# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Catherine E Housecroft' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Edwin Constable' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Eugenio Coronado' '' '' 'Markus Neuburger' '' '' 'Guoqi Zhang.' '' '' _publ_contact_author_name 'Catherine E Housecroft' _publ_contact_author_email CATHERINE.HOUSECROFT@UNIBAS.CH _publ_section_title ; Not just size and shape: spherically symmetrical d5 and d10 metal ions give different coordination nets with 4,2':6',4"-terpyridines ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_name_full ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? _publ_contact_author_address ; Chemical Crystallography Laboratory, Department of Chemistry, University of Nowhere, Nowhere, NO1 4T, UK. ; _publ_contact_author_fax '+44 1865 000000' _publ_contact_author_phone '+44 1865 000000' # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica E. The figures will be sent by e-mail. ; _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' _publ_requested_journal 'Section E' # Attachment 'gq25.cif' data_gq25_123k _database_code_depnum_ccdc_archive 'CCDC 758780' #TrackingRef 'gq25.cif' _audit_creation_date 08-09-09 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'gq25_123k_0ma in P2(1)/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 26.2828(19) _cell_length_b 13.5030(9) _cell_length_c 21.8199(16) _cell_angle_alpha 90 _cell_angle_beta 106.818(4) _cell_angle_gamma 90 _cell_volume 7412.6(9) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 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 0.0033 0.0016 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 0.0061 0.0033 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 0.0106 0.0060 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' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C80 H68 Br4 Mn2 N12 O8 # Dc = 1.57 Fooo = 3524.00 Mu = 25.63 M = 1754.97 # Found Formula = C75.80 H63.20 Br3 Mn3 N9 O15 # Dc = 1.56 FOOO = 3524.00 Mu = 21.93 M = 1744.68 _chemical_formula_sum 'C75.80 H63.20 Br3 Mn3 N9 O15' _chemical_formula_moiety 'C75 H60 Br3 Mn3 N9 O12, 0.8(C H4 O), 2.2(H2 O)' _chemical_compound_source ? _chemical_formula_weight 1744.68 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 123 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.21 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.35 _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 3524.000 _exptl_absorpt_coefficient_mu 2.193 # Sheldrick geometric approximatio 0.58 0.63 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.63 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 123 _diffrn_reflns_number 254702 _reflns_number_total 24605 _diffrn_reflns_av_R_equivalents 0.061 # Number of reflections with Friedels Law is 24605 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 24617 _diffrn_reflns_theta_min 1.712 _diffrn_reflns_theta_max 31.480 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 31.480 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _reflns_limit_h_min -38 _reflns_limit_h_max 36 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.69 _refine_diff_density_max 1.49 _refine_ls_number_reflns 10897 _refine_ls_number_restraints 101 _refine_ls_number_parameters 994 #_refine_ls_R_factor_ref 0.0444 _refine_ls_wR_factor_ref 0.0465 _refine_ls_goodness_of_fit_ref 1.1229 #_reflns_number_all 24501 _refine_ls_R_factor_all 0.1143 _refine_ls_wR_factor_all 0.0769 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10897 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_gt 0.0465 _refine_ls_shift/su_max 0.005484 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _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: 1.26 1.53 0.796 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint # start Validation Reply Form _vrf_PLAT220_gq25_123k ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.66 Ratio RESPONSE: Peripherical substitutents have high adp's, splitting does not seem to be sensible. ; _vrf_PLAT222_gq25_123k ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.80 Ratio RESPONSE: Peripherical substitutents have high adp's, splitting does not seem to be sensible. Therefore also the corresponding hydrogen atoms have high isotropic U-values. ; _vrf_PLAT430_gq25_123k ; PROBLEM: Short Inter D...A Contact O62 .. O64 .. 2.10 Ang. RESPONSE: The s.o.f.'s of the involved positions are 0.5. ; # end Validation Reply Form 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Mn1 Mn 0.0000 0.5000 0.5000 0.0245 1.0000 Uani S . . . . . Mn2 Mn 0.026831(19) 0.43358(3) 0.68277(3) 0.0241 1.0000 Uani . . . . . . Mn3 Mn 0.5000 0.5000 0.5000 0.0353 1.0000 Uani S . . . . . Mn4 Mn 0.52604(2) 0.41243(4) 0.68240(4) 0.0374 1.0000 Uani . . . . . . N1 N 0.07101(11) 0.40597(19) 0.49762(15) 0.0266 1.0000 Uani . . . . . . N2 N 0.24852(10) 0.28060(18) 0.48928(13) 0.0216 1.0000 Uani . . . . . . N3 N 0.42455(11) 0.4115(2) 0.48038(18) 0.0339 1.0000 Uani . . . . . . N4 N 0.09412(10) 0.33369(18) 0.66965(14) 0.0221 1.0000 Uani . . . . . . N5 N 0.26758(10) 0.19654(18) 0.65538(13) 0.0203 1.0000 Uani . . . . . . N6 N 0.44957(12) 0.3189(2) 0.6628(2) 0.0413 1.0000 Uani . . . . . . N7 N 0.59757(11) 0.5106(2) 0.68594(16) 0.0285 1.0000 Uani . . . . . . N8 N 0.77125(9) 0.64745(18) 0.67593(13) 0.0181 1.0000 Uani . . . . . . N9 N 0.95116(10) 0.52484(18) 0.67582(15) 0.0235 1.0000 Uani . . . . . . O1 O 0.05037(11) 0.59731(19) 0.56987(14) 0.0359 1.0000 Uani . . . . . . O2 O 0.06723(9) 0.56530(16) 0.67411(13) 0.0293 1.0000 Uani . . . . . . O3 O -0.01339(9) 0.40360(16) 0.57404(13) 0.0275 1.0000 Uani . . . . . . O4 O -0.02710(9) 0.30560(16) 0.64811(13) 0.0296 1.0000 Uani . . . . . . O5 O 0.05292(10) 0.41624(17) 0.78190(13) 0.0322 1.0000 Uani . . . . . . O6 O 0.08414(15) 0.4358(3) 0.88658(16) 0.0570 1.0000 Uani . . . . . . O11 O 0.47335(13) 0.5882(2) 0.5669(2) 0.0611 1.0000 Uani . U . . . . O12 O 0.47622(11) 0.5367(2) 0.6671(2) 0.0605 1.0000 Uani . U . . . . O13 O 0.53206(12) 0.3895(2) 0.5752(2) 0.0579 1.0000 Uani . . . . . . O14 O 0.56566(13) 0.2860(2) 0.6500(2) 0.0594 1.0000 Uani . . . . . . O15 O 0.55554(13) 0.3988(3) 0.7828(2) 0.0592 1.0000 Uani . U . . . . O16 O 0.5782(2) 0.4197(3) 0.8854(3) 0.0921 1.0000 Uani . U . . . . O51 O 0.1046(2) 0.5212(4) 1.0080(3) 0.0817 0.8000 Uani D U . . . . O61 O 0.5715(5) 0.5107(7) 0.9941(9) 0.1368 0.5000 Uani . U . . . . O62 O 0.6029(3) 0.5545(7) 1.1272(7) 0.1222 0.5000 Uani . U . . . . O63 O 0.5762(4) 0.4141(9) 1.2165(8) 0.1233 0.5000 Uani . U . . . . O64 O 0.5956(4) 0.4240(13) 1.1765(9) 0.1551 0.5000 Uani . U . . . . C1 C 0.13205(12) 0.1711(2) 0.67026(16) 0.0209 1.0000 Uani . . . . . . C2 C 0.09187(12) 0.2349(2) 0.67518(17) 0.0229 1.0000 Uani . . . . . . C3 C 0.13780(12) 0.3703(2) 0.65835(17) 0.0238 1.0000 Uani . . . . . . C4 C 0.18012(12) 0.3121(2) 0.65343(16) 0.0212 1.0000 Uani . . . . . . C5 C 0.17792(11) 0.20953(19) 0.65975(15) 0.0171 1.0000 Uani . . . . . . C6 C 0.22324(11) 0.1469(2) 0.65544(15) 0.0177 1.0000 Uani . . . . . . C7 C 0.21989(11) 0.0438(2) 0.65135(15) 0.0187 1.0000 Uani . . . . . . C8 C 0.26411(12) -0.01062(19) 0.64860(16) 0.0197 1.0000 Uani . . . . . . C9 C 0.31055(12) 0.0409(2) 0.65008(16) 0.0211 1.0000 Uani . . . . . . C10 C 0.31024(12) 0.1441(2) 0.65286(16) 0.0201 1.0000 Uani . . . . . . C11 C 0.35843(11) 0.2030(2) 0.65466(17) 0.0225 1.0000 Uani . . . . . . C12 C 0.40682(15) 0.1601(3) 0.6559(3) 0.0499 1.0000 Uani . . . . . . C13 C 0.45015(15) 0.2205(3) 0.6599(3) 0.0599 1.0000 Uani . . . . . . C14 C 0.40284(14) 0.3585(3) 0.6608(3) 0.0453 1.0000 Uani . . . . . . C15 C 0.35739(14) 0.3047(2) 0.6566(2) 0.0373 1.0000 Uani . . . . . . C16 C 0.26244(12) -0.12029(19) 0.64585(16) 0.0210 1.0000 Uani . . . . . . C17 C 0.21653(13) -0.1709(2) 0.61334(18) 0.0256 1.0000 Uani . . . . . . C18 C 0.21480(14) -0.2731(2) 0.61196(18) 0.0277 1.0000 Uani . . . . . . C19 C 0.25922(15) -0.3251(2) 0.64464(19) 0.0289 1.0000 Uani . . . . . . C20 C 0.30598(14) -0.2783(2) 0.67761(19) 0.0293 1.0000 Uani . . . . . . C21 C 0.30767(13) -0.1753(2) 0.67725(17) 0.0252 1.0000 Uani . . . . . . C22 C 0.06484(12) 0.6213(2) 0.62746(18) 0.0266 1.0000 Uani . . . . . . C23 C 0.08076(18) 0.7287(3) 0.6427(2) 0.0419 1.0000 Uani . . . . . . C24 C -0.03530(12) 0.3276(2) 0.5902(2) 0.0280 1.0000 Uani . . . . . . C25 C -0.07065(19) 0.2631(3) 0.5397(2) 0.0510 1.0000 Uani . . . . . . C26 C 0.05338(16) 0.4582(3) 0.8338(2) 0.0384 1.0000 Uani D U . . . . C27 C 0.0115(3) 0.5359(6) 0.8357(4) 0.0469 0.6000 Uani D U . . . . C28 C 0.0417(8) 0.5667(6) 0.8213(7) 0.0634 0.4000 Uani D U . . . . C31 C 0.11044(12) 0.2462(2) 0.49406(18) 0.0268 1.0000 Uani . . . . . . C32 C 0.06848(12) 0.3069(2) 0.49630(18) 0.0269 1.0000 Uani . . . . . . C33 C 0.11750(14) 0.4466(2) 0.49732(19) 0.0290 1.0000 Uani . . . . . . C34 C 0.16152(13) 0.3918(2) 0.49523(17) 0.0250 1.0000 Uani . . . . . . C35 C 0.15852(12) 0.2885(2) 0.49334(16) 0.0197 1.0000 Uani . . . . . . C36 C 0.20525(12) 0.2287(2) 0.49012(15) 0.0191 1.0000 Uani . . . . . . C37 C 0.20370(12) 0.1253(2) 0.48779(16) 0.0206 1.0000 Uani . . . . . . C38 C 0.24823(12) 0.0733(2) 0.48368(16) 0.0205 1.0000 Uani . . . . . . C39 C 0.29280(12) 0.1278(2) 0.48222(16) 0.0222 1.0000 Uani . . . . . . C40 C 0.29150(11) 0.2306(2) 0.48506(16) 0.0199 1.0000 Uani . . . . . . C41 C 0.33807(12) 0.2917(2) 0.48304(17) 0.0245 1.0000 Uani . . . . . . C42 C 0.38433(14) 0.2518(3) 0.4767(2) 0.0406 1.0000 Uani . . . . . . C43 C 0.42606(16) 0.3129(3) 0.4753(3) 0.0467 1.0000 Uani . . . . . . C44 C 0.37942(14) 0.4500(3) 0.4837(2) 0.0431 1.0000 Uani . . . . . . C45 C 0.33562(13) 0.3941(2) 0.4862(2) 0.0398 1.0000 Uani . . . . . . C46 C 0.24827(12) -0.0367(2) 0.47943(16) 0.0225 1.0000 Uani . . . . . . C47 C 0.20249(14) -0.0877(2) 0.44682(17) 0.0253 1.0000 Uani . . . . . . C48 C 0.20301(15) -0.1903(2) 0.44213(19) 0.0312 1.0000 Uani . . . . . . C49 C 0.24922(16) -0.2412(2) 0.47091(18) 0.0315 1.0000 Uani . . . . . . C50 C 0.29493(15) -0.1926(3) 0.50377(18) 0.0318 1.0000 Uani . . . . . . C51 C 0.29465(14) -0.0901(2) 0.50753(18) 0.0270 1.0000 Uani . . . . . . C52 C 0.45776(15) 0.5837(3) 0.6181(3) 0.0491 1.0000 Uani . U . . . . C53 C 0.4106(2) 0.6491(4) 0.6141(3) 0.0701 1.0000 Uani . U . . . . C54 C 0.55978(15) 0.3125(3) 0.5931(3) 0.0521 1.0000 Uani . U . . . . C55 C 0.5852(3) 0.2546(5) 0.5539(4) 0.0773 1.0000 Uani . . . . . . C56 C 0.5463(2) 0.3872(4) 0.8312(4) 0.0714 1.0000 Uani . U . . . . C57 C 0.4969(3) 0.3334(5) 0.8315(5) 0.0952 1.0000 Uani . U . . . . C61 C 0.68667(12) 0.5318(2) 0.68168(18) 0.0269 1.0000 Uani . . . . . . C62 C 0.64415(13) 0.4733(2) 0.68380(19) 0.0299 1.0000 Uani . . . . . . C63 C 0.59369(13) 0.6088(3) 0.6881(2) 0.0331 1.0000 Uani . . . . . . C64 C 0.63476(12) 0.6731(2) 0.68638(19) 0.0297 1.0000 Uani . . . . . . C65 C 0.68277(12) 0.6342(2) 0.68310(16) 0.0204 1.0000 Uani . . . . . . C66 C 0.72825(11) 0.6973(2) 0.68083(15) 0.0191 1.0000 Uani . . . . . . C67 C 0.72704(11) 0.8000(2) 0.68450(15) 0.0192 1.0000 Uani . . . . . . C68 C 0.77121(11) 0.8551(2) 0.68126(15) 0.0180 1.0000 Uani . . . . . . C69 C 0.81524(11) 0.8022(2) 0.67396(15) 0.0188 1.0000 Uani . . . . . . C70 C 0.81394(11) 0.69932(19) 0.67286(15) 0.0168 1.0000 Uani . . . . . . C71 C 0.86066(11) 0.63993(19) 0.67110(15) 0.0174 1.0000 Uani . . . . . . C72 C 0.85972(12) 0.5370(2) 0.67343(17) 0.0242 1.0000 Uani . . . . . . C73 C 0.90486(13) 0.4826(2) 0.67553(19) 0.0267 1.0000 Uani . . . . . . C74 C 0.95162(12) 0.6239(2) 0.67230(19) 0.0281 1.0000 Uani . . . . . . C75 C 0.90824(12) 0.6841(2) 0.66988(17) 0.0244 1.0000 Uani . . . . . . C76 C 0.77262(12) 0.9643(2) 0.68702(15) 0.0197 1.0000 Uani . . . . . . C77 C 0.82118(13) 1.0134(2) 0.71028(17) 0.0242 1.0000 Uani . . . . . . C78 C 0.82338(14) 1.1153(2) 0.71767(18) 0.0273 1.0000 Uani . . . . . . C79 C 0.77623(14) 1.1684(2) 0.70205(18) 0.0268 1.0000 Uani . . . . . . C80 C 0.72793(15) 1.1225(2) 0.67814(18) 0.0296 1.0000 Uani . . . . . . C81 C 0.72573(13) 1.0202(2) 0.67001(17) 0.0252 1.0000 Uani . . . . . . O91 O 0.0206(10) 0.4491(18) 0.9784(11) 0.0829 0.2000 Uani . U . . . . C92 C 0.0669(4) 0.5142(6) 1.0408(5) 0.0938 0.8000 Uani D U . . . . Br1 Br 0.24971(2) -0.38158(3) 0.46625(2) 0.0509 1.0000 Uani . . . . . . Br2 Br 0.257136(19) -0.46575(2) 0.64484(2) 0.0430 1.0000 Uani . . . . . . Br3 Br 0.779470(17) 1.30814(2) 0.71208(2) 0.0371 1.0000 Uani . . . . . . H11 H 0.1284 0.1029 0.6739 0.0252 1.0000 Uiso R . . . . . H21 H 0.0615 0.2078 0.6824 0.0294 1.0000 Uiso R . . . . . H31 H 0.1398 0.4388 0.6532 0.0276 1.0000 Uiso R . . . . . H41 H 0.2105 0.3408 0.6464 0.0255 1.0000 Uiso R . . . . . H71 H 0.1884 0.0124 0.6497 0.0230 1.0000 Uiso R . . . . . H91 H 0.3409 0.0068 0.6490 0.0277 1.0000 Uiso R . . . . . H121 H 0.4102 0.0918 0.6538 0.0610 1.0000 Uiso R . . . . . H131 H 0.4820 0.1903 0.6612 0.0729 1.0000 Uiso R . . . . . H141 H 0.4005 0.4272 0.6617 0.0564 1.0000 Uiso R . . . . . H151 H 0.3262 0.3372 0.6558 0.0461 1.0000 Uiso R . . . . . H171 H 0.1860 -0.1352 0.5920 0.0318 1.0000 Uiso R . . . . . H181 H 0.1839 -0.3059 0.5903 0.0347 1.0000 Uiso R . . . . . H201 H 0.3361 -0.3143 0.7000 0.0377 1.0000 Uiso R . . . . . H211 H 0.3392 -0.1433 0.6980 0.0317 1.0000 Uiso R . . . . . H231 H 0.0628 0.7563 0.6718 0.0631 1.0000 Uiso R . . . . . H232 H 0.0721 0.7669 0.6037 0.0635 1.0000 Uiso R . . . . . H233 H 0.1184 0.7324 0.6627 0.0633 1.0000 Uiso R . . . . . H251 H -0.0851 0.2106 0.5589 0.0750 1.0000 Uiso R . . . . . H252 H -0.0990 0.3006 0.5126 0.0753 1.0000 Uiso R . . . . . H253 H -0.0510 0.2348 0.5139 0.0754 1.0000 Uiso R . . . . . H271 H -0.0007 0.5227 0.8724 0.0528 0.6000 Uiso R . . . . . H272 H 0.0267 0.6006 0.8392 0.0528 0.6000 Uiso R . . . . . H273 H -0.0186 0.5325 0.7976 0.0528 0.6000 Uiso R . . . . . H281 H 0.0485 0.6063 0.8616 0.0735 0.4000 Uiso R . . . . . H282 H 0.0545 0.6001 0.7923 0.0735 0.4000 Uiso R . . . . . H283 H 0.0030 0.5674 0.8058 0.0735 0.4000 Uiso R . . . . . H311 H 0.1064 0.1772 0.4930 0.0330 1.0000 Uiso R . . . . . H321 H 0.0363 0.2772 0.4961 0.0344 1.0000 Uiso R . . . . . H331 H 0.1201 0.5149 0.4990 0.0361 1.0000 Uiso R . . . . . H341 H 0.1930 0.4237 0.4940 0.0306 1.0000 Uiso R . . . . . H371 H 0.1736 0.0908 0.4892 0.0242 1.0000 Uiso R . . . . . H391 H 0.3234 0.0955 0.4796 0.0278 1.0000 Uiso R . . . . . H421 H 0.3875 0.1838 0.4722 0.0510 1.0000 Uiso R . . . . . H431 H 0.4566 0.2842 0.4705 0.0578 1.0000 Uiso R . . . . . H441 H 0.3768 0.5189 0.4849 0.0522 1.0000 Uiso R . . . . . H451 H 0.3050 0.4248 0.4903 0.0468 1.0000 Uiso R . . . . . H471 H 0.1711 -0.0522 0.4277 0.0317 1.0000 Uiso R . . . . . H481 H 0.1726 -0.2234 0.4204 0.0394 1.0000 Uiso R . . . . . H501 H 0.3258 -0.2282 0.5240 0.0409 1.0000 Uiso R . . . . . H511 H 0.3259 -0.0560 0.5293 0.0329 1.0000 Uiso R . . . . . H531 H 0.4118 0.6718 0.6558 0.1051 1.0000 Uiso R . . . . . H532 H 0.4122 0.7055 0.5881 0.1049 1.0000 Uiso R . . . . . H533 H 0.3781 0.6138 0.5954 0.1050 1.0000 Uiso R . . . . . H551 H 0.5830 0.1858 0.5633 0.1196 1.0000 Uiso R . . . . . H552 H 0.6220 0.2729 0.5648 0.1199 1.0000 Uiso R . . . . . H553 H 0.5683 0.2676 0.5099 0.1200 1.0000 Uiso R . . . . . H571 H 0.4974 0.3170 0.8749 0.1193 1.0000 Uiso R . . . . . H572 H 0.4946 0.2733 0.8070 0.1193 1.0000 Uiso R . . . . . H573 H 0.4661 0.3746 0.8123 0.1193 1.0000 Uiso R . . . . . H611 H 0.7182 0.5009 0.6794 0.0341 1.0000 Uiso R . . . . . H621 H 0.6473 0.4052 0.6825 0.0359 1.0000 Uiso R . . . . . H631 H 0.5613 0.6365 0.6910 0.0420 1.0000 Uiso R . . . . . H641 H 0.6298 0.7424 0.6868 0.0359 1.0000 Uiso R . . . . . H671 H 0.6972 0.8318 0.6887 0.0207 1.0000 Uiso R . . . . . H691 H 0.8446 0.8361 0.6702 0.0235 1.0000 Uiso R . . . . . H721 H 0.8289 0.5037 0.6739 0.0306 1.0000 Uiso R . . . . . H731 H 0.9031 0.4143 0.6761 0.0350 1.0000 Uiso R . . . . . H741 H 0.9832 0.6551 0.6713 0.0350 1.0000 Uiso R . . . . . H751 H 0.9110 0.7524 0.6678 0.0300 1.0000 Uiso R . . . . . H771 H 0.8527 0.9774 0.7216 0.0297 1.0000 Uiso R . . . . . H781 H 0.8555 1.1473 0.7331 0.0315 1.0000 Uiso R . . . . . H801 H 0.6965 1.1590 0.6665 0.0381 1.0000 Uiso R . . . . . H811 H 0.6924 0.9893 0.6529 0.0311 1.0000 Uiso R . . . . . H920 H 0.0914 0.4908 0.9721 0.1380 0.8000 Uiso R . . . . . H921 H 0.0815 0.5478 1.0812 0.1222 0.8000 Uiso R . . . . . H922 H 0.0614 0.4452 1.0499 0.1222 0.8000 Uiso R . . . . . H923 H 0.0338 0.5431 1.0185 0.1222 0.8000 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 Mn1 0.0201(3) 0.0142(2) 0.0406(4) -0.0030(3) 0.0109(3) -0.0008(2) Mn2 0.0168(2) 0.01427(18) 0.0425(3) -0.00124(19) 0.0104(2) 0.00197(16) Mn3 0.0152(3) 0.0184(3) 0.0737(6) -0.0059(3) 0.0150(4) -0.0035(2) Mn4 0.0185(2) 0.0226(2) 0.0743(5) -0.0004(3) 0.0185(3) -0.00479(19) N1 0.0224(13) 0.0171(11) 0.0427(18) -0.0014(11) 0.0133(13) 0.0021(10) N2 0.0213(12) 0.0177(10) 0.0274(15) 0.0013(10) 0.0097(11) -0.0025(9) N3 0.0193(13) 0.0243(13) 0.059(2) -0.0016(13) 0.0124(14) -0.0069(10) N4 0.0153(11) 0.0164(10) 0.0336(16) 0.0004(10) 0.0058(11) 0.0026(9) N5 0.0180(12) 0.0151(10) 0.0286(14) -0.0001(10) 0.0079(11) -0.0026(9) N6 0.0192(14) 0.0225(13) 0.082(3) 0.0013(15) 0.0139(15) -0.0081(11) N7 0.0171(12) 0.0218(12) 0.0478(19) 0.0007(12) 0.0114(13) -0.0037(10) N8 0.0129(11) 0.0157(10) 0.0262(15) 0.0003(9) 0.0066(10) -0.0005(8) N9 0.0171(12) 0.0150(10) 0.0406(17) -0.0032(10) 0.0117(12) 0.0011(9) O1 0.0351(14) 0.0263(11) 0.0455(17) -0.0081(11) 0.0106(12) -0.0098(10) O2 0.0206(11) 0.0183(9) 0.0495(16) -0.0012(10) 0.0111(11) -0.0020(8) O3 0.0210(10) 0.0173(9) 0.0447(15) -0.0026(9) 0.0101(10) -0.0025(8) O4 0.0227(11) 0.0178(9) 0.0517(16) -0.0013(10) 0.0163(11) -0.0021(8) O5 0.0291(13) 0.0234(11) 0.0455(16) 0.0028(10) 0.0127(12) 0.0062(9) O6 0.070(2) 0.0491(18) 0.049(2) 0.0094(15) 0.0140(17) 0.0260(16) O11 0.0366(16) 0.0411(16) 0.109(3) -0.0178(18) 0.0270(18) -0.0013(13) O12 0.0210(13) 0.0277(13) 0.130(3) 0.0131(17) 0.0177(17) -0.0062(11) O13 0.0359(16) 0.0289(14) 0.103(3) -0.0070(16) 0.0099(17) 0.0003(12) O14 0.0450(18) 0.0340(15) 0.111(3) -0.0129(18) 0.040(2) -0.0137(13) O15 0.0374(17) 0.0564(19) 0.083(3) 0.0179(19) 0.0163(17) -0.0037(14) O16 0.103(4) 0.051(2) 0.121(4) 0.004(2) 0.030(3) -0.006(2) O51 0.097(4) 0.056(3) 0.090(4) -0.003(3) 0.025(3) 0.026(3) O61 0.110(8) 0.042(5) 0.256(11) 0.005(7) 0.049(9) -0.005(5) O62 0.032(4) 0.071(5) 0.252(10) 0.044(6) 0.022(5) 0.005(3) O63 0.062(6) 0.099(7) 0.203(11) 0.028(7) 0.029(6) -0.019(5) O64 0.054(5) 0.179(10) 0.232(12) 0.071(9) 0.041(7) -0.018(6) C1 0.0195(13) 0.0133(11) 0.0313(18) 0.0028(11) 0.0097(13) 0.0005(10) C2 0.0166(13) 0.0167(12) 0.0380(19) 0.0023(12) 0.0121(13) -0.0002(10) C3 0.0203(14) 0.0132(11) 0.0382(19) -0.0011(12) 0.0090(14) -0.0017(10) C4 0.0177(13) 0.0157(11) 0.0325(17) -0.0005(12) 0.0109(12) -0.0022(10) C5 0.0141(12) 0.0128(11) 0.0242(16) -0.0021(10) 0.0051(11) -0.0011(9) C6 0.0153(13) 0.0150(11) 0.0233(16) 0.0007(11) 0.0064(12) -0.0007(10) C7 0.0157(13) 0.0138(11) 0.0288(17) -0.0006(11) 0.0098(12) -0.0029(9) C8 0.0221(14) 0.0123(11) 0.0282(17) 0.0007(11) 0.0130(13) -0.0027(10) C9 0.0175(13) 0.0151(11) 0.0341(18) -0.0011(11) 0.0129(13) 0.0006(10) C10 0.0172(13) 0.0183(12) 0.0278(17) -0.0028(11) 0.0111(12) -0.0039(10) C11 0.0145(13) 0.0185(12) 0.0357(18) 0.0012(12) 0.0091(13) -0.0038(10) C12 0.0238(17) 0.0202(14) 0.115(4) -0.006(2) 0.034(2) -0.0058(13) C13 0.0202(17) 0.0293(18) 0.137(5) -0.003(2) 0.034(2) -0.0029(14) C14 0.0224(17) 0.0168(14) 0.101(4) 0.0021(17) 0.024(2) -0.0055(12) C15 0.0210(15) 0.0165(13) 0.077(3) 0.0034(16) 0.0181(17) -0.0009(12) C16 0.0224(14) 0.0121(11) 0.0339(18) -0.0020(11) 0.0169(14) -0.0027(10) C17 0.0266(15) 0.0167(12) 0.038(2) -0.0026(12) 0.0165(14) -0.0042(11) C18 0.0283(16) 0.0201(13) 0.038(2) -0.0069(13) 0.0151(15) -0.0076(12) C19 0.0409(19) 0.0116(11) 0.042(2) -0.0018(12) 0.0239(16) -0.0044(12) C20 0.0303(17) 0.0176(12) 0.046(2) 0.0017(13) 0.0201(16) 0.0005(12) C21 0.0221(15) 0.0191(13) 0.040(2) -0.0022(12) 0.0170(14) -0.0012(11) C22 0.0161(14) 0.0195(13) 0.045(2) -0.0052(13) 0.0099(14) -0.0020(10) C23 0.050(2) 0.0195(14) 0.054(3) -0.0042(16) 0.011(2) -0.0094(15) C24 0.0180(14) 0.0158(12) 0.053(2) -0.0034(13) 0.0145(15) -0.0025(10) C25 0.053(3) 0.044(2) 0.055(3) -0.009(2) 0.014(2) -0.030(2) C26 0.043(2) 0.0224(15) 0.048(2) 0.0026(15) 0.0097(19) 0.0122(14) C27 0.054(4) 0.042(4) 0.041(4) -0.005(3) 0.009(3) 0.033(3) C28 0.102(10) 0.032(5) 0.054(8) -0.014(5) 0.019(7) 0.022(6) C31 0.0207(14) 0.0142(12) 0.047(2) -0.0014(12) 0.0118(14) -0.0008(10) C32 0.0192(14) 0.0183(12) 0.046(2) -0.0030(13) 0.0132(14) -0.0027(11) C33 0.0278(16) 0.0144(12) 0.049(2) -0.0008(13) 0.0169(16) -0.0023(11) C34 0.0211(15) 0.0166(12) 0.039(2) 0.0003(12) 0.0117(14) -0.0041(11) C35 0.0186(13) 0.0172(12) 0.0248(16) 0.0029(11) 0.0086(12) 0.0007(10) C36 0.0191(14) 0.0151(11) 0.0248(16) 0.0005(11) 0.0088(12) -0.0002(10) C37 0.0201(14) 0.0174(12) 0.0242(17) 0.0005(11) 0.0062(12) -0.0041(10) C38 0.0188(14) 0.0169(12) 0.0266(17) 0.0026(11) 0.0079(13) 0.0017(10) C39 0.0182(14) 0.0214(13) 0.0282(18) 0.0020(12) 0.0088(13) 0.0004(10) C40 0.0153(13) 0.0177(12) 0.0276(17) 0.0006(11) 0.0074(12) -0.0021(10) C41 0.0202(14) 0.0210(13) 0.0326(18) 0.0007(12) 0.0081(13) -0.0048(11) C42 0.0277(17) 0.0253(16) 0.076(3) -0.0149(17) 0.0257(19) -0.0104(13) C43 0.0320(19) 0.0327(18) 0.084(3) -0.018(2) 0.031(2) -0.0135(15) C44 0.0189(16) 0.0203(14) 0.088(3) 0.0098(17) 0.0129(18) -0.0018(12) C45 0.0169(15) 0.0183(14) 0.083(3) 0.0062(16) 0.0127(18) 0.0003(11) C46 0.0233(15) 0.0162(11) 0.0323(18) 0.0022(12) 0.0148(14) 0.0015(11) C47 0.0305(16) 0.0144(11) 0.0354(19) -0.0001(12) 0.0163(15) 0.0019(11) C48 0.0396(19) 0.0186(13) 0.041(2) -0.0031(14) 0.0202(16) -0.0030(13) C49 0.051(2) 0.0176(13) 0.033(2) 0.0042(13) 0.0234(17) 0.0080(14) C50 0.0394(19) 0.0250(15) 0.036(2) 0.0078(14) 0.0188(16) 0.0128(14) C51 0.0278(16) 0.0236(14) 0.0328(19) 0.0056(13) 0.0137(15) 0.0051(12) C52 0.0212(17) 0.0301(18) 0.099(4) -0.014(2) 0.022(2) -0.0011(14) C53 0.043(3) 0.054(3) 0.116(5) 0.012(3) 0.026(3) 0.018(2) C54 0.0234(17) 0.0218(15) 0.107(4) -0.001(2) 0.012(2) -0.0012(13) C55 0.079(4) 0.060(3) 0.104(5) -0.019(3) 0.043(4) 0.011(3) C56 0.067(3) 0.035(2) 0.121(4) 0.020(3) 0.040(3) 0.000(2) C57 0.066(3) 0.075(4) 0.159(6) 0.031(4) 0.055(4) -0.008(3) C61 0.0143(13) 0.0187(12) 0.049(2) 0.0073(13) 0.0115(14) 0.0010(10) C62 0.0164(14) 0.0207(13) 0.052(2) 0.0037(14) 0.0092(15) -0.0028(11) C63 0.0128(14) 0.0270(15) 0.061(3) -0.0097(15) 0.0138(16) -0.0043(11) C64 0.0164(14) 0.0209(13) 0.054(2) -0.0054(14) 0.0137(15) -0.0031(11) C65 0.0145(13) 0.0195(12) 0.0291(17) 0.0018(11) 0.0093(12) -0.0010(10) C66 0.0117(12) 0.0172(11) 0.0293(17) 0.0003(11) 0.0072(12) -0.0020(10) C67 0.0121(12) 0.0177(12) 0.0282(16) 0.0023(11) 0.0066(12) 0.0026(10) C68 0.0169(13) 0.0147(11) 0.0244(17) 0.0022(10) 0.0092(12) 0.0002(10) C69 0.0140(12) 0.0127(10) 0.0314(17) 0.0008(11) 0.0091(12) -0.0004(9) C70 0.0143(12) 0.0135(10) 0.0243(15) -0.0005(10) 0.0082(11) 0.0007(9) C71 0.0153(13) 0.0135(11) 0.0247(16) -0.0021(10) 0.0079(12) -0.0014(9) C72 0.0201(14) 0.0145(11) 0.043(2) -0.0003(12) 0.0161(14) -0.0008(10) C73 0.0228(15) 0.0102(11) 0.052(2) -0.0021(12) 0.0193(15) -0.0014(10) C74 0.0160(14) 0.0147(12) 0.056(2) -0.0039(13) 0.0142(15) -0.0020(10) C75 0.0182(14) 0.0123(11) 0.047(2) -0.0016(12) 0.0158(14) -0.0001(10) C76 0.0190(13) 0.0153(11) 0.0265(17) 0.0024(11) 0.0094(12) 0.0022(10) C77 0.0220(14) 0.0165(12) 0.0355(19) 0.0016(12) 0.0106(14) 0.0019(10) C78 0.0298(17) 0.0161(12) 0.036(2) 0.0008(12) 0.0099(15) -0.0019(11) C79 0.0356(17) 0.0149(12) 0.035(2) 0.0006(12) 0.0177(15) 0.0051(11) C80 0.0328(18) 0.0211(13) 0.038(2) 0.0076(14) 0.0151(16) 0.0096(13) C81 0.0209(15) 0.0190(13) 0.037(2) 0.0039(12) 0.0115(14) 0.0053(11) O91 0.094(9) 0.088(12) 0.081(11) 0.004(10) 0.047(10) 0.037(8) C92 0.114(7) 0.053(4) 0.123(7) 0.015(4) 0.047(6) 0.023(4) Br1 0.0885(4) 0.01532(14) 0.0543(3) 0.00291(15) 0.0291(3) 0.00832(17) Br2 0.0612(3) 0.01211(12) 0.0601(3) -0.00147(15) 0.0244(2) -0.00540(15) Br3 0.0563(2) 0.01341(12) 0.0483(2) 0.00243(14) 0.02589(19) 0.00720(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.07039(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mn1 . O3 2_566 2.181(2) yes Mn1 . O1 2_566 2.153(3) yes Mn1 . N1 2_566 2.270(3) yes Mn1 . N1 . 2.270(3) yes Mn1 . O1 . 2.153(3) yes Mn1 . O3 . 2.181(2) yes Mn2 . N9 1_455 2.307(2) yes Mn2 . N4 . 2.307(2) yes Mn2 . O2 . 2.108(2) yes Mn2 . O3 . 2.336(3) yes Mn2 . O4 . 2.224(2) yes Mn2 . O5 . 2.085(3) yes Mn3 . O13 2_666 2.197(4) yes Mn3 . N3 2_666 2.248(3) yes Mn3 . O11 2_666 2.152(4) yes Mn3 . N3 . 2.248(3) yes Mn3 . O11 . 2.152(4) yes Mn3 . O13 . 2.197(4) yes Mn4 . N6 . 2.306(3) yes Mn4 . N7 . 2.283(3) yes Mn4 . O12 . 2.095(3) yes Mn4 . O13 . 2.410(4) yes Mn4 . O14 . 2.219(3) yes Mn4 . O15 . 2.109(4) yes N1 . C32 . 1.339(4) yes N1 . C33 . 1.341(4) yes N2 . C36 . 1.341(4) yes N2 . C40 . 1.342(4) yes N3 . C43 . 1.337(5) yes N3 . C44 . 1.316(5) yes N4 . C2 . 1.342(4) yes N4 . C3 . 1.337(4) yes N5 . C6 . 1.344(4) yes N5 . C10 . 1.340(4) yes N6 . C13 . 1.331(5) yes N6 . C14 . 1.328(5) yes N7 . C62 . 1.337(4) yes N7 . C63 . 1.332(4) yes N8 . C66 . 1.346(4) yes N8 . C70 . 1.341(4) yes N9 . C73 . 1.343(4) yes N9 . C74 . 1.341(4) yes O1 . C22 . 1.246(5) yes O2 . C22 . 1.255(4) yes O3 . C24 . 1.276(4) yes O4 . C24 . 1.255(5) yes O5 . C26 . 1.262(5) yes O6 . C26 . 1.238(5) yes O11 . C52 . 1.299(7) yes O12 . C52 . 1.216(7) yes O13 . C54 . 1.265(5) yes O14 . C54 . 1.257(7) yes O15 . C56 . 1.161(8) yes O16 . C56 . 1.312(9) yes O51 . C92 . 1.385(8) yes O51 . H920 . 0.862 no O63 . O64 . 1.14(2) yes C1 . C2 . 1.391(4) yes C1 . C5 . 1.391(4) yes C1 . H11 . 0.932 no C2 . H21 . 0.932 no C3 . C4 . 1.392(4) yes C3 . H31 . 0.935 no C4 . C5 . 1.394(4) yes C4 . H41 . 0.941 no C5 . C6 . 1.485(4) yes C6 . C7 . 1.396(4) yes C7 . C8 . 1.391(4) yes C7 . H71 . 0.921 no C8 . C9 . 1.397(4) yes C8 . C16 . 1.482(4) yes C9 . C10 . 1.395(4) yes C9 . H91 . 0.927 no C10 . C11 . 1.486(4) yes C11 . C12 . 1.390(5) yes C11 . C15 . 1.375(4) yes C12 . C13 . 1.382(5) yes C12 . H121 . 0.929 no C13 . H131 . 0.924 no C14 . C15 . 1.379(5) yes C14 . H141 . 0.930 no C15 . H151 . 0.926 no C16 . C17 . 1.390(4) yes C16 . C21 . 1.401(5) yes C17 . C18 . 1.380(4) yes C17 . H171 . 0.936 no C18 . C19 . 1.372(5) yes C18 . H181 . 0.925 no C19 . C20 . 1.384(5) yes C19 . Br2 . 1.900(3) yes C20 . C21 . 1.392(4) yes C20 . H201 . 0.936 no C21 . H211 . 0.928 no C22 . C23 . 1.519(5) yes C23 . H231 . 0.969 no C23 . H232 . 0.965 no C23 . H233 . 0.960 no C24 . C25 . 1.497(5) yes C25 . H251 . 0.956 no C25 . H252 . 0.953 no C25 . H253 . 0.947 no C26 . C27 . 1.531(6) yes C26 . C28 . 1.507(8) yes C27 . H271 . 0.963 no C27 . H272 . 0.955 no C27 . H273 . 0.967 no C27 . H283 . 0.756 no C28 . H281 . 1.000 no C28 . H282 . 0.917 no C28 . H283 . 0.973 no C31 . C32 . 1.386(4) yes C31 . C35 . 1.391(4) yes C31 . H311 . 0.937 no C32 . H321 . 0.936 no C33 . C34 . 1.386(5) yes C33 . H331 . 0.924 no C34 . C35 . 1.396(4) yes C34 . H341 . 0.940 no C35 . C36 . 1.489(4) yes C36 . C37 . 1.397(4) yes C37 . C38 . 1.390(4) yes C37 . H371 . 0.927 no C38 . C39 . 1.392(4) yes C38 . C46 . 1.487(4) yes C39 . C40 . 1.391(4) yes C39 . H391 . 0.930 no C40 . C41 . 1.487(4) yes C41 . C42 . 1.373(5) yes C41 . C45 . 1.388(4) yes C42 . C43 . 1.380(5) yes C42 . H421 . 0.929 no C43 . H431 . 0.924 no C44 . C45 . 1.391(5) yes C44 . H441 . 0.933 no C45 . H451 . 0.933 no C46 . C47 . 1.391(5) yes C46 . C51 . 1.397(5) yes C47 . C48 . 1.389(4) yes C47 . H471 . 0.941 no C48 . C49 . 1.379(5) yes C48 . H481 . 0.920 no C49 . C50 . 1.375(6) yes C49 . Br1 . 1.898(3) yes C50 . C51 . 1.385(5) yes C50 . H501 . 0.937 no C51 . H511 . 0.943 no C52 . C53 . 1.504(6) yes C53 . H531 . 0.951 no C53 . H532 . 0.958 no C53 . H533 . 0.960 no C54 . C55 . 1.456(7) yes C55 . H551 . 0.956 no C55 . H552 . 0.958 no C55 . H553 . 0.951 no C56 . C57 . 1.490(8) yes C57 . H571 . 0.969 no C57 . H572 . 0.965 no C57 . H573 . 0.971 no C61 . C62 . 1.380(4) yes C61 . C65 . 1.388(4) yes C61 . H611 . 0.942 no C62 . H621 . 0.924 no C63 . C64 . 1.394(4) yes C63 . H631 . 0.949 no C64 . C65 . 1.388(4) yes C64 . H641 . 0.944 no C65 . C66 . 1.480(4) yes C66 . C67 . 1.389(4) yes C67 . C68 . 1.398(4) yes C67 . H671 . 0.921 no C68 . C69 . 1.408(4) yes C68 . C76 . 1.479(4) yes C69 . C70 . 1.390(4) yes C69 . H691 . 0.922 no C70 . C71 . 1.476(4) yes C71 . C72 . 1.392(4) yes C71 . C75 . 1.393(4) yes C72 . C73 . 1.385(4) yes C72 . H721 . 0.930 no C73 . H731 . 0.923 no C74 . C75 . 1.389(4) yes C74 . H741 . 0.936 no C75 . H751 . 0.926 no C76 . C77 . 1.397(4) yes C76 . C81 . 1.401(4) yes C77 . C78 . 1.385(4) yes C77 . H771 . 0.930 no C78 . C79 . 1.386(5) yes C78 . H781 . 0.920 no C79 . C80 . 1.373(5) yes C79 . Br3 . 1.899(3) yes C80 . C81 . 1.392(4) yes C80 . H801 . 0.932 no C81 . H811 . 0.943 no C92 . H921 . 0.967 no C92 . H922 . 0.972 no C92 . H923 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 2_566 Mn1 . O1 2_566 92.16(10) yes O3 2_566 Mn1 . N1 2_566 89.60(9) yes O1 2_566 Mn1 . N1 2_566 90.94(10) yes O3 2_566 Mn1 . N1 . 90.40(9) yes O1 2_566 Mn1 . N1 . 89.06(10) yes N1 2_566 Mn1 . N1 . 179.995 yes O3 2_566 Mn1 . O1 . 87.84(10) yes O1 2_566 Mn1 . O1 . 179.995 yes N1 2_566 Mn1 . O1 . 89.06(10) yes N1 . Mn1 . O1 . 90.94(10) yes O3 2_566 Mn1 . O3 . 179.995 yes O1 2_566 Mn1 . O3 . 87.84(10) yes N1 2_566 Mn1 . O3 . 90.40(9) yes N1 . Mn1 . O3 . 89.60(9) yes O1 . Mn1 . O3 . 92.16(10) yes N9 1_455 Mn2 . N4 . 168.93(10) yes N9 1_455 Mn2 . O2 . 89.45(9) yes N4 . Mn2 . O2 . 93.34(9) yes N9 1_455 Mn2 . O3 . 84.13(9) yes N4 . Mn2 . O3 . 84.87(9) yes O2 . Mn2 . O3 . 98.45(10) yes N9 1_455 Mn2 . O4 . 86.57(9) yes N4 . Mn2 . O4 . 86.53(9) yes O2 . Mn2 . O4 . 155.95(11) yes O3 . Mn2 . O4 . 57.56(9) yes N9 1_455 Mn2 . O5 . 98.43(10) yes N4 . Mn2 . O5 . 91.68(10) yes O2 . Mn2 . O5 . 99.48(10) yes O3 . Mn2 . O5 . 161.91(9) yes O4 . Mn2 . O5 . 104.56(10) yes O13 2_666 Mn3 . N3 2_666 84.70(12) yes O13 2_666 Mn3 . O11 2_666 89.98(15) yes N3 2_666 Mn3 . O11 2_666 88.93(12) yes O13 2_666 Mn3 . N3 . 95.30(12) yes N3 2_666 Mn3 . N3 . 179.995 yes O11 2_666 Mn3 . N3 . 91.07(12) yes O13 2_666 Mn3 . O11 . 90.02(15) yes N3 2_666 Mn3 . O11 . 91.07(12) yes O11 2_666 Mn3 . O11 . 179.995 yes N3 . Mn3 . O11 . 88.93(12) yes O13 2_666 Mn3 . O13 . 179.995 yes N3 2_666 Mn3 . O13 . 95.30(12) yes O11 2_666 Mn3 . O13 . 90.02(15) yes N3 . Mn3 . O13 . 84.70(12) yes O11 . Mn3 . O13 . 89.98(15) yes N6 . Mn4 . N7 . 171.45(13) yes N6 . Mn4 . O12 . 86.45(11) yes N7 . Mn4 . O12 . 90.62(10) yes N6 . Mn4 . O13 . 92.74(13) yes N7 . Mn4 . O13 . 79.80(11) yes O12 . Mn4 . O13 . 99.28(15) yes N6 . Mn4 . O14 . 89.08(11) yes N7 . Mn4 . O14 . 89.98(10) yes O12 . Mn4 . O14 . 153.44(18) yes O13 . Mn4 . O14 . 54.77(14) yes N6 . Mn4 . O15 . 100.58(14) yes N7 . Mn4 . O15 . 87.93(12) yes O12 . Mn4 . O15 . 105.13(16) yes O13 . Mn4 . O15 . 152.75(12) yes O14 . Mn4 . O15 . 101.43(16) yes Mn1 . N1 . C32 . 121.5(2) yes Mn1 . N1 . C33 . 121.8(2) yes C32 . N1 . C33 . 116.7(3) yes C36 . N2 . C40 . 118.2(2) yes Mn3 . N3 . C43 . 120.0(2) yes Mn3 . N3 . C44 . 122.6(2) yes C43 . N3 . C44 . 116.5(3) yes Mn2 . N4 . C2 . 121.0(2) yes Mn2 . N4 . C3 . 122.46(19) yes C2 . N4 . C3 . 116.5(3) yes C6 . N5 . C10 . 118.2(2) yes Mn4 . N6 . C13 . 122.3(2) yes Mn4 . N6 . C14 . 122.3(2) yes C13 . N6 . C14 . 115.0(3) yes Mn4 . N7 . C62 . 122.2(2) yes Mn4 . N7 . C63 . 120.6(2) yes C62 . N7 . C63 . 117.2(3) yes C66 . N8 . C70 . 118.5(2) yes Mn2 1_655 N9 . C73 . 122.43(19) yes Mn2 1_655 N9 . C74 . 121.0(2) yes C73 . N9 . C74 . 116.6(3) yes Mn1 . O1 . C22 . 145.0(2) yes Mn2 . O2 . C22 . 132.3(2) yes Mn1 . O3 . Mn2 . 121.75(10) yes Mn1 . O3 . C24 . 150.1(2) yes Mn2 . O3 . C24 . 88.1(2) yes Mn2 . O4 . C24 . 93.77(18) yes Mn2 . O5 . C26 . 142.6(2) yes Mn3 . O11 . C52 . 143.5(3) yes Mn4 . O12 . C52 . 129.1(3) yes Mn3 . O13 . Mn4 . 121.24(14) yes Mn3 . O13 . C54 . 148.4(4) yes Mn4 . O13 . C54 . 89.9(4) yes Mn4 . O14 . C54 . 99.2(3) yes Mn4 . O15 . C56 . 147.7(4) yes C92 . O51 . H920 . 106.1 no C2 . C1 . C5 . 119.7(2) yes C2 . C1 . H11 . 120.5 no C5 . C1 . H11 . 119.8 no C1 . C2 . N4 . 123.7(3) yes C1 . C2 . H21 . 118.5 no N4 . C2 . H21 . 117.9 no N4 . C3 . C4 . 123.6(3) yes N4 . C3 . H31 . 118.0 no C4 . C3 . H31 . 118.4 no C3 . C4 . C5 . 119.8(3) yes C3 . C4 . H41 . 121.0 no C5 . C4 . H41 . 119.2 no C4 . C5 . C1 . 116.7(3) yes C4 . C5 . C6 . 120.1(2) yes C1 . C5 . C6 . 123.2(2) yes C5 . C6 . N5 . 115.3(2) yes C5 . C6 . C7 . 122.3(2) yes N5 . C6 . C7 . 122.4(3) yes C6 . C7 . C8 . 119.5(3) yes C6 . C7 . H71 . 120.1 no C8 . C7 . H71 . 120.4 no C7 . C8 . C9 . 118.1(2) yes C7 . C8 . C16 . 121.0(3) yes C9 . C8 . C16 . 120.9(3) yes C8 . C9 . C10 . 118.8(3) yes C8 . C9 . H91 . 120.3 no C10 . C9 . H91 . 120.9 no C9 . C10 . N5 . 123.0(3) yes C9 . C10 . C11 . 121.3(3) yes N5 . C10 . C11 . 115.7(2) yes C10 . C11 . C12 . 123.1(3) yes C10 . C11 . C15 . 120.7(3) yes C12 . C11 . C15 . 116.2(3) yes C11 . C12 . C13 . 119.2(3) yes C11 . C12 . H121 . 120.8 no C13 . C12 . H121 . 120.0 no C12 . C13 . N6 . 124.9(4) yes C12 . C13 . H131 . 117.6 no N6 . C13 . H131 . 117.5 no N6 . C14 . C15 . 124.4(3) yes N6 . C14 . H141 . 117.8 no C15 . C14 . H141 . 117.7 no C14 . C15 . C11 . 120.2(3) yes C14 . C15 . H151 . 119.8 no C11 . C15 . H151 . 119.9 no C8 . C16 . C17 . 121.6(3) yes C8 . C16 . C21 . 119.9(3) yes C17 . C16 . C21 . 118.5(3) yes C16 . C17 . C18 . 121.4(3) yes C16 . C17 . H171 . 119.5 no C18 . C17 . H171 . 119.1 no C17 . C18 . C19 . 118.8(3) yes C17 . C18 . H181 . 120.6 no C19 . C18 . H181 . 120.6 no C18 . C19 . C20 . 122.1(3) yes C18 . C19 . Br2 . 119.5(3) yes C20 . C19 . Br2 . 118.5(3) yes C19 . C20 . C21 . 118.6(3) yes C19 . C20 . H201 . 121.5 no C21 . C20 . H201 . 119.9 no C16 . C21 . C20 . 120.6(3) yes C16 . C21 . H211 . 120.3 no C20 . C21 . H211 . 119.2 no O2 . C22 . O1 . 126.2(3) yes O2 . C22 . C23 . 116.9(3) yes O1 . C22 . C23 . 116.9(3) yes C22 . C23 . H231 . 110.8 no C22 . C23 . H232 . 109.8 no H231 . C23 . H232 . 109.7 no C22 . C23 . H233 . 109.4 no H231 . C23 . H233 . 108.3 no H232 . C23 . H233 . 108.9 no O3 . C24 . O4 . 120.5(3) yes O3 . C24 . C25 . 119.9(4) yes O4 . C24 . C25 . 119.5(3) yes C24 . C25 . H251 . 110.5 no C24 . C25 . H252 . 110.8 no H251 . C25 . H252 . 109.1 no C24 . C25 . H253 . 110.1 no H251 . C25 . H253 . 108.4 no H252 . C25 . H253 . 107.9 no O5 . C26 . O6 . 124.0(3) yes O5 . C26 . C27 . 120.8(4) yes O6 . C26 . C27 . 115.0(4) yes O5 . C26 . C28 . 109.0(6) yes O6 . C26 . C28 . 116.7(6) yes C26 . C27 . H271 . 108.1 no C26 . C27 . H272 . 110.0 no H271 . C27 . H272 . 109.6 no C26 . C27 . H273 . 111.1 no H271 . C27 . H273 . 108.7 no H272 . C27 . H273 . 109.3 no C26 . C28 . H281 . 112.7 no H281 . C28 . H282 . 109.7 no C26 . C28 . H283 . 102.1 no H281 . C28 . H283 . 101.7 no H282 . C28 . H283 . 108.1 no C32 . C31 . C35 . 119.5(3) yes C32 . C31 . H311 . 120.1 no C35 . C31 . H311 . 120.4 no C31 . C32 . N1 . 123.8(3) yes C31 . C32 . H321 . 118.3 no N1 . C32 . H321 . 117.9 no N1 . C33 . C34 . 123.5(3) yes N1 . C33 . H331 . 117.7 no C34 . C33 . H331 . 118.8 no C33 . C34 . C35 . 119.6(3) yes C33 . C34 . H341 . 120.4 no C35 . C34 . H341 . 120.0 no C34 . C35 . C31 . 117.0(3) yes C34 . C35 . C36 . 120.2(3) yes C31 . C35 . C36 . 122.8(3) yes C35 . C36 . N2 . 115.6(2) yes C35 . C36 . C37 . 121.9(3) yes N2 . C36 . C37 . 122.5(3) yes C36 . C37 . C38 . 119.4(3) yes C36 . C37 . H371 . 121.1 no C38 . C37 . H371 . 119.5 no C37 . C38 . C39 . 117.7(3) yes C37 . C38 . C46 . 121.6(3) yes C39 . C38 . C46 . 120.7(3) yes C38 . C39 . C40 . 119.7(3) yes C38 . C39 . H391 . 120.1 no C40 . C39 . H391 . 120.2 no C39 . C40 . N2 . 122.5(3) yes C39 . C40 . C41 . 121.4(3) yes N2 . C40 . C41 . 116.1(3) yes C40 . C41 . C42 . 123.1(3) yes C40 . C41 . C45 . 120.1(3) yes C42 . C41 . C45 . 116.8(3) yes C41 . C42 . C43 . 120.0(3) yes C41 . C42 . H421 . 120.4 no C43 . C42 . H421 . 119.5 no C42 . C43 . N3 . 123.4(4) yes C42 . C43 . H431 . 118.3 no N3 . C43 . H431 . 118.3 no N3 . C44 . C45 . 123.8(3) yes N3 . C44 . H441 . 118.0 no C45 . C44 . H441 . 118.2 no C44 . C45 . C41 . 119.2(3) yes C44 . C45 . H451 . 120.7 no C41 . C45 . H451 . 120.1 no C38 . C46 . C47 . 120.7(3) yes C38 . C46 . C51 . 120.3(3) yes C47 . C46 . C51 . 119.0(3) yes C46 . C47 . C48 . 120.4(3) yes C46 . C47 . H471 . 119.5 no C48 . C47 . H471 . 120.1 no C47 . C48 . C49 . 119.4(3) yes C47 . C48 . H481 . 119.8 no C49 . C48 . H481 . 120.8 no C48 . C49 . C50 . 121.4(3) yes C48 . C49 . Br1 . 119.5(3) yes C50 . C49 . Br1 . 119.1(3) yes C49 . C50 . C51 . 119.3(3) yes C49 . C50 . H501 . 120.5 no C51 . C50 . H501 . 120.2 no C46 . C51 . C50 . 120.6(3) yes C46 . C51 . H511 . 119.5 no C50 . C51 . H511 . 119.9 no O11 . C52 . O12 . 129.4(4) yes O11 . C52 . C53 . 112.5(5) yes O12 . C52 . C53 . 118.1(5) yes C52 . C53 . H531 . 109.5 no C52 . C53 . H532 . 108.9 no H531 . C53 . H532 . 108.4 no C52 . C53 . H533 . 110.5 no H531 . C53 . H533 . 110.3 no H532 . C53 . H533 . 109.1 no O13 . C54 . O14 . 115.8(5) yes O13 . C54 . C55 . 125.5(6) yes O14 . C54 . C55 . 118.7(4) yes C54 . C55 . H551 . 109.2 no C54 . C55 . H552 . 108.5 no H551 . C55 . H552 . 108.5 no C54 . C55 . H553 . 109.6 no H551 . C55 . H553 . 110.7 no H552 . C55 . H553 . 110.3 no O16 . C56 . O15 . 121.8(6) yes O16 . C56 . C57 . 119.3(7) yes O15 . C56 . C57 . 118.9(7) yes C56 . C57 . H571 . 110.6 no C56 . C57 . H572 . 108.7 no H571 . C57 . H572 . 109.4 no C56 . C57 . H573 . 109.6 no H571 . C57 . H573 . 109.1 no H572 . C57 . H573 . 109.4 no C62 . C61 . C65 . 120.3(3) yes C62 . C61 . H611 . 118.8 no C65 . C61 . H611 . 121.0 no C61 . C62 . N7 . 122.9(3) yes C61 . C62 . H621 . 119.2 no N7 . C62 . H621 . 117.8 no N7 . C63 . C64 . 123.5(3) yes N7 . C63 . H631 . 118.3 no C64 . C63 . H631 . 118.2 no C63 . C64 . C65 . 119.2(3) yes C63 . C64 . H641 . 120.5 no C65 . C64 . H641 . 120.3 no C61 . C65 . C64 . 116.9(3) yes C61 . C65 . C66 . 120.5(3) yes C64 . C65 . C66 . 122.6(3) yes C65 . C66 . N8 . 114.8(2) yes C65 . C66 . C67 . 122.7(3) yes N8 . C66 . C67 . 122.5(3) yes C66 . C67 . C68 . 119.7(3) yes C66 . C67 . H671 . 120.3 no C68 . C67 . H671 . 120.0 no C67 . C68 . C69 . 117.3(3) yes C67 . C68 . C76 . 121.8(3) yes C69 . C68 . C76 . 120.9(3) yes C68 . C69 . C70 . 119.5(3) yes C68 . C69 . H691 . 119.8 no C70 . C69 . H691 . 120.8 no C69 . C70 . N8 . 122.6(3) yes C69 . C70 . C71 . 121.8(2) yes N8 . C70 . C71 . 115.6(2) yes C70 . C71 . C72 . 121.2(2) yes C70 . C71 . C75 . 121.7(2) yes C72 . C71 . C75 . 117.0(3) yes C71 . C72 . C73 . 120.5(3) yes C71 . C72 . H721 . 120.5 no C73 . C72 . H721 . 119.0 no C72 . C73 . N9 . 122.8(3) yes C72 . C73 . H731 . 118.9 no N9 . C73 . H731 . 118.3 no N9 . C74 . C75 . 124.4(3) yes N9 . C74 . H741 . 118.2 no C75 . C74 . H741 . 117.4 no C71 . C75 . C74 . 118.7(3) yes C71 . C75 . H751 . 120.7 no C74 . C75 . H751 . 120.6 no C68 . C76 . C77 . 120.1(3) yes C68 . C76 . C81 . 121.1(3) yes C77 . C76 . C81 . 118.8(3) yes C76 . C77 . C78 . 121.2(3) yes C76 . C77 . H771 . 119.8 no C78 . C77 . H771 . 119.0 no C77 . C78 . C79 . 118.7(3) yes C77 . C78 . H781 . 120.8 no C79 . C78 . H781 . 120.5 no C78 . C79 . C80 . 121.5(3) yes C78 . C79 . Br3 . 118.6(3) yes C80 . C79 . Br3 . 119.9(2) yes C79 . C80 . C81 . 119.8(3) yes C79 . C80 . H801 . 120.9 no C81 . C80 . H801 . 119.3 no C76 . C81 . C80 . 120.0(3) yes C76 . C81 . H811 . 120.8 no C80 . C81 . H811 . 119.2 no O51 . C92 . H921 . 106.6 no O51 . C92 . H922 . 110.0 no H921 . C92 . H922 . 107.9 no O51 . C92 . H923 . 113.1 no H921 . C92 . H923 . 109.8 no H922 . C92 . H923 . 109.3 no C28 . H283 . C27 . 71.3 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_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 O51 . H920 . O6 . 161 0.86 1.97 2.795(2) yes O91 2_567 H923 . O51 . 174 1.46 1.96 3.414(2) yes # Attachment 'gq31.cif' data_gq31_3_123k _database_code_depnum_ccdc_archive 'CCDC 758781' #TrackingRef 'gq31.cif' _audit_creation_date 08-10-21 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'gq31_3_123k_0m in C2/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 26.0368(8) _cell_length_b 15.0774(5) _cell_length_c 8.0056(3) _cell_angle_alpha 90 _cell_angle_beta 107.238(2) _cell_angle_gamma 90 _cell_volume 3001.57(18) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 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 0.0033 0.0016 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 0.0061 0.0033 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 0.0106 0.0060 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' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C29 H26 Br1 N3 O8 Zn1 # Dc = 1.53 Fooo = 1520.00 Mu = 22.03 M = 344.91 # Found Formula = C29 H26 Br1 N3 O8 Zn2 # Dc = 1.67 FOOO = 1520.00 Mu = 29.84 M = 377.60 _chemical_formula_sum 'C29 H26 Br1 N3 O8 Zn2' _chemical_formula_moiety 'C29 H26 Br N3 O8 Zn2' _chemical_compound_source ? _chemical_formula_weight 755.20 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 123 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 2.984 # Sheldrick geometric approximatio 0.76 0.79 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.79 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 123 _diffrn_reflns_number 43719 _reflns_number_total 6308 _diffrn_reflns_av_R_equivalents 0.040 # Number of reflections with Friedels Law is 6308 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6316 _diffrn_reflns_theta_min 2.702 _diffrn_reflns_theta_max 34.408 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 34.408 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -41 _reflns_limit_h_max 39 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.34 _refine_diff_density_max 0.83 _refine_ls_number_reflns 3885 _refine_ls_number_restraints 0 _refine_ls_number_parameters 197 #_refine_ls_R_factor_ref 0.0260 _refine_ls_wR_factor_ref 0.0285 _refine_ls_goodness_of_fit_ref 1.0291 #_reflns_number_all 6301 _refine_ls_R_factor_all 0.0476 _refine_ls_wR_factor_all 0.0441 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 3885 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_gt 0.0285 _refine_ls_shift/su_max 0.002247 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _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: 0.312 0.601E-01 0.101 -0.712E-01 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Br1 Br 0.5000 -0.101417(17) 0.7500 0.0395 1.0000 Uani S T . . . . Zn1 Zn 0.289338(7) 0.691701(11) 0.11368(2) 0.0149 1.0000 Uani . . . . . . O1 O 0.25042(5) 0.60200(8) -0.06998(17) 0.0242 1.0000 Uani . . . . . . O2 O 0.18770(6) 0.69043(8) -0.23785(17) 0.0301 1.0000 Uani . . . . . . O3 O 0.33299(5) 0.72875(8) -0.05143(16) 0.0234 1.0000 Uani . . . . . . O4 O 0.27130(5) 0.81647(10) -0.22588(17) 0.0296 1.0000 Uani . . . . . . N1 N 0.34372(5) 0.61203(8) 0.28121(16) 0.0149 1.0000 Uani . . . . . . N2 N 0.5000 0.49359(11) 0.7500 0.0125 1.0000 Uani S T . . . . C1 C 0.5000 0.02425(15) 0.7500 0.0240 1.0000 Uani S T . . . . C2 C 0.45148(7) 0.06928(11) 0.6945(2) 0.0246 1.0000 Uani . . . . . . C3 C 0.45173(6) 0.16161(11) 0.6946(2) 0.0209 1.0000 Uani . . . . . . C4 C 0.5000 0.20894(13) 0.7500 0.0162 1.0000 Uani S T . . . . C5 C 0.5000 0.30726(14) 0.7500 0.0143 1.0000 Uani S T . . . . C6 C 0.45993(5) 0.35534(9) 0.62891(18) 0.0149 1.0000 Uani . . . . . . C7 C 0.46123(5) 0.44811(9) 0.63431(17) 0.0126 1.0000 Uani . . . . . . C8 C 0.41979(5) 0.50373(9) 0.51092(17) 0.0121 1.0000 Uani . . . . . . C9 C 0.37475(5) 0.46757(10) 0.38896(19) 0.0156 1.0000 Uani . . . . . . C10 C 0.33810(6) 0.52361(10) 0.27738(19) 0.0167 1.0000 Uani . . . . . . C11 C 0.38664(6) 0.64726(10) 0.40047(19) 0.0165 1.0000 Uani . . . . . . C12 C 0.42491(6) 0.59606(10) 0.51654(18) 0.0155 1.0000 Uani . . . . . . C13 C 0.21033(6) 0.61657(10) -0.19924(19) 0.0176 1.0000 Uani . . . . . . C14 C 0.18779(8) 0.53998(11) -0.3196(2) 0.0280 1.0000 Uani . . . . . . C15 C 0.31619(6) 0.77947(10) -0.1809(2) 0.0187 1.0000 Uani . . . . . . C16 C 0.35441(8) 0.79757(15) -0.2878(3) 0.0335 1.0000 Uani . . . . . . H21 H 0.4197 0.0374 0.6565 0.0304 1.0000 Uiso R . . . . . H31 H 0.4195 0.1925 0.6561 0.0254 1.0000 Uiso R . . . . . H61 H 0.4326 0.3261 0.5469 0.0175 1.0000 Uiso R . . . . . H91 H 0.3693 0.4069 0.3821 0.0179 1.0000 Uiso R . . . . . H101 H 0.3088 0.4993 0.1956 0.0196 1.0000 Uiso R . . . . . H111 H 0.3900 0.7085 0.4033 0.0184 1.0000 Uiso R . . . . . H121 H 0.4541 0.6240 0.5990 0.0179 1.0000 Uiso R . . . . . H141 H 0.1492 0.5458 -0.3615 0.0399 1.0000 Uiso R . . . . . H142 H 0.2019 0.5422 -0.4163 0.0410 1.0000 Uiso R . . . . . H143 H 0.1978 0.4855 -0.2587 0.0403 1.0000 Uiso R . . . . . H161 H 0.3342 0.7957 -0.4051 0.0559 1.0000 Uiso R . . . . . H162 H 0.3686 0.8542 -0.2573 0.0564 1.0000 Uiso R . . . . . H163 H 0.3814 0.7544 -0.2626 0.0558 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 Br1 0.03875(15) 0.01462(10) 0.0682(2) 0.0000 0.02079(15) 0.0000 Zn1 0.01347(7) 0.01417(7) 0.01393(6) 0.00222(6) -0.00054(5) 0.00301(6) O1 0.0217(5) 0.0206(5) 0.0237(5) -0.0038(4) -0.0034(4) 0.0012(4) O2 0.0348(7) 0.0181(5) 0.0267(6) -0.0030(5) -0.0076(5) 0.0049(5) O3 0.0199(5) 0.0251(6) 0.0257(6) 0.0094(5) 0.0073(4) 0.0040(4) O4 0.0247(6) 0.0392(7) 0.0274(6) 0.0128(5) 0.0118(5) 0.0153(5) N1 0.0130(5) 0.0161(5) 0.0137(5) 0.0014(4) 0.0010(4) 0.0019(4) N2 0.0097(6) 0.0147(7) 0.0117(6) 0.0000 0.0012(5) 0.0000 C1 0.0241(10) 0.0149(9) 0.0329(12) 0.0000 0.0084(9) 0.0000 C2 0.0194(7) 0.0172(6) 0.0352(9) -0.0021(6) 0.0051(6) -0.0041(5) C3 0.0144(6) 0.0178(6) 0.0270(7) -0.0014(5) 0.0011(5) -0.0010(5) C4 0.0130(7) 0.0141(8) 0.0193(8) 0.0000 0.0013(6) 0.0000 C5 0.0106(7) 0.0153(7) 0.0153(7) 0.0000 0.0011(5) 0.0000 C6 0.0117(5) 0.0155(5) 0.0147(6) -0.0003(4) -0.0005(4) -0.0003(4) C7 0.0092(5) 0.0159(5) 0.0113(5) 0.0011(4) 0.0010(4) 0.0006(4) C8 0.0095(5) 0.0146(5) 0.0112(5) 0.0011(4) 0.0016(4) 0.0008(4) C9 0.0121(5) 0.0152(6) 0.0156(6) 0.0017(4) -0.0018(4) -0.0013(4) C10 0.0130(5) 0.0176(6) 0.0159(6) 0.0020(5) -0.0013(4) 0.0000(5) C11 0.0163(6) 0.0151(6) 0.0153(6) 0.0001(4) 0.0002(5) 0.0015(4) C12 0.0129(5) 0.0157(6) 0.0149(6) 0.0000(4) -0.0005(5) -0.0006(4) C13 0.0179(6) 0.0174(6) 0.0165(6) -0.0023(5) 0.0038(5) -0.0008(5) C14 0.0297(8) 0.0201(7) 0.0272(8) -0.0079(6) -0.0025(6) -0.0004(6) C15 0.0192(6) 0.0180(6) 0.0192(6) 0.0014(5) 0.0062(5) 0.0031(5) C16 0.0343(9) 0.0402(11) 0.0336(9) 0.0140(8) 0.0219(8) 0.0117(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.12487(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 . C1 . 1.895(2) yes Zn1 . Zn1 4_565 2.8965(3) yes Zn1 . O4 4_565 2.0385(13) yes Zn1 . O2 4_565 2.0375(13) yes Zn1 . O1 . 2.0334(12) yes Zn1 . O3 . 2.0595(12) yes Zn1 . N1 . 2.0301(12) yes O1 . C13 . 1.2524(18) yes O2 . C13 . 1.2550(19) yes O3 . C15 . 1.2576(19) yes O4 . C15 . 1.2479(19) yes N1 . C10 . 1.3405(19) yes N1 . C11 . 1.3454(18) yes N2 . C7 5_656 1.3390(15) yes N2 . C7 . 1.3390(15) yes C1 . C2 5_656 1.386(2) yes C1 . C2 . 1.386(2) yes C2 . C3 . 1.392(2) yes C2 . H21 . 0.928 no C3 . C4 . 1.3982(18) yes C3 . H31 . 0.930 no C4 . C5 . 1.482(3) yes C5 . C6 5_656 1.3981(17) yes C5 . C6 . 1.3981(17) yes C6 . C7 . 1.3994(19) yes C6 . H61 . 0.924 no C7 . C8 . 1.4871(18) yes C8 . C9 . 1.3955(18) yes C8 . C12 . 1.398(2) yes C9 . C10 . 1.3846(19) yes C9 . H91 . 0.925 no C10 . H101 . 0.922 no C11 . C12 . 1.3797(19) yes C11 . H111 . 0.927 no C12 . H121 . 0.946 no C13 . C14 . 1.507(2) yes C14 . H141 . 0.965 no C14 . H142 . 0.951 no C14 . H143 . 0.951 no C15 . C16 . 1.517(2) yes C16 . H161 . 0.931 no C16 . H162 . 0.934 no C16 . H163 . 0.935 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Zn1 4_565 Zn1 . O4 4_565 79.49(4) yes Zn1 4_565 Zn1 . O2 4_565 80.09(4) yes O4 4_565 Zn1 . O2 4_565 89.50(6) yes Zn1 4_565 Zn1 . O1 . 80.86(3) yes O4 4_565 Zn1 . O1 . 89.62(6) yes O2 4_565 Zn1 . O1 . 160.77(5) yes Zn1 4_565 Zn1 . O3 . 81.61(3) yes O4 4_565 Zn1 . O3 . 161.09(5) yes O2 4_565 Zn1 . O3 . 86.48(6) yes O1 . Zn1 . O3 . 88.16(6) yes Zn1 4_565 Zn1 . N1 . 177.74(4) yes O4 4_565 Zn1 . N1 . 98.79(5) yes O2 4_565 Zn1 . N1 . 98.48(5) yes O1 . Zn1 . N1 . 100.64(5) yes O3 . Zn1 . N1 . 100.08(5) yes Zn1 . O1 . C13 . 126.55(11) yes Zn1 4_565 O2 . C13 . 127.25(10) yes Zn1 . O3 . C15 . 124.77(11) yes Zn1 4_565 O4 . C15 . 128.84(11) yes Zn1 . N1 . C10 . 121.55(9) yes Zn1 . N1 . C11 . 120.35(10) yes C10 . N1 . C11 . 118.10(12) yes C7 5_656 N2 . C7 . 118.39(17) yes Br1 . C1 . C2 5_656 119.33(10) yes Br1 . C1 . C2 . 119.33(10) yes C2 5_656 C1 . C2 . 121.3(2) yes C1 . C2 . C3 . 119.07(15) yes C1 . C2 . H21 . 119.4 no C3 . C2 . H21 . 121.5 no C2 . C3 . C4 . 120.95(15) yes C2 . C3 . H31 . 119.8 no C4 . C3 . H31 . 119.2 no C3 5_656 C4 . C3 . 118.62(19) yes C3 5_656 C4 . C5 . 120.69(9) yes C3 . C4 . C5 . 120.69(9) yes C4 . C5 . C6 5_656 121.24(9) yes C4 . C5 . C6 . 121.24(9) yes C6 5_656 C5 . C6 . 117.53(18) yes C5 . C6 . C7 . 119.38(13) yes C5 . C6 . H61 . 120.3 no C7 . C6 . H61 . 120.3 no C6 . C7 . N2 . 122.66(12) yes C6 . C7 . C8 . 122.48(12) yes N2 . C7 . C8 . 114.86(13) yes C7 . C8 . C9 . 122.57(12) yes C7 . C8 . C12 . 119.78(12) yes C9 . C8 . C12 . 117.64(12) yes C8 . C9 . C10 . 119.25(13) yes C8 . C9 . H91 . 120.7 no C10 . C9 . H91 . 120.0 no C9 . C10 . N1 . 122.85(13) yes C9 . C10 . H101 . 118.8 no N1 . C10 . H101 . 118.3 no N1 . C11 . C12 . 122.64(13) yes N1 . C11 . H111 . 117.6 no C12 . C11 . H111 . 119.8 no C8 . C12 . C11 . 119.51(12) yes C8 . C12 . H121 . 121.0 no C11 . C12 . H121 . 119.5 no O2 . C13 . O1 . 125.07(14) yes O2 . C13 . C14 . 117.20(14) yes O1 . C13 . C14 . 117.73(14) yes C13 . C14 . H141 . 108.7 no C13 . C14 . H142 . 108.8 no H141 . C14 . H142 . 109.2 no C13 . C14 . H143 . 109.8 no H141 . C14 . H143 . 110.8 no H142 . C14 . H143 . 109.5 no O3 . C15 . O4 . 125.25(15) yes O3 . C15 . C16 . 116.61(14) yes O4 . C15 . C16 . 118.13(14) yes C15 . C16 . H161 . 107.1 no C15 . C16 . H162 . 106.9 no H161 . C16 . H162 . 110.7 no C15 . C16 . H163 . 109.3 no H161 . C16 . H163 . 111.2 no H162 . C16 . H163 . 111.5 no # Attachment 'gq86.cif' data_gq86 _database_code_depnum_ccdc_archive 'CCDC 758782' #TrackingRef 'gq86.cif' _audit_creation_date 09-10-15 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 'gq86_123k_0ma in P2(1)/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.1338(4) _cell_length_b 14.9020(7) _cell_length_c 25.2700(10) _cell_angle_alpha 90 _cell_angle_beta 90.457(3) _cell_angle_gamma 90 _cell_volume 3062.9(2) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 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 0.0033 0.0016 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 0.0061 0.0033 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 0.0106 0.0060 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C30 H29 N3 O8 S1 Zn2 # Dc = 1.57 Fooo = 1480.00 Mu = 16.89 M = 722.40 # Found Formula = C30 H29 N3 O8 S1 Zn2 # Dc = 1.57 FOOO = 1480.00 Mu = 16.89 M = 722.40 _chemical_formula_sum 'C30 H29 N3 O8 S1 Zn2' _chemical_formula_moiety 'C30 H29 N3 O8 S1 Zn2' _chemical_compound_source ? _chemical_formula_weight 722.40 _cell_measurement_reflns_used 4893 _cell_measurement_theta_min 3 _cell_measurement_theta_max 26 _cell_measurement_temperature 123 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.09 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 1.689 # Sheldrick geometric approximatio 0.75 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.86 _diffrn_measurement_device 'Bruker Kappa Apex2' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 123 _diffrn_reflns_number 42659 _reflns_number_total 7103 _diffrn_reflns_av_R_equivalents 0.077 # Number of reflections with Friedels Law is 7103 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7101 _diffrn_reflns_theta_min 1.612 _diffrn_reflns_theta_max 27.594 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.594 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _oxford_diffrn_Wilson_B_factor 1.54 _oxford_diffrn_Wilson_scale 371.85 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.47 _refine_diff_density_max 1.14 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 4056 _refine_ls_number_restraints 0 _refine_ls_number_parameters 397 _oxford_refine_ls_R_factor_ref 0.0389 _refine_ls_wR_factor_ref 0.0406 _refine_ls_goodness_of_fit_ref 1.1055 _refine_ls_shift/su_max 0.000203 # The values computed from all data _oxford_reflns_number_all 7078 _refine_ls_R_factor_all 0.0861 _refine_ls_wR_factor_all 0.1174 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4056 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_gt 0.0406 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _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: 0.167 0.150 0.552E-01 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Zn1 Zn -0.18277(6) -0.18650(3) 0.289527(16) 0.0168 1.0000 Uani . . . . . . . Zn2 Zn -0.31705(6) -0.29456(3) 0.204838(17) 0.0188 1.0000 Uani . . . . . . . N1 N -0.0711(4) -0.10817(19) 0.34475(11) 0.0155 1.0000 Uani . . . . . . . N2 N 0.2497(4) 0.00150(19) 0.49976(12) 0.0148 1.0000 Uani . . . . . . . N3 N 0.5696(4) -0.1253(2) 0.65126(11) 0.0172 1.0000 Uani . . . . . . . C1 C -0.0613(5) -0.0189(2) 0.33968(14) 0.0187 1.0000 Uani . . . . . . . C2 C 0.0144(4) 0.0357(2) 0.37627(13) 0.0169 1.0000 Uani . . . . . . . C3 C 0.0869(4) -0.0034(2) 0.42095(13) 0.0147 1.0000 Uani . . . . . . . C4 C 0.0786(4) -0.0958(2) 0.42577(13) 0.0150 1.0000 Uani . . . . . . . C5 C -0.0004(4) -0.1453(2) 0.38756(14) 0.0166 1.0000 Uani . . . . . . . C6 C 0.1712(4) 0.0509(2) 0.46280(13) 0.0136 1.0000 Uani . . . . . . . C7 C 0.1698(5) 0.1437(2) 0.46342(14) 0.0186 1.0000 Uani . . . . . . . C8 C 0.2529(5) 0.1901(2) 0.50328(14) 0.0183 1.0000 Uani . . . . . . . C9 C 0.3362(4) 0.1378(2) 0.54131(13) 0.0156 1.0000 Uani . . . . . . . C10 C 0.3299(4) 0.0453(2) 0.53846(13) 0.0139 1.0000 Uani . . . . . . . C11 C 0.4967(4) -0.1586(2) 0.60762(14) 0.0180 1.0000 Uani . . . . . . . C12 C 0.4168(5) -0.1054(2) 0.57107(14) 0.0180 1.0000 Uani . . . . . . . C13 C 0.4119(4) -0.0136(2) 0.57833(13) 0.0146 1.0000 Uani . . . . . . . C14 C 0.4848(5) 0.0214(3) 0.62416(14) 0.0203 1.0000 Uani . . . . . . . C15 C 0.5614(5) -0.0362(3) 0.65873(14) 0.0213 1.0000 Uani . . . . . . . C16 C 0.2551(5) 0.2888(2) 0.50587(15) 0.0212 1.0000 Uani . . . . . . . C17 C 0.2842(5) 0.3335(3) 0.55407(16) 0.0276 1.0000 Uani . . . . . . . C18 C 0.2871(6) 0.4255(3) 0.55722(18) 0.0342 1.0000 Uani . . . . . . . C19 C 0.2596(6) 0.4773(3) 0.51250(18) 0.0330 1.0000 Uani . . . . . . . C20 C 0.2307(6) 0.4349(3) 0.46463(19) 0.0350 1.0000 Uani . . . . . . . C21 C 0.2292(5) 0.3422(3) 0.46145(17) 0.0273 1.0000 Uani . . . . . . . S1 S 0.2694(2) 0.59502(8) 0.52210(6) 0.0506 1.0000 Uani . . . . . . . C22 C 0.2017(9) 0.6336(4) 0.4624(3) 0.0740 1.0000 Uani . . . . . . . O1 O -0.0001(3) -0.18732(18) 0.23413(10) 0.0259 1.0000 Uani . . . . . . . O2 O -0.1026(3) -0.26503(18) 0.16656(11) 0.0290 1.0000 Uani . . . . . . . O3 O -0.3048(4) -0.09009(18) 0.24783(11) 0.0290 1.0000 Uani . . . . . . . O4 O -0.4006(4) -0.17259(19) 0.18111(11) 0.0316 1.0000 Uani . . . . . . . O5 O -0.4011(3) -0.21615(19) 0.32600(11) 0.0285 1.0000 Uani . . . . . . . O6 O -0.5018(4) -0.2960(2) 0.25926(11) 0.0331 1.0000 Uani . . . . . . . O7 O -0.0997(4) -0.30799(17) 0.31515(11) 0.0274 1.0000 Uani . . . . . . . O8 O -0.1918(4) -0.38921(18) 0.24701(11) 0.0297 1.0000 Uani . . . . . . . C23 C 0.0097(5) -0.2227(2) 0.18939(14) 0.0202 1.0000 Uani . . . . . . . C24 C 0.1693(6) -0.2131(3) 0.1606(2) 0.0415 1.0000 Uani . . . . . . . C25 C -0.3843(5) -0.1001(3) 0.20528(15) 0.0208 1.0000 Uani . . . . . . . C26 C -0.4659(6) -0.0183(3) 0.18240(18) 0.0355 1.0000 Uani . . . . . . . C27 C -0.5146(5) -0.2577(2) 0.30294(15) 0.0207 1.0000 Uani . . . . . . . C28 C -0.6793(6) -0.2619(3) 0.32938(19) 0.0399 1.0000 Uani . . . . . . . C29 C -0.1144(5) -0.3801(2) 0.29007(15) 0.0189 1.0000 Uani . . . . . . . C30 C -0.0308(6) -0.4623(3) 0.31236(17) 0.0320 1.0000 Uani . . . . . . . H221 H 0.1974 0.6970 0.4652 0.1100 1.0000 Uiso R . . . . . . H223 H 0.0964 0.6102 0.4550 0.1097 1.0000 Uiso R . . . . . . H222 H 0.2774 0.6164 0.4359 0.1098 1.0000 Uiso R . . . . . . H11 H -0.1075 0.0063 0.3097 0.0228 1.0000 Uiso R . . . . . . H21 H 0.0192 0.0973 0.3712 0.0202 1.0000 Uiso R . . . . . . H41 H 0.1246 -0.1238 0.4547 0.0186 1.0000 Uiso R . . . . . . H51 H -0.0084 -0.2063 0.3914 0.0200 1.0000 Uiso R . . . . . . H71 H 0.1126 0.1750 0.4373 0.0230 1.0000 Uiso R . . . . . . H91 H 0.3965 0.1652 0.5683 0.0196 1.0000 Uiso R . . . . . . H111 H 0.5013 -0.2199 0.6021 0.0218 1.0000 Uiso R . . . . . . H121 H 0.3694 -0.1307 0.5411 0.0220 1.0000 Uiso R . . . . . . H141 H 0.4807 0.0825 0.6312 0.0251 1.0000 Uiso R . . . . . . H151 H 0.6076 -0.0130 0.6884 0.0246 1.0000 Uiso R . . . . . . H171 H 0.2998 0.3001 0.5844 0.0344 1.0000 Uiso R . . . . . . H181 H 0.3086 0.4535 0.5898 0.0412 1.0000 Uiso R . . . . . . H201 H 0.2114 0.4682 0.4340 0.0418 1.0000 Uiso R . . . . . . H211 H 0.2123 0.3153 0.4288 0.0324 1.0000 Uiso R . . . . . . H241 H 0.1728 -0.2514 0.1302 0.0630 1.0000 Uiso R . . . . . . H243 H 0.2592 -0.2266 0.1838 0.0637 1.0000 Uiso R . . . . . . H242 H 0.1798 -0.1524 0.1491 0.0638 1.0000 Uiso R . . . . . . H261 H -0.4470 -0.0156 0.1451 0.0543 1.0000 Uiso R . . . . . . H262 H -0.5808 -0.0218 0.1887 0.0546 1.0000 Uiso R . . . . . . H263 H -0.4248 0.0345 0.1989 0.0549 1.0000 Uiso R . . . . . . H282 H -0.7287 -0.3194 0.3243 0.0612 1.0000 Uiso R . . . . . . H281 H -0.6661 -0.2507 0.3663 0.0608 1.0000 Uiso R . . . . . . H283 H -0.7497 -0.2174 0.3142 0.0618 1.0000 Uiso R . . . . . . H302 H -0.0799 -0.5147 0.2990 0.0486 1.0000 Uiso R . . . . . . H301 H -0.0371 -0.4622 0.3502 0.0479 1.0000 Uiso R . . . . . . H303 H 0.0824 -0.4613 0.3028 0.0485 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 Zn1 0.0174(3) 0.0169(2) 0.0161(2) -0.00468(17) -0.00404(16) -0.00088(17) Zn2 0.0174(3) 0.0217(2) 0.0172(2) -0.00754(18) -0.00369(17) -0.00210(18) N1 0.0147(17) 0.0170(15) 0.0148(15) 0.0004(12) -0.0018(12) -0.0008(12) N2 0.0117(12) 0.0192(15) 0.0136(13) 0.0015(12) 0.0003(10) 0.0012(12) N3 0.0134(17) 0.0246(16) 0.0137(15) 0.0059(12) -0.0009(12) 0.0000(12) C1 0.020(2) 0.0196(18) 0.0165(18) 0.0024(14) -0.0044(15) -0.0003(14) C2 0.017(2) 0.0185(17) 0.0154(17) 0.0029(14) -0.0043(14) -0.0027(14) C3 0.012(2) 0.0195(17) 0.0130(17) -0.0005(14) 0.0009(14) -0.0020(14) C4 0.016(2) 0.0156(16) 0.0139(17) 0.0025(13) -0.0044(14) 0.0044(13) C5 0.017(2) 0.0131(16) 0.0193(19) 0.0018(14) 0.0006(15) -0.0009(14) C6 0.009(2) 0.0174(17) 0.0141(18) -0.0009(13) 0.0026(14) 0.0008(13) C7 0.018(2) 0.0234(19) 0.0148(18) 0.0030(15) -0.0014(15) -0.0001(15) C8 0.0187(15) 0.0219(18) 0.0144(15) 0.0014(15) -0.0004(12) -0.0010(14) C9 0.0118(19) 0.0233(18) 0.0118(17) -0.0003(14) -0.0015(14) -0.0013(14) C10 0.011(2) 0.0212(18) 0.0102(17) 0.0009(14) 0.0005(14) -0.0003(14) C11 0.017(2) 0.0185(17) 0.0184(18) 0.0012(14) -0.0003(15) 0.0003(14) C12 0.019(2) 0.0229(18) 0.0121(17) 0.0001(14) -0.0019(15) -0.0006(15) C13 0.012(2) 0.0211(18) 0.0110(17) 0.0009(14) 0.0031(14) 0.0048(14) C14 0.023(2) 0.0218(18) 0.0157(18) -0.0018(15) -0.0045(15) 0.0046(15) C15 0.023(2) 0.027(2) 0.0134(18) -0.0017(15) -0.0063(15) -0.0004(16) C16 0.0210(17) 0.0192(19) 0.0235(19) 0.0008(15) -0.0004(15) -0.0016(16) C17 0.039(3) 0.022(2) 0.022(2) -0.0034(16) -0.0061(18) -0.0021(17) C18 0.046(3) 0.026(2) 0.031(2) -0.0056(18) -0.006(2) -0.0028(19) C19 0.034(2) 0.025(2) 0.041(3) -0.0061(18) 0.002(2) -0.0005(18) C20 0.041(3) 0.028(2) 0.036(3) 0.0057(19) -0.005(2) 0.0022(19) C21 0.032(2) 0.023(2) 0.027(2) 0.0010(16) -0.0046(18) 0.0019(17) S1 0.0718(10) 0.0252(6) 0.0545(8) -0.0049(6) -0.0101(7) 0.0004(6) C22 0.101(6) 0.054(4) 0.067(4) -0.023(3) 0.001(4) -0.008(4) O1 0.0238(16) 0.0309(15) 0.0230(14) -0.0074(12) 0.0039(11) -0.0055(11) O2 0.0247(17) 0.0300(15) 0.0323(16) -0.0122(12) 0.0019(12) -0.0080(12) O3 0.0353(18) 0.0234(14) 0.0282(15) -0.0014(12) -0.0111(13) 0.0069(12) O4 0.0336(19) 0.0272(15) 0.0337(16) -0.0037(13) -0.0132(13) 0.0038(13) O5 0.0236(16) 0.0302(15) 0.0317(15) -0.0099(12) 0.0014(12) -0.0045(12) O6 0.0274(18) 0.0433(18) 0.0287(15) -0.0165(13) 0.0029(12) -0.0089(13) O7 0.0348(18) 0.0202(14) 0.0269(14) -0.0029(11) -0.0091(12) 0.0005(11) O8 0.0377(18) 0.0235(14) 0.0277(15) -0.0054(12) -0.0138(13) 0.0031(12) C23 0.023(2) 0.0169(17) 0.0212(19) -0.0027(15) 0.0022(15) 0.0031(15) C24 0.026(3) 0.049(3) 0.050(3) -0.013(2) 0.019(2) -0.009(2) C25 0.017(2) 0.0238(19) 0.0214(19) 0.0009(16) -0.0035(15) -0.0004(15) C26 0.039(3) 0.030(2) 0.037(3) 0.0068(19) -0.011(2) 0.0071(19) C27 0.017(2) 0.0225(18) 0.023(2) 0.0002(15) 0.0026(15) -0.0005(15) C28 0.027(3) 0.050(3) 0.043(3) -0.013(2) 0.012(2) -0.007(2) C29 0.016(2) 0.0168(17) 0.024(2) -0.0009(15) 0.0016(15) -0.0014(14) C30 0.037(3) 0.025(2) 0.034(2) 0.0040(18) -0.0088(19) 0.0091(18) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.04043(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . Zn2 . 2.8859(5) yes Zn1 . N1 . 2.028(3) yes Zn1 . O1 . 2.050(3) yes Zn1 . O3 . 2.035(3) yes Zn1 . O5 . 2.056(3) yes Zn1 . O7 . 2.036(3) yes Zn2 . N3 4_444 2.022(3) yes Zn2 . O2 . 2.049(3) yes Zn2 . O4 . 2.029(3) yes Zn2 . O6 . 2.045(3) yes Zn2 . O8 . 2.036(3) yes N1 . C1 . 1.339(5) yes N1 . C5 . 1.341(4) yes N2 . C6 . 1.346(4) yes N2 . C10 . 1.341(4) yes N3 . C11 . 1.343(5) yes N3 . C15 . 1.343(5) yes C1 . C2 . 1.374(5) yes C1 . H11 . 0.922 no C2 . C3 . 1.397(5) yes C2 . H21 . 0.928 no C3 . C4 . 1.384(5) yes C3 . C6 . 1.494(5) yes C4 . C5 . 1.371(5) yes C4 . H41 . 0.918 no C5 . H51 . 0.916 no C6 . C7 . 1.383(5) yes C7 . C8 . 1.393(5) yes C7 . H71 . 0.931 no C8 . C9 . 1.407(5) yes C8 . C16 . 1.473(5) yes C9 . C10 . 1.381(5) yes C9 . H91 . 0.932 no C10 . C13 . 1.490(5) yes C11 . C12 . 1.377(5) yes C11 . H111 . 0.925 no C12 . C13 . 1.381(5) yes C12 . H121 . 0.927 no C13 . C14 . 1.398(5) yes C14 . C15 . 1.371(5) yes C14 . H141 . 0.928 no C15 . H151 . 0.905 no C16 . C17 . 1.407(5) yes C16 . C21 . 1.391(5) yes C17 . C18 . 1.374(6) yes C17 . H171 . 0.923 no C18 . C19 . 1.385(6) yes C18 . H181 . 0.939 no C19 . C20 . 1.383(6) yes C19 . S1 . 1.773(4) yes C20 . C21 . 1.383(6) yes C20 . H201 . 0.932 no C21 . H211 . 0.925 no S1 . C22 . 1.702(7) yes C22 . H221 . 0.949 no C22 . H223 . 0.942 no C22 . H222 . 0.948 no O1 . C23 . 1.250(4) yes O2 . C23 . 1.247(4) yes O3 . C25 . 1.259(4) yes O4 . C25 . 1.247(5) yes O5 . C27 . 1.251(4) yes O6 . C27 . 1.247(5) yes O7 . C29 . 1.253(4) yes O8 . C29 . 1.260(4) yes C23 . C24 . 1.501(6) yes C24 . H241 . 0.957 no C24 . H243 . 0.955 no C24 . H242 . 0.954 no C25 . C26 . 1.501(5) yes C26 . H261 . 0.958 no C26 . H262 . 0.951 no C26 . H263 . 0.951 no C27 . C28 . 1.503(6) yes C28 . H282 . 0.955 no C28 . H281 . 0.953 no C28 . H283 . 0.956 no C29 . C30 . 1.508(5) yes C30 . H302 . 0.939 no C30 . H301 . 0.957 no C30 . H303 . 0.954 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Zn2 . Zn1 . N1 . 174.87(9) yes Zn2 . Zn1 . O1 . 76.26(7) yes N1 . Zn1 . O1 . 98.64(11) yes Zn2 . Zn1 . O3 . 80.20(8) yes N1 . Zn1 . O3 . 99.42(11) yes O1 . Zn1 . O3 . 90.22(12) yes Zn2 . Zn1 . O5 . 83.64(7) yes N1 . Zn1 . O5 . 101.47(11) yes O1 . Zn1 . O5 . 159.83(10) yes O3 . Zn1 . O5 . 87.96(12) yes Zn2 . Zn1 . O7 . 82.09(7) yes N1 . Zn1 . O7 . 98.47(11) yes O1 . Zn1 . O7 . 88.36(12) yes O3 . Zn1 . O7 . 162.06(11) yes O5 . Zn1 . O7 . 87.24(12) yes Zn1 . Zn2 . N3 4_444 173.64(9) yes Zn1 . Zn2 . O2 . 84.93(7) yes N3 4_444 Zn2 . O2 . 101.30(11) yes Zn1 . Zn2 . O4 . 80.98(8) yes N3 4_444 Zn2 . O4 . 100.45(12) yes O2 . Zn2 . O4 . 87.28(12) yes Zn1 . Zn2 . O6 . 77.46(8) yes N3 4_444 Zn2 . O6 . 96.36(11) yes O2 . Zn2 . O6 . 162.25(11) yes O4 . Zn2 . O6 . 87.82(13) yes Zn1 . Zn2 . O8 . 79.26(7) yes N3 4_444 Zn2 . O8 . 99.49(12) yes O2 . Zn2 . O8 . 88.36(12) yes O4 . Zn2 . O8 . 160.06(11) yes O6 . Zn2 . O8 . 90.47(13) yes Zn1 . N1 . C1 . 122.2(2) yes Zn1 . N1 . C5 . 120.3(2) yes C1 . N1 . C5 . 117.5(3) yes C6 . N2 . C10 . 117.7(3) yes Zn2 4_645 N3 . C11 . 121.8(2) yes Zn2 4_645 N3 . C15 . 120.9(2) yes C11 . N3 . C15 . 117.3(3) yes N1 . C1 . C2 . 123.4(3) yes N1 . C1 . H11 . 117.3 no C2 . C1 . H11 . 119.3 no C1 . C2 . C3 . 118.7(3) yes C1 . C2 . H21 . 120.8 no C3 . C2 . H21 . 120.5 no C2 . C3 . C4 . 117.8(3) yes C2 . C3 . C6 . 122.3(3) yes C4 . C3 . C6 . 119.9(3) yes C3 . C4 . C5 . 119.7(3) yes C3 . C4 . H41 . 120.1 no C5 . C4 . H41 . 120.1 no C4 . C5 . N1 . 122.8(3) yes C4 . C5 . H51 . 119.5 no N1 . C5 . H51 . 117.7 no C3 . C6 . N2 . 114.0(3) yes C3 . C6 . C7 . 123.1(3) yes N2 . C6 . C7 . 122.9(3) yes C6 . C7 . C8 . 120.0(3) yes C6 . C7 . H71 . 119.9 no C8 . C7 . H71 . 120.1 no C7 . C8 . C9 . 116.6(3) yes C7 . C8 . C16 . 122.3(3) yes C9 . C8 . C16 . 121.2(3) yes C8 . C9 . C10 . 120.0(3) yes C8 . C9 . H91 . 120.3 no C10 . C9 . H91 . 119.7 no C9 . C10 . N2 . 122.8(3) yes C9 . C10 . C13 . 122.4(3) yes N2 . C10 . C13 . 114.8(3) yes N3 . C11 . C12 . 122.8(3) yes N3 . C11 . H111 . 118.0 no C12 . C11 . H111 . 119.2 no C11 . C12 . C13 . 119.7(3) yes C11 . C12 . H121 . 120.3 no C13 . C12 . H121 . 119.9 no C10 . C13 . C12 . 120.5(3) yes C10 . C13 . C14 . 121.7(3) yes C12 . C13 . C14 . 117.8(3) yes C13 . C14 . C15 . 118.8(3) yes C13 . C14 . H141 . 120.6 no C15 . C14 . H141 . 120.6 no C14 . C15 . N3 . 123.6(3) yes C14 . C15 . H151 . 118.2 no N3 . C15 . H151 . 118.2 no C8 . C16 . C17 . 120.9(3) yes C8 . C16 . C21 . 122.3(3) yes C17 . C16 . C21 . 116.8(4) yes C16 . C17 . C18 . 121.7(4) yes C16 . C17 . H171 . 119.1 no C18 . C17 . H171 . 119.2 no C17 . C18 . C19 . 120.4(4) yes C17 . C18 . H181 . 119.9 no C19 . C18 . H181 . 119.7 no C18 . C19 . C20 . 119.0(4) yes C18 . C19 . S1 . 115.6(3) yes C20 . C19 . S1 . 125.4(4) yes C19 . C20 . C21 . 120.5(4) yes C19 . C20 . H201 . 120.6 no C21 . C20 . H201 . 118.8 no C16 . C21 . C20 . 121.6(4) yes C16 . C21 . H211 . 119.4 no C20 . C21 . H211 . 119.0 no C19 . S1 . C22 . 101.5(3) yes S1 . C22 . H221 . 106.4 no S1 . C22 . H223 . 109.8 no H221 . C22 . H223 . 110.4 no S1 . C22 . H222 . 109.1 no H221 . C22 . H222 . 110.3 no H223 . C22 . H222 . 110.8 no Zn1 . O1 . C23 . 132.2(3) yes Zn2 . O2 . C23 . 120.9(2) yes Zn1 . O3 . C25 . 127.1(2) yes Zn2 . O4 . C25 . 126.7(2) yes Zn1 . O5 . C27 . 122.3(2) yes Zn2 . O6 . C27 . 131.1(3) yes Zn1 . O7 . C29 . 124.9(2) yes Zn2 . O8 . C29 . 128.5(2) yes O1 . C23 . O2 . 125.5(4) yes O1 . C23 . C24 . 117.4(4) yes O2 . C23 . C24 . 117.2(3) yes C23 . C24 . H241 . 111.4 no C23 . C24 . H243 . 110.0 no H241 . C24 . H243 . 109.8 no C23 . C24 . H242 . 108.6 no H241 . C24 . H242 . 108.6 no H243 . C24 . H242 . 108.5 no O3 . C25 . O4 . 124.9(4) yes O3 . C25 . C26 . 117.1(3) yes O4 . C25 . C26 . 118.0(3) yes C25 . C26 . H261 . 109.9 no C25 . C26 . H262 . 108.9 no H261 . C26 . H262 . 109.4 no C25 . C26 . H263 . 110.5 no H261 . C26 . H263 . 109.9 no H262 . C26 . H263 . 108.3 no O5 . C27 . O6 . 124.9(4) yes O5 . C27 . C28 . 118.0(4) yes O6 . C27 . C28 . 117.1(4) yes C27 . C28 . H282 . 110.7 no C27 . C28 . H281 . 109.5 no H282 . C28 . H281 . 109.5 no C27 . C28 . H283 . 109.0 no H282 . C28 . H283 . 108.6 no H281 . C28 . H283 . 109.5 no O8 . C29 . O7 . 125.0(3) yes O8 . C29 . C30 . 117.1(3) yes O7 . C29 . C30 . 117.8(3) yes C29 . C30 . H302 . 110.6 no C29 . C30 . H301 . 110.1 no H302 . C30 . H301 . 109.6 no C29 . C30 . H303 . 109.0 no H302 . C30 . H303 . 109.4 no H301 . C30 . H303 . 108.2 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_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 C2 . H21 . O2 3_555 158 0.93 2.36 3.243(6) yes C5 . H51 . O7 . 122 0.92 2.56 3.139(6) yes C14 . H141 . O5 2_556 158 0.93 2.36 3.238(6) yes # start Validation Reply Form _vrf_PLAT220_global ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.48 Ratio RESPONSE: Peripherical substitutents have high adp's, splitting does not seem to be sensible. ; _vrf_PLAT222_global ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.91 Ratio RESPONSE: Peripherical substitutents have high adp's, splitting does not seem to be sensible. Therefore also the corresponding hydrogen atoms have high isotropic U-values. ; # end Validation Reply Form