8) . ? C7 C6 1.392(8) . ? C24 C25 1.381(9) . ? C24 C23 1.394(10) . ? C24 C28B 1.516(10) . ? C24 C28A 1.516(10) . ? C36 C41A 1.408(12) . ? C36 C35 1.508(10) . ? C36 C49 1.547(9) . ? C36 C41B 1.666(12) . ? C15 C14 1.531(9) . ? C20 C25 1.385(9) . ? C20 C19 1.535(8) . ? C38 C39 1.506(10) . ? C18 C19 1.508(10) . ? C13 C14 1.550(8) . ? C35 C34 1.499(12) . ? C9 C8 1.370(8) . ? C9 C10 1.383(8) . ? C33 C34 1.528(9) . ? C22 C23 1.365(9) . ? C39 C40B 1.316(14) . ? C39 C40A 1.669(13) . ? C28A C29A 1.521(14) . ? C28A C30A 1.524(13) . ? C28B C30B 1.443(15) . ? C28B C29B 1.490(15) . ? C8 C3 1.477(7) 2_655 ? C40A C41A 1.3900 . ? C40A C45A 1.3900 . ? C41A C42A 1.3900 . ? C42A C43A 1.3900 . ? C43A C44A 1.3900 . ? C44A C45A 1.3900 . ? C44A C46A 1.568(15) . ? C46A C47A 1.514(17) . ? C46A C48A 1.519(17) . ? C40B C41B 1.3900 . ? C40B C45B 1.3900 . ? C41B C42B 1.3900 . ? C42B C43B 1.3900 . ? C43B C44B 1.3900 . ? C44B C45B 1.3900 . ? C44B C46B 1.587(15) . ? C46B C47B 1.498(16) . ? C46B C48B 1.508(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ni1 O4 97.60(16) . 4_556 ? O3 Ni1 O5 90.71(12) . . ? O4 Ni1 O5 94.86(13) 4_556 . ? O3 Ni1 O2 87.49(15) . . ? O4 Ni1 O2 171.98(13) 4_556 . ? O5 Ni1 O2 91.26(12) . . ? O3 Ni1 N2 83.99(15) . . ? O4 Ni1 N2 86.27(16) 4_556 . ? O5 Ni1 N2 174.69(13) . . ? O2 Ni1 N2 88.12(15) . . ? O3 Ni1 N1 172.80(15) . . ? O4 Ni1 N1 87.08(16) 4_556 . ? O5 Ni1 N1 94.35(14) . . ? O2 Ni1 N1 87.29(16) . . ? N2 Ni1 N1 90.89(16) . . ? C11 O2 Ni1 127.1(3) . . ? Ni1 O5 Ni1 114.7(2) 4_556 . ? C31 O3 Ni1 136.8(3) . . ? C31 O4 Ni1 132.9(3) . 4_556 ? C1 N1 C5 117.3(4) . . ? C1 N1 Ni1 123.7(3) . . ? C5 N1 Ni1 118.4(3) . . ? C6 N2 C10 115.8(5) . . ? C6 N2 Ni1 123.4(4) . . ? C10 N2 Ni1 120.6(4) . . ? C38 C37 C36 111.0(5) . . ? C38 C37 C32 112.8(5) . . ? C36 C37 C32 119.7(5) . . ? C2 C3 C4 115.8(5) . . ? C2 C3 C8 123.4(5) . 3_664 ? C4 C3 C8 120.8(5) . 3_664 ? C46 C32 C33 111.1(5) . . ? C46 C32 C37 113.7(5) . . ? C33 C32 C37 108.3(5) . . ? C46 C32 C31 109.7(4) . . ? C33 C32 C31 107.1(4) . . ? C37 C32 C31 106.6(4) . . ? C18 C17 C12 113.4(4) . . ? C18 C17 C16 110.0(4) . . ? C12 C17 C16 117.6(5) . . ? C26 C12 C13 111.2(5) . . ? C26 C12 C17 114.5(5) . . ? C13 C12 C17 109.2(5) . . ? C26 C12 C11 108.7(5) . . ? C13 C12 C11 104.9(4) . . ? C17 C12 C11 107.8(4) . . ? C21 C16 C15 110.8(5) . . ? C21 C16 C17 107.5(5) . . ? C15 C16 C17 108.3(4) . . ? C21 C16 C27 106.6(5) . . ? C15 C16 C27 108.6(5) . . ? C17 C16 C27 115.0(5) . . ? C20 C21 C22 116.4(6) . . ? C20 C21 C16 122.5(5) . . ? C22 C21 C16 121.1(5) . . ? O3 C31 O4 125.3(4) . . ? O3 C31 C32 115.0(4) . . ? O4 C31 C32 119.6(4) . . ? C3 C2 C1 121.3(5) . . ? C5 C4 C3 119.8(5) . . ? N1 C1 C2 122.5(5) . . ? N1 C5 C4 123.2(5) . . ? C8 C7 C6 120.6(5) . . ? C25 C24 C23 115.8(6) . . ? C25 C24 C28B 121.0(7) . . ? C23 C24 C28B 123.1(7) . . ? C25 C24 C28A 121.0(7) . . ? C23 C24 C28A 123.1(7) . . ? C28B C24 C28A 0.0(7) . . ? C41A C36 C35 107.6(10) . . ? C41A C36 C37 115.5(9) . . ? C35 C36 C37 106.8(5) . . ? C41A C36 C49 104.5(11) . . ? C35 C36 C49 108.8(7) . . ? C37 C36 C49 113.4(5) . . ? C41A C36 C41B 13.9(10) . . ? C35 C36 C41B 116.8(9) . . ? C37 C36 C41B 101.9(7) . . ? C49 C36 C41B 109.1(9) . . ? C14 C15 C16 112.2(5) . . ? O1 C11 O2 124.0(5) . . ? O1 C11 C12 117.1(5) . . ? O2 C11 C12 118.7(4) . . ? C25 C20 C21 120.4(6) . . ? C25 C20 C19 118.0(6) . . ? C21 C20 C19 121.6(6) . . ? C24 C25 C20 123.4(7) . . ? C39 C38 C37 109.5(6) . . ? C19 C18 C17 112.4(5) . . ? N2 C6 C7 123.5(6) . . ? C12 C13 C14 112.2(5) . . ? C34 C35 C36 114.0(6) . . ? C8 C9 C10 120.4(6) . . ? C15 C14 C13 110.9(5) . . ? C18 C19 C20 114.3(5) . . ? C34 C33 C32 111.6(6) . . ? C23 C22 C21 122.4(7) . . ? C35 C34 C33 112.2(6) . . ? C22 C23 C24 121.6(6) . . ? C40B C39 C38 122.1(10) . . ? C40B C39 C40A 13.3(12) . . ? C38 C39 C40A 109.5(8) . . ? N2 C10 C9 123.9(6) . . ? C24 C28A C29A 112.3(9) . . ? C24 C28A C30A 115.0(9) . . ? C29A C28A C30A 106.7(10) . . ? C30B C28B C29B 120.6(14) . . ? C30B C28B C24 116.3(13) . . ? C29B C28B C24 114.8(10) . . ? C7 C8 C9 115.6(5) . . ? C7 C8 C3 122.2(5) . 2_655 ? C9 C8 C3 122.1(5) . 2_655 ? C41A C40A C45A 120.0 . . ? C41A C40A C39 124.5(10) . . ? C45A C40A C39 115.4(9) . . ? C40A C41A C42A 120.0 . . ? C40A C41A C36 117.6(11) . . ? C42A C41A C36 122.3(11) . . ? C43A C42A C41A 120.0 . . ? C42A C43A C44A 120.0 . . ? C45A C44A C43A 120.0 . . ? C45A C44A C46A 119.0(12) . . ? C43A C44A C46A 120.7(12) . . ? C44A C45A C40A 120.0 . . ? C47A C46A C48A 106.5(18) . . ? C47A C46A C44A 119.1(17) . . ? C48A C46A C44A 110.7(16) . . ? C39 C40B C41B 119.5(12) . . ? C39 C40B C45B 120.4(12) . . ? C41B C40B C45B 120.0 . . ? C42B C41B C40B 120.0 . . ? C42B C41B C36 115.3(9) . . ? C40B C41B C36 124.7(9) . . ? C43B C42B C41B 120.0 . . ? C44B C43B C42B 120.0 . . ? C43B C44B C45B 120.0 . . ? C43B C44B C46B 123.6(12) . . ? C45B C44B C46B 116.4(12) . . ? C44B C45B C40B 120.0 . . ? C47B C46B C48B 110.8(16) . . ? C47B C46B C44B 110.1(16) . . ? C48B C46B C44B 112.3(13) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.393 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.068