#------------------------------------------------------------------------------ #$Date: 2024-04-06 01:42:31 +0300 (Sat, 06 Apr 2024) $ #$Revision: 291101 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/83/7248385.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7248385 loop_ _publ_author_name 'Mendoza-Baez, Raul' 'Molina-Renteria, Alan' 'Olgu\'in, Juan' _publ_section_title ; Nitro group and K+ based secondary building unit for the self-assembly of 3D coordination polymers built on dinuclear dianionic helicate connectors ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00255E _journal_year 2024 _chemical_formula_moiety 'C83 H57 K2 N13 Ni2 O18' _chemical_formula_sum 'C83 H57 K2 N13 Ni2 O18' _chemical_formula_weight 1720.03 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2024-01-18 deposited with the CCDC. 2024-04-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.921(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.7610(11) _cell_length_b 14.5644(9) _cell_length_c 36.558(3) _cell_measurement_reflns_used 9939 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 21.8964 _cell_measurement_theta_min 2.2504 _cell_volume 8311.8(10) _computing_cell_refinement 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_data_collection 'Bruker Instrument Service (Bruker AXS Inc., 2015)' _computing_data_reduction 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_molecular_graphics 'XP V 5.1 (Bruker, 1998)' _computing_publication_material 'XP V 5.1 (Bruker, 1998)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2012 (Bruker, 2013)' _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker D8 VENTURE diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1132 _diffrn_reflns_av_unetI/netI 0.0458 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_number 204178 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.026 _diffrn_reflns_theta_max 25.026 _diffrn_reflns_theta_min 2.250 _diffrn_source 'microfocus sealed tube' _exptl_absorpt_coefficient_mu 0.629 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Sheldrick, 2012)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 3536 _exptl_crystal_size_max 0.384 _exptl_crystal_size_mid 0.217 _exptl_crystal_size_min 0.056 _exptl_transmission_factor_max 0.7452 _exptl_transmission_factor_min 0.6704 _refine_diff_density_max 0.795 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.079 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 551 _refine_ls_number_reflns 7322 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0642 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0984P)^2^+16.4832P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1671 _refine_ls_wR_factor_ref 0.1879 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5052 _reflns_number_total 7322 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00255e2.cif _cod_data_source_block JOAMR137B _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. data item '_exptl_crystal_density_meas' value 'not measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_original_cell_volume 8311.7(10) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7248385 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.6704 _shelx_estimated_absorpt_t_max 0.7452 _shelx_res_file ; JOAMR137B.res created by SHELXL-2014/7 TITL mo_JO_amr_137_0m_a.res in C2/c REM Old TITL mo_JO_amr_137_0m in C2/c REM SHELXT solution in C2/c REM R1 0.196, Rweak 0.046, Alpha 0.088, Orientation as input REM Formula found by SHELXT: C93 N4 O14 K2 Ni2 CELL 0.71073 15.7610 14.5644 36.5576 90.000 97.921 90.000 ZERR 4.000 0.0011 0.0009 0.0027 0.000 0.002 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H N O K NI UNIT 332 228 52 72 8 8 TEMP 23.230 L.S. 20 BOND $H LIST 4 OMIT -2 0 4 OMIT -3 1 6 OMIT -1 1 5 OMIT -1 1 3 OMIT 2 2 1 OMIT -2 2 7 OMIT 0 2 3 OMIT -3 1 8 FMAP 2 ACTA EQIV $1 -x, y, -z+1/2 HTAB C35 O9_$1 EQIV $2 x-1/2, -y+1/2, z-1/2 HTAB C11 O6_$2 CONF PLAN 20 WGHT 0.098400 16.483200 FVAR 0.20096 O3 4 0.459408 0.906927 0.068315 11.00000 0.18644 0.12860 = 0.10745 -0.01284 0.03932 -0.10667 N3 3 0.634345 0.444280 0.380452 11.00000 0.04381 0.05356 = 0.04315 0.01234 0.00969 0.01291 C3 1 0.239572 0.606595 0.251931 11.00000 0.04617 0.04944 = 0.04464 0.00044 0.01305 0.01362 AFIX 43 H3 2 0.194177 0.591513 0.264573 11.00000 -1.20000 AFIX 0 O2 4 0.433543 0.871273 0.011543 11.00000 0.13966 0.10378 = 0.08046 0.02124 0.04439 -0.02968 C2 1 0.316172 0.632895 0.271836 11.00000 0.05151 0.04130 = 0.04390 -0.00180 0.00749 0.01860 N2 3 0.426017 0.856662 0.043481 11.00000 0.09064 0.07794 = 0.07850 0.00481 0.02461 -0.02440 O4 4 0.810437 0.384083 0.405066 11.00000 0.04425 0.05985 = 0.06058 0.01908 0.00881 0.01014 C4 1 0.227722 0.601808 0.214022 11.00000 0.04867 0.04646 = 0.04684 -0.00399 0.00761 0.00494 AFIX 43 H4 2 0.174733 0.584948 0.201384 11.00000 -1.20000 AFIX 0 N4 3 0.662613 0.107740 0.478738 11.00000 0.09691 0.07249 = 0.08656 0.03712 0.01417 0.00026 O6 4 0.710019 0.052101 0.496181 11.00000 0.12340 0.10803 = 0.13610 0.08243 0.00612 0.01134 N6 3 -0.149681 0.413919 0.196626 11.00000 0.04714 0.07672 = 0.10947 -0.01776 0.03281 0.00065 C6 1 0.371936 0.651459 0.214120 11.00000 0.05169 0.05924 = 0.04579 -0.00101 0.01030 -0.00238 AFIX 43 H6 2 0.417221 0.666961 0.201478 11.00000 -1.20000 AFIX 0 O5 4 0.586246 0.105607 0.478180 11.00000 0.09211 0.10755 = 0.14504 0.06206 0.03932 -0.00160 N5 3 0.224472 0.407666 0.173475 11.00000 0.03648 0.04626 = 0.05423 -0.00497 0.01291 -0.00159 C5 1 0.295341 0.622295 0.194645 11.00000 0.05065 0.04111 = 0.03945 -0.00444 0.00663 0.00364 O7 4 0.118174 0.535232 0.125813 11.00000 0.04635 0.05976 = 0.05431 -0.00104 0.01191 0.00025 C7 1 0.382011 0.657856 0.252223 11.00000 0.05135 0.05721 = 0.04483 -0.00490 -0.00073 0.00041 AFIX 43 H7 2 0.433509 0.679134 0.264859 11.00000 -1.20000 AFIX 0 O8 4 -0.223154 0.433235 0.182458 11.00000 0.04335 0.13307 = 0.14373 -0.01179 0.02840 -0.00256 C8 1 0.313767 0.681946 0.138117 11.00000 0.06040 0.05208 = 0.04678 -0.00888 0.00636 -0.00562 AFIX 43 H8 2 0.332313 0.732020 0.152874 11.00000 -1.20000 AFIX 0 C9 1 0.319705 0.691869 0.099182 11.00000 0.05670 0.05120 = 0.04277 -0.00281 0.01126 -0.00780 O9 4 -0.133507 0.370833 0.225205 11.00000 0.07239 0.13263 = 0.13998 0.04193 0.05367 0.00950 C1 1 0.331255 0.633354 0.313752 11.00000 0.05536 0.05798 = 0.03942 -0.00157 0.00811 0.02081 AFIX 23 H1A 2 0.281629 0.606684 0.322723 11.00000 -1.20000 H1B 2 0.335835 0.696564 0.322150 11.00000 -1.20000 AFIX 0 K1 5 0.085297 0.513892 0.047457 11.00000 0.05660 0.08711 = 0.05371 0.00255 0.00084 -0.01621 NI1 6 0.241224 0.489839 0.127289 11.00000 0.04026 0.04779 = 0.04325 -0.00836 0.00894 -0.00672 N1 3 0.286187 0.612919 0.154993 11.00000 0.05039 0.04376 = 0.03945 -0.00242 0.00870 -0.00505 O1 4 0.240675 0.558561 0.078731 11.00000 0.05922 0.06660 = 0.04174 -0.00516 0.00401 -0.02326 C20 1 0.450830 0.516734 0.312211 11.00000 0.05568 0.05737 = 0.04891 -0.00746 -0.00248 0.01695 AFIX 43 H20 2 0.427709 0.501278 0.288215 11.00000 -1.20000 AFIX 0 C21 1 0.621691 0.381384 0.403643 11.00000 0.04276 0.06476 = 0.05070 0.01351 0.01505 0.00773 AFIX 43 H21 2 0.565661 0.375367 0.408619 11.00000 -1.20000 AFIX 0 C22 1 0.683244 0.318579 0.423068 11.00000 0.04980 0.05543 = 0.05064 0.01903 0.01512 0.00921 C23 1 0.773352 0.323002 0.422165 11.00000 0.05568 0.05245 = 0.04596 0.01184 0.00431 0.00830 C24 1 0.824488 0.253140 0.441903 11.00000 0.05421 0.07476 = 0.07416 0.02560 0.00626 0.00980 AFIX 43 H24 2 0.883630 0.254764 0.442425 11.00000 -1.20000 AFIX 0 C25 1 0.789205 0.184634 0.459870 11.00000 0.07695 0.06604 = 0.07443 0.02781 -0.00073 0.01418 AFIX 43 H25 2 0.824093 0.140138 0.472477 11.00000 -1.20000 AFIX 0 C26 1 0.701218 0.180768 0.459488 11.00000 0.07485 0.06261 = 0.06007 0.02506 0.01195 0.00386 C27 1 0.650542 0.247774 0.441957 11.00000 0.05812 0.06682 = 0.06057 0.01584 0.01402 0.00488 AFIX 43 H27 2 0.591854 0.245672 0.442763 11.00000 -1.20000 AFIX 0 C28 1 0.500000 0.194515 0.250000 10.50000 0.04548 0.03506 = 0.08702 0.00000 0.00432 0.00000 H28 2 0.474730 0.155730 0.267660 11.00000 0.07568 C29 1 0.428114 0.250477 0.229628 11.00000 0.03958 0.03283 = 0.07416 -0.00071 0.01297 -0.00494 C30 1 0.388433 0.318862 0.248029 11.00000 0.05120 0.04756 = 0.05674 -0.00581 0.00527 0.00275 AFIX 43 H30 2 0.407339 0.330303 0.272842 11.00000 -1.20000 AFIX 0 C31 1 0.321406 0.369814 0.229862 11.00000 0.04652 0.04589 = 0.05906 -0.00715 0.01425 0.00830 AFIX 43 H31 2 0.294998 0.414401 0.242592 11.00000 -1.20000 AFIX 0 C32 1 0.293558 0.354533 0.192744 11.00000 0.03604 0.04021 = 0.05386 -0.00136 0.01342 -0.00326 C33 1 0.331301 0.286558 0.174299 11.00000 0.04234 0.04365 = 0.05293 -0.01075 0.01375 -0.00942 AFIX 43 H33 2 0.312321 0.274956 0.149505 11.00000 -1.20000 AFIX 0 C34 1 0.397583 0.235833 0.192991 11.00000 0.03977 0.03665 = 0.07136 -0.01055 0.01704 -0.00588 AFIX 43 H34 2 0.422547 0.190006 0.180325 11.00000 -1.20000 AFIX 0 C35 1 0.152303 0.396801 0.185508 11.00000 0.04721 0.04806 = 0.05320 -0.00221 0.01498 -0.00346 AFIX 43 H35 2 0.152352 0.356921 0.205379 11.00000 -1.20000 AFIX 0 C36 1 0.070564 0.439234 0.171858 11.00000 0.04160 0.04831 = 0.05880 -0.00495 0.01557 0.00009 C37 1 0.058099 0.505198 0.142695 11.00000 0.04674 0.05155 = 0.04766 -0.01612 0.00685 -0.00053 C38 1 -0.027959 0.537817 0.132107 11.00000 0.04433 0.07125 = 0.06211 -0.00963 0.00599 0.00582 AFIX 43 H38 2 -0.038508 0.580929 0.113264 11.00000 -1.20000 AFIX 0 C39 1 -0.093836 0.507323 0.148881 11.00000 0.03826 0.07375 = 0.07698 -0.02416 0.00322 0.00845 AFIX 43 H39 2 -0.149090 0.528163 0.140958 11.00000 -1.20000 AFIX 0 C40 1 -0.079810 0.445960 0.177459 11.00000 0.04093 0.05773 = 0.07879 -0.01864 0.01874 -0.00559 C41 1 0.000909 0.412374 0.189252 11.00000 0.05103 0.05387 = 0.07389 -0.00436 0.02073 -0.00089 AFIX 43 H41 2 0.009216 0.371468 0.208955 11.00000 -1.20000 AFIX 0 C10 1 0.283802 0.627980 0.071579 11.00000 0.04794 0.06002 = 0.04133 0.00040 0.00508 -0.00543 C11 1 0.299963 0.644488 0.035040 11.00000 0.07663 0.08115 = 0.04389 -0.00396 0.00404 -0.02517 AFIX 43 H11 2 0.278554 0.603332 0.016600 11.00000 -1.20000 AFIX 0 C12 1 0.345369 0.717840 0.025861 11.00000 0.07407 0.08306 = 0.04929 0.00724 0.01330 -0.01414 AFIX 43 H12 2 0.355337 0.726342 0.001603 11.00000 -1.20000 AFIX 0 C13 1 0.376758 0.779991 0.052994 11.00000 0.06576 0.06683 = 0.05828 0.00483 0.01244 -0.02019 C14 1 0.364497 0.767276 0.088917 11.00000 0.06601 0.06298 = 0.04938 -0.00597 0.01047 -0.01550 AFIX 43 H14 2 0.386511 0.809802 0.106710 11.00000 -1.20000 AFIX 0 C16 1 0.444704 0.598455 0.367061 11.00000 0.05864 0.07389 = 0.04960 -0.01149 0.00560 0.02762 AFIX 43 H16 2 0.418624 0.641674 0.380567 11.00000 -1.20000 AFIX 0 C15 1 0.410590 0.581699 0.330923 11.00000 0.04416 0.04936 = 0.03730 0.00232 0.01061 0.00990 C17 1 0.516847 0.552651 0.383840 11.00000 0.05130 0.08690 = 0.04123 -0.00488 -0.00176 0.01829 AFIX 43 H17 2 0.537225 0.563767 0.408542 11.00000 -1.20000 AFIX 0 C19 1 0.525355 0.473560 0.328335 11.00000 0.05588 0.05045 = 0.05631 -0.00311 0.00930 0.01909 AFIX 43 H19 2 0.553120 0.432334 0.314595 11.00000 -1.20000 AFIX 0 C18 1 0.558133 0.491199 0.364198 11.00000 0.03895 0.05152 = 0.04242 0.01242 0.01236 0.01143 C42 1 0.404926 0.246419 0.394303 10.50000 0.05867 0.15141 = 0.05936 0.03943 -0.00237 -0.02534 C43 1 0.390902 0.281118 0.359642 10.50000 0.07642 0.11050 = 0.13136 0.01827 0.00535 -0.03731 AFIX 137 H43A 2 0.344657 0.248438 0.345488 10.50000 -1.50000 H43B 2 0.441810 0.274558 0.348168 10.50000 -1.50000 H43C 2 0.376295 0.344965 0.360691 10.50000 -1.50000 AFIX 0 N7 3 0.416943 0.239237 0.423701 10.50000 0.08642 0.24008 = 0.13936 0.01836 -0.00303 -0.06487 HKLF 4 REM mo_JO_amr_137_0m_a.res in C2/c REM R1 = 0.0642 for 5052 Fo > 4sig(Fo) and 0.1076 for all 7322 data REM 551 parameters refined using 0 restraints END WGHT 0.0984 14.4960 REM Highest difference peak 0.795, deepest hole -0.267, 1-sigma level 0.079 Q1 1 1.0000 0.0000 0.5000 10.50000 0.05 0.79 Q2 1 0.3284 0.4224 0.4220 11.00000 0.05 0.66 Q3 1 0.3887 0.3660 0.4371 11.00000 0.05 0.54 Q4 1 0.3903 0.3071 0.4078 11.00000 0.05 0.51 Q5 1 0.3790 0.3150 0.3991 11.00000 0.05 0.49 Q6 1 0.9433 -0.0404 0.4708 11.00000 0.05 0.48 Q7 1 0.9982 0.0705 0.5092 11.00000 0.05 0.46 Q8 1 0.3972 0.2398 0.3783 11.00000 0.05 0.38 Q9 1 0.3979 0.2438 0.3576 11.00000 0.05 0.35 Q10 1 0.2349 0.5424 0.1068 11.00000 0.05 0.32 Q11 1 0.0589 0.4571 0.0608 11.00000 0.05 0.31 Q12 1 0.4083 0.2193 0.4301 11.00000 0.05 0.29 Q13 1 0.0541 0.5602 0.0592 11.00000 0.05 0.28 Q14 1 0.0802 0.4787 0.1642 11.00000 0.05 0.27 Q15 1 0.2348 0.4337 0.1596 11.00000 0.05 0.26 Q16 1 0.2496 0.6424 0.2026 11.00000 0.05 0.23 Q17 1 0.3636 0.3777 0.2343 11.00000 0.05 0.22 Q18 1 0.3811 0.9104 0.0519 11.00000 0.05 0.22 Q19 1 0.3646 0.6051 0.2433 11.00000 0.05 0.22 Q20 1 0.1081 0.4381 0.1873 11.00000 0.05 0.22 ; _shelx_res_checksum 36248 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O3 O 0.4594(4) 0.9069(4) 0.06832(15) 0.139(2) Uani 1 1 d . . . . . N3 N 0.6343(2) 0.4443(2) 0.38045(9) 0.0465(9) Uani 1 1 d . . . . . C3 C 0.2396(3) 0.6066(3) 0.25193(11) 0.0461(10) Uani 1 1 d . . . . . H3 H 0.1942 0.5915 0.2646 0.055 Uiso 1 1 calc R U . . . O2 O 0.4335(3) 0.8713(3) 0.01154(12) 0.1052(15) Uani 1 1 d . . . . . C2 C 0.3162(3) 0.6329(3) 0.27184(11) 0.0455(10) Uani 1 1 d . . . . . N2 N 0.4260(3) 0.8567(3) 0.04348(15) 0.0811(14) Uani 1 1 d . . . . . O4 O 0.81044(18) 0.3841(2) 0.40507(8) 0.0547(8) Uani 1 1 d . . . . . C4 C 0.2277(3) 0.6018(3) 0.21402(11) 0.0472(10) Uani 1 1 d . . . . . H4 H 0.1747 0.5849 0.2014 0.057 Uiso 1 1 calc R U . . . N4 N 0.6626(4) 0.1077(3) 0.47874(14) 0.0852(15) Uani 1 1 d . . . . . O6 O 0.7100(3) 0.0521(4) 0.49618(15) 0.1236(19) Uani 1 1 d . . . . . N6 N -0.1497(3) 0.4139(3) 0.19663(16) 0.0757(13) Uani 1 1 d . . . . . C6 C 0.3719(3) 0.6515(3) 0.21412(12) 0.0519(11) Uani 1 1 d . . . . . H6 H 0.4172 0.6670 0.2015 0.062 Uiso 1 1 calc R U . . . O5 O 0.5862(3) 0.1056(3) 0.47818(15) 0.1127(17) Uani 1 1 d . . . . . N5 N 0.2245(2) 0.4077(2) 0.17347(9) 0.0450(8) Uani 1 1 d . . . . . C5 C 0.2953(3) 0.6223(3) 0.19464(11) 0.0437(10) Uani 1 1 d . . . . . O7 O 0.11817(19) 0.5352(2) 0.12581(8) 0.0530(8) Uani 1 1 d . . . . . C7 C 0.3820(3) 0.6579(3) 0.25222(12) 0.0518(11) Uani 1 1 d . . . . . H7 H 0.4335 0.6791 0.2649 0.062 Uiso 1 1 calc R U . . . O8 O -0.2232(2) 0.4332(4) 0.18246(14) 0.1053(15) Uani 1 1 d . . . . . C8 C 0.3138(3) 0.6819(3) 0.13812(12) 0.0532(11) Uani 1 1 d . . . . . H8 H 0.3323 0.7320 0.1529 0.064 Uiso 1 1 calc R U . . . C9 C 0.3197(3) 0.6919(3) 0.09918(11) 0.0498(11) Uani 1 1 d . . . . . O9 O -0.1335(3) 0.3708(4) 0.22521(16) 0.1113(17) Uani 1 1 d . . . . . C1 C 0.3313(3) 0.6334(3) 0.31375(11) 0.0508(11) Uani 1 1 d . . . . . H1A H 0.2816 0.6067 0.3227 0.061 Uiso 1 1 calc R U . . . H1B H 0.3358 0.6966 0.3222 0.061 Uiso 1 1 calc R U . . . K1 K 0.08530(7) 0.51389(9) 0.04746(3) 0.0664(3) Uani 1 1 d . . . . . Ni1 Ni 0.24122(3) 0.48984(4) 0.12729(2) 0.0435(2) Uani 1 1 d . . . . . N1 N 0.2862(2) 0.6129(2) 0.15499(9) 0.0443(8) Uani 1 1 d . . . . . O1 O 0.2407(2) 0.5586(2) 0.07873(8) 0.0561(8) Uani 1 1 d . . . . . C20 C 0.4508(3) 0.5167(3) 0.31221(13) 0.0549(12) Uani 1 1 d . . . . . H20 H 0.4277 0.5013 0.2882 0.066 Uiso 1 1 calc R U . . . C21 C 0.6217(3) 0.3814(3) 0.40364(12) 0.0519(11) Uani 1 1 d . . . . . H21 H 0.5657 0.3754 0.4086 0.062 Uiso 1 1 calc R U . . . C22 C 0.6832(3) 0.3186(3) 0.42307(12) 0.0512(11) Uani 1 1 d . . . . . C23 C 0.7734(3) 0.3230(3) 0.42216(12) 0.0516(11) Uani 1 1 d . . . . . C24 C 0.8245(3) 0.2531(4) 0.44190(14) 0.0680(14) Uani 1 1 d . . . . . H24 H 0.8836 0.2548 0.4424 0.082 Uiso 1 1 calc R U . . . C25 C 0.7892(4) 0.1846(4) 0.45987(15) 0.0735(15) Uani 1 1 d . . . . . H25 H 0.8241 0.1401 0.4725 0.088 Uiso 1 1 calc R U . . . C26 C 0.7012(4) 0.1808(4) 0.45949(14) 0.0656(14) Uani 1 1 d . . . . . C27 C 0.6505(3) 0.2478(3) 0.44196(13) 0.0613(13) Uani 1 1 d . . . . . H27 H 0.5919 0.2457 0.4428 0.074 Uiso 1 1 calc R U . . . C28 C 0.5000 0.1945(4) 0.2500 0.0563(17) Uani 1 2 d S T P . . H28 H 0.475(3) 0.156(4) 0.2677(13) 0.076(15) Uiso 1 1 d . . . . . C29 C 0.4281(3) 0.2505(3) 0.22963(13) 0.0484(11) Uani 1 1 d . . . . . C30 C 0.3884(3) 0.3189(3) 0.24803(13) 0.0520(11) Uani 1 1 d . . . . . H30 H 0.4073 0.3303 0.2728 0.062 Uiso 1 1 calc R U . . . C31 C 0.3214(3) 0.3698(3) 0.22986(12) 0.0498(11) Uani 1 1 d . . . . . H31 H 0.2950 0.4144 0.2426 0.060 Uiso 1 1 calc R U . . . C32 C 0.2936(3) 0.3545(3) 0.19274(12) 0.0427(10) Uani 1 1 d . . . . . C33 C 0.3313(3) 0.2866(3) 0.17430(12) 0.0456(10) Uani 1 1 d . . . . . H33 H 0.3123 0.2750 0.1495 0.055 Uiso 1 1 calc R U . . . C34 C 0.3976(3) 0.2358(3) 0.19299(13) 0.0484(11) Uani 1 1 d . . . . . H34 H 0.4225 0.1900 0.1803 0.058 Uiso 1 1 calc R U . . . C35 C 0.1523(3) 0.3968(3) 0.18551(12) 0.0487(11) Uani 1 1 d . . . . . H35 H 0.1524 0.3569 0.2054 0.058 Uiso 1 1 calc R U . . . C36 C 0.0706(3) 0.4392(3) 0.17186(12) 0.0488(11) Uani 1 1 d . . . . . C37 C 0.0581(3) 0.5052(3) 0.14270(12) 0.0486(11) Uani 1 1 d . . . . . C38 C -0.0280(3) 0.5378(4) 0.13211(14) 0.0594(12) Uani 1 1 d . . . . . H38 H -0.0385 0.5809 0.1133 0.071 Uiso 1 1 calc R U . . . C39 C -0.0938(3) 0.5073(4) 0.14888(15) 0.0634(14) Uani 1 1 d . . . . . H39 H -0.1491 0.5282 0.1410 0.076 Uiso 1 1 calc R U . . . C40 C -0.0798(3) 0.4460(3) 0.17746(15) 0.0582(12) Uani 1 1 d . . . . . C41 C 0.0009(3) 0.4124(3) 0.18925(14) 0.0585(12) Uani 1 1 d . . . . . H41 H 0.0092 0.3715 0.2090 0.070 Uiso 1 1 calc R U . . . C10 C 0.2838(3) 0.6280(3) 0.07158(11) 0.0499(11) Uani 1 1 d . . . . . C11 C 0.3000(3) 0.6445(4) 0.03504(13) 0.0676(14) Uani 1 1 d . . . . . H11 H 0.2786 0.6033 0.0166 0.081 Uiso 1 1 calc R U . . . C12 C 0.3454(3) 0.7178(4) 0.02586(14) 0.0684(14) Uani 1 1 d . . . . . H12 H 0.3553 0.7263 0.0016 0.082 Uiso 1 1 calc R U . . . C13 C 0.3768(3) 0.7800(4) 0.05299(13) 0.0633(13) Uani 1 1 d . . . . . C14 C 0.3645(3) 0.7673(3) 0.08892(13) 0.0592(12) Uani 1 1 d . . . . . H14 H 0.3865 0.8098 0.1067 0.071 Uiso 1 1 calc R U . . . C16 C 0.4447(3) 0.5985(4) 0.36706(13) 0.0609(13) Uani 1 1 d . . . . . H16 H 0.4186 0.6417 0.3806 0.073 Uiso 1 1 calc R U . . . C15 C 0.4106(3) 0.5817(3) 0.33092(11) 0.0431(10) Uani 1 1 d . . . . . C17 C 0.5168(3) 0.5527(4) 0.38384(12) 0.0606(13) Uani 1 1 d . . . . . H17 H 0.5372 0.5638 0.4085 0.073 Uiso 1 1 calc R U . . . C19 C 0.5254(3) 0.4736(3) 0.32834(12) 0.0541(12) Uani 1 1 d . . . . . H19 H 0.5531 0.4323 0.3146 0.065 Uiso 1 1 calc R U . . . C18 C 0.5581(3) 0.4912(3) 0.36420(11) 0.0437(10) Uani 1 1 d . . . . . C42 C 0.4049(8) 0.2464(11) 0.3943(4) 0.091(4) Uani 0.5 1 d . . P . . C43 C 0.3909(8) 0.2811(10) 0.3596(4) 0.107(5) Uani 0.5 1 d . . P . . H43A H 0.3447 0.2484 0.3455 0.160 Uiso 0.5 1 calc R U P . . H43B H 0.4418 0.2746 0.3482 0.160 Uiso 0.5 1 calc R U P . . H43C H 0.3763 0.3450 0.3607 0.160 Uiso 0.5 1 calc R U P . . N7 N 0.4169(9) 0.2392(14) 0.4237(5) 0.157(7) Uani 0.5 1 d . . P . . 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 O3 0.186(6) 0.129(4) 0.107(4) -0.013(3) 0.039(4) -0.107(4) N3 0.044(2) 0.054(2) 0.0432(19) 0.0123(17) 0.0097(16) 0.0129(17) C3 0.046(3) 0.049(3) 0.045(2) 0.0004(19) 0.013(2) 0.014(2) O2 0.140(4) 0.104(3) 0.080(3) 0.021(2) 0.044(3) -0.030(3) C2 0.052(3) 0.041(2) 0.044(2) -0.0018(18) 0.007(2) 0.019(2) N2 0.091(4) 0.078(3) 0.078(3) 0.005(3) 0.025(3) -0.024(3) O4 0.0443(17) 0.0598(19) 0.0606(19) 0.0191(16) 0.0088(14) 0.0101(15) C4 0.049(3) 0.046(2) 0.047(3) -0.0040(19) 0.008(2) 0.005(2) N4 0.097(4) 0.072(3) 0.087(3) 0.037(3) 0.014(3) 0.000(3) O6 0.123(4) 0.108(4) 0.136(4) 0.082(3) 0.006(3) 0.011(3) N6 0.047(3) 0.077(3) 0.109(4) -0.018(3) 0.033(3) 0.001(2) C6 0.052(3) 0.059(3) 0.046(3) -0.001(2) 0.010(2) -0.002(2) O5 0.092(3) 0.108(4) 0.145(4) 0.062(3) 0.039(3) -0.002(3) N5 0.036(2) 0.046(2) 0.054(2) -0.0050(16) 0.0129(16) -0.0016(16) C5 0.051(3) 0.041(2) 0.039(2) -0.0044(18) 0.0066(19) 0.004(2) O7 0.0464(17) 0.0598(19) 0.0543(18) -0.0010(15) 0.0119(15) 0.0003(15) C7 0.051(3) 0.057(3) 0.045(3) -0.005(2) -0.001(2) 0.000(2) O8 0.043(2) 0.133(4) 0.144(4) -0.012(3) 0.028(2) -0.003(2) C8 0.060(3) 0.052(3) 0.047(3) -0.009(2) 0.006(2) -0.006(2) C9 0.057(3) 0.051(3) 0.043(2) -0.003(2) 0.011(2) -0.008(2) O9 0.072(3) 0.133(4) 0.140(4) 0.042(4) 0.054(3) 0.009(3) C1 0.055(3) 0.058(3) 0.039(2) -0.002(2) 0.008(2) 0.021(2) K1 0.0566(7) 0.0871(8) 0.0537(6) 0.0026(5) 0.0008(5) -0.0162(6) Ni1 0.0403(3) 0.0478(4) 0.0433(3) -0.0084(2) 0.0089(2) -0.0067(2) N1 0.050(2) 0.044(2) 0.0395(19) -0.0024(16) 0.0087(16) -0.0050(17) O1 0.0592(19) 0.067(2) 0.0417(16) -0.0052(15) 0.0040(14) -0.0233(17) C20 0.056(3) 0.057(3) 0.049(3) -0.007(2) -0.002(2) 0.017(2) C21 0.043(2) 0.065(3) 0.051(3) 0.014(2) 0.015(2) 0.008(2) C22 0.050(3) 0.055(3) 0.051(3) 0.019(2) 0.015(2) 0.009(2) C23 0.056(3) 0.052(3) 0.046(2) 0.012(2) 0.004(2) 0.008(2) C24 0.054(3) 0.075(4) 0.074(3) 0.026(3) 0.006(2) 0.010(3) C25 0.077(4) 0.066(3) 0.074(3) 0.028(3) -0.001(3) 0.014(3) C26 0.075(4) 0.063(3) 0.060(3) 0.025(3) 0.012(3) 0.004(3) C27 0.058(3) 0.067(3) 0.061(3) 0.016(2) 0.014(2) 0.005(3) C28 0.045(4) 0.035(3) 0.087(5) 0.000 0.004(4) 0.000 C29 0.040(2) 0.033(2) 0.074(3) -0.001(2) 0.013(2) -0.0049(19) C30 0.051(3) 0.048(3) 0.057(3) -0.006(2) 0.005(2) 0.003(2) C31 0.047(3) 0.046(3) 0.059(3) -0.007(2) 0.014(2) 0.008(2) C32 0.036(2) 0.040(2) 0.054(3) -0.0014(19) 0.0134(19) -0.0033(19) C33 0.042(2) 0.044(2) 0.053(2) -0.011(2) 0.014(2) -0.009(2) C34 0.040(2) 0.037(2) 0.071(3) -0.011(2) 0.017(2) -0.0059(19) C35 0.047(3) 0.048(3) 0.053(3) -0.002(2) 0.015(2) -0.003(2) C36 0.042(2) 0.048(3) 0.059(3) -0.005(2) 0.016(2) 0.000(2) C37 0.047(3) 0.052(3) 0.048(2) -0.016(2) 0.007(2) -0.001(2) C38 0.044(3) 0.071(3) 0.062(3) -0.010(2) 0.006(2) 0.006(2) C39 0.038(3) 0.074(4) 0.077(3) -0.024(3) 0.003(2) 0.008(2) C40 0.041(3) 0.058(3) 0.079(3) -0.019(3) 0.019(2) -0.006(2) C41 0.051(3) 0.054(3) 0.074(3) -0.004(2) 0.021(2) -0.001(2) C10 0.048(3) 0.060(3) 0.041(2) 0.000(2) 0.005(2) -0.005(2) C11 0.077(3) 0.081(4) 0.044(3) -0.004(2) 0.004(2) -0.025(3) C12 0.074(3) 0.083(4) 0.049(3) 0.007(3) 0.013(2) -0.014(3) C13 0.066(3) 0.067(3) 0.058(3) 0.005(2) 0.012(2) -0.020(3) C14 0.066(3) 0.063(3) 0.049(3) -0.006(2) 0.010(2) -0.016(3) C16 0.059(3) 0.074(3) 0.050(3) -0.011(2) 0.006(2) 0.028(3) C15 0.044(2) 0.049(2) 0.037(2) 0.0023(18) 0.0106(18) 0.010(2) C17 0.051(3) 0.087(4) 0.041(2) -0.005(2) -0.002(2) 0.018(3) C19 0.056(3) 0.050(3) 0.056(3) -0.003(2) 0.009(2) 0.019(2) C18 0.039(2) 0.052(3) 0.042(2) 0.0124(19) 0.0124(19) 0.011(2) C42 0.059(7) 0.151(13) 0.059(7) 0.039(8) -0.002(6) -0.025(7) C43 0.076(9) 0.111(11) 0.131(12) 0.018(9) 0.005(8) -0.037(8) N7 0.086(9) 0.240(19) 0.139(13) 0.018(13) -0.003(9) -0.065(11) 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' K K 0.2009 0.2494 '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' 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 N2 O3 K1 113.0(4) . 3 ? C21 N3 C18 114.6(4) . . ? C21 N3 Ni1 122.8(3) . 2_655 ? C18 N3 Ni1 122.0(3) . 2_655 ? C4 C3 C2 122.3(4) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? N2 O2 K1 149.5(4) . 7_565 ? N2 O2 K1 83.6(3) . 3 ? K1 O2 K1 85.54(11) 7_565 3 ? C3 C2 C7 117.6(4) . . ? C3 C2 C1 122.6(4) . . ? C7 C2 C1 119.7(4) . . ? O2 N2 O3 121.4(5) . . ? O2 N2 C13 120.1(5) . . ? O3 N2 C13 118.5(5) . . ? O2 N2 K1 75.6(3) . 3 ? O3 N2 K1 47.5(3) . 3 ? C13 N2 K1 160.3(4) . 3 ? C23 O4 Ni1 129.6(3) . 2_655 ? C23 O4 K1 114.8(3) . 2_655 ? Ni1 O4 K1 90.16(11) 2_655 2_655 ? C3 C4 C5 119.7(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? O5 N4 O6 122.1(5) . . ? O5 N4 C26 119.7(5) . . ? O6 N4 C26 118.1(6) . . ? O5 N4 K1 62.8(3) . 8_556 ? O6 N4 K1 61.9(3) . 8_556 ? C26 N4 K1 161.1(4) . 8_556 ? N4 O6 K1 97.5(4) . 8_556 ? O9 N6 O8 123.5(5) . . ? O9 N6 C40 119.6(5) . . ? O8 N6 C40 116.8(6) . . ? C5 C6 C7 120.7(4) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? N4 O5 K1 149.5(5) . 4_545 ? N4 O5 K1 96.8(3) . 8_556 ? K1 O5 K1 84.28(11) 4_545 8_556 ? C35 N5 C32 114.3(4) . . ? C35 N5 Ni1 123.8(3) . . ? C32 N5 Ni1 121.7(2) . . ? C6 C5 C4 118.7(4) . . ? C6 C5 N1 120.4(4) . . ? C4 C5 N1 120.9(4) . . ? C37 O7 Ni1 129.9(3) . . ? C37 O7 K1 113.8(3) . . ? Ni1 O7 K1 91.81(11) . . ? C6 C7 C2 120.8(4) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? N1 C8 C9 128.5(4) . . ? N1 C8 H8 115.8 . . ? C9 C8 H8 115.8 . . ? C14 C9 C10 119.4(4) . . ? C14 C9 C8 116.8(4) . . ? C10 C9 C8 123.8(4) . . ? C2 C1 C15 114.9(3) . . ? C2 C1 H1A 108.6 . . ? C15 C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? C15 C1 H1B 108.6 . . ? H1A C1 H1B 107.5 . . ? O1 K1 O2 100.71(13) . 7_565 ? O1 K1 O3 133.72(15) . 3_445 ? O2 K1 O3 124.97(17) 7_565 3_445 ? O1 K1 O7 60.61(9) . . ? O2 K1 O7 135.64(13) 7_565 . ? O3 K1 O7 79.59(13) 3_445 . ? O1 K1 O4 59.23(9) . 2_655 ? O2 K1 O4 149.76(13) 7_565 2_655 ? O3 K1 O4 80.47(16) 3_445 2_655 ? O7 K1 O4 57.60(9) . 2_655 ? O1 K1 O5 139.21(12) . 4 ? O2 K1 O5 59.32(15) 7_565 4 ? O3 K1 O5 71.68(18) 3_445 4 ? O7 K1 O5 106.95(11) . 4 ? O4 K1 O5 150.61(13) 2_655 4 ? O1 K1 O6 72.89(11) . 8_455 ? O2 K1 O6 73.44(16) 7_565 8_455 ? O3 K1 O6 123.33(17) 3_445 8_455 ? O7 K1 O6 127.36(12) . 8_455 ? O4 K1 O6 78.67(13) 2_655 8_455 ? O5 K1 O6 124.66(15) 4 8_455 ? O1 K1 O5 112.77(13) . 8_455 ? O2 K1 O5 72.93(15) 7_565 8_455 ? O3 K1 O5 89.61(16) 3_445 8_455 ? O7 K1 O5 150.08(13) . 8_455 ? O4 K1 O5 93.27(13) 2_655 8_455 ? O5 K1 O5 95.72(11) 4 8_455 ? O6 K1 O5 40.47(12) 8_455 8_455 ? O1 K1 O2 155.01(13) . 3_445 ? O2 K1 O2 94.46(11) 7_565 3_445 ? O3 K1 O2 39.87(13) 3_445 3_445 ? O7 K1 O2 119.25(10) . 3_445 ? O4 K1 O2 98.44(11) 2_655 3_445 ? O5 K1 O2 65.77(13) 4 3_445 ? O6 K1 O2 92.88(12) 8_455 3_445 ? O5 K1 O2 53.25(13) 8_455 3_445 ? O1 K1 N2 145.49(12) . 3_445 ? O2 K1 N2 112.55(14) 7_565 3_445 ? O3 K1 N2 19.49(13) 3_445 3_445 ? O7 K1 N2 98.49(11) . 3_445 ? O4 K1 N2 86.60(11) 2_655 3_445 ? O5 K1 N2 70.24(13) 4 3_445 ? O6 K1 N2 107.28(13) 8_455 3_445 ? O5 K1 N2 70.70(14) 8_455 3_445 ? O2 K1 N2 20.77(10) 3_445 3_445 ? O1 K1 N4 92.44(12) . 8_455 ? O2 K1 N4 75.36(14) 7_565 8_455 ? O3 K1 N4 104.86(16) 3_445 8_455 ? O7 K1 N4 139.16(12) . 8_455 ? O4 K1 N4 82.71(11) 2_655 8_455 ? O5 K1 N4 113.01(14) 4 8_455 ? O6 K1 N4 20.65(12) 8_455 8_455 ? O5 K1 N4 20.34(11) 8_455 8_455 ? O2 K1 N4 72.24(13) 3_445 8_455 ? N2 K1 N4 87.44(14) 3_445 8_455 ? O1 K1 N7 71.4(2) . 4 ? O2 K1 N7 69.6(3) 7_565 4 ? O3 K1 N7 114.9(3) 3_445 4 ? O7 K1 N7 66.3(3) . 4 ? O4 K1 N7 117.6(3) 2_655 4 ? O5 K1 N7 68.3(2) 4 4 ? O6 K1 N7 121.5(3) 8_455 4 ? O5 K1 N7 142.4(3) 8_455 4 ? O2 K1 N7 133.1(2) 3_445 4 ? N2 K1 N7 128.2(3) 3_445 4 ? N4 K1 N7 137.3(3) 8_455 4 ? O1 Ni1 O4 84.97(12) . 2_655 ? O1 Ni1 O7 85.87(12) . . ? O4 Ni1 O7 85.84(12) 2_655 . ? O1 Ni1 N5 170.94(12) . . ? O4 Ni1 N5 87.24(13) 2_655 . ? O7 Ni1 N5 88.95(13) . . ? O1 Ni1 N3 86.02(13) . 2_655 ? O4 Ni1 N3 89.37(12) 2_655 2_655 ? O7 Ni1 N3 170.91(12) . 2_655 ? N5 Ni1 N3 98.55(13) . 2_655 ? O1 Ni1 N1 87.83(12) . . ? O4 Ni1 N1 171.72(13) 2_655 . ? O7 Ni1 N1 89.58(13) . . ? N5 Ni1 N1 99.58(13) . . ? N3 Ni1 N1 94.21(13) 2_655 . ? O1 Ni1 K1 47.03(8) . . ? O4 Ni1 K1 54.89(9) 2_655 . ? O7 Ni1 K1 53.24(8) . . ? N5 Ni1 K1 124.15(9) . . ? N3 Ni1 K1 117.79(9) 2_655 . ? N1 Ni1 K1 116.94(10) . . ? C8 N1 C5 114.5(3) . . ? C8 N1 Ni1 122.8(3) . . ? C5 N1 Ni1 122.5(3) . . ? C10 O1 Ni1 129.4(3) . . ? C10 O1 K1 126.9(3) . . ? Ni1 O1 K1 98.55(12) . . ? C15 C20 C19 121.5(4) . . ? C15 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? N3 C21 C22 128.4(4) . . ? N3 C21 H21 115.8 . . ? C22 C21 H21 115.8 . . ? C27 C22 C23 119.1(4) . . ? C27 C22 C21 116.5(4) . . ? C23 C22 C21 124.2(4) . . ? O4 C23 C22 124.6(4) . . ? O4 C23 C24 118.6(4) . . ? C22 C23 C24 116.7(4) . . ? C25 C24 C23 121.9(5) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C26 120.1(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 119.7(5) . . ? C27 C26 N4 119.6(5) . . ? C25 C26 N4 120.6(5) . . ? C26 C27 C22 122.3(5) . . ? C26 C27 H27 118.8 . . ? C22 C27 H27 118.8 . . ? C29 C28 C29 114.5(5) 2_655 . ? C29 C28 H28 109(3) 2_655 . ? C29 C28 H28 107(3) . . ? C34 C29 C30 117.4(4) . . ? C34 C29 C28 122.4(4) . . ? C30 C29 C28 120.2(4) . . ? C31 C30 C29 120.9(4) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 120.1(4) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 119.7(4) . . ? C33 C32 N5 119.7(4) . . ? C31 C32 N5 120.6(4) . . ? C32 C33 C34 119.4(4) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C29 C34 C33 122.5(4) . . ? C29 C34 H34 118.7 . . ? C33 C34 H34 118.7 . . ? N5 C35 C36 127.9(4) . . ? N5 C35 H35 116.0 . . ? C36 C35 H35 116.0 . . ? C41 C36 C37 119.5(4) . . ? C41 C36 C35 116.0(4) . . ? C37 C36 C35 124.5(4) . . ? O7 C37 C36 123.8(4) . . ? O7 C37 C38 119.4(4) . . ? C36 C37 C38 116.8(4) . . ? C39 C38 C37 121.6(5) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C38 C39 C40 120.5(5) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C39 C40 C41 121.1(4) . . ? C39 C40 N6 121.4(5) . . ? C41 C40 N6 117.5(5) . . ? C40 C41 C36 120.5(5) . . ? C40 C41 H41 119.7 . . ? C36 C41 H41 119.7 . . ? O1 C10 C11 120.2(4) . . ? O1 C10 C9 123.0(4) . . ? C11 C10 C9 116.8(4) . . ? C12 C11 C10 122.6(5) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C11 C12 C13 119.2(5) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C14 C13 C12 121.1(4) . . ? C14 C13 N2 119.5(5) . . ? C12 C13 N2 119.3(5) . . ? C13 C14 C9 120.9(4) . . ? C13 C14 H14 119.6 . . ? C9 C14 H14 119.6 . . ? C15 C16 C17 121.8(4) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C20 C15 C16 117.0(4) . . ? C20 C15 C1 123.1(4) . . ? C16 C15 C1 119.9(4) . . ? C18 C17 C16 120.2(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C18 C19 C20 120.5(4) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C18 C17 118.9(4) . . ? C19 C18 N3 119.4(4) . . ? C17 C18 N3 121.7(4) . . ? N7 C42 C43 164(2) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 N7 K1 113.1(15) . 4_545 ? 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 O3 N2 1.227(6) . ? O3 K1 2.713(5) 3 ? N3 C21 1.282(5) . ? N3 C18 1.437(5) . ? N3 Ni1 2.126(3) 2_655 ? C3 C4 1.374(6) . ? C3 C2 1.375(6) . ? C3 H3 0.9300 . ? O2 N2 1.209(6) . ? O2 K1 2.713(4) 7_565 ? O2 K1 3.301(5) 3 ? C2 C7 1.389(6) . ? C2 C1 1.518(6) . ? N2 C13 1.430(7) . ? N2 K1 3.386(5) 3 ? O4 C23 1.275(5) . ? O4 Ni1 2.042(3) 2_655 ? O4 K1 2.916(3) 2_655 ? C4 C5 1.391(6) . ? C4 H4 0.9300 . ? N4 O5 1.201(6) . ? N4 O6 1.221(6) . ? N4 C26 1.454(7) . ? N4 K1 3.432(5) 8_556 ? O6 K1 3.052(5) 8_556 ? N6 O9 1.215(6) . ? N6 O8 1.234(6) . ? N6 C40 1.461(7) . ? C6 C5 1.381(6) . ? C6 C7 1.383(6) . ? C6 H6 0.9300 . ? O5 K1 3.045(6) 4_545 ? O5 K1 3.075(4) 8_556 ? N5 C35 1.285(5) . ? N5 C32 1.439(5) . ? N5 Ni1 2.116(4) . ? C5 N1 1.443(5) . ? O7 C37 1.277(5) . ? O7 Ni1 2.043(3) . ? O7 K1 2.857(3) . ? C7 H7 0.9300 . ? C8 N1 1.286(5) . ? C8 C9 1.446(6) . ? C8 H8 0.9300 . ? C9 C14 1.385(6) . ? C9 C10 1.431(6) . ? C1 C15 1.519(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? K1 O1 2.637(3) . ? K1 O2 2.713(4) 7_565 ? K1 O3 2.713(5) 3_445 ? K1 O4 2.916(3) 2_655 ? K1 O5 3.045(6) 4 ? K1 O6 3.052(5) 8_455 ? K1 O5 3.075(4) 8_455 ? K1 O2 3.301(5) 3_445 ? K1 N2 3.386(5) 3_445 ? K1 N4 3.432(5) 8_455 ? K1 N7 3.449(19) 4 ? Ni1 O1 2.037(3) . ? Ni1 O4 2.042(3) 2_655 ? Ni1 N3 2.126(3) 2_655 ? Ni1 N1 2.132(3) . ? O1 C10 1.266(5) . ? C20 C15 1.373(6) . ? C20 C19 1.390(6) . ? C20 H20 0.9300 . ? C21 C22 1.446(6) . ? C21 H21 0.9300 . ? C22 C27 1.380(6) . ? C22 C23 1.427(6) . ? C23 C24 1.430(6) . ? C24 C25 1.355(7) . ? C24 H24 0.9300 . ? C25 C26 1.386(7) . ? C25 H25 0.9300 . ? C26 C27 1.364(7) . ? C27 H27 0.9300 . ? C28 C29 1.507(6) 2_655 ? C28 C29 1.507(6) . ? C28 H28 0.98(5) . ? C29 C34 1.376(6) . ? C29 C30 1.397(6) . ? C30 C31 1.384(6) . ? C30 H30 0.9300 . ? C31 C32 1.385(6) . ? C31 H31 0.9300 . ? C32 C33 1.378(6) . ? C33 C34 1.381(6) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.454(6) . ? C35 H35 0.9300 . ? C36 C41 1.398(6) . ? C36 C37 1.428(6) . ? C37 C38 1.439(6) . ? C38 C39 1.352(7) . ? C38 H38 0.9300 . ? C39 C40 1.369(7) . ? C39 H39 0.9300 . ? C40 C41 1.376(7) . ? C41 H41 0.9300 . ? C10 C11 1.414(6) . ? C11 C12 1.354(7) . ? C11 H11 0.9300 . ? C12 C13 1.383(7) . ? C12 H12 0.9300 . ? C13 C14 1.366(6) . ? C14 H14 0.9300 . ? C16 C15 1.378(6) . ? C16 C17 1.386(6) . ? C16 H16 0.9300 . ? C17 C18 1.367(6) . ? C17 H17 0.9300 . ? C19 C18 1.366(6) . ? C19 H19 0.9300 . ? C42 N7 1.070(16) . ? C42 C43 1.354(17) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? N7 K1 3.449(19) 4_545 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C35 H35 O9 0.93 2.60 3.339(7) 136.5 2 C11 H11 O6 0.93 2.57 3.416(7) 150.8 8_455 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 C3 C2 C7 2.0(6) . . . . ? C4 C3 C2 C1 -176.6(4) . . . . ? K1 O2 N2 O3 -56.4(11) 7_565 . . . ? K1 O2 N2 O3 13.4(6) 3 . . . ? K1 O2 N2 C13 123.0(7) 7_565 . . . ? K1 O2 N2 C13 -167.2(5) 3 . . . ? K1 O2 N2 K1 -69.8(7) 7_565 . . 3 ? K1 O3 N2 O2 -17.7(8) 3 . . . ? K1 O3 N2 C13 162.8(4) 3 . . . ? C2 C3 C4 C5 1.3(6) . . . . ? O5 N4 O6 K1 -18.7(7) . . . 8_556 ? C26 N4 O6 K1 158.6(4) . . . 8_556 ? O6 N4 O5 K1 -71.8(10) . . . 4_545 ? C26 N4 O5 K1 111.0(7) . . . 4_545 ? K1 N4 O5 K1 -90.3(6) 8_556 . . 4_545 ? O6 N4 O5 K1 18.6(7) . . . 8_556 ? C26 N4 O5 K1 -158.7(5) . . . 8_556 ? C7 C6 C5 C4 1.7(6) . . . . ? C7 C6 C5 N1 -178.0(4) . . . . ? C3 C4 C5 C6 -3.1(6) . . . . ? C3 C4 C5 N1 176.5(4) . . . . ? C5 C6 C7 C2 1.7(7) . . . . ? C3 C2 C7 C6 -3.5(6) . . . . ? C1 C2 C7 C6 175.2(4) . . . . ? N1 C8 C9 C14 -169.9(5) . . . . ? N1 C8 C9 C10 8.8(8) . . . . ? C3 C2 C1 C15 127.6(4) . . . . ? C7 C2 C1 C15 -50.9(6) . . . . ? C9 C8 N1 C5 175.2(4) . . . . ? C9 C8 N1 Ni1 0.5(7) . . . . ? C6 C5 N1 C8 -47.3(6) . . . . ? C4 C5 N1 C8 133.0(4) . . . . ? C6 C5 N1 Ni1 127.4(4) . . . . ? C4 C5 N1 Ni1 -52.3(5) . . . . ? C18 N3 C21 C22 176.2(4) . . . . ? Ni1 N3 C21 C22 -12.8(7) 2_655 . . . ? N3 C21 C22 C27 -169.9(5) . . . . ? N3 C21 C22 C23 6.8(8) . . . . ? Ni1 O4 C23 C22 -2.5(7) 2_655 . . . ? K1 O4 C23 C22 110.2(4) 2_655 . . . ? Ni1 O4 C23 C24 177.3(3) 2_655 . . . ? K1 O4 C23 C24 -70.0(5) 2_655 . . . ? C27 C22 C23 O4 178.6(5) . . . . ? C21 C22 C23 O4 2.1(8) . . . . ? C27 C22 C23 C24 -1.1(7) . . . . ? C21 C22 C23 C24 -177.7(5) . . . . ? O4 C23 C24 C25 -178.2(5) . . . . ? C22 C23 C24 C25 1.6(8) . . . . ? C23 C24 C25 C26 0.0(9) . . . . ? C24 C25 C26 C27 -2.1(9) . . . . ? C24 C25 C26 N4 -179.8(5) . . . . ? O5 N4 C26 C27 2.1(9) . . . . ? O6 N4 C26 C27 -175.3(6) . . . . ? K1 N4 C26 C27 -90.4(13) 8_556 . . . ? O5 N4 C26 C25 179.8(6) . . . . ? O6 N4 C26 C25 2.4(9) . . . . ? K1 N4 C26 C25 87.3(13) 8_556 . . . ? C25 C26 C27 C22 2.6(8) . . . . ? N4 C26 C27 C22 -179.7(5) . . . . ? C23 C22 C27 C26 -0.9(8) . . . . ? C21 C22 C27 C26 175.9(5) . . . . ? C29 C28 C29 C34 128.8(4) 2_655 . . . ? C29 C28 C29 C30 -52.7(3) 2_655 . . . ? C34 C29 C30 C31 -0.3(6) . . . . ? C28 C29 C30 C31 -178.9(4) . . . . ? C29 C30 C31 C32 -1.1(7) . . . . ? C30 C31 C32 C33 1.9(6) . . . . ? C30 C31 C32 N5 -179.4(4) . . . . ? C35 N5 C32 C33 115.2(4) . . . . ? Ni1 N5 C32 C33 -61.3(4) . . . . ? C35 N5 C32 C31 -63.5(5) . . . . ? Ni1 N5 C32 C31 119.9(4) . . . . ? C31 C32 C33 C34 -1.3(6) . . . . ? N5 C32 C33 C34 -180.0(4) . . . . ? C30 C29 C34 C33 0.9(6) . . . . ? C28 C29 C34 C33 179.5(4) . . . . ? C32 C33 C34 C29 -0.2(6) . . . . ? C32 N5 C35 C36 -179.1(4) . . . . ? Ni1 N5 C35 C36 -2.7(6) . . . . ? N5 C35 C36 C41 177.6(4) . . . . ? N5 C35 C36 C37 -2.8(7) . . . . ? Ni1 O7 C37 C36 10.8(6) . . . . ? K1 O7 C37 C36 125.2(4) . . . . ? Ni1 O7 C37 C38 -168.6(3) . . . . ? K1 O7 C37 C38 -54.2(4) . . . . ? C41 C36 C37 O7 178.4(4) . . . . ? C35 C36 C37 O7 -1.2(7) . . . . ? C41 C36 C37 C38 -2.2(6) . . . . ? C35 C36 C37 C38 178.2(4) . . . . ? O7 C37 C38 C39 179.3(4) . . . . ? C36 C37 C38 C39 -0.2(7) . . . . ? C37 C38 C39 C40 2.0(7) . . . . ? C38 C39 C40 C41 -1.4(7) . . . . ? C38 C39 C40 N6 178.4(4) . . . . ? O9 N6 C40 C39 -168.8(5) . . . . ? O8 N6 C40 C39 10.8(7) . . . . ? O9 N6 C40 C41 11.0(7) . . . . ? O8 N6 C40 C41 -169.4(5) . . . . ? C39 C40 C41 C36 -1.0(7) . . . . ? N6 C40 C41 C36 179.2(4) . . . . ? C37 C36 C41 C40 2.8(7) . . . . ? C35 C36 C41 C40 -177.6(4) . . . . ? Ni1 O1 C10 C11 155.5(4) . . . . ? K1 O1 C10 C11 -55.4(6) . . . . ? Ni1 O1 C10 C9 -23.3(7) . . . . ? K1 O1 C10 C9 125.8(4) . . . . ? C14 C9 C10 O1 -178.6(4) . . . . ? C8 C9 C10 O1 2.7(7) . . . . ? C14 C9 C10 C11 2.6(7) . . . . ? C8 C9 C10 C11 -176.1(5) . . . . ? O1 C10 C11 C12 179.7(5) . . . . ? C9 C10 C11 C12 -1.5(8) . . . . ? C10 C11 C12 C13 -0.7(9) . . . . ? C11 C12 C13 C14 1.6(8) . . . . ? C11 C12 C13 N2 178.9(5) . . . . ? O2 N2 C13 C14 -176.2(5) . . . . ? O3 N2 C13 C14 3.3(9) . . . . ? K1 N2 C13 C14 43.7(14) 3 . . . ? O2 N2 C13 C12 6.5(8) . . . . ? O3 N2 C13 C12 -174.0(6) . . . . ? K1 N2 C13 C12 -133.7(9) 3 . . . ? C12 C13 C14 C9 -0.4(8) . . . . ? N2 C13 C14 C9 -177.7(5) . . . . ? C10 C9 C14 C13 -1.8(8) . . . . ? C8 C9 C14 C13 177.0(5) . . . . ? C19 C20 C15 C16 -3.5(7) . . . . ? C19 C20 C15 C1 177.3(4) . . . . ? C17 C16 C15 C20 0.6(7) . . . . ? C17 C16 C15 C1 179.8(5) . . . . ? C2 C1 C15 C20 -19.5(6) . . . . ? C2 C1 C15 C16 161.4(4) . . . . ? C15 C16 C17 C18 2.3(8) . . . . ? C15 C20 C19 C18 3.6(8) . . . . ? C20 C19 C18 C17 -0.6(7) . . . . ? C20 C19 C18 N3 178.8(4) . . . . ? C16 C17 C18 C19 -2.3(7) . . . . ? C16 C17 C18 N3 178.4(4) . . . . ? C21 N3 C18 C19 -106.4(5) . . . . ? Ni1 N3 C18 C19 82.5(5) 2_655 . . . ? C21 N3 C18 C17 73.0(6) . . . . ? Ni1 N3 C18 C17 -98.1(4) 2_655 . . . ? C43 C42 N7 K1 176(5) . . . 4_545 ?