#------------------------------------------------------------------------------ #$Date: 2017-05-06 00:54:06 +0300 (Sat, 06 May 2017) $ #$Revision: 196377 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/80/7228064.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_7228064 loop_ _publ_author_name 'Morshedi, Mahbod' 'White, Nicholas G.' _publ_section_title ; Mixed halide/oxoanion-templated frameworks ; _journal_issue 17 _journal_name_full CrystEngComm _journal_page_first 2367 _journal_paper_doi 10.1039/C7CE00265C _journal_volume 19 _journal_year 2017 _chemical_compound_source synthesized _chemical_formula_moiety '2(C29 H32 N8), 8(N O3), 3(C H4 O), H2 O' _chemical_formula_sum 'C61 H78 N24 O28' _chemical_formula_weight 1595.44 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary other _audit_update_record ; 2017-02-06 deposited with the CCDC. 2017-04-12 downloaded from the CCDC. ; _cell_angle_alpha 101.982(7) _cell_angle_beta 91.167(8) _cell_angle_gamma 90.664(8) _cell_formula_units_Z 2 _cell_length_a 11.6729(15) _cell_length_b 11.8954(9) _cell_length_c 26.963(2) _cell_measurement_reflns_used 4419 _cell_measurement_temperature 150 _cell_measurement_theta_max 68.3 _cell_measurement_theta_min 3.85 _cell_volume 3661.1(6) _computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)' _computing_data_collection 'CrysAlisPro, (Agilent, 2011)' _computing_data_reduction 'CrysAlisPro, (Agilent, 2011)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _diffrn_ambient_temperature 150 _diffrn_measured_fraction_theta_full 0.963 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measurement_device Area _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_method \w _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 22057 _diffrn_reflns_theta_full 68.252 _diffrn_reflns_theta_max 68.252 _diffrn_reflns_theta_min 3.788 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.994 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1671.990 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.15 _refine_diff_density_min -0.88 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 0.9703 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1019 _refine_ls_number_reflns 11000 _refine_ls_number_restraints 169 _refine_ls_R_factor_all 0.1618 _refine_ls_R_factor_gt 0.1386 _refine_ls_shift/su_max 0.0001955 _refine_ls_shift/su_mean 0.0000140 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.341E+04 0.560E+04 0.338E+04 0.137E+04 325. ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.3474 _refine_ls_wR_factor_gt 0.3309 _refine_ls_wR_factor_ref 0.3474 _reflns_limit_h_max 14 _reflns_limit_h_min -14 _reflns_limit_k_max 14 _reflns_limit_k_min -14 _reflns_limit_l_max 32 _reflns_limit_l_min 0 _reflns_number_gt 7779 _reflns_number_total 12917 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 3.74 _oxford_diffrn_Wilson_scale 0.14 _oxford_refine_ls_r_factor_ref 0.1618 _oxford_refine_ls_scale 3.54(9) _oxford_reflns_number_all 11000 _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _cod_data_source_file c7ce00265c2.cif _cod_data_source_block 1NO3 _cod_depositor_comments ; The following automatic conversions were performed: '_atom_sites_solution_primary' value 'Other' changed to 'other' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas Adding full bibliography for 7228063--7228067.cif. ; _cod_original_cell_volume 3661.1(3) _cod_original_sg_symbol_H-M 'P -1 ' _cod_database_code 7228064 _iucr_refine_instructions_details_constraints ; # # Punched on 24/10/16 at 14:40:58 # #LIST 12 BLOCK SCALE X'S U'S SUMFIX ELEMENT SCALES RIDE N ( 1,X'S) H ( 11,X'S) H ( 12,X'S) RIDE N ( 2,X'S) H ( 21,X'S) H ( 22,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE N ( 11,X'S) H ( 111,X'S) H ( 112,X'S) RIDE N ( 12,X'S) H ( 121,X'S) H ( 122,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE N ( 21,X'S) H ( 211,X'S) H ( 212,X'S) RIDE N ( 22,X'S) H ( 221,X'S) H ( 222,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE N ( 31,X'S) H ( 311,X'S) H ( 312,X'S) RIDE N ( 32,X'S) H ( 321,X'S) H ( 322,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE N ( 51,X'S) H ( 511,X'S) H ( 512,X'S) RIDE N ( 52,X'S) H ( 521,X'S) H ( 522,X'S) RIDE C ( 55,X'S) H ( 551,X'S) RIDE C ( 56,X'S) H ( 561,X'S) RIDE C ( 58,X'S) H ( 581,X'S) RIDE C ( 59,X'S) H ( 591,X'S) RIDE N ( 61,X'S) H ( 611,X'S) H ( 612,X'S) RIDE N ( 62,X'S) H ( 621,X'S) H ( 622,X'S) RIDE C ( 65,X'S) H ( 651,X'S) RIDE C ( 66,X'S) H ( 661,X'S) RIDE C ( 68,X'S) H ( 681,X'S) RIDE C ( 69,X'S) H ( 691,X'S) RIDE N ( 71,X'S) H ( 711,X'S) H ( 712,X'S) RIDE N ( 72,X'S) H ( 721,X'S) H ( 722,X'S) RIDE C ( 75,X'S) H ( 751,X'S) RIDE C ( 76,X'S) H ( 761,X'S) RIDE C ( 78,X'S) H ( 781,X'S) RIDE C ( 79,X'S) H ( 791,X'S) RIDE N ( 81,X'S) H ( 811,X'S) H ( 812,X'S) RIDE N ( 82,X'S) H ( 821,X'S) H ( 822,X'S) RIDE C ( 85,X'S) H ( 851,X'S) RIDE C ( 86,X'S) H ( 861,X'S) RIDE C ( 88,X'S) H ( 881,X'S) RIDE C ( 89,X'S) H ( 891,X'S) RIDE O ( 201,X'S) H (2011,X'S) RIDE C ( 202,X'S) H (2021,X'S) H (2022,X'S) H (2023,X'S) RIDE O ( 211,X'S) H (2111,X'S) RIDE C ( 212,X'S) H (2121,X'S) H (2122,X'S) H (2123,X'S) RIDE O ( 221,X'S) H (2211,X'S) RIDE C ( 222,X'S) H (2221,X'S) H (2222,X'S) H (2223,X'S) RIDE O ( 231,X'S) H (2311,X'S) H (2312,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 24/10/16 at 14:40:58 # #LIST 16 REM REM MEOHS REM DIST 1.45, 0.01 = O(201) TO C(202), O(211) TO C(212) CONT O(221) TO C(222) REM REM NITRATES REM DIST 0, 0.01 = MEAN N(101) TO O(102), N(101) TO O(103) CONT N(101) TO O(104) CONT N(111) TO O(112), N(111) TO O(113) CONT N(111) TO O(114) CONT N(121) TO O(122), N(121) TO O(123) CONT N(121) TO O(124) CONT N(131) TO O(132), N(131) TO O(133) CONT N(131) TO O(134) CONT N(141) TO O(142), N(141) TO O(143) CONT N(141) TO O(144) CONT N(151) TO O(152), N(151) TO O(153) CONT N(151) TO O(154) CONT N(161) TO O(162), N(161) TO O(163) CONT N(161) TO O(164) CONT N(171) TO O(172), N(171) TO O(173) CONT N(171) TO O(174) PLANAR N(141) O(142) O(143) O(144) PLANAR N(161) O(162) O(163) O(164) ANGL 120, 1 = O(142) TO N(141) TO O(143) CONT O(142) TO N(141) TO O(144) CONT O(143) TO N(141) TO O(144) CONT O(162) TO N(161) TO O(163) CONT O(162) TO N(161) TO O(164) CONT O(163) TO N(161) TO O(164) REM REM PHENYLS REM DIST 0, 0.01 = MEAN C(4) TO C(5), C(5) TO C(6) CONT C(6) TO C(7), C(7) TO C(8) CONT C(8) TO C(9), C(9) TO C(4) CONT C(14) TO C(15), C(15) TO C(16) CONT C(16) TO C(17), C(17) TO C(18) CONT C(18) TO C(19), C(19) TO C(14) CONT C(24) TO C(25), C(25) TO C(26) CONT C(26) TO C(27), C(27) TO C(28) CONT C(28) TO C(29), C(29) TO C(24) CONT C(34) TO C(35), C(35) TO C(36) CONT C(36) TO C(37), C(37) TO C(38) CONT C(38) TO C(39), C(39) TO C(34) CONT C(54) TO C(55), C(55) TO C(56) CONT C(56) TO C(57), C(57) TO C(58) CONT C(58) TO C(59), C(59) TO C(54) CONT C(64) TO C(65), C(65) TO C(66) CONT C(66) TO C(67), C(67) TO C(68) CONT C(68) TO C(69), C(69) TO C(64) CONT C(74) TO C(75), C(75) TO C(76) CONT C(76) TO C(77), C(77) TO C(78) CONT C(78) TO C(79), C(79) TO C(74) CONT C(84) TO C(85), C(85) TO C(86) CONT C(86) TO C(87), C(87) TO C(88) CONT C(88) TO C(89), C(89) TO C(84) REM REM OTHER REM DIST 0, 0.01 = MEAN N(1) TO C(3), N(2) TO C(3) CONT N(11) TO C(13), N(12) TO C(13) CONT N(21) TO C(23), N(22) TO C(23) CONT N(31) TO C(33), N(32) TO C(33) CONT N(51) TO C(53), N(52) TO C(53) CONT N(61) TO C(63), N(62) TO C(63) CONT N(71) TO C(73), N(72) TO C(73) CONT N(81) TO C(83), N(82) TO C(83) DIST 0, 0.01 = MEAN C(3) TO C(4), C(13) TO C(14) CONT C(23) TO C(24), C(33) TO C(34) CONT C(53) TO C(54), C(63) TO C(64) CONT C(73) TO C(74), C(83) TO C(84) DIST 0, 0.01 = MEAN C(7) TO C(10), C(17) TO C(10) CONT C(27) TO C(10), C(37) TO C(10) CONT C(57) TO C(60), C(67) TO C(60) CONT C(77) TO C(60), C(87) TO C(60) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00100 = N(141) TO O(142) VIBR .0, 0.00100 = N(141) TO O(143) VIBR .0, 0.00100 = N(141) TO O(144) VIBR .0, 0.00200 = O(143) TO O(142) VIBR .0, 0.00200 = O(144) TO O(142) VIBR .0, 0.00200 = O(144) TO O(143) VIBR .0, 0.00100 = N(161) TO O(162) VIBR .0, 0.00100 = N(161) TO O(163) VIBR .0, 0.00100 = N(161) TO O(164) VIBR .0, 0.00200 = O(163) TO O(162) VIBR .0, 0.00200 = O(164) TO O(162) VIBR .0, 0.00200 = O(164) TO O(163) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.01000 = N(141) TO O(142) U(IJ) .0, 0.01000 = N(141) TO O(143) U(IJ) .0, 0.01000 = N(141) TO O(144) U(IJ) .0, 0.01000 = N(161) TO O(162) U(IJ) .0, 0.01000 = N(161) TO O(163) U(IJ) .0, 0.01000 = N(161) TO O(164) REM THERMSIM END (DO NOT REMOVE THIS LINE) END ; loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp N1 N 0.6255(7) 0.4161(6) 0.4458(3) 0.0569 1.0000 Uani D . N2 N 0.5944(7) 0.3364(6) 0.5138(3) 0.0580 1.0000 Uani D . C3 C 0.6405(7) 0.4175(6) 0.4940(3) 0.0455 1.0000 Uani D . C4 C 0.7103(7) 0.5101(5) 0.5267(3) 0.0408 1.0000 Uani D . C5 C 0.7121(7) 0.6222(5) 0.5191(3) 0.0412 1.0000 Uani D . C6 C 0.7805(7) 0.7044(6) 0.5502(3) 0.0396 1.0000 Uani D . C7 C 0.8464(7) 0.6816(5) 0.5908(3) 0.0405 1.0000 Uani D . C8 C 0.8439(7) 0.5691(5) 0.5969(3) 0.0454 1.0000 Uani D . C9 C 0.7782(7) 0.4844(6) 0.5659(3) 0.0460 1.0000 Uani D . C10 C 0.9197(6) 0.7791(5) 0.6239(2) 0.0373 1.0000 Uani D . N11 N 1.2114(8) 0.5765(7) 0.8012(3) 0.0674 1.0000 Uani D . N12 N 1.2975(7) 0.4974(6) 0.7273(3) 0.0594 1.0000 Uani D . C13 C 1.2217(8) 0.5662(7) 0.7519(3) 0.0534 1.0000 Uani D . C14 C 1.1445(6) 0.6271(7) 0.7221(3) 0.0486 1.0000 Uani D . C15 C 1.0288(6) 0.6376(7) 0.7314(3) 0.0496 1.0000 Uani D . C16 C 0.9593(7) 0.6885(7) 0.6996(3) 0.0447 1.0000 Uani D . C17 C 1.0034(6) 0.7300(6) 0.6590(3) 0.0386 1.0000 Uani D . C18 C 1.1218(6) 0.7246(7) 0.6531(3) 0.0461 1.0000 Uani D . C19 C 1.1927(7) 0.6729(7) 0.6837(3) 0.0466 1.0000 Uani D . N21 N 1.2974(7) 1.0663(6) 0.5286(3) 0.0597 1.0000 Uani D . N22 N 1.2632(7) 0.9328(7) 0.4560(3) 0.0621 1.0000 Uani D . C23 C 1.2370(7) 0.9790(7) 0.5027(3) 0.0518 1.0000 Uani D . C24 C 1.1447(6) 0.9291(6) 0.5283(3) 0.0449 1.0000 Uani D . C25 C 1.0745(7) 1.0008(7) 0.5615(3) 0.0517 1.0000 Uani D . C26 C 0.9994(7) 0.9530(6) 0.5909(3) 0.0461 1.0000 Uani D . C27 C 0.9897(6) 0.8348(5) 0.5869(3) 0.0388 1.0000 Uani D . C28 C 1.0509(7) 0.7662(6) 0.5490(3) 0.0449 1.0000 Uani D . C29 C 1.1291(7) 0.8109(6) 0.5205(3) 0.0477 1.0000 Uani D . N31 N 0.6081(7) 1.2079(6) 0.7286(3) 0.0581 1.0000 Uani D . N32 N 0.6360(8) 1.1269(8) 0.7976(3) 0.0687 1.0000 Uani D . C33 C 0.6519(7) 1.1302(6) 0.7501(3) 0.0468 1.0000 Uani D . C34 C 0.7212(6) 1.0390(6) 0.7189(3) 0.0405 1.0000 Uani D . C35 C 0.8372(6) 1.0313(6) 0.7273(3) 0.0470 1.0000 Uani D . C36 C 0.9004(7) 0.9479(6) 0.6965(3) 0.0459 1.0000 Uani D . C37 C 0.8458(6) 0.8677(6) 0.6580(2) 0.0381 1.0000 Uani D . C38 C 0.7282(6) 0.8750(7) 0.6505(3) 0.0494 1.0000 Uani D . C39 C 0.6674(7) 0.9605(7) 0.6804(3) 0.0480 1.0000 Uani D . N51 N 0.6490(7) 0.5570(7) 0.7936(3) 0.0625 1.0000 Uani D . N52 N 0.7195(9) 0.4616(8) 0.7183(3) 0.0773 1.0000 Uani D . C53 C 0.7193(7) 0.4836(7) 0.7679(3) 0.0580 1.0000 Uani D . C54 C 0.8064(7) 0.4257(7) 0.7947(3) 0.0512 1.0000 Uani D . C55 C 0.7902(9) 0.4162(11) 0.8445(4) 0.0771 1.0000 Uani D . C56 C 0.8691(7) 0.3621(9) 0.8706(4) 0.0628 1.0000 Uani D . C57 C 0.9659(7) 0.3128(7) 0.8468(3) 0.0506 1.0000 Uani D . C58 C 0.9799(8) 0.3170(7) 0.7966(3) 0.0527 1.0000 Uani D . C59 C 0.9011(8) 0.3727(7) 0.7716(3) 0.0589 1.0000 Uani D . C60 C 1.0532(6) 0.2567(6) 0.8775(3) 0.0455 1.0000 Uani D . N61 N 1.3797(8) 0.6930(7) 0.9959(4) 0.0799 1.0000 Uani D . N62 N 1.3944(8) 0.5655(9) 1.0486(3) 0.0779 1.0000 Uani D . C63 C 1.3571(9) 0.5933(8) 1.0067(3) 0.0679 1.0000 Uani D . C64 C 1.2823(7) 0.5078(6) 0.9721(3) 0.0576 1.0000 Uani D . C65 C 1.3041(7) 0.3911(6) 0.9641(3) 0.0504 1.0000 Uani D . C66 C 1.2301(7) 0.3128(7) 0.9336(3) 0.0468 1.0000 Uani D . C67 C 1.1364(6) 0.3485(6) 0.9082(3) 0.0444 1.0000 Uani D . C68 C 1.1169(8) 0.4657(6) 0.9149(3) 0.0511 1.0000 Uani D . C69 C 1.1908(8) 0.5440(8) 0.9456(3) 0.0622 1.0000 Uani D . N71 N 0.7917(8) 0.0475(8) 1.0554(3) 0.0715 1.0000 Uani D . N72 N 0.6834(11) -0.0255(14) 0.9856(4) 0.1376 1.0000 Uani D . C73 C 0.7720(8) 0.0342(9) 1.0066(3) 0.0671 1.0000 Uani D . C74 C 0.8474(7) 0.0901(8) 0.9748(3) 0.0562 1.0000 Uani D . C75 C 0.9421(8) 0.1538(9) 0.9953(3) 0.0679 1.0000 Uani D . C76 C 1.0077(8) 0.2087(8) 0.9648(3) 0.0573 1.0000 Uani D . C77 C 0.9854(7) 0.1956(7) 0.9133(3) 0.0484 1.0000 Uani D . C78 C 0.8913(7) 0.1271(8) 0.8943(3) 0.0597 1.0000 Uani D . C79 C 0.8234(8) 0.0717(9) 0.9238(3) 0.0609 1.0000 Uani D . N81 N 1.3850(9) -0.1470(7) 0.7584(4) 0.0819 1.0000 Uani D . N82 N 1.3474(8) -0.0546(7) 0.6937(3) 0.0678 1.0000 Uani D . C83 C 1.3366(8) -0.0641(7) 0.7407(3) 0.0584 1.0000 Uani D . C84 C 1.2626(7) 0.0159(6) 0.7748(3) 0.0525 1.0000 Uani D . C85 C 1.2791(8) 0.1340(6) 0.7819(3) 0.0552 1.0000 Uani D . C86 C 1.2132(7) 0.2074(7) 0.8161(3) 0.0463 1.0000 Uani D . C87 C 1.1261(6) 0.1674(6) 0.8424(3) 0.0442 1.0000 Uani D . C88 C 1.1103(8) 0.0497(6) 0.8343(3) 0.0559 1.0000 Uani D . C89 C 1.1781(8) -0.0256(8) 0.8016(3) 0.0668 1.0000 Uani D . N101 N 0.4832(6) 0.2874(7) 0.6234(2) 0.0577 1.0000 Uani D . O102 O 0.5896(6) 0.2873(6) 0.6210(3) 0.0673 1.0000 Uani D . O103 O 0.4195(6) 0.2776(6) 0.5852(2) 0.0627 1.0000 Uani D . O104 O 0.4356(7) 0.2919(7) 0.6657(2) 0.0762 1.0000 Uani D . N111 N 0.4501(6) 0.3916(6) 0.8293(2) 0.0529 1.0000 Uani D . O112 O 0.5142(6) 0.3327(6) 0.8512(2) 0.0703 1.0000 Uani D . O113 O 0.4391(6) 0.3631(5) 0.78213(19) 0.0509 1.0000 Uani D . O114 O 0.3970(7) 0.4728(6) 0.8541(2) 0.0734 1.0000 Uani D . N121 N 0.5265(7) 0.6513(6) 0.6728(2) 0.0558 1.0000 Uani D . O122 O 0.5694(8) 0.5626(7) 0.6489(3) 0.0903 1.0000 Uani D . O123 O 0.4727(5) 0.7164(5) 0.6503(2) 0.0539 1.0000 Uani D . O124 O 0.5432(8) 0.6773(6) 0.7195(2) 0.0815 1.0000 Uani D . N131 N 0.4644(7) 0.0997(7) 0.9120(3) 0.0612 1.0000 Uani D . O132 O 0.5581(8) 0.1221(13) 0.8966(4) 0.1390 1.0000 Uani D . O133 O 0.3937(8) 0.0331(7) 0.8867(3) 0.0858 1.0000 Uani D . O134 O 0.4469(7) 0.1493(7) 0.9558(3) 0.0805 1.0000 Uani D . N141 N 0.9889(9) 0.7420(8) 0.8722(3) 0.1555 1.0000 Uani D U O142 O 1.0912(10) 0.7570(9) 0.8694(3) 0.1548 1.0000 Uani D U O143 O 0.9455(10) 0.6475(8) 0.8511(3) 0.1462 1.0000 Uani D U O144 O 0.9317(12) 0.8195(9) 0.8974(3) 0.1908 1.0000 Uani D U N151 N 0.4855(6) 0.9155(5) 0.5704(2) 0.0470 1.0000 Uani D . O152 O 0.5407(6) 0.8543(5) 0.5360(3) 0.0652 1.0000 Uani D . O153 O 0.3977(6) 0.8730(6) 0.5854(2) 0.0651 1.0000 Uani D . O154 O 0.5171(6) 1.0153(5) 0.5890(2) 0.0610 1.0000 Uani D . N161 N 0.4555(8) 0.7729(7) 0.8822(3) 0.1210 1.0000 Uani D U O162 O 0.4953(9) 0.7641(6) 0.8396(3) 0.1130 1.0000 Uani D U O163 O 0.5188(10) 0.8043(7) 0.9204(3) 0.1345 1.0000 Uani D U O164 O 0.3544(9) 0.7496(7) 0.8878(4) 0.1488 1.0000 Uani D U N171 N 0.8751(7) 0.2692(5) 0.6333(2) 0.0467 1.0000 Uani D . O172 O 0.9126(9) 0.2273(7) 0.5918(3) 0.0956 1.0000 Uani D . O173 O 0.8197(10) 0.2076(9) 0.6565(4) 0.1175 1.0000 Uani D . O174 O 0.9038(11) 0.3682(6) 0.6543(3) 0.1091 1.0000 Uani D . O201 O 0.2564(6) 0.4376(6) 0.6126(3) 0.0675 1.0000 Uani D . C202 C 0.1393(9) 0.4131(12) 0.5945(5) 0.0952 1.0000 Uani D . O211 O 0.2574(8) 0.1334(7) 0.6521(3) 0.0826 1.0000 Uani D . C212 C 0.1591(10) 0.1969(11) 0.6743(5) 0.0823 1.0000 Uani D . O221 O 0.6859(9) 0.9156(7) 0.8268(3) 0.0976 1.0000 Uani D . C222 C 0.7629(13) 0.8340(10) 0.7995(5) 0.1004 1.0000 Uani D . O231 O 0.6694(15) 0.6408(9) 0.9096(4) 0.1623 1.0000 Uani . . H51 H 0.6687 0.6412 0.4923 0.0554 1.0000 Uiso R . H61 H 0.7805 0.7784 0.5445 0.0483 1.0000 Uiso R . H81 H 0.8898 0.5495 0.6220 0.0542 1.0000 Uiso R . H91 H 0.7782 0.4088 0.5715 0.0588 1.0000 Uiso R . H151 H 0.9984 0.6121 0.7583 0.0580 1.0000 Uiso R . H161 H 0.8805 0.6945 0.7050 0.0540 1.0000 Uiso R . H181 H 1.1558 0.7565 0.6285 0.0570 1.0000 Uiso R . H191 H 1.2713 0.6684 0.6780 0.0626 1.0000 Uiso R . H251 H 1.0770 1.0799 0.5648 0.0608 1.0000 Uiso R . H261 H 0.9541 1.0013 0.6137 0.0542 1.0000 Uiso R . H281 H 1.0407 0.6865 0.5435 0.0503 1.0000 Uiso R . H291 H 1.1710 0.7620 0.4962 0.0548 1.0000 Uiso R . H351 H 0.8727 1.0826 0.7542 0.0558 1.0000 Uiso R . H361 H 0.9794 0.9453 0.7018 0.0567 1.0000 Uiso R . H381 H 0.6895 0.8220 0.6254 0.0579 1.0000 Uiso R . H391 H 0.5891 0.9651 0.6745 0.0598 1.0000 Uiso R . H551 H 0.7264 0.4495 0.8615 0.0888 1.0000 Uiso R . H561 H 0.8566 0.3579 0.9040 0.0821 1.0000 Uiso R . H581 H 1.0422 0.2804 0.7792 0.0640 1.0000 Uiso R . H591 H 0.9136 0.3754 0.7379 0.0691 1.0000 Uiso R . H651 H 1.3670 0.3646 0.9802 0.0641 1.0000 Uiso R . H661 H 1.2454 0.2349 0.9281 0.0582 1.0000 Uiso R . H681 H 1.0545 0.4922 0.8984 0.0631 1.0000 Uiso R . H691 H 1.1781 0.6220 0.9486 0.0752 1.0000 Uiso R . H751 H 0.9624 0.1622 1.0295 0.0818 1.0000 Uiso R . H761 H 1.0697 0.2547 0.9790 0.0691 1.0000 Uiso R . H781 H 0.8720 0.1172 0.8601 0.0791 1.0000 Uiso R . H791 H 0.7630 0.0224 0.9094 0.0741 1.0000 Uiso R . H851 H 1.3351 0.1646 0.7638 0.0678 1.0000 Uiso R . H861 H 1.2262 0.2862 0.8209 0.0562 1.0000 Uiso R . H881 H 1.0529 0.0198 0.8513 0.0670 1.0000 Uiso R . H891 H 1.1676 -0.1043 0.7976 0.0739 1.0000 Uiso R . H2221 H 0.8298 0.8741 0.7928 0.1209 1.0000 Uiso R . H2222 H 0.7836 0.7779 0.8184 0.1209 1.0000 Uiso R . H2223 H 0.7268 0.7972 0.7684 0.1209 1.0000 Uiso R . H2021 H 0.1142 0.4765 0.5810 0.1082 1.0000 Uiso R . H2022 H 0.0913 0.4038 0.6215 0.1082 1.0000 Uiso R . H2023 H 0.1357 0.3453 0.5687 0.1082 1.0000 Uiso R . H2121 H 0.0950 0.1456 0.6704 0.1039 1.0000 Uiso R . H2122 H 0.1753 0.2253 0.7094 0.1039 1.0000 Uiso R . H2123 H 0.1422 0.2593 0.6585 0.1039 1.0000 Uiso R . H311 H 0.5585 1.2534 0.7447 0.0700 1.0000 Uiso R . H312 H 0.5724 1.1861 0.6995 0.0700 1.0000 Uiso R . H321 H 0.6055 1.1841 0.8175 0.0858 1.0000 Uiso R . H322 H 0.6553 1.0672 0.8090 0.0858 1.0000 Uiso R . H211 H 1.3699 1.0733 0.5241 0.0714 1.0000 Uiso R . H212 H 1.2739 1.1010 0.5576 0.0714 1.0000 Uiso R . H221 H 1.3106 0.9677 0.4395 0.0785 1.0000 Uiso R . H222 H 1.2240 0.8743 0.4396 0.0785 1.0000 Uiso R . H111 H 1.2571 0.5419 0.8182 0.0813 1.0000 Uiso R . H112 H 1.1773 0.6352 0.8182 0.0813 1.0000 Uiso R . H121 H 1.3543 0.4747 0.7432 0.0730 1.0000 Uiso R . H122 H 1.2842 0.4672 0.6957 0.0730 1.0000 Uiso R . H11 H 0.6629 0.4631 0.4318 0.0648 1.0000 Uiso R . H12 H 0.6239 0.3536 0.4234 0.0648 1.0000 Uiso R . H21 H 0.6174 0.3301 0.5436 0.0691 1.0000 Uiso R . H22 H 0.5667 0.2739 0.4949 0.0691 1.0000 Uiso R . H621 H 1.3962 0.6168 1.0762 0.0957 1.0000 Uiso R . H622 H 1.3642 0.5073 1.0583 0.0957 1.0000 Uiso R . H611 H 1.4346 0.7347 1.0120 0.0930 1.0000 Uiso R . H612 H 1.3612 0.7043 0.9660 0.0930 1.0000 Uiso R . H811 H 1.3720 -0.1525 0.7913 0.0949 1.0000 Uiso R . H812 H 1.4182 -0.2015 0.7382 0.0949 1.0000 Uiso R . H821 H 1.2995 -0.0146 0.6803 0.0815 1.0000 Uiso R . H822 H 1.4008 -0.0924 0.6756 0.0815 1.0000 Uiso R . H711 H 0.8441 0.0943 1.0711 0.0904 1.0000 Uiso R . H712 H 0.7510 0.0947 1.0762 0.0904 1.0000 Uiso R . H721 H 0.6285 -0.0447 1.0089 0.1641 1.0000 Uiso R . H722 H 0.6523 -0.0129 0.9580 0.1641 1.0000 Uiso R . H521 H 0.6965 0.5131 0.7026 0.0923 1.0000 Uiso R . H522 H 0.7650 0.4128 0.7019 0.0923 1.0000 Uiso R . H511 H 0.6583 0.5814 0.8261 0.0833 1.0000 Uiso R . H512 H 0.5930 0.5834 0.7780 0.0833 1.0000 Uiso R . H2311 H 0.6212 0.6947 0.9129 0.1966 1.0000 Uiso R . H2312 H 0.7337 0.6424 0.8955 0.1966 1.0000 Uiso R . H2011 H 0.3074 0.3873 0.6040 0.0811 1.0000 Uiso R . H2111 H 0.3123 0.1823 0.6563 0.0981 1.0000 Uiso R . H2211 H 0.6287 0.8704 0.8305 0.1179 1.0000 Uiso R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.071(5) 0.042(4) 0.053(5) 0.000(3) -0.014(4) -0.003(4) N2 0.070(5) 0.040(4) 0.062(5) 0.008(4) -0.010(4) -0.015(4) C3 0.050(5) 0.038(4) 0.048(5) 0.009(4) 0.001(4) 0.001(4) C4 0.050(5) 0.034(4) 0.037(4) 0.007(3) -0.003(4) 0.003(4) C5 0.054(5) 0.035(4) 0.038(4) 0.016(3) -0.004(4) 0.000(4) C6 0.051(5) 0.029(4) 0.041(4) 0.015(3) -0.005(4) 0.008(4) C7 0.049(5) 0.033(4) 0.040(4) 0.009(3) 0.005(4) 0.001(4) C8 0.056(5) 0.038(4) 0.046(5) 0.017(4) -0.005(4) 0.007(4) C9 0.056(5) 0.028(4) 0.055(5) 0.013(4) -0.013(4) 0.004(4) C10 0.047(5) 0.030(4) 0.040(4) 0.019(3) -0.004(3) 0.005(3) N11 0.084(6) 0.067(5) 0.059(5) 0.030(4) -0.009(4) 0.023(5) N12 0.072(6) 0.049(4) 0.056(5) 0.010(4) -0.007(4) 0.021(4) C13 0.070(6) 0.048(5) 0.042(5) 0.008(4) -0.011(4) 0.004(5) C14 0.068(6) 0.033(4) 0.046(5) 0.011(4) -0.011(4) 0.001(4) C15 0.054(6) 0.044(5) 0.052(5) 0.012(4) 0.001(4) 0.001(4) C16 0.050(5) 0.037(4) 0.054(5) 0.027(4) -0.006(4) 0.002(4) C17 0.042(5) 0.033(4) 0.040(4) 0.006(3) -0.008(3) 0.010(3) C18 0.062(6) 0.033(4) 0.046(5) 0.016(4) -0.004(4) -0.002(4) C19 0.050(5) 0.045(5) 0.045(5) 0.009(4) -0.004(4) 0.005(4) N21 0.054(5) 0.054(5) 0.074(5) 0.023(4) -0.003(4) -0.004(4) N22 0.072(6) 0.062(5) 0.059(5) 0.026(4) 0.004(4) 0.001(4) C23 0.056(6) 0.049(5) 0.057(6) 0.026(4) -0.007(4) 0.008(4) C24 0.048(5) 0.041(5) 0.050(5) 0.021(4) -0.003(4) -0.002(4) C25 0.072(6) 0.033(4) 0.053(5) 0.016(4) 0.003(5) -0.009(4) C26 0.060(5) 0.032(4) 0.049(5) 0.013(4) 0.002(4) 0.005(4) C27 0.046(5) 0.030(4) 0.045(4) 0.018(3) -0.008(4) 0.003(3) C28 0.062(6) 0.029(4) 0.046(5) 0.014(4) -0.004(4) -0.003(4) C29 0.056(5) 0.045(5) 0.042(5) 0.011(4) -0.005(4) 0.010(4) N31 0.072(5) 0.054(5) 0.049(4) 0.010(4) 0.005(4) 0.024(4) N32 0.090(7) 0.070(5) 0.049(5) 0.016(4) 0.021(4) 0.031(5) C33 0.049(5) 0.040(4) 0.056(5) 0.021(4) 0.000(4) 0.000(4) C34 0.057(5) 0.030(4) 0.039(4) 0.016(3) 0.001(4) 0.002(4) C35 0.066(6) 0.032(4) 0.044(5) 0.008(4) -0.003(4) -0.002(4) C36 0.054(5) 0.038(4) 0.051(5) 0.021(4) -0.003(4) 0.001(4) C37 0.048(5) 0.033(4) 0.036(4) 0.016(3) -0.003(3) 0.002(4) C38 0.064(6) 0.041(5) 0.043(5) 0.009(4) -0.007(4) -0.004(4) C39 0.041(5) 0.058(5) 0.048(5) 0.017(4) 0.004(4) 0.009(4) N51 0.066(5) 0.053(5) 0.077(6) 0.032(4) -0.004(4) 0.007(4) N52 0.089(7) 0.075(6) 0.080(7) 0.045(5) -0.010(5) -0.009(5) C53 0.062(6) 0.055(6) 0.066(6) 0.038(5) -0.018(5) -0.017(5) C54 0.046(5) 0.049(5) 0.065(6) 0.028(4) -0.008(4) 0.000(4) C55 0.054(6) 0.103(9) 0.090(8) 0.058(7) 0.007(6) 0.022(6) C56 0.046(5) 0.092(8) 0.063(6) 0.045(6) 0.005(4) 0.019(5) C57 0.058(6) 0.046(5) 0.052(5) 0.022(4) -0.015(4) -0.005(4) C58 0.062(6) 0.044(5) 0.049(5) 0.003(4) -0.004(4) 0.003(4) C59 0.090(8) 0.045(5) 0.049(5) 0.027(4) -0.010(5) -0.013(5) C60 0.051(5) 0.046(5) 0.043(4) 0.017(4) -0.006(4) 0.008(4) N61 0.076(6) 0.064(6) 0.089(7) -0.006(5) -0.010(5) -0.010(5) N62 0.081(6) 0.096(7) 0.048(5) -0.003(5) -0.017(4) 0.000(5) C63 0.067(7) 0.072(7) 0.054(6) -0.009(5) -0.005(5) 0.009(6) C64 0.058(6) 0.058(6) 0.049(5) -0.006(4) -0.002(4) 0.011(5) C65 0.044(5) 0.060(6) 0.049(5) 0.016(4) -0.003(4) 0.006(4) C66 0.055(5) 0.041(5) 0.045(5) 0.011(4) -0.001(4) 0.006(4) C67 0.048(5) 0.045(5) 0.042(4) 0.013(4) 0.005(4) 0.002(4) C68 0.059(6) 0.048(5) 0.046(5) 0.007(4) -0.008(4) 0.010(4) C69 0.082(7) 0.047(5) 0.054(6) 0.005(4) -0.003(5) 0.006(5) N71 0.091(7) 0.072(6) 0.056(5) 0.026(4) 0.011(5) -0.007(5) N72 0.114(10) 0.216(16) 0.086(8) 0.045(9) -0.012(7) -0.093(11) C73 0.063(7) 0.069(7) 0.075(7) 0.025(6) 0.022(5) 0.001(5) C74 0.046(5) 0.064(6) 0.061(6) 0.019(5) 0.014(4) 0.006(5) C75 0.086(8) 0.080(7) 0.041(5) 0.021(5) 0.001(5) -0.012(6) C76 0.051(5) 0.067(6) 0.052(5) 0.008(5) 0.006(4) -0.005(5) C77 0.058(6) 0.050(5) 0.039(4) 0.015(4) -0.001(4) 0.005(4) C78 0.058(6) 0.074(7) 0.055(6) 0.033(5) -0.004(5) -0.004(5) C79 0.055(6) 0.068(6) 0.069(6) 0.036(5) -0.002(5) -0.010(5) N81 0.089(7) 0.069(6) 0.075(6) -0.013(5) -0.007(5) 0.026(5) N82 0.077(6) 0.059(5) 0.061(5) -0.004(4) 0.002(4) 0.006(4) C83 0.068(7) 0.048(5) 0.057(6) 0.007(4) 0.001(5) -0.012(5) C84 0.062(6) 0.039(5) 0.055(5) 0.009(4) -0.006(4) -0.003(4) C85 0.058(6) 0.047(5) 0.059(6) 0.009(4) -0.012(5) 0.002(4) C86 0.052(5) 0.044(5) 0.044(5) 0.011(4) 0.004(4) -0.006(4) C87 0.047(5) 0.046(5) 0.040(4) 0.014(4) -0.008(4) -0.006(4) C88 0.064(6) 0.058(6) 0.047(5) 0.014(4) -0.001(4) -0.003(5) C89 0.094(8) 0.042(5) 0.057(6) -0.004(4) -0.016(6) 0.000(5) N101 0.073(6) 0.052(5) 0.049(5) 0.013(4) -0.005(4) 0.003(4) O102 0.061(5) 0.072(5) 0.067(4) 0.011(4) -0.001(3) 0.001(4) O103 0.085(5) 0.060(4) 0.043(4) 0.011(3) -0.009(3) 0.004(4) O104 0.095(6) 0.089(5) 0.044(4) 0.013(4) -0.002(4) 0.007(4) N111 0.055(5) 0.051(4) 0.050(5) 0.005(4) -0.004(4) 0.010(4) O112 0.076(5) 0.080(5) 0.053(4) 0.010(3) -0.013(3) 0.035(4) O113 0.069(4) 0.052(3) 0.032(3) 0.010(3) -0.004(3) 0.013(3) O114 0.093(6) 0.079(5) 0.045(4) 0.003(3) 0.000(4) 0.042(4) N121 0.071(5) 0.041(4) 0.054(5) 0.007(4) 0.002(4) 0.011(4) O122 0.123(7) 0.086(6) 0.064(5) 0.018(4) 0.007(5) 0.040(5) O123 0.058(4) 0.050(3) 0.056(4) 0.016(3) -0.012(3) 0.013(3) O124 0.129(7) 0.067(5) 0.047(4) 0.009(3) -0.015(4) 0.043(5) N131 0.064(6) 0.062(5) 0.060(5) 0.020(4) -0.005(4) -0.001(4) O132 0.085(7) 0.260(15) 0.080(6) 0.056(8) 0.005(5) -0.059(8) O133 0.113(7) 0.080(5) 0.067(5) 0.022(4) 0.005(5) -0.021(5) O134 0.074(5) 0.088(6) 0.075(5) 0.006(4) 0.012(4) -0.017(4) N141 0.193(9) 0.142(7) 0.105(6) -0.035(5) -0.041(7) 0.054(6) O142 0.201(9) 0.126(7) 0.117(7) -0.020(6) -0.035(8) 0.035(7) O143 0.184(9) 0.134(7) 0.106(7) -0.009(5) -0.023(7) 0.040(6) O144 0.219(10) 0.184(8) 0.129(8) -0.061(6) -0.061(7) 0.089(8) N151 0.058(5) 0.044(4) 0.042(4) 0.015(3) -0.002(3) -0.002(4) O152 0.079(5) 0.043(4) 0.069(4) 0.000(3) 0.009(4) -0.004(3) O153 0.082(5) 0.065(4) 0.050(4) 0.016(3) 0.009(3) -0.011(4) O154 0.073(5) 0.047(4) 0.060(4) 0.004(3) -0.003(3) 0.000(3) N161 0.154(7) 0.110(6) 0.089(4) -0.006(5) 0.013(4) 0.001(6) O162 0.157(7) 0.100(6) 0.081(4) 0.017(5) 0.000(5) 0.013(6) O163 0.183(8) 0.133(7) 0.082(4) 0.010(6) 0.002(5) 0.007(7) O164 0.164(7) 0.114(7) 0.146(7) -0.028(6) 0.035(5) -0.011(7) N171 0.082(5) 0.031(4) 0.029(4) 0.011(3) 0.005(3) 0.010(4) O172 0.143(8) 0.062(5) 0.079(6) 0.010(4) -0.007(5) 0.015(5) O173 0.129(9) 0.129(8) 0.101(7) 0.037(6) 0.014(6) -0.019(7) O174 0.199(11) 0.068(6) 0.064(5) 0.025(4) 0.007(6) -0.001(6) O201 0.082(5) 0.058(4) 0.061(4) 0.009(3) -0.005(4) 0.017(4) C202 0.088(10) 0.096(10) 0.101(10) 0.019(8) 0.007(8) -0.015(8) O211 0.104(6) 0.076(5) 0.071(5) 0.024(4) 0.010(4) -0.012(5) C212 0.087(9) 0.092(9) 0.075(8) 0.035(7) 0.010(7) -0.002(7) O221 0.151(9) 0.069(5) 0.081(6) 0.034(4) 0.000(6) 0.009(6) C222 0.158(14) 0.059(7) 0.092(9) 0.034(7) 0.012(9) -0.009(8) O231 0.294(18) 0.116(8) 0.089(7) 0.049(6) -0.028(9) 0.064(10) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 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_publ_flag C3 N1 H11 120.3 no C3 N1 H12 122.1 no H11 N1 H12 104.0 no C3 N2 H21 118.3 no C3 N2 H22 121.3 no H21 N2 H22 115.0 no N2 C3 N1 120.1(7) yes N2 C3 C4 119.5(6) yes N1 C3 C4 120.4(6) yes C3 C4 C5 122.2(6) yes C3 C4 C9 119.4(6) yes C5 C4 C9 118.4(6) yes C4 C5 C6 119.5(6) yes C4 C5 H51 120.0 no C6 C5 H51 120.5 no C5 C6 C7 123.1(6) yes C5 C6 H61 118.1 no C7 C6 H61 118.7 no C6 C7 C8 115.9(6) yes C6 C7 C10 119.6(5) yes C8 C7 C10 124.5(6) yes C7 C8 C9 122.5(7) yes C7 C8 H81 118.6 no C9 C8 H81 118.9 no C4 C9 C8 120.5(6) yes C4 C9 H91 119.6 no C8 C9 H91 119.8 no C7 C10 C17 110.6(5) yes C7 C10 C27 106.5(5) yes C17 C10 C27 109.1(5) yes C7 C10 C37 112.0(6) yes C17 C10 C37 107.1(5) yes C27 C10 C37 111.5(5) yes C13 N11 H111 120.9 no C13 N11 H112 119.2 no H111 N11 H112 116.1 no C13 N12 H121 120.5 no C13 N12 H122 118.8 no H121 N12 H122 120.0 no N11 C13 N12 120.5(7) yes N11 C13 C14 121.6(7) yes N12 C13 C14 117.8(7) yes C13 C14 C15 122.0(7) yes C13 C14 C19 117.6(7) yes C15 C14 C19 120.5(7) yes C14 C15 C16 119.1(7) yes C14 C15 H151 120.1 no C16 C15 H151 120.8 no C15 C16 C17 122.1(7) yes C15 C16 H161 119.8 no C17 C16 H161 118.1 no C10 C17 C16 118.8(6) yes C10 C17 C18 124.3(6) yes C16 C17 C18 116.9(6) yes C17 C18 C19 122.1(7) yes C17 C18 H181 120.2 no C19 C18 H181 117.7 no C14 C19 C18 119.1(7) yes C14 C19 H191 120.9 no C18 C19 H191 120.0 no C23 N21 H211 121.5 no C23 N21 H212 118.9 no H211 N21 H212 115.1 no C23 N22 H221 120.5 no C23 N22 H222 119.7 no H221 N22 H222 118.8 no N21 C23 N22 120.4(8) yes N21 C23 C24 118.8(7) yes N22 C23 C24 120.7(7) yes C23 C24 C25 119.8(6) yes C23 C24 C29 120.5(7) yes C25 C24 C29 119.6(7) yes C24 C25 C26 119.3(7) yes C24 C25 H251 121.8 no C26 C25 H251 119.0 no C25 C26 C27 121.8(7) yes C25 C26 H261 119.0 no C27 C26 H261 119.2 no C10 C27 C26 123.2(6) yes C10 C27 C28 119.8(5) yes C26 C27 C28 116.9(6) yes C27 C28 C29 122.3(7) yes C27 C28 H281 118.6 no C29 C28 H281 119.0 no C24 C29 C28 119.4(7) yes C24 C29 H291 120.6 no C28 C29 H291 120.0 no C33 N31 H311 118.8 no C33 N31 H312 118.5 no H311 N31 H312 100.2 no C33 N32 H321 120.1 no C33 N32 H322 120.3 no H321 N32 H322 119.6 no N32 C33 N31 123.0(7) yes N32 C33 C34 118.6(6) yes N31 C33 C34 118.4(6) yes C33 C34 C35 121.8(6) yes C33 C34 C39 118.8(7) yes C35 C34 C39 119.4(7) yes C34 C35 C36 120.6(7) yes C34 C35 H351 119.1 no C36 C35 H351 120.3 no C35 C36 C37 120.0(7) yes C35 C36 H361 119.7 no C37 C36 H361 120.2 no C10 C37 C36 118.2(6) yes C10 C37 C38 122.9(6) yes C36 C37 C38 118.9(7) yes C37 C38 C39 120.3(7) yes C37 C38 H381 120.6 no C39 C38 H381 119.1 no C34 C39 C38 120.8(7) yes C34 C39 H391 120.0 no C38 C39 H391 119.2 no C53 N51 H511 121.1 no C53 N51 H512 119.8 no H511 N51 H512 119.0 no C53 N52 H521 119.1 no C53 N52 H522 121.0 no H521 N52 H522 115.2 no N52 C53 N51 121.8(8) yes N52 C53 C54 117.7(8) yes N51 C53 C54 120.4(7) yes C53 C54 C55 120.2(7) yes C53 C54 C59 123.2(7) yes C55 C54 C59 116.4(7) yes C54 C55 C56 121.8(9) yes C54 C55 H551 119.5 no C56 C55 H551 118.6 no C55 C56 C57 120.5(8) yes C55 C56 H561 120.0 no C57 C56 H561 119.5 no C56 C57 C58 118.1(7) yes C56 C57 C60 119.0(6) yes C58 C57 C60 122.9(7) yes C57 C58 C59 120.5(8) yes C57 C58 H581 119.7 no C59 C58 H581 119.8 no C58 C59 C54 122.6(8) yes C58 C59 H591 118.5 no C54 C59 H591 118.9 no C57 C60 C67 110.5(6) yes C57 C60 C77 107.8(6) yes C67 C60 C77 110.6(6) yes C57 C60 C87 111.5(6) yes C67 C60 C87 107.5(6) yes C77 C60 C87 109.0(6) yes C63 N61 H611 119.1 no C63 N61 H612 119.1 no H611 N61 H612 117.1 no C63 N62 H621 119.0 no C63 N62 H622 119.6 no H621 N62 H622 102.1 no N62 C63 N61 122.4(9) yes N62 C63 C64 117.3(8) yes N61 C63 C64 120.3(8) yes C63 C64 C65 121.1(7) yes C63 C64 C69 120.5(7) yes C65 C64 C69 118.4(7) yes C64 C65 C66 120.0(7) yes C64 C65 H651 120.3 no C66 C65 H651 119.7 no C65 C66 C67 121.6(7) yes C65 C66 H661 119.7 no C67 C66 H661 118.6 no C60 C67 C66 118.9(6) yes C60 C67 C68 122.7(6) yes C66 C67 C68 118.3(7) yes C67 C68 C69 120.1(7) yes C67 C68 H681 120.2 no C69 C68 H681 119.7 no C64 C69 C68 121.4(8) yes C64 C69 H691 119.7 no C68 C69 H691 118.9 no C73 N71 H711 122.0 no C73 N71 H712 119.5 no H711 N71 H712 79.0 no C73 N72 H721 115.1 no C73 N72 H722 121.0 no H721 N72 H722 113.2 no N71 C73 N72 120.0(9) yes N71 C73 C74 121.0(8) yes N72 C73 C74 119.0(9) yes C73 C74 C75 121.0(7) yes C73 C74 C79 118.3(7) yes C75 C74 C79 120.7(7) yes C74 C75 C76 119.3(8) yes C74 C75 H751 121.3 no C76 C75 H751 119.4 no C75 C76 C77 122.3(8) yes C75 C76 H761 119.5 no C77 C76 H761 118.2 no C60 C77 C76 124.8(7) yes C60 C77 C78 119.3(6) yes C76 C77 C78 115.8(7) yes C77 C78 C79 123.4(8) yes C77 C78 H781 118.9 no C79 C78 H781 117.7 no C78 C79 C74 118.3(8) yes C78 C79 H791 121.3 no C74 C79 H791 120.4 no C83 N81 H811 118.9 no C83 N81 H812 120.0 no H811 N81 H812 120.3 no C83 N82 H821 120.2 no C83 N82 H822 119.4 no H821 N82 H822 120.3 no N81 C83 N82 121.9(9) yes N81 C83 C84 118.1(8) yes N82 C83 C84 119.9(8) yes C83 C84 C85 120.8(7) yes C83 C84 C89 120.5(7) yes C85 C84 C89 118.7(8) yes C84 C85 C86 120.0(8) yes C84 C85 H851 120.5 no C86 C85 H851 119.5 no C85 C86 C87 122.1(8) yes C85 C86 H861 119.1 no C87 C86 H861 118.7 no C60 C87 C86 118.1(6) yes C60 C87 C88 125.1(6) yes C86 C87 C88 116.8(7) yes C87 C88 C89 122.0(8) yes C87 C88 H881 119.2 no C89 C88 H881 118.8 no C88 C89 C84 120.3(8) yes C88 C89 H891 120.5 no C84 C89 H891 119.1 no O102 N101 O103 122.6(7) yes O102 N101 O104 120.0(7) yes O103 N101 O104 117.3(7) yes O112 N111 O113 117.8(6) yes O112 N111 O114 120.5(7) yes O113 N111 O114 121.7(6) yes O122 N121 O123 120.6(7) yes O122 N121 O124 118.6(7) yes O123 N121 O124 120.7(7) yes O132 N131 O133 124.0(9) yes O132 N131 O134 113.7(9) yes O133 N131 O134 122.3(8) yes O142 N141 O143 118.9(7) yes O142 N141 O144 118.8(7) yes O143 N141 O144 122.2(7) yes O152 N151 O153 118.0(7) yes O152 N151 O154 120.9(7) yes O153 N151 O154 121.1(7) yes O162 N161 O163 119.7(7) yes O162 N161 O164 121.1(7) yes O163 N161 O164 119.2(7) yes O172 N171 O173 119.4(8) yes O172 N171 O174 119.6(8) yes O173 N171 O174 120.4(8) yes C202 O201 H2011 119.8 no O201 C202 H2021 107.4 no O201 C202 H2022 110.8 no H2021 C202 H2022 109.5 no O201 C202 H2023 110.2 no H2021 C202 H2023 109.5 no H2022 C202 H2023 109.5 no C212 O211 H2111 105.1 no O211 C212 H2121 108.2 no O211 C212 H2122 108.5 no H2121 C212 H2122 109.5 no O211 C212 H2123 111.7 no H2121 C212 H2123 109.5 no H2122 C212 H2123 109.5 no C222 O221 H2211 100.5 no O221 C222 H2221 108.4 no O221 C222 H2222 111.3 no H2221 C222 H2222 109.5 no O221 C222 H2223 108.7 no H2221 C222 H2223 109.5 no H2222 C222 H2223 109.5 no H2311 O231 H2312 124.1 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag N1 C3 1.305(7) yes N1 H11 0.856 no N1 H12 0.854 no N2 C3 1.310(7) yes N2 H21 0.860 no N2 H22 0.865 no C3 C4 1.484(7) yes C4 C5 1.391(7) yes C4 C9 1.394(7) yes C5 C6 1.382(7) yes C5 H51 0.940 no C6 C7 1.398(7) yes C6 H61 0.926 no C7 C8 1.381(7) yes C7 C10 1.546(7) yes C8 C9 1.383(7) yes C8 H81 0.925 no C9 H91 0.942 no C10 C17 1.548(7) yes C10 C27 1.548(7) yes C10 C37 1.535(7) yes N11 C13 1.317(8) yes N11 H111 0.858 no N11 H112 0.858 no N12 C13 1.306(8) yes N12 H121 0.859 no N12 H122 0.864 no C13 C14 1.487(7) yes C14 C15 1.380(8) yes C14 C19 1.393(8) yes C15 C16 1.399(8) yes C15 H151 0.919 no C16 C17 1.395(7) yes C16 H161 0.936 no C17 C18 1.395(8) yes C18 C19 1.393(7) yes C18 H181 0.923 no C19 H191 0.934 no N21 C23 1.314(7) yes N21 H211 0.862 no N21 H212 0.858 no N22 C23 1.307(7) yes N22 H221 0.872 no N22 H222 0.864 no C23 C24 1.475(8) yes C24 C25 1.388(8) yes C24 C29 1.387(7) yes C25 C26 1.388(8) yes C25 H251 0.927 no C26 C27 1.391(7) yes C26 H261 0.928 no C27 C28 1.385(7) yes C28 C29 1.376(8) yes C28 H281 0.934 no C29 H291 0.931 no N31 C33 1.294(7) yes N31 H311 0.858 no N31 H312 0.871 no N32 C33 1.307(7) yes N32 H321 0.861 no N32 H322 0.861 no C33 C34 1.486(7) yes C34 C35 1.374(8) yes C34 C39 1.378(8) yes C35 C36 1.385(8) yes C35 H351 0.934 no C36 C37 1.392(7) yes C36 H361 0.933 no C37 C38 1.390(8) yes C38 C39 1.374(8) yes C38 H381 0.929 no C39 H391 0.929 no N51 C53 1.305(8) yes N51 H511 0.869 no N51 H512 0.867 no N52 C53 1.308(8) yes N52 H521 0.857 no N52 H522 0.851 no C53 C54 1.492(8) yes C54 C55 1.386(8) yes C54 C59 1.375(8) yes C55 C56 1.391(8) yes C55 H551 0.931 no C56 C57 1.385(8) yes C56 H561 0.927 no C57 C58 1.378(8) yes C57 C60 1.541(7) yes C58 C59 1.385(8) yes C58 H581 0.936 no C59 H591 0.928 no C60 C67 1.546(7) yes C60 C77 1.548(7) yes C60 C87 1.543(8) yes N61 C63 1.305(8) yes N61 H611 0.859 no N61 H612 0.866 no N62 C63 1.310(8) yes N62 H621 0.858 no N62 H622 0.862 no C63 C64 1.490(8) yes C64 C65 1.388(8) yes C64 C69 1.394(8) yes C65 C66 1.387(8) yes C65 H651 0.937 no C66 C67 1.396(7) yes C66 H661 0.928 no C67 C68 1.390(7) yes C68 C69 1.388(8) yes C68 H681 0.938 no C69 H691 0.929 no N71 C73 1.306(8) yes N71 H711 0.864 no N71 H712 0.861 no N72 C73 1.299(8) yes N72 H721 0.964 no N72 H722 0.863 no C73 C74 1.487(8) yes C74 C75 1.374(8) yes C74 C79 1.368(8) yes C75 C76 1.388(8) yes C75 H751 0.932 no C76 C77 1.385(8) yes C76 H761 0.929 no C77 C78 1.384(8) yes C78 C79 1.389(8) yes C78 H781 0.928 no C79 H791 0.936 no N81 C83 1.310(8) yes N81 H811 0.918 no N81 H812 0.858 no N82 C83 1.303(8) yes N82 H821 0.860 no N82 H822 0.871 no C83 C84 1.479(8) yes C84 C85 1.388(8) yes C84 C89 1.381(8) yes C85 C86 1.383(8) yes C85 H851 0.936 no C86 C87 1.386(7) yes C86 H861 0.930 no C87 C88 1.382(8) yes C88 C89 1.386(8) yes C88 H881 0.928 no C89 H891 0.927 no N101 O102 1.245(7) yes N101 O103 1.241(7) yes N101 O104 1.272(7) yes N111 O112 1.251(7) yes N111 O113 1.250(7) yes N111 O114 1.235(7) yes N121 O122 1.234(7) yes N121 O123 1.246(7) yes N121 O124 1.244(7) yes N131 O132 1.224(8) yes N131 O133 1.229(7) yes N131 O134 1.227(7) yes N141 O142 1.212(9) yes N141 O143 1.246(8) yes N141 O144 1.237(8) yes N151 O152 1.248(7) yes N151 O153 1.248(7) yes N151 O154 1.237(7) yes N161 O162 1.235(8) yes N161 O163 1.245(8) yes N161 O164 1.227(8) yes N171 O172 1.219(7) yes N171 O173 1.241(8) yes N171 O174 1.235(7) yes O201 C202 1.447(8) yes O201 H2011 0.850 no C202 H2021 0.950 no C202 H2022 0.950 no C202 H2023 0.950 no O211 C212 1.452(8) yes O211 H2111 0.850 no C212 H2121 0.950 no C212 H2122 0.950 no C212 H2123 0.950 no O221 C222 1.430(9) yes O221 H2211 0.872 no C222 H2221 0.950 no C222 H2222 0.950 no C222 H2223 0.950 no O231 H2311 0.850 no O231 H2312 0.850 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C8 H81 C16 . 124.1(2) 0.925 2.495 3.109(12) yes C8 H81 O174 . 131.5(3) 0.925 2.494 3.183(12) yes C15 H151 O143 . 150.4(3) 0.919 2.539 3.369(12) yes C18 H181 C28 . 120.9(2) 0.923 2.472 3.050(12) yes C19 H191 O123 1_655 160.55(19) 0.934 2.575 3.470(12) yes C26 H261 C36 . 120.3(2) 0.928 2.532 3.106(12) yes C38 H381 C6 . 124.7(2) 0.929 2.478 3.102(12) yes C55 H551 O231 . 138.0(5) 0.931 2.480 3.233(12) yes C58 H581 C86 . 127.1(2) 0.936 2.459 3.114(12) yes C59 H591 O174 . 167.4(4) 0.928 2.238 3.150(12) yes C75 H751 O144 2_767 161.8(4) 0.932 2.275 3.173(12) yes C76 H761 C66 . 126.4(3) 0.929 2.427 3.070(12) yes C79 H791 O221 1_545 141.7(3) 0.936 2.470 3.256(12) yes C85 H851 O113 1_655 131.1(2) 0.936 2.593 3.285(12) yes C88 H881 C78 . 125.9(3) 0.928 2.462 3.099(12) yes C202 H2022 O174 1_455 151.4(4) 0.950 2.443 3.309(12) yes N31 H311 O113 1_565 179.1(2) 0.858 2.054 2.911(12) yes N31 H312 O104 1_565 125.5(3) 0.871 2.329 2.922(12) yes N32 H321 O112 1_565 167.0(3) 0.861 2.121 2.966(12) yes N32 H322 O221 . 171.4(4) 0.861 1.995 2.849(12) yes N21 H211 O152 2_776 128.9(3) 0.862 2.256 2.876(12) yes N21 H212 O211 1_665 154.7(3) 0.858 2.508 3.304(12) yes N22 H221 O154 2_776 149.3(3) 0.872 2.190 2.973(12) yes N22 H222 N171 2_766 161.4(2) 0.864 2.566 3.396(12) yes N22 H222 O172 2_766 160.8(3) 0.864 2.047 2.877(12) yes N11 H111 O114 1_655 168.6(3) 0.858 2.139 2.985(12) yes N11 H112 O142 . 168.9(3) 0.858 2.068 2.915(12) yes N12 H121 O113 1_655 154.9(3) 0.859 2.100 2.900(12) yes N12 H122 O201 1_655 164.7(3) 0.864 2.213 3.055(12) yes N1 H11 O201 2_666 171.1(3) 0.856 2.080 2.928(12) yes N1 H12 O123 2_666 136.6(2) 0.854 2.261 2.940(12) yes N2 H21 O102 . 152.7(3) 0.860 2.278 3.067(12) yes N2 H22 O152 2_666 162.0(3) 0.865 1.994 2.830(12) yes N2 H22 O153 2_666 142.5(2) 0.865 2.528 3.258(12) yes N62 H621 O112 2_767 142.6(3) 0.858 2.169 2.898(12) yes N62 H622 O231 2_767 165.7(5) 0.862 2.154 2.997(12) yes N61 H611 O134 2_767 171.1(4) 0.859 1.995 2.846(12) yes N61 H612 O164 1_655 166.9(4) 0.866 2.284 3.134(12) yes N81 H811 O162 1_645 124.1(4) 0.918 2.291 2.906(12) yes N81 H812 N121 1_645 173.9(3) 0.858 2.576 3.430(12) yes N81 H812 O123 1_645 147.1(2) 0.858 2.468 3.222(12) yes N81 H812 O124 1_645 153.6(3) 0.858 2.058 2.852(12) yes N82 H821 O211 1_655 151.3(3) 0.860 2.116 2.899(12) yes N82 H822 O123 1_645 141.0(3) 0.871 2.402 3.126(12) yes N82 H822 O153 1_645 122.6(3) 0.871 2.381 2.943(12) yes N71 H711 O142 2_767 154.2(4) 0.864 2.239 3.040(12) yes N71 H712 O164 2_667 162.7(3) 0.861 2.290 3.122(12) yes N72 H721 O134 2_657 153.4(6) 0.964 1.932 2.827(12) yes N52 H521 O122 . 147.3(3) 0.857 2.221 2.978(12) yes N52 H522 O173 . 153.2(3) 0.851 2.587 3.368(12) yes N52 H522 O174 . 152.1(3) 0.851 2.091 2.872(12) yes N51 H511 O231 . 176.1(5) 0.869 2.216 3.084(12) yes N51 H512 O124 . 146.4(3) 0.867 2.186 2.948(12) yes O231 H2311 N161 . 148.8(3) 0.850 2.363 3.122(12) yes O231 H2311 O163 . 178.6(6) 0.850 1.761 2.611(12) yes O201 H2011 N101 . 151.1(2) 0.850 2.483 3.253(12) yes O201 H2011 O103 . 179.8(3) 0.850 1.861 2.711(12) yes O211 H2111 O104 . 179.9(3) 0.850 1.908 2.758(12) yes O221 H2211 O162 . 179.5(3) 0.872 2.045 2.917(12) yes loop_ _oxford_twin_element_scale_factors 0.648(4) 0.352(4) loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag -2 -3 1 x 3 0 4 x -2 0 7 x -2 -1 6 x 1 -2 6 x -2 2 0 x 2 2 0 x 1 -2 9 x -1 -2 7 x -2 -1 7 x -2 -2 8 x 3 -2 6 x 1 -1 8 x -2 2 2 x -1 -2 6 x -3 -2 8 x 1 -2 9 x 2 3 1 x -2 3 0 x -3 2 0 x -4 -5 11 x 2 -2 6 x -5 -2 7 x -3 -4 9 x 3 1 4 x -5 -4 9 x -5 -5 11 x -3 -3 13 x -4 -4 12 x 4 2 1 x 1 -4 12 x 1 -3 12 x -3 3 0 x 3 1 2 x -2 0 4 x -3 -2 9 x 1 -3 10 x 3 -4 10 x -4 -2 8 x -2 1 4 x -2 1 2 x -3 0 4 x