# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ocMOM-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C144 H72 O44 P3 In6) (NO3-)2 (C2H6O)106.67] ' _chemical_formula_sum 'C357.33 H712 In6 N2 O156.67 P3' _chemical_formula_weight 8325.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -1.6620 3.1820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0349 0.0309 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 31.1023(19) _cell_length_b 31.1023(19) _cell_length_c 45.205(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 37870(4) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13387 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9713 _exptl_absorpt_correction_T_max 0.9713 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.41328 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXII CCD' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46316 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0976 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 0.68 _diffrn_reflns_theta_max 13.43 _reflns_number_total 23627 _reflns_number_gt 15024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_cell_refinement 'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'APEX2 (Bruker, 2010)' _refine_special_details ; DFIX 1.39 0.01 C23 C18 C19 C18 C20 C19 C23 C22 C4 C3 C5 C4 C6 C5 C7 C6 DFIX 1.39 0.01 C56 C55 C57 C56 C55 C54 C54 C53 C70 C69 C69 C68 C73 C68 C73 C72 DFIX 1.39 0.01 C52 C22 C52 C20 C71 C3 C71 C7 DFIX 1.39 0.01 C53 C52 C57 C52 C72 C71 C71 C70 DFIX 1.49 C18 C12 C8 C5 DFIX 1.49 C68 C62 C58 C55 DFIX 1.49 0.001 C97 C94 C97 C38 C90 C45 C90 C87 DFIX 1.49 0.01 C79 C91 C33 C35 C83 C84 C29 C42 C66 C75 C16 C25 SADI C43 C29 C47 C29 FLAT 0.02 C90 C45 C46 C44 C43 C47 C42 C29 FLAT 0.04 C29 C28 C30 C42 FLAT 0.06 C98 C83 C82 C84 FLAT 0.01 C79 C96 C91 C92 C93 C94 C95 C97 flat 0.02 c34 c25 c26 c16 flat 0.02 c15 c16 c17 c25 flat 0.02 c98 c75 c76 c66 flat 0.02 c67 c66 c65 c75 DELU C44 C88 C45 C87 O5 C24 C1 C71 C7 C24 C52 C61 C62 C60 C18 C55 C19 C56 = C20 C57 C54 C23 C53 C22 C70 C6 C69 C4 C73 C3 C72 C5 C68 C66 C64 C65 DELU C36 C92 C37 C93 C38 C94 C39 C95 SIMU C20 C19 C18 C22 C23 simu C54 C53 C55 C56 C57 FLAT 0.04 C52 C20 C19 C18 C23 C22 FLAT 0.04 C7 C71 C3 C4 C5 C6 FLAT 0.04 c71 c72 c73 c68 c69 c70 FLAT 0.04 c52 c57 c56 c55 c54 c53 Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.088(8) _refine_ls_number_reflns 23627 _refine_ls_number_parameters 1015 _refine_ls_number_restraints 380 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.7529(2) -0.4174(2) -0.67015(11) 0.0888(15) Uani 1 1 d . A . C3 C -0.8034(5) -0.4287(5) -0.7180(3) 0.122(4) Uani 0.50 1 d PDU A 1 H3 H -0.8073 -0.4008 -0.7140 0.147 Uiso 0.50 1 calc PR A 1 C4 C -0.8237(5) -0.4569(6) -0.7453(3) 0.116(4) Uani 0.50 1 d PDU A 1 H4 H -0.8394 -0.4457 -0.7589 0.139 Uiso 0.50 1 calc PR A 1 C5 C -0.8214(7) -0.4997(8) -0.7526(5) 0.121(4) Uani 0.50 1 d PU A 1 C6 C -0.8047(5) -0.5230(6) -0.7314(3) 0.134(3) Uani 0.50 1 d PU A 1 H6 H -0.8076 -0.5544 -0.7351 0.160 Uiso 0.50 1 calc PR A 1 C7 C -0.7815(5) -0.4934(5) -0.7020(3) 0.122(3) Uani 0.50 1 d PU A 1 H7 H -0.7695 -0.5062 -0.6870 0.146 Uiso 0.50 1 calc PR A 1 C8 C -0.8435(5) -0.5253(5) -0.7798(3) 0.069(3) Uani 0.50 1 d P A 1 C9 C -0.8223(9) -0.5021(9) -0.8087(6) 0.092(7) Uani 0.50 1 d P A 1 H9 H -0.7932 -0.4703 -0.8090 0.110 Uiso 0.50 1 calc PR A 1 C10 C -0.8424(5) -0.5238(4) -0.8337(3) 0.065(3) Uani 0.50 1 d P A 1 C11 C -0.8203(6) -0.4980(7) -0.8598(5) 0.076(4) Uani 0.50 1 d PD A 1 H11 H -0.7922 -0.4656 -0.8589 0.091 Uiso 0.50 1 calc PR A 1 C12 C -0.8385(4) -0.5188(5) -0.8855(3) 0.081(3) Uani 0.50 1 d PD A 1 C13 C -0.8779(5) -0.5654(4) -0.8879(3) 0.109(3) Uani 0.50 1 d PD A 1 H13 H -0.8897 -0.5803 -0.9067 0.131 Uiso 0.50 1 calc PR A 1 C14 C -0.9003(4) -0.5905(4) -0.8623(3) 0.093(3) Uani 0.50 1 d P A 1 H14 H -0.9270 -0.6238 -0.8633 0.112 Uiso 0.50 1 calc PR A 1 C15 C -0.8842(5) -0.5676(4) -0.8346(2) 0.077(3) Uani 0.50 1 d P A 1 C16 C -0.9066(3) -0.5944(3) -0.8063(2) 0.075(2) Uani 0.50 1 d P A 1 C17 C -0.8847(4) -0.5734(4) -0.7807(2) 0.077(3) Uani 0.50 1 d P A 1 C18 C -0.8197(6) -0.4952(6) -0.9145(4) 0.124(3) Uani 0.50 1 d PDU A 1 C19 C -0.8290(5) -0.4574(5) -0.9227(3) 0.138(3) Uani 0.50 1 d PDU A 1 H19 H -0.8491 -0.4486 -0.9113 0.165 Uiso 0.50 1 calc PR A 1 C20 C -0.8047(4) -0.4323(5) -0.9505(3) 0.142(4) Uani 0.50 1 d PDU A 1 H20 H -0.8077 -0.4046 -0.9564 0.171 Uiso 0.50 1 calc PR A 1 C22 C -0.7726(5) -0.4871(5) -0.9603(3) 0.142(4) Uani 0.50 1 d PDU A 1 H22 H -0.7537 -0.4971 -0.9720 0.171 Uiso 0.50 1 calc PR A 1 C23 C -0.7964(5) -0.5145(5) -0.9334(3) 0.140(3) Uani 0.50 1 d PDU A 1 H23 H -0.7966 -0.5443 -0.9286 0.168 Uiso 0.50 1 calc PR A 1 C24 C -0.7520(2) -0.4188(2) -0.99577(12) 0.0933(16) Uani 1 1 d . A . C25 C -0.9527(3) -0.6436(4) -0.8059(2) 0.078(2) Uani 0.50 1 d P A 1 C26 C -0.9970(3) -0.6463(4) -0.8203(2) 0.095(3) Uani 0.50 1 d P A 1 C98 C -1.0183(3) -0.6227(3) -0.8731(2) 0.074(2) Uani 0.50 1 d P A 2 C27 C -0.9985(4) -0.6053(4) -0.8331(2) 0.093(3) Uani 0.50 1 d P A 1 H27 H -0.9715 -0.5726 -0.8302 0.111 Uiso 0.50 1 calc PR A 1 C28 C -1.0385(4) -0.6126(4) -0.8495(3) 0.108(3) Uani 0.50 1 d P A 1 H28 H -1.0366 -0.5855 -0.8604 0.129 Uiso 0.50 1 calc PR A 1 C29 C -1.0821(5) -0.6586(4) -0.8508(3) 0.095(3) Uani 0.50 1 d P A 1 C30 C -1.0815(5) -0.7003(5) -0.8417(3) 0.084(4) Uani 0.50 1 d P A 1 H30 H -1.1084 -0.7321 -0.8468 0.101 Uiso 0.50 1 calc PR A 1 C31 C -1.0398(4) -0.6970(4) -0.8240(3) 0.083(3) Uani 0.50 1 d P A 1 C32 C -1.0377(6) -0.7359(6) -0.8107(3) 0.084(4) Uani 0.50 1 d P A 1 H32 H -1.0653 -0.7684 -0.8130 0.100 Uiso 0.50 1 calc PR A 1 C33 C -0.9966(5) -0.7301(5) -0.7936(3) 0.086(4) Uani 0.50 1 d P A 1 C34 C -0.9563(4) -0.6837(4) -0.7943(2) 0.076(2) Uani 0.50 1 d P A 1 C35 C -0.9998(6) -0.7757(5) -0.7827(3) 0.085(5) Uani 0.50 1 d P A 1 C36 C -0.9583(4) -0.7811(4) -0.7839(2) 0.077(3) Uani 0.50 1 d PU A 1 H36 H -0.9290 -0.7561 -0.7932 0.092 Uiso 0.50 1 calc PR A 1 C37 C -0.9584(5) -0.8236(5) -0.7714(3) 0.084(3) Uani 0.50 1 d PU A 1 H37 H -0.9297 -0.8270 -0.7711 0.101 Uiso 0.50 1 calc PR A 1 C38 C -1.0026(9) -0.8584(8) -0.7602(5) 0.091(3) Uani 0.50 1 d PU A 1 C39 C -1.0420(5) -0.8536(5) -0.7599(3) 0.081(3) Uani 0.50 1 d PU A 1 H39 H -1.0714 -0.8777 -0.7503 0.097 Uiso 0.50 1 calc PR A 1 C40 C -1.0407(4) -0.8145(4) -0.7735(3) 0.078(3) Uani 0.50 1 d P A 1 H40 H -1.0712 -0.8150 -0.7765 0.094 Uiso 0.50 1 calc PR A 1 C42 C -1.1270(5) -0.6616(6) -0.8647(3) 0.113(5) Uani 0.50 1 d PD A 1 C43 C -1.1297(7) -0.6204(6) -0.8659(3) 0.164(8) Uani 0.50 1 d PD A 1 H43 H -1.1065 -0.5901 -0.8567 0.196 Uiso 0.50 1 calc PR A 1 C44 C -1.1702(5) -0.6263(7) -0.8823(3) 0.104(4) Uani 0.50 1 d PDU A 1 H44 H -1.1755 -0.5988 -0.8828 0.124 Uiso 0.50 1 calc PR A 1 C45 C -1.2022(5) -0.6667(7) -0.8972(3) 0.087(4) Uani 0.50 1 d PDU A 1 C46 C -1.1955(7) -0.7053(7) -0.8921(3) 0.153(9) Uani 0.50 1 d PD A 1 H46 H -1.2196 -0.7367 -0.8997 0.183 Uiso 0.50 1 calc PR A 1 C47 C -1.1566(5) -0.7031(6) -0.8769(3) 0.106(5) Uani 0.50 1 d PD A 1 H47 H -1.1518 -0.7308 -0.8754 0.127 Uiso 0.50 1 calc PR A 1 C52 C -0.7771(2) -0.4464(2) -0.96924(14) 0.1067(17) Uani 1 1 d D . . C53 C -0.7614(5) -0.4672(3) -0.9477(2) 0.118(3) Uani 0.50 1 d PDU A 2 H53 H -0.7308 -0.4667 -0.9502 0.141 Uiso 0.50 1 calc PR A 2 C54 C -0.7903(4) -0.4895(4) -0.9217(3) 0.109(3) Uani 0.50 1 d PDU A 2 H54 H -0.7787 -0.5037 -0.9075 0.131 Uiso 0.50 1 calc PR A 2 C55 C -0.8347(4) -0.4908(5) -0.9169(3) 0.107(3) Uani 0.50 1 d PDU A 2 C56 C -0.8537(5) -0.4715(4) -0.9376(3) 0.118(3) Uani 0.50 1 d PDU A 2 H56 H -0.8845 -0.4729 -0.9344 0.141 Uiso 0.50 1 calc PR A 2 C57 C -0.8251(4) -0.4493(4) -0.9639(3) 0.113(3) Uani 0.50 1 d PDU A 2 H57 H -0.8376 -0.4361 -0.9782 0.136 Uiso 0.50 1 calc PR A 2 C58 C -0.8593(4) -0.5099(4) -0.8866(3) 0.070(3) Uani 0.50 1 d PD A 2 C59 C -0.8366(7) -0.4891(7) -0.8604(5) 0.078(4) Uani 0.50 1 d PD A 2 H59 H -0.8054 -0.4593 -0.8611 0.094 Uiso 0.50 1 calc PR A 2 C60 C -0.8560(5) -0.5085(5) -0.8329(3) 0.067(4) Uani 0.50 1 d P A 2 C61 C -0.8313(8) -0.4879(8) -0.8060(5) 0.079(5) Uani 0.50 1 d P A 2 H61 H -0.7984 -0.4603 -0.8060 0.095 Uiso 0.50 1 calc PR A 2 C62 C -0.8517(7) -0.5052(7) -0.7834(5) 0.102(6) Uani 0.50 1 d P A 2 C63 C -0.9012(4) -0.5446(4) -0.7796(3) 0.107(3) Uani 0.50 1 d P A 2 H63 H -0.9163 -0.5540 -0.7607 0.129 Uiso 0.50 1 calc PR A 2 C64 C -0.9247(4) -0.5673(4) -0.8038(3) 0.098(3) Uani 0.50 1 d P A 2 H64 H -0.9568 -0.5959 -0.8024 0.118 Uiso 0.50 1 calc PR A 2 C65 C -0.9028(5) -0.5496(5) -0.8324(3) 0.082(3) Uani 0.50 1 d P A 2 C66 C -0.9279(3) -0.5727(3) -0.8606(2) 0.068(2) Uani 0.50 1 d P A 2 C67 C -0.9075(4) -0.5511(3) -0.8861(3) 0.078(3) Uani 0.50 1 d PD A 2 C68 C -0.8292(7) -0.4872(7) -0.7508(5) 0.141(5) Uani 0.50 1 d PDU A 2 C69 C -0.7859(6) -0.4877(6) -0.7441(4) 0.157(4) Uani 0.50 1 d PDU A 2 H69 H -0.7712 -0.5016 -0.7565 0.188 Uiso 0.50 1 calc PR A 2 C70 C -0.7662(6) -0.4647(6) -0.7161(4) 0.154(4) Uani 0.50 1 d PDU A 2 H70 H -0.7383 -0.4670 -0.7098 0.184 Uiso 0.50 1 calc PR A 2 C71 C -0.7789(2) -0.4419(2) -0.69831(15) 0.1061(17) Uani 1 1 d D . . C72 C -0.8226(6) -0.4446(6) -0.7046(3) 0.140(4) Uani 0.50 1 d PDU A 2 H72 H -0.8362 -0.4316 -0.6909 0.168 Uiso 0.50 1 calc PR A 2 C73 C -0.8491(6) -0.4665(5) -0.7314(3) 0.144(4) Uani 0.50 1 d PDU A 2 H73 H -0.8792 -0.4671 -0.7358 0.173 Uiso 0.50 1 calc PR A 2 C75 C -0.9766(3) -0.6190(3) -0.8601(2) 0.072(2) Uani 0.50 1 d P A 2 C76 C -0.9798(4) -0.6634(3) -0.8456(2) 0.089(3) Uani 0.50 1 d P A 2 C77 C -0.9397(4) -0.6664(4) -0.8333(2) 0.089(3) Uani 0.50 1 d P A 2 H77 H -0.9070 -0.6400 -0.8370 0.107 Uiso 0.50 1 calc PR A 2 C78 C -0.9456(4) -0.7053(4) -0.8162(3) 0.108(3) Uani 0.50 1 d P A 2 H78 H -0.9177 -0.7050 -0.8074 0.130 Uiso 0.50 1 calc PR A 2 C79 C -0.9936(4) -0.7456(5) -0.8120(4) 0.089(3) Uani 0.50 1 d P A 2 C80 C -1.0330(5) -0.7478(5) -0.8255(3) 0.085(4) Uani 0.50 1 d P A 2 H80 H -1.0642 -0.7774 -0.8236 0.101 Uiso 0.50 1 calc PR A 2 C81 C -1.0307(4) -0.7075(4) -0.8429(3) 0.079(3) Uani 0.50 1 d P A 2 C82 C -1.0676(6) -0.7025(7) -0.8569(4) 0.097(5) Uani 0.50 1 d P A 2 H82 H -1.0995 -0.7315 -0.8565 0.116 Uiso 0.50 1 calc PR A 2 C83 C -1.0659(4) -0.6637(4) -0.8708(3) 0.075(3) Uani 0.50 1 d P A 2 C84 C -1.1114(3) -0.6657(3) -0.8825(2) 0.070(3) Uani 0.50 1 d PD A 2 C85 C -1.1477(4) -0.7077(4) -0.8950(2) 0.082(4) Uani 0.50 1 d PD A 2 H85 H -1.1446 -0.7365 -0.8954 0.099 Uiso 0.50 1 calc PR A 2 C86 C -1.1903(4) -0.7096(5) -0.9075(3) 0.080(4) Uani 0.50 1 d PD A 2 H86 H -1.2161 -0.7396 -0.9156 0.096 Uiso 0.50 1 calc PR A 2 C87 C -1.1936(4) -0.6683(6) -0.9077(2) 0.073(3) Uani 0.50 1 d PDU A 2 C88 C -1.1574(4) -0.6252(6) -0.8957(2) 0.081(3) Uani 0.50 1 d PDU A 2 H88 H -1.1597 -0.5959 -0.8958 0.097 Uiso 0.50 1 calc PR A 2 C89 C -1.1168(4) -0.6258(4) -0.8832(2) 0.083(4) Uani 0.50 1 d PD A 2 H89 H -1.0914 -0.5959 -0.8746 0.100 Uiso 0.50 1 calc PR A 2 C90 C -1.23918(19) -0.6682(2) -0.92001(11) 0.0930(14) Uani 1 1 d D . . C91 C -0.9959(5) -0.7905(7) -0.7988(4) 0.096(5) Uani 0.50 1 d PD A 2 C92 C -0.9556(5) -0.7970(5) -0.7995(3) 0.113(3) Uani 0.50 1 d PDU A 2 H92 H -0.9265 -0.7747 -0.8101 0.136 Uiso 0.50 1 calc PR A 2 C93 C -0.9581(6) -0.8363(6) -0.7844(3) 0.109(3) Uani 0.50 1 d PDU A 2 H93 H -0.9313 -0.8426 -0.7858 0.131 Uiso 0.50 1 calc PR A 2 C94 C -0.9985(8) -0.8668(7) -0.7673(5) 0.086(3) Uani 0.50 1 d PDU A 2 C95 C -1.0405(5) -0.8655(6) -0.7758(3) 0.106(3) Uani 0.50 1 d PU A 2 H95 H -1.0729 -0.8916 -0.7711 0.127 Uiso 0.50 1 calc PR A 2 C96 C -1.0323(10) -0.8218(9) -0.7922(4) 0.129(7) Uani 0.50 1 d P A 2 H96 H -1.0609 -0.8201 -0.7977 0.155 Uiso 0.50 1 calc PR A 2 C97 C -1.0017(2) -0.9055(2) -0.74640(12) 0.0875(14) Uani 1 1 d . . . In1 In -0.935639(12) -0.934224(12) -0.707269(6) 0.07879(16) Uani 1 1 d . . . In2 In -0.731005(11) -0.331902(11) -0.626011(6) 0.07676(15) Uani 1 1 d . . . O1 O -0.76055(13) -0.38394(16) -0.66270(8) 0.1126(12) Uani 1 1 d . . . O2 O -0.79893(15) -0.32905(16) -0.62628(10) 0.1389(14) Uani 1 1 d . . . O3 O -1.0000 -1.0000 -0.70853(12) 0.0808(14) Uani 1 3 d S . . O4 O -0.72718(16) -0.43119(14) -0.65892(9) 0.1228(14) Uani 1 1 d . . . O5 O -0.76496(15) -0.39380(17) -1.00752(9) 0.1276(15) Uani 1 1 d . . . O6 O -0.71696(17) -0.42678(13) -1.00380(9) 0.1179(12) Uani 1 1 d . . . O7 O -1.23548(12) -0.62737(14) -0.92525(8) 0.1020(11) Uani 1 1 d . . . O8 O -1.27302(12) -0.70937(13) -0.92901(8) 0.0987(11) Uani 1 1 d . A . O9 O -1.04263(14) -0.93966(12) -0.73802(9) 0.1043(11) Uani 1 1 d . A . O10 O -0.96101(14) -0.90229(12) -0.74131(8) 0.0993(10) Uani 1 1 d . A . O11 O -0.6667 -0.3333 -0.62522(12) 0.0800(14) Uani 1 3 d S . . O12 O -0.9059(2) -0.6000(2) -0.75482(15) 0.0907(17) Uani 0.50 1 d P A 1 O13 O -0.86750(15) -0.86321(15) -0.70698(10) 0.1372(14) Uani 1 1 d . A . O14 O -0.9159(2) -0.6786(2) -0.77871(14) 0.0879(17) Uani 0.50 1 d P A 1 O15 O -0.8527(3) -0.6377(3) -0.74205(18) 0.127(2) Uani 0.50 1 d P A 1 O19 O -0.9338(2) -0.5727(2) -0.91224(14) 0.0840(16) Uani 0.50 1 d P A 2 O16 O -0.9409(3) -0.6752(3) -0.7283(2) 0.134(3) Uani 0.50 1 d P A 1 O20 O -1.0108(2) -0.5813(2) -0.88812(14) 0.0869(17) Uani 0.50 1 d P A 2 O17 O -1.0089(3) -0.6094(3) -0.93933(19) 0.132(3) Uani 0.50 1 d P A 2 O18 O -0.9710(3) -0.5190(3) -0.92490(18) 0.125(2) Uani 0.50 1 d P A 2 P1 P -0.90186(13) -0.64931(11) -0.74756(7) 0.1037(9) Uani 0.50 1 d P A 1 P2 P -0.98273(11) -0.56853(12) -0.91923(7) 0.1030(9) Uani 0.50 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.096(4) 0.092(4) 0.053(3) -0.017(3) -0.014(3) 0.027(3) C3 0.123(8) 0.146(8) 0.096(9) 0.021(6) 0.002(6) 0.066(8) C4 0.093(8) 0.148(8) 0.086(9) 0.016(6) -0.009(6) 0.044(8) C5 0.062(7) 0.165(9) 0.110(7) 0.000(6) 0.007(6) 0.037(6) C6 0.117(7) 0.136(9) 0.118(9) 0.009(6) 0.003(6) 0.040(7) C7 0.106(7) 0.133(9) 0.110(8) 0.007(6) 0.012(6) 0.048(7) C8 0.058(7) 0.082(9) 0.051(7) -0.002(6) -0.009(5) 0.023(7) C9 0.066(9) 0.078(11) 0.12(2) -0.021(9) 0.008(10) 0.029(7) C10 0.074(8) 0.059(8) 0.063(8) -0.009(6) 0.002(6) 0.034(7) C11 0.072(10) 0.079(9) 0.078(10) 0.005(7) 0.011(9) 0.038(6) C12 0.092(10) 0.081(8) 0.076(8) 0.018(6) 0.014(7) 0.048(7) C13 0.113(9) 0.092(8) 0.099(10) 0.011(7) 0.002(7) 0.034(8) C14 0.088(7) 0.086(7) 0.095(9) 0.005(7) 0.010(6) 0.036(6) C15 0.079(7) 0.073(8) 0.062(8) -0.001(6) -0.008(5) 0.025(7) C16 0.066(6) 0.080(6) 0.074(8) -0.015(6) -0.016(5) 0.031(5) C17 0.082(7) 0.075(7) 0.089(8) 0.002(6) 0.003(6) 0.050(6) C18 0.141(6) 0.099(5) 0.117(6) -0.008(4) -0.004(5) 0.047(5) C19 0.153(6) 0.114(6) 0.126(6) 0.001(5) -0.002(5) 0.050(5) C20 0.158(7) 0.119(6) 0.125(7) -0.001(5) -0.008(6) 0.050(6) C22 0.150(7) 0.135(8) 0.129(8) -0.006(6) 0.005(6) 0.062(7) C23 0.145(6) 0.120(6) 0.134(7) 0.001(5) 0.000(5) 0.051(5) C24 0.099(4) 0.087(4) 0.061(4) 0.009(3) 0.020(3) 0.021(3) C25 0.068(6) 0.089(7) 0.085(7) 0.002(5) -0.002(5) 0.044(5) C26 0.074(6) 0.082(7) 0.103(8) -0.009(6) 0.003(6) 0.019(6) C98 0.072(6) 0.070(6) 0.082(7) 0.002(5) 0.007(5) 0.036(5) C27 0.095(7) 0.095(7) 0.102(8) 0.006(6) -0.002(6) 0.057(6) C28 0.107(9) 0.099(8) 0.120(10) 0.004(7) -0.015(8) 0.055(8) C29 0.094(9) 0.085(9) 0.101(10) 0.004(7) -0.015(8) 0.039(7) C30 0.066(8) 0.072(7) 0.102(12) 0.027(8) 0.000(7) 0.026(6) C31 0.084(7) 0.084(8) 0.083(9) -0.002(7) -0.011(7) 0.044(6) C32 0.108(9) 0.073(8) 0.067(10) 0.002(7) 0.008(8) 0.043(6) C33 0.097(9) 0.097(10) 0.079(9) 0.001(7) -0.006(7) 0.060(8) C34 0.069(6) 0.068(7) 0.090(8) 0.001(6) -0.001(5) 0.032(6) C35 0.107(11) 0.085(11) 0.071(9) -0.023(7) -0.014(7) 0.054(10) C36 0.075(5) 0.089(6) 0.081(7) 0.005(5) 0.003(5) 0.052(4) C37 0.085(4) 0.086(5) 0.087(7) 0.008(5) 0.007(5) 0.047(4) C38 0.085(4) 0.095(6) 0.091(7) 0.010(5) 0.006(5) 0.044(4) C39 0.080(4) 0.088(6) 0.079(7) 0.007(5) 0.006(5) 0.045(4) C40 0.043(5) 0.069(7) 0.098(10) 0.047(7) 0.009(6) 0.009(5) C42 0.115(11) 0.113(11) 0.104(12) -0.024(10) -0.036(9) 0.051(9) C43 0.24(2) 0.141(13) 0.144(18) -0.017(13) -0.079(16) 0.125(14) C44 0.105(7) 0.099(5) 0.090(8) -0.009(7) -0.011(6) 0.039(5) C45 0.084(6) 0.093(5) 0.083(8) 0.004(7) -0.020(6) 0.043(5) C46 0.23(2) 0.123(12) 0.116(17) -0.030(12) -0.078(15) 0.101(13) C47 0.124(11) 0.140(13) 0.080(11) 0.003(10) -0.025(9) 0.085(10) C52 0.111(4) 0.097(4) 0.108(5) 0.007(3) 0.001(4) 0.048(3) C53 0.133(6) 0.102(6) 0.118(7) -0.022(5) -0.004(5) 0.058(6) C54 0.134(6) 0.081(5) 0.106(6) -0.002(4) -0.015(5) 0.049(5) C55 0.136(6) 0.079(5) 0.113(5) -0.003(4) -0.007(5) 0.059(5) C56 0.136(6) 0.101(5) 0.101(6) -0.006(5) -0.025(5) 0.047(5) C57 0.122(7) 0.105(7) 0.096(7) -0.022(5) -0.025(5) 0.044(6) C58 0.076(8) 0.076(7) 0.070(8) 0.018(5) 0.016(6) 0.046(6) C59 0.076(11) 0.078(8) 0.075(10) -0.001(8) 0.000(8) 0.035(6) C60 0.064(8) 0.071(8) 0.073(9) -0.007(6) -0.006(6) 0.039(7) C61 0.080(10) 0.102(14) 0.036(8) -0.023(9) 0.014(7) 0.030(7) C62 0.103(11) 0.108(12) 0.118(15) -0.040(10) -0.047(10) 0.071(10) C63 0.090(8) 0.099(8) 0.100(10) 0.006(7) -0.004(7) 0.022(8) C64 0.100(8) 0.104(8) 0.097(10) -0.020(7) -0.016(8) 0.056(7) C65 0.087(9) 0.087(8) 0.073(9) 0.002(6) 0.003(6) 0.044(8) C66 0.065(6) 0.069(5) 0.071(7) 0.007(5) 0.011(5) 0.034(5) C67 0.062(6) 0.074(6) 0.102(9) 0.006(6) 0.008(6) 0.036(5) C68 0.072(7) 0.185(13) 0.103(7) -0.004(8) 0.019(6) 0.016(7) C69 0.138(8) 0.170(10) 0.142(10) -0.021(7) -0.009(7) 0.061(8) C70 0.126(8) 0.176(10) 0.143(10) -0.017(7) -0.015(7) 0.064(8) C71 0.093(4) 0.100(4) 0.106(5) -0.003(4) 0.003(3) 0.034(3) C72 0.148(9) 0.163(9) 0.105(10) 0.014(7) -0.003(7) 0.074(8) C73 0.135(9) 0.158(8) 0.117(10) 0.010(7) -0.009(6) 0.057(8) C75 0.064(5) 0.071(5) 0.080(7) 0.004(5) 0.000(5) 0.033(5) C76 0.084(7) 0.072(6) 0.096(8) 0.004(5) -0.001(6) 0.029(5) C77 0.081(6) 0.085(6) 0.101(8) 0.003(6) -0.012(6) 0.041(5) C78 0.107(9) 0.101(8) 0.126(11) 0.009(8) -0.006(7) 0.059(8) C79 0.071(8) 0.076(8) 0.112(11) 0.023(8) -0.014(8) 0.029(6) C80 0.090(8) 0.070(8) 0.078(11) 0.004(7) 0.001(8) 0.029(6) C81 0.078(7) 0.070(7) 0.085(9) 0.011(6) 0.001(6) 0.034(6) C82 0.059(8) 0.121(11) 0.093(12) -0.009(10) 0.001(7) 0.033(7) C83 0.081(8) 0.066(7) 0.078(8) 0.006(6) -0.019(6) 0.038(6) C84 0.060(6) 0.054(6) 0.082(8) -0.002(6) -0.022(6) 0.019(5) C85 0.098(8) 0.053(6) 0.085(10) 0.000(6) -0.025(7) 0.029(6) C86 0.085(7) 0.067(7) 0.085(11) -0.026(7) -0.058(6) 0.037(5) C87 0.080(5) 0.079(4) 0.063(7) -0.007(6) -0.007(5) 0.042(4) C88 0.091(6) 0.083(4) 0.067(7) -0.006(6) -0.010(6) 0.042(4) C89 0.095(8) 0.071(7) 0.077(9) -0.013(6) -0.042(6) 0.037(6) C90 0.093(4) 0.105(4) 0.080(4) -0.013(3) -0.007(3) 0.048(4) C91 0.052(7) 0.072(9) 0.128(15) 0.029(10) 0.002(9) 0.005(6) C92 0.110(5) 0.108(7) 0.106(8) 0.017(5) 0.005(6) 0.043(5) C93 0.105(4) 0.099(6) 0.105(8) 0.012(5) 0.015(6) 0.039(5) C94 0.089(4) 0.083(6) 0.097(7) 0.011(5) -0.001(5) 0.051(4) C95 0.096(4) 0.109(6) 0.104(8) 0.009(6) -0.008(6) 0.044(5) C96 0.19(2) 0.162(17) 0.086(13) 0.006(13) -0.004(13) 0.126(17) C97 0.092(4) 0.088(4) 0.081(4) 0.008(3) 0.004(3) 0.044(3) In1 0.0782(2) 0.0787(3) 0.0798(4) -0.00680(18) 0.00336(17) 0.03942(19) In2 0.0776(2) 0.0787(2) 0.0734(4) 0.01015(17) 0.00243(17) 0.03869(19) O1 0.106(3) 0.136(3) 0.092(3) -0.040(2) -0.030(2) 0.057(2) O2 0.130(3) 0.149(3) 0.147(4) 0.007(3) -0.001(3) 0.078(3) O3 0.079(2) 0.079(2) 0.085(4) 0.000 0.000 0.0395(10) O4 0.149(3) 0.126(3) 0.103(3) -0.038(2) -0.069(3) 0.076(3) O5 0.126(3) 0.156(4) 0.108(3) 0.078(3) 0.037(2) 0.077(3) O6 0.150(3) 0.101(3) 0.097(3) 0.026(2) 0.033(3) 0.059(3) O7 0.106(3) 0.097(2) 0.113(3) -0.007(2) -0.022(2) 0.057(2) O8 0.080(2) 0.098(2) 0.117(3) -0.014(2) -0.049(2) 0.0433(19) O9 0.097(2) 0.080(2) 0.129(3) 0.042(2) 0.002(2) 0.039(2) O10 0.093(2) 0.094(2) 0.118(3) 0.0283(19) 0.011(2) 0.052(2) O11 0.078(2) 0.078(2) 0.083(4) 0.000 0.000 0.0392(10) O12 0.096(4) 0.093(4) 0.079(5) 0.012(4) 0.002(4) 0.044(4) O13 0.124(3) 0.129(3) 0.144(4) 0.000(3) 0.006(3) 0.052(2) O14 0.091(4) 0.086(4) 0.086(5) 0.004(3) -0.005(4) 0.044(3) O15 0.139(7) 0.137(6) 0.115(6) -0.006(5) -0.012(5) 0.076(5) O19 0.080(4) 0.080(4) 0.083(5) -0.001(3) -0.009(3) 0.033(3) O16 0.154(7) 0.128(6) 0.127(7) 0.000(5) -0.002(6) 0.075(6) O20 0.088(4) 0.086(4) 0.085(5) 0.009(4) 0.001(3) 0.042(3) O17 0.124(6) 0.150(7) 0.116(7) 0.005(5) -0.008(5) 0.063(5) O18 0.126(6) 0.139(6) 0.121(6) 0.023(5) 0.008(5) 0.074(5) P1 0.096(2) 0.101(2) 0.088(2) 0.0273(18) -0.0187(18) 0.0294(17) P2 0.0924(19) 0.100(2) 0.088(2) 0.0267(18) -0.0204(17) 0.0267(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O4 1.194(6) . ? C1 O1 1.225(6) . ? C1 C71 1.496(8) . ? C3 C71 1.362(9) . ? C3 C4 1.463(9) . ? C3 H3 0.9500 . ? C4 C5 1.41(2) . ? C4 H4 0.9500 . ? C5 C8 1.44(2) . ? C5 C6 1.45(3) . ? C6 C7 1.573(18) . ? C6 H6 0.9500 . ? C7 C71 1.572(16) . ? C7 H7 0.9500 . ? C8 C17 1.400(15) . ? C8 C9 1.48(3) . ? C9 C10 1.31(3) . ? C9 H9 0.9500 . ? C10 C15 1.332(15) . ? C10 C11 1.40(2) . ? C11 C12 1.31(2) . ? C11 H11 0.9500 . ? C12 C13 1.356(16) . ? C12 C18 1.47(2) . ? C13 C14 1.374(14) . ? C13 H13 0.9500 . ? C14 C15 1.403(14) . ? C14 H14 0.9500 . ? C15 C16 1.497(14) . ? C16 C17 1.336(12) . ? C16 C25 1.484(12) . ? C17 O12 1.393(11) . ? C18 C19 1.393(15) . ? C18 C23 1.431(15) . ? C19 C20 1.474(14) . ? C19 H19 0.9500 . ? C20 C52 1.422(13) . ? C20 H20 0.9500 . ? C22 C52 1.402(13) . ? C22 C23 1.455(14) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 O5 1.168(7) . ? C24 O6 1.285(6) . ? C24 C52 1.454(8) . ? C25 C34 1.306(12) . ? C25 C26 1.487(13) . ? C26 C27 1.423(13) . ? C26 C31 1.479(14) . ? C98 O20 1.368(10) . ? C98 C75 1.375(11) . ? C98 C83 1.393(13) . ? C27 C28 1.367(13) . ? C27 H27 0.9500 . ? C28 C29 1.398(15) . ? C28 H28 0.9500 . ? C29 C30 1.370(16) . ? C29 C42 1.492(18) . ? C30 C31 1.481(17) . ? C30 H30 0.9500 . ? C31 C32 1.383(17) . ? C32 C33 1.425(19) . ? C32 H32 0.9500 . ? C33 C34 1.358(15) . ? C33 C35 1.46(2) . ? C34 O14 1.378(10) . ? C35 C40 1.309(18) . ? C35 C36 1.382(19) . ? C36 C37 1.435(14) . ? C36 H36 0.9500 . ? C37 C38 1.352(19) . ? C37 H37 0.9500 . ? C38 C39 1.31(2) . ? C38 C97 1.61(3) . ? C39 C40 1.345(16) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C42 C47 1.275(14) . ? C42 C43 1.327(15) . ? C43 C44 1.389(15) . ? C43 H43 0.9500 . ? C44 C45 1.335(13) . ? C44 H44 0.9500 . ? C45 C46 1.339(15) . ? C45 C90 1.528(9) . ? C46 C47 1.363(15) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C52 C53 1.387(9) . ? C52 C57 1.471(12) . ? C53 C54 1.430(9) . ? C53 H53 0.9500 . ? C54 C55 1.379(9) . ? C54 H54 0.9500 . ? C55 C56 1.393(9) . ? C55 C58 1.533(19) . ? C56 C57 1.437(13) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 C59 1.37(2) . ? C58 C67 1.404(15) . ? C59 C60 1.38(2) . ? C59 H59 0.9500 . ? C60 C65 1.378(15) . ? C60 C61 1.41(3) . ? C61 C62 1.18(2) . ? C61 H61 0.9500 . ? C62 C63 1.42(2) . ? C62 C68 1.61(3) . ? C63 C64 1.307(14) . ? C63 H63 0.9500 . ? C64 C65 1.438(15) . ? C64 H64 0.9500 . ? C65 C66 1.481(14) . ? C66 C67 1.324(12) . ? C66 C75 1.479(11) . ? C67 O19 1.401(11) . ? C68 C69 1.389(10) . ? C68 C73 1.403(10) . ? C69 C70 1.434(9) . ? C69 H69 0.9500 . ? C70 C71 1.259(18) . ? C70 H70 0.9500 . ? C71 C72 1.351(17) . ? C72 C73 1.429(9) . ? C72 H72 0.9500 . ? C73 H73 0.9500 . ? C75 C76 1.487(12) . ? C76 C77 1.409(12) . ? C76 C81 1.494(13) . ? C77 C78 1.368(13) . ? C77 H77 0.9500 . ? C78 C79 1.402(15) . ? C78 H78 0.9500 . ? C79 C80 1.339(17) . ? C79 C91 1.485(19) . ? C80 C81 1.451(17) . ? C80 H80 0.9500 . ? C81 C82 1.385(19) . ? C82 C83 1.341(19) . ? C82 H82 0.9500 . ? C83 C84 1.481(14) . ? C84 C89 1.334(12) . ? C84 C85 1.351(12) . ? C85 C86 1.415(13) . ? C85 H85 0.9500 . ? C86 C87 1.338(14) . ? C86 H86 0.9500 . ? C87 C88 1.359(12) . ? C87 C90 1.525(9) . ? C88 C89 1.391(13) . ? C88 H88 0.9500 . ? C89 H89 0.9500 . ? C90 O7 1.239(6) . ? C90 O8 1.252(6) . ? C91 C96 1.10(2) . ? C91 C92 1.366(15) . ? C92 C93 1.366(14) . ? C92 H92 0.9500 . ? C93 C94 1.374(15) . ? C93 H93 0.9500 . ? C94 C95 1.38(2) . ? C94 C97 1.50(2) . ? C95 C96 1.45(2) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C97 O10 1.239(6) . ? C97 O9 1.242(6) . ? In1 O3 2.0249(4) . ? In1 O13 2.165(4) . ? In1 O6 2.172(4) 5_345 ? In1 O9 2.181(3) 3_435 ? In1 O10 2.182(4) . ? In1 O5 2.185(4) 6_335 ? In2 O11 2.0240(3) . ? In2 O2 2.158(4) . ? In2 O8 2.169(3) 6_335 ? In2 O1 2.174(4) . ? In2 O4 2.180(4) 3_445 ? In2 O7 2.181(4) 5_355 ? O3 In1 2.0250(4) 3_435 ? O3 In1 2.0250(4) 2_345 ? O4 In2 2.180(4) 2_455 ? O5 In1 2.185(4) 8_344 ? O6 In1 2.172(4) 9_434 ? O7 In2 2.181(4) 9_334 ? O8 In2 2.169(3) 8_344 ? O9 In1 2.181(3) 2_345 ? O11 In2 2.0239(4) 3_445 ? O11 In2 2.0239(4) 2_455 ? O12 P1 1.635(7) . ? O14 P1 1.614(7) . ? O15 P1 1.408(8) . ? O19 P2 1.623(7) . ? O16 P1 1.379(9) . ? O20 P2 1.597(7) . ? O17 P2 1.438(9) . ? O18 P2 1.417(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 C1 O1 129.7(5) . . ? O4 C1 C71 117.8(6) . . ? O1 C1 C71 112.5(6) . . ? C71 C3 C4 120.6(12) . . ? C71 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 123.7(14) . . ? C5 C4 H4 118.2 . . ? C3 C4 H4 118.2 . . ? C4 C5 C8 119.3(17) . . ? C4 C5 C6 121.3(18) . . ? C8 C5 C6 118.7(17) . . ? C5 C6 C7 116.3(15) . . ? C5 C6 H6 121.8 . . ? C7 C6 H6 121.8 . . ? C71 C7 C6 117.4(12) . . ? C71 C7 H7 121.3 . . ? C6 C7 H7 121.3 . . ? C17 C8 C5 122.9(14) . . ? C17 C8 C9 116.3(14) . . ? C5 C8 C9 120.7(16) . . ? C10 C9 C8 122(2) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C15 121.6(16) . . ? C9 C10 C11 117.6(18) . . ? C15 C10 C11 120.7(15) . . ? C12 C11 C10 119.7(17) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 122.3(15) . . ? C11 C12 C18 125.1(15) . . ? C13 C12 C18 112.6(14) . . ? C12 C13 C14 118.0(12) . . ? C12 C13 H13 121.0 . . ? C14 C13 H13 121.0 . . ? C13 C14 C15 120.8(10) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C10 C15 C14 117.6(11) . . ? C10 C15 C16 119.3(10) . . ? C14 C15 C16 122.1(9) . . ? C17 C16 C25 119.3(9) . . ? C17 C16 C15 119.0(8) . . ? C25 C16 C15 121.6(8) . . ? C16 C17 O12 117.4(9) . . ? C16 C17 C8 121.2(10) . . ? O12 C17 C8 121.3(10) . . ? C19 C18 C23 123.8(17) . . ? C19 C18 C12 117.3(13) . . ? C23 C18 C12 118.6(12) . . ? C18 C19 C20 113.8(15) . . ? C18 C19 H19 123.1 . . ? C20 C19 H19 123.1 . . ? C52 C20 C19 125.1(13) . . ? C52 C20 H20 117.4 . . ? C19 C20 H20 117.4 . . ? C52 C22 C23 121.2(14) . . ? C52 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C18 C23 C22 118.0(15) . . ? C18 C23 H23 121.0 . . ? C22 C23 H23 121.0 . . ? O5 C24 O6 127.5(5) . . ? O5 C24 C52 120.4(6) . . ? O6 C24 C52 112.1(6) . . ? C34 C25 C16 124.5(9) . . ? C34 C25 C26 119.2(9) . . ? C16 C25 C26 116.3(9) . . ? C27 C26 C31 119.5(10) . . ? C27 C26 C25 124.9(9) . . ? C31 C26 C25 115.2(9) . . ? O20 C98 C75 115.1(8) . . ? O20 C98 C83 120.1(8) . . ? C75 C98 C83 124.8(9) . . ? C28 C27 C26 120.5(10) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 121.9(11) . . ? C27 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C30 C29 C28 119.5(11) . . ? C30 C29 C42 121.6(12) . . ? C28 C29 C42 118.7(11) . . ? C29 C30 C31 121.4(12) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C32 C31 C26 118.1(11) . . ? C32 C31 C30 126.7(12) . . ? C26 C31 C30 115.3(10) . . ? C31 C32 C33 123.9(13) . . ? C31 C32 H32 118.0 . . ? C33 C32 H32 118.0 . . ? C34 C33 C32 114.5(12) . . ? C34 C33 C35 128.3(12) . . ? C32 C33 C35 116.1(13) . . ? C25 C34 C33 128.1(10) . . ? C25 C34 O14 117.2(8) . . ? C33 C34 O14 114.5(9) . . ? C40 C35 C36 115.9(12) . . ? C40 C35 C33 124.5(13) . . ? C36 C35 C33 119.4(15) . . ? C35 C36 C37 121.6(12) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C38 C37 C36 114.7(13) . . ? C38 C37 H37 122.6 . . ? C36 C37 H37 122.6 . . ? C39 C38 C37 123.2(17) . . ? C39 C38 C97 123.0(14) . . ? C37 C38 C97 113.7(16) . . ? C38 C39 C40 119.5(12) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C35 C40 C39 123.7(11) . . ? C35 C40 H40 118.2 . . ? C39 C40 H40 118.2 . . ? C47 C42 C43 126.7(16) . . ? C47 C42 C29 115.0(14) . . ? C43 C42 C29 117.9(14) . . ? C42 C43 C44 112.7(17) . . ? C42 C43 H43 123.7 . . ? C44 C43 H43 123.6 . . ? C45 C44 C43 126.4(16) . . ? C45 C44 H44 116.8 . . ? C43 C44 H44 116.8 . . ? C44 C45 C46 112.4(12) . . ? C44 C45 C90 124.5(13) . . ? C46 C45 C90 122.9(14) . . ? C45 C46 C47 125.1(15) . . ? C45 C46 H46 117.5 . . ? C47 C46 H46 117.5 . . ? C42 C47 C46 116.3(15) . . ? C42 C47 H47 121.9 . . ? C46 C47 H47 121.9 . . ? C53 C52 C22 32.6(5) . . ? C53 C52 C20 97.6(9) . . ? C22 C52 C20 117.0(10) . . ? C53 C52 C24 130.2(8) . . ? C22 C52 C24 120.4(9) . . ? C20 C52 C24 122.6(8) . . ? C53 C52 C57 116.0(9) . . ? C22 C52 C57 116.9(9) . . ? C20 C52 C57 33.9(5) . . ? C24 C52 C57 113.7(7) . . ? C52 C53 C54 121.3(11) . . ? C52 C53 H53 119.3 . . ? C54 C53 H53 119.3 . . ? C55 C54 C53 121.6(12) . . ? C55 C54 H54 119.2 . . ? C53 C54 H54 119.2 . . ? C54 C55 C56 120.8(14) . . ? C54 C55 C58 116.9(10) . . ? C56 C55 C58 122.1(10) . . ? C55 C56 C57 118.1(13) . . ? C55 C56 H56 121.0 . . ? C57 C56 H56 121.0 . . ? C56 C57 C52 122.1(11) . . ? C56 C57 H57 119.0 . . ? C52 C57 H57 119.0 . . ? C59 C58 C67 118.8(13) . . ? C59 C58 C55 123.4(13) . . ? C67 C58 C55 117.7(11) . . ? C58 C59 C60 124.4(17) . . ? C58 C59 H59 117.8 . . ? C60 C59 H59 117.8 . . ? C65 C60 C59 116.7(14) . . ? C65 C60 C61 119.4(15) . . ? C59 C60 C61 123.9(17) . . ? C62 C61 C60 119(2) . . ? C62 C61 H61 120.3 . . ? C60 C61 H61 120.3 . . ? C61 C62 C63 127.0(18) . . ? C61 C62 C68 126.3(19) . . ? C63 C62 C68 106.7(18) . . ? C64 C63 C62 116.0(13) . . ? C64 C63 H63 122.0 . . ? C62 C63 H63 122.0 . . ? C63 C64 C65 121.0(11) . . ? C63 C64 H64 119.5 . . ? C65 C64 H64 119.5 . . ? C60 C65 C64 116.7(11) . . ? C60 C65 C66 119.5(11) . . ? C64 C65 C66 123.9(10) . . ? C67 C66 C75 120.3(9) . . ? C67 C66 C65 120.2(9) . . ? C75 C66 C65 119.5(9) . . ? C66 C67 O19 118.3(8) . . ? C66 C67 C58 119.9(10) . . ? O19 C67 C58 121.7(10) . . ? C69 C68 C73 121.5(19) . . ? C69 C68 C62 116.9(15) . . ? C73 C68 C62 121.2(14) . . ? C68 C69 C70 111.1(17) . . ? C68 C69 H69 124.4 . . ? C70 C69 H69 124.4 . . ? C71 C70 C69 132.1(16) . . ? C71 C70 H70 114.0 . . ? C69 C70 H70 114.0 . . ? C70 C71 C72 114.8(12) . . ? C70 C71 C3 97.6(12) . . ? C72 C71 C3 35.2(7) . . ? C70 C71 C1 126.1(10) . . ? C72 C71 C1 118.8(9) . . ? C3 C71 C1 130.0(9) . . ? C70 C71 C7 39.6(7) . . ? C72 C71 C7 112.1(10) . . ? C3 C71 C7 119.2(10) . . ? C1 C71 C7 110.4(7) . . ? C71 C72 C73 122.1(15) . . ? C71 C72 H72 119.0 . . ? C73 C72 H72 119.0 . . ? C68 C73 C72 117.9(17) . . ? C68 C73 H73 121.1 . . ? C72 C73 H73 121.1 . . ? C98 C75 C66 122.5(8) . . ? C98 C75 C76 119.3(8) . . ? C66 C75 C76 118.1(8) . . ? C77 C76 C75 125.9(8) . . ? C77 C76 C81 118.2(9) . . ? C75 C76 C81 115.9(9) . . ? C78 C77 C76 123.4(9) . . ? C78 C77 H77 118.3 . . ? C76 C77 H77 118.3 . . ? C77 C78 C79 118.6(10) . . ? C77 C78 H78 120.7 . . ? C79 C78 H78 120.7 . . ? C80 C79 C78 121.4(12) . . ? C80 C79 C91 121.5(12) . . ? C78 C79 C91 115.1(11) . . ? C79 C80 C81 123.7(12) . . ? C79 C80 H80 118.2 . . ? C81 C80 H80 118.2 . . ? C82 C81 C80 131.1(12) . . ? C82 C81 C76 114.7(11) . . ? C80 C81 C76 114.2(10) . . ? C83 C82 C81 130.8(14) . . ? C83 C82 H82 114.6 . . ? C81 C82 H82 114.6 . . ? C82 C83 C98 113.9(11) . . ? C82 C83 C84 121.5(11) . . ? C98 C83 C84 124.7(9) . . ? C89 C84 C85 117.1(10) . . ? C89 C84 C83 122.1(9) . . ? C85 C84 C83 120.7(9) . . ? C84 C85 C86 121.4(10) . . ? C84 C85 H85 119.3 . . ? C86 C85 H85 119.3 . . ? C87 C86 C85 118.8(9) . . ? C87 C86 H86 120.6 . . ? C85 C86 H86 120.6 . . ? C86 C87 C88 121.3(9) . . ? C86 C87 C90 121.4(11) . . ? C88 C87 C90 117.2(10) . . ? C87 C88 C89 117.4(11) . . ? C87 C88 H88 121.3 . . ? C89 C88 H88 121.3 . . ? C84 C89 C88 124.0(11) . . ? C84 C89 H89 118.0 . . ? C88 C89 H89 118.0 . . ? O7 C90 O8 125.9(5) . . ? O7 C90 C87 117.5(8) . . ? O8 C90 C87 115.0(8) . . ? O7 C90 C45 114.6(9) . . ? O8 C90 C45 119.0(9) . . ? C87 C90 C45 21.1(8) . . ? C96 C91 C92 119.1(18) . . ? C96 C91 C79 119.0(14) . . ? C92 C91 C79 120.9(13) . . ? C93 C92 C91 118.5(14) . . ? C93 C92 H92 120.8 . . ? C91 C92 H92 120.8 . . ? C92 C93 C94 121.3(15) . . ? C92 C93 H93 119.3 . . ? C94 C93 H93 119.3 . . ? C93 C94 C95 112.2(16) . . ? C93 C94 C97 125.4(15) . . ? C95 C94 C97 121.1(14) . . ? C94 C95 C96 116.3(15) . . ? C94 C95 H95 121.9 . . ? C96 C95 H95 121.9 . . ? C91 C96 C95 125.9(19) . . ? C91 C96 H96 117.1 . . ? C95 C96 H96 117.1 . . ? O10 C97 O9 125.6(5) . . ? O10 C97 C94 113.6(9) . . ? O9 C97 C94 120.5(9) . . ? O10 C97 C38 118.7(10) . . ? O9 C97 C38 114.9(9) . . ? C94 C97 C38 16.9(11) . . ? O3 In1 O13 178.40(18) . . ? O3 In1 O6 93.20(16) . 5_345 ? O13 In1 O6 88.39(16) . 5_345 ? O3 In1 O9 94.46(13) . 3_435 ? O13 In1 O9 85.47(15) . 3_435 ? O6 In1 O9 89.66(16) 5_345 3_435 ? O3 In1 O10 92.30(14) . . ? O13 In1 O10 86.12(15) . . ? O6 In1 O10 172.59(15) 5_345 . ? O9 In1 O10 94.86(14) 3_435 . ? O3 In1 O5 94.34(15) . 6_335 ? O13 In1 O5 85.82(16) . 6_335 ? O6 In1 O5 86.59(18) 5_345 6_335 ? O9 In1 O5 170.61(15) 3_435 6_335 ? O10 In1 O5 88.04(16) . 6_335 ? O11 In2 O2 178.83(16) . . ? O11 In2 O8 94.94(13) . 6_335 ? O2 In2 O8 85.35(15) . 6_335 ? O11 In2 O1 92.97(16) . . ? O2 In2 O1 88.17(16) . . ? O8 In2 O1 88.99(15) 6_335 . ? O11 In2 O4 93.57(15) . 3_445 ? O2 In2 O4 86.21(16) . 3_445 ? O8 In2 O4 170.77(14) 6_335 3_445 ? O1 In2 O4 87.03(17) . 3_445 ? O11 In2 O7 92.93(14) . 5_355 ? O2 In2 O7 85.91(15) . 5_355 ? O8 In2 O7 95.07(14) 6_335 5_355 ? O1 In2 O7 172.52(15) . 5_355 ? O4 In2 O7 88.02(16) 3_445 5_355 ? C1 O1 In2 130.7(4) . . ? In1 O3 In1 119.919(16) . 3_435 ? In1 O3 In1 119.923(16) . 2_345 ? In1 O3 In1 119.921(16) 3_435 2_345 ? C1 O4 In2 133.5(4) . 2_455 ? C24 O5 In1 134.6(4) . 8_344 ? C24 O6 In1 131.2(4) . 9_434 ? C90 O7 In2 132.6(3) . 9_334 ? C90 O8 In2 134.1(3) . 8_344 ? C97 O9 In1 133.9(3) . 2_345 ? C97 O10 In1 132.9(3) . . ? In2 O11 In2 119.969(11) 3_445 2_455 ? In2 O11 In2 119.969(11) 3_445 . ? In2 O11 In2 119.968(11) 2_455 . ? C17 O12 P1 119.3(6) . . ? C34 O14 P1 119.0(6) . . ? C67 O19 P2 118.0(6) . . ? C98 O20 P2 119.0(6) . . ? O16 P1 O15 124.4(5) . . ? O16 P1 O14 108.1(5) . . ? O15 P1 O14 104.6(5) . . ? O16 P1 O12 102.5(5) . . ? O15 P1 O12 112.3(4) . . ? O14 P1 O12 103.2(3) . . ? O18 P2 O17 124.7(5) . . ? O18 P2 O20 103.9(5) . . ? O17 P2 O20 109.9(4) . . ? O18 P2 O19 112.4(4) . . ? O17 P2 O19 101.0(5) . . ? O20 P2 O19 103.1(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 13.43 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.599 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.039 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.005 -0.009 -0.002 28926 8510 ' ' _platon_squeeze_details ; there is no significant amount of DMF molecules in the void of the structure or coordinated to metal atoms. The solvent molecules removed by the SQUEEZE process could be regarded as EtOH molecules as well as nitrate anions. In every single unit cell, there are 6 nitrate anions containing 186 electrons, so the rest of 8510 C 186 = 8324 electrons are belongs to EtOH molecules. As a result, there are 320 EtOH molecules per unit cell. The theoretical occupied volume of single EtOH molecule and nitrate anion are 49.41and 38.61 respectively, indicating total volume of free molecules is 49.41*320 + 38.61*6 = 16042 per unit cell which is much smaller than 28926 calculated by PLATON. ; _database_code_depnum_ccdc_archive 'CCDC 936187' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ocMOM-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H19 Cd2 O20 P' _chemical_formula_weight 1219.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 17.4396(10) _cell_length_b 22.4040(15) _cell_length_c 29.2728(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11437.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 230(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 64.37 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0.708 _exptl_crystal_density_diffrn 0.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 3.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8250 _exptl_absorpt_correction_T_max 0.8250 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 230(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXII CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 96572 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 64.74 _reflns_number_total 19193 _reflns_number_gt 16705 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_cell_refinement 'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'APEX2 (Bruker, 2010)' _refine_special_details ; DELU O15 C1D O12 DELU O6 C8 DELU O21 C18 SIMU O21 C18 Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0054P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(3) _refine_ls_number_reflns 19193 _refine_ls_number_parameters 676 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0713 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.116089(11) 0.622325(9) 0.492078(7) 0.04500(5) Uani 1 1 d . . . Cd2 Cd 0.842418(13) 0.772001(11) 0.065295(8) 0.05586(6) Uani 1 1 d . . . P3 P 0.36249(6) 0.59629(6) 0.40439(3) 0.0780(3) Uani 1 1 d . . . O1 O 0.78216(12) 0.62996(12) 0.43791(8) 0.0628(6) Uani 1 1 d . . . O2 O 0.22409(14) 0.71718(14) -0.02558(8) 0.0781(8) Uani 1 1 d . . . O3 O 0.77212(13) 0.68600(11) 0.49775(10) 0.0767(8) Uani 1 1 d . . . O4 O 0.44438(14) 0.79898(10) 0.47648(8) 0.0641(6) Uani 1 1 d . . . C5 C 0.42021(16) 0.62095(17) 0.30207(9) 0.0520(7) Uani 1 1 d . . . O6 O -0.03563(16) 0.61988(16) 0.41441(11) 0.0944(9) Uani 1 1 d U . . C7 C 0.33578(17) 0.61643(17) 0.29566(10) 0.0550(8) Uani 1 1 d . . . O8 O -0.04528(13) 0.75246(14) 0.11866(9) 0.0832(9) Uani 1 1 d . . . O9 O 0.40151(12) 0.65108(11) 0.37837(7) 0.0600(6) Uani 1 1 d . . . O10 O 0.32747(12) 0.55780(10) 0.36300(7) 0.0562(5) Uani 1 1 d . . . C11 C 0.12469(19) 0.73132(19) 0.05056(11) 0.0675(9) Uani 1 1 d . . . H11 H 0.1034 0.7357 0.0216 0.081 Uiso 1 1 calc R . . O12 O 0.77609(14) 0.70885(11) 0.11293(8) 0.0642(6) Uani 1 1 d U . . O13 O 0.60584(18) 0.42667(12) 0.06430(9) 0.0812(7) Uani 1 1 d . . . C14 C 0.6632(2) 0.51714(15) 0.08543(10) 0.0555(8) Uani 1 1 d . . . O15 O 0.81261(16) 0.65809(14) 0.05240(9) 0.0856(8) Uani 1 1 d U . . C16 C 0.6184(2) 0.52417(14) 0.12498(9) 0.0531(7) Uani 1 1 d . . . H16 H 0.5826 0.4951 0.1326 0.064 Uiso 1 1 calc R . . C17 C 0.62673(18) 0.57336(15) 0.15244(10) 0.0524(7) Uani 1 1 d . . . O18 O 0.11290(17) 0.36870(11) 0.44189(10) 0.0824(7) Uani 1 1 d . . . C19 C 0.63585(16) 0.66125(14) 0.40632(10) 0.0493(7) Uani 1 1 d . . . H19 H 0.6631 0.6327 0.3899 0.059 Uiso 1 1 calc R . . C20 C 0.2542(2) 0.7244(2) 0.01307(14) 0.0736(11) Uani 1 1 d . . . C21 C 0.67851(17) 0.61669(16) 0.14067(10) 0.0520(7) Uani 1 1 d . . . H21 H 0.6831 0.6502 0.1592 0.062 Uiso 1 1 calc R . . O22 O 0.19142(16) 0.36023(12) 0.38549(10) 0.0815(8) Uani 1 1 d . . . O23 O -0.03351(13) 0.74466(12) 0.04471(9) 0.0705(7) Uani 1 1 d . . . C24 C 0.1092(2) 0.7206(2) 0.13077(11) 0.0773(11) Uani 1 1 d . . . H24 H 0.0773 0.7195 0.1562 0.093 Uiso 1 1 calc R . . C25 C 0.6531(2) 0.46428(16) 0.05543(11) 0.0626(9) Uani 1 1 d . . . O26 O 0.32450(13) 0.72802(15) 0.01801(9) 0.0829(8) Uani 1 1 d . . . C27 C 0.72386(18) 0.61241(16) 0.10255(11) 0.0553(8) Uani 1 1 d . . . C28 C 0.71669(19) 0.56219(16) 0.07460(11) 0.0580(8) Uani 1 1 d . . . H28 H 0.7473 0.5584 0.0487 0.070 Uiso 1 1 calc R . . C29 C 0.57824(17) 0.64315(15) 0.31135(10) 0.0527(8) Uani 1 1 d . . . H29 H 0.6303 0.6511 0.3143 0.063 Uiso 1 1 calc R . . O30 O -0.03756(15) 0.55118(12) 0.46518(9) 0.0801(8) Uani 1 1 d . . . C31 C 0.55037(16) 0.62000(17) 0.27012(10) 0.0526(7) Uani 1 1 d . . . C32 C 0.10161(17) 0.57203(16) 0.37595(10) 0.0538(8) Uani 1 1 d . . . H32 H 0.0899 0.6112 0.3681 0.065 Uiso 1 1 calc R . . C33 C 0.52353(17) 0.72261(16) 0.41628(10) 0.0536(7) Uani 1 1 d . . . H33 H 0.4751 0.7350 0.4069 0.064 Uiso 1 1 calc R . . O34 O 0.69488(16) 0.45899(13) 0.02034(9) 0.0830(8) Uani 1 1 d . . . O35 O 0.4215(2) 0.55597(17) 0.42612(11) 0.1122(12) Uani 1 1 d . . . C36 C 0.16392(18) 0.54519(15) 0.35593(10) 0.0517(7) Uani 1 1 d . . . C37 C 0.20305(18) 0.72316(19) 0.05496(11) 0.0652(9) Uani 1 1 d . . . C38 C 0.17839(17) 0.48593(16) 0.36661(11) 0.0572(8) Uani 1 1 d . . . H38 H 0.2191 0.4663 0.3527 0.069 Uiso 1 1 calc R . . C39 C 0.66826(16) 0.68557(14) 0.44511(10) 0.0492(7) Uani 1 1 d . . . C40 C 0.07785(18) 0.73302(19) 0.08836(12) 0.0638(9) Uani 1 1 d . . . C41 C 0.56275(16) 0.67840(15) 0.39087(10) 0.0485(7) Uani 1 1 d . . . O42 O 0.29969(19) 0.62402(18) 0.43153(11) 0.1115(11) Uani 1 1 d . . . C43 C 0.07353(18) 0.48408(16) 0.41789(11) 0.0568(8) Uani 1 1 d . . . H43 H 0.0441 0.4637 0.4393 0.068 Uiso 1 1 calc R . . C44 C 0.57397(18) 0.58197(16) 0.19307(10) 0.0560(8) Uani 1 1 d . . . C46 C 0.45151(18) 0.64148(14) 0.34244(10) 0.0491(7) Uani 1 1 d . . . C47 C 0.62884(17) 0.72971(16) 0.46973(11) 0.0572(8) Uani 1 1 d . . . H47 H 0.6506 0.7469 0.4956 0.069 Uiso 1 1 calc R . . C48 C 0.60115(17) 0.60713(14) 0.23297(10) 0.0521(8) Uani 1 1 d . . . H48 H 0.6531 0.6158 0.2358 0.062 Uiso 1 1 calc R . . C49 C 0.44596(18) 0.57750(19) 0.22460(11) 0.0665(10) Uani 1 1 d . . . H49 H 0.3949 0.5660 0.2221 0.080 Uiso 1 1 calc R . . C50 C 0.53013(16) 0.65441(15) 0.34774(10) 0.0488(7) Uani 1 1 d . . . C1 C 0.13368(18) 0.45597(15) 0.39734(10) 0.0557(8) Uani 1 1 d . . . C2 C 0.05585(18) 0.54294(15) 0.40718(11) 0.0542(8) Uani 1 1 d . . . C3 C -0.00628(19) 0.74343(16) 0.08383(13) 0.0598(9) Uani 1 1 d . . . C4 C 0.21723(18) 0.63829(19) 0.25233(11) 0.0648(10) Uani 1 1 d . . . C6 C 0.55580(17) 0.74748(15) 0.45451(12) 0.0569(8) Uani 1 1 d . . . C8 C -0.01100(18) 0.57464(16) 0.43030(13) 0.0579(8) Uani 1 1 d U . . C9 C 0.74575(18) 0.66603(16) 0.46123(11) 0.0548(8) Uani 1 1 d . . . C10 C 0.47221(17) 0.60628(16) 0.26531(10) 0.0553(8) Uani 1 1 d . . . C12 C 0.17564(18) 0.60471(17) 0.28458(11) 0.0627(9) Uani 1 1 d . . . H12 H 0.1231 0.5998 0.2806 0.075 Uiso 1 1 calc R . . C13 C 0.3355(2) 0.68494(18) 0.22868(12) 0.0692(10) Uani 1 1 d . . . H13 H 0.3860 0.6959 0.2345 0.083 Uiso 1 1 calc R . . C15 C 0.29915(18) 0.64657(18) 0.25879(11) 0.0632(10) Uani 1 1 d . . . C18 C 0.5137(2) 0.79602(18) 0.48076(14) 0.0739(11) Uani 1 1 d U . . C1A C 0.23394(19) 0.71324(19) 0.09682(12) 0.0711(11) Uani 1 1 d . . . H1A H 0.2868 0.7088 0.0995 0.085 Uiso 1 1 calc R . . C1B C 0.18223(19) 0.6608(2) 0.21204(12) 0.0735(11) Uani 1 1 d . . . H1B H 0.1305 0.6535 0.2069 0.088 Uiso 1 1 calc R . . C1C C 0.29163(17) 0.58503(16) 0.32651(10) 0.0531(8) Uani 1 1 d . . . C1D C 0.77528(18) 0.66320(19) 0.08837(12) 0.0622(9) Uani 1 1 d U . . C1E C 0.21056(17) 0.57903(16) 0.32188(11) 0.0544(8) Uani 1 1 d . . . C1F C 0.49519(19) 0.56678(18) 0.18941(11) 0.0627(9) Uani 1 1 d . . . H1F H 0.4770 0.5493 0.1627 0.075 Uiso 1 1 calc R . . C1G C 0.2226(2) 0.6928(2) 0.18094(12) 0.0698(10) Uani 1 1 d . . . C1H C 0.29962(19) 0.7075(2) 0.19033(13) 0.0742(12) Uani 1 1 d . . . H1H H 0.3264 0.7325 0.1706 0.089 Uiso 1 1 calc R . . O21 O 0.5519(2) 0.8331(2) 0.50081(19) 0.177(2) Uani 1 1 d U . . C22 C 0.18773(18) 0.7094(2) 0.13647(12) 0.0777(13) Uani 1 1 d . . . C23 C 0.1479(2) 0.39098(15) 0.40889(13) 0.0623(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03756(10) 0.05086(11) 0.04659(10) -0.00203(9) -0.00272(8) 0.00250(9) Cd2 0.04004(11) 0.06717(14) 0.06038(13) 0.00801(12) 0.00030(10) -0.00744(10) P3 0.0699(7) 0.1072(8) 0.0568(6) -0.0003(5) 0.0051(4) -0.0094(5) O1 0.0410(12) 0.0926(17) 0.0549(12) 0.0000(14) -0.0081(10) 0.0219(12) O2 0.0563(15) 0.122(2) 0.0560(15) 0.0170(15) 0.0090(12) 0.0068(14) O3 0.0523(14) 0.0836(17) 0.094(2) -0.0301(15) -0.0374(13) 0.0128(11) O4 0.0574(16) 0.0591(14) 0.0759(16) -0.0125(11) 0.0060(11) 0.0133(11) C5 0.0388(16) 0.080(2) 0.0375(15) -0.0034(16) -0.0023(11) -0.0018(15) O6 0.0727(19) 0.097(2) 0.114(2) 0.015(2) 0.0285(15) 0.0279(17) C7 0.0329(15) 0.084(2) 0.0483(16) 0.0040(16) -0.0006(12) -0.0056(16) O8 0.0420(14) 0.130(3) 0.0772(17) 0.0232(16) 0.0059(12) 0.0025(13) O9 0.0404(12) 0.0882(16) 0.0513(12) -0.0067(11) 0.0105(9) 0.0035(10) O10 0.0483(13) 0.0650(14) 0.0553(13) 0.0057(10) 0.0018(10) -0.0005(10) C11 0.0475(19) 0.103(3) 0.0516(18) 0.0253(18) -0.0017(15) -0.0021(19) O12 0.0635(15) 0.0662(16) 0.0630(15) 0.0060(12) 0.0035(11) -0.0158(11) O13 0.111(2) 0.0687(16) 0.0635(15) -0.0151(13) -0.0034(16) -0.0175(16) C14 0.058(2) 0.065(2) 0.0436(16) 0.0004(14) 0.0022(14) 0.0063(16) O15 0.0823(19) 0.104(2) 0.0706(18) 0.0020(15) 0.0295(14) -0.0235(15) C16 0.0546(18) 0.0594(19) 0.0454(16) -0.0014(14) 0.0043(15) -0.0073(15) C17 0.0461(18) 0.066(2) 0.0450(16) -0.0034(14) 0.0051(13) -0.0043(15) O18 0.0948(19) 0.0538(14) 0.0987(19) 0.0109(14) 0.0175(17) 0.0120(14) C19 0.0391(18) 0.0615(19) 0.0473(17) -0.0068(14) 0.0010(12) 0.0052(13) C20 0.051(2) 0.099(3) 0.071(3) 0.034(2) 0.0059(17) 0.0107(19) C21 0.0502(18) 0.0589(19) 0.0470(16) -0.0005(15) 0.0030(12) -0.0036(14) O22 0.0778(18) 0.0689(18) 0.098(2) -0.0066(14) 0.0120(15) 0.0202(13) O23 0.0451(13) 0.095(2) 0.0718(16) 0.0001(13) -0.0081(12) 0.0029(11) C24 0.048(2) 0.130(3) 0.0538(19) 0.023(2) -0.0011(16) -0.014(2) C25 0.073(2) 0.066(2) 0.048(2) -0.0016(16) -0.0159(17) 0.010(2) O26 0.0478(16) 0.128(2) 0.0730(17) 0.0197(17) 0.0097(11) -0.0063(14) C27 0.0483(18) 0.066(2) 0.0517(18) -0.0012(16) 0.0010(13) -0.0090(15) C28 0.055(2) 0.067(2) 0.0513(19) -0.0026(16) 0.0108(14) 0.0073(15) C29 0.0287(15) 0.078(2) 0.0511(18) -0.0065(15) -0.0019(12) 0.0004(13) O30 0.0795(19) 0.0729(17) 0.0878(18) -0.0033(14) 0.0438(15) 0.0069(13) C31 0.0327(15) 0.080(2) 0.0456(16) -0.0032(17) 0.0079(12) -0.0070(15) C32 0.0407(18) 0.066(2) 0.0549(18) 0.0052(15) 0.0082(13) 0.0070(14) C33 0.0410(16) 0.070(2) 0.0502(17) -0.0035(16) -0.0061(13) 0.0077(15) O34 0.0808(19) 0.100(2) 0.0684(18) -0.0329(15) 0.0024(14) 0.0062(15) O35 0.119(3) 0.132(3) 0.085(2) 0.023(2) -0.0425(19) -0.014(2) C36 0.0371(17) 0.070(2) 0.0480(17) 0.0018(15) 0.0030(13) 0.0030(14) C37 0.0446(19) 0.101(3) 0.050(2) 0.0141(19) 0.0038(14) -0.0046(18) C38 0.0416(18) 0.072(2) 0.0576(19) -0.0078(17) 0.0049(13) 0.0056(14) C39 0.0349(16) 0.0591(18) 0.0535(18) -0.0022(14) -0.0047(13) 0.0012(13) C40 0.0360(17) 0.094(3) 0.061(2) 0.0128(19) -0.0074(14) -0.0018(16) C41 0.0284(15) 0.065(2) 0.0519(18) -0.0011(15) -0.0038(12) 0.0014(13) O42 0.115(2) 0.134(3) 0.086(2) -0.029(2) 0.0454(18) -0.032(2) C43 0.0500(19) 0.068(2) 0.0522(19) 0.0021(16) 0.0105(14) -0.0046(15) C44 0.0485(19) 0.074(2) 0.0454(18) -0.0016(16) 0.0075(13) -0.0100(15) C46 0.0478(18) 0.0572(19) 0.0422(16) 0.0004(13) -0.0052(13) 0.0057(13) C47 0.0484(18) 0.0624(19) 0.0608(18) -0.0131(16) -0.0065(14) -0.0006(15) C48 0.0354(17) 0.073(2) 0.0476(16) -0.0093(14) 0.0038(12) -0.0043(13) C49 0.0367(18) 0.116(3) 0.0463(18) -0.0100(19) 0.0026(13) -0.0194(18) C50 0.0328(16) 0.075(2) 0.0389(16) -0.0025(14) 0.0010(12) 0.0083(13) C1 0.051(2) 0.069(2) 0.0476(17) 0.0029(15) -0.0006(13) 0.0008(14) C2 0.0427(18) 0.067(2) 0.0526(18) -0.0101(16) 0.0100(14) -0.0044(14) C3 0.0456(19) 0.064(2) 0.070(2) 0.0076(17) -0.0022(18) 0.0007(14) C4 0.0354(17) 0.112(3) 0.0469(18) 0.0057(18) -0.0030(13) -0.0055(16) C6 0.0373(17) 0.069(2) 0.065(2) -0.0098(16) -0.0028(14) 0.0082(14) C8 0.0442(18) 0.061(2) 0.068(2) -0.0025(18) 0.0070(16) -0.0037(15) C9 0.0438(18) 0.064(2) 0.057(2) 0.0069(16) -0.0078(15) -0.0070(15) C10 0.0401(17) 0.087(3) 0.0383(16) -0.0046(15) 0.0006(12) -0.0039(15) C12 0.0349(18) 0.095(3) 0.058(2) 0.0100(18) 0.0046(14) -0.0032(15) C13 0.0438(19) 0.103(3) 0.061(2) 0.0207(19) -0.0034(16) -0.0119(18) C15 0.0354(17) 0.108(3) 0.0460(18) 0.0042(17) 0.0013(13) -0.0060(16) C18 0.053(2) 0.078(3) 0.090(3) -0.035(2) -0.0087(18) 0.0137(17) C1A 0.0319(17) 0.113(3) 0.069(2) 0.026(2) 0.0017(15) -0.0018(17) C1B 0.0314(18) 0.127(3) 0.062(2) 0.019(2) -0.0006(14) -0.0033(18) C1C 0.0407(18) 0.075(2) 0.0440(17) 0.0035(15) -0.0004(13) 0.0006(15) C1D 0.0419(19) 0.089(3) 0.056(2) 0.0153(19) 0.0058(15) -0.0050(17) C1E 0.0420(18) 0.072(2) 0.0494(18) 0.0012(16) 0.0067(13) -0.0043(15) C1F 0.052(2) 0.090(3) 0.0454(18) -0.0052(17) -0.0021(14) -0.0135(17) C1G 0.051(2) 0.104(3) 0.054(2) 0.025(2) 0.0000(16) 0.0059(19) C1H 0.0362(18) 0.120(3) 0.066(2) 0.035(2) 0.0013(15) -0.0046(18) O21 0.085(2) 0.186(4) 0.262(6) -0.161(4) -0.031(3) 0.025(2) C22 0.0317(18) 0.146(4) 0.055(2) 0.027(2) -0.0029(14) 0.0035(19) C23 0.055(2) 0.061(2) 0.071(2) -0.0016(18) -0.0057(17) 0.0047(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O30 2.244(2) . ? Cd1 O4 2.251(2) 3_466 ? Cd1 O1 2.386(2) 1_455 ? Cd1 O13 2.389(2) 2_565 ? Cd1 O3 2.421(2) 1_455 ? Cd1 O34 2.427(3) 2_565 ? Cd1 C9 2.753(3) 1_455 ? Cd2 O12 2.299(2) . ? Cd2 O18 2.312(2) 4_655 ? Cd2 O23 2.328(2) 1_655 ? Cd2 O2 2.381(2) 3_565 ? Cd2 O26 2.458(3) 3_565 ? Cd2 O22 2.516(3) 4_655 ? Cd2 O8 2.543(3) 1_655 ? Cd2 O15 2.632(3) . ? P3 O42 1.489(3) . ? P3 O35 1.510(4) . ? P3 O9 1.597(3) . ? P3 O10 1.608(2) . ? O1 C9 1.234(4) . ? O1 Cd1 2.386(2) 1_655 ? O2 C20 1.258(5) . ? O2 Cd2 2.381(2) 3_465 ? O3 C9 1.247(4) . ? O3 Cd1 2.421(2) 1_655 ? O4 C18 1.217(4) . ? O4 Cd1 2.251(2) 3_566 ? C5 C46 1.381(4) . ? C5 C10 1.445(4) . ? C5 C7 1.488(4) . ? O6 C8 1.195(4) . ? C7 C1C 1.380(4) . ? C7 C15 1.424(5) . ? O8 C3 1.242(4) . ? O8 Cd2 2.543(3) 1_455 ? O9 C46 1.383(4) . ? O10 C1C 1.380(4) . ? C11 C40 1.376(5) . ? C11 C37 1.385(5) . ? C11 H11 0.9300 . ? O12 C1D 1.250(4) . ? O13 C25 1.207(5) . ? O13 Cd1 2.389(2) 2_564 ? C14 C16 1.406(4) . ? C14 C28 1.411(5) . ? C14 C25 1.485(5) . ? O15 C1D 1.243(4) . ? C16 C17 1.372(4) . ? C16 H16 0.9300 . ? C17 C21 1.370(4) . ? C17 C44 1.516(4) . ? O18 C23 1.247(4) . ? O18 Cd2 2.312(2) 4_645 ? C19 C39 1.381(4) . ? C19 C41 1.406(4) . ? C19 H19 0.9300 . ? C20 O26 1.238(4) . ? C20 C37 1.516(5) . ? C21 C27 1.371(4) . ? C21 H21 0.9300 . ? O22 C23 1.233(4) . ? O22 Cd2 2.516(3) 4_645 ? O23 C3 1.240(4) . ? O23 Cd2 2.328(2) 1_455 ? C24 C40 1.385(5) . ? C24 C22 1.401(5) . ? C24 H24 0.9300 . ? C25 O34 1.264(4) . ? O26 Cd2 2.458(3) 3_465 ? C27 C28 1.397(5) . ? C27 C1D 1.507(5) . ? C28 H28 0.9300 . ? C29 C50 1.379(4) . ? C29 C31 1.401(4) . ? C29 H29 0.9300 . ? O30 C8 1.238(4) . ? C31 C10 1.404(4) . ? C31 C48 1.432(4) . ? C32 C36 1.373(4) . ? C32 C2 1.377(4) . ? C32 H32 0.9300 . ? C33 C6 1.371(4) . ? C33 C41 1.415(4) . ? C33 H33 0.9300 . ? O34 Cd1 2.427(3) 2_564 ? C36 C38 1.387(5) . ? C36 C1E 1.493(4) . ? C37 C1A 1.357(5) . ? C38 C1 1.367(5) . ? C38 H38 0.9300 . ? C39 C47 1.403(4) . ? C39 C9 1.497(4) . ? C40 C3 1.491(5) . ? C41 C50 1.486(4) . ? C43 C1 1.364(5) . ? C43 C2 1.390(5) . ? C43 H43 0.9300 . ? C44 C48 1.381(4) . ? C44 C1F 1.419(5) . ? C46 C50 1.410(4) . ? C47 C6 1.407(4) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C1F 1.362(5) . ? C49 C10 1.430(4) . ? C49 H49 0.9300 . ? C1 C23 1.515(5) . ? C2 C8 1.524(5) . ? C4 C12 1.408(5) . ? C4 C1B 1.421(5) . ? C4 C15 1.453(5) . ? C6 C18 1.521(5) . ? C9 Cd1 2.753(3) 1_655 ? C12 C1E 1.376(5) . ? C12 H12 0.9300 . ? C13 C1H 1.381(5) . ? C13 C15 1.385(5) . ? C13 H13 0.9300 . ? C18 O21 1.217(5) . ? C1A C22 1.415(5) . ? C1A H1A 0.9300 . ? C1B C1G 1.356(5) . ? C1B H1B 0.9300 . ? C1C C1E 1.427(4) . ? C1F H1F 0.9300 . ? C1G C1H 1.410(5) . ? C1G C22 1.484(5) . ? C1H H1H 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O30 Cd1 O4 114.44(10) . 3_466 ? O30 Cd1 O1 105.76(10) . 1_455 ? O4 Cd1 O1 124.33(9) 3_466 1_455 ? O30 Cd1 O13 86.48(10) . 2_565 ? O4 Cd1 O13 87.89(9) 3_466 2_565 ? O1 Cd1 O13 132.59(10) 1_455 2_565 ? O30 Cd1 O3 159.03(10) . 1_455 ? O4 Cd1 O3 83.56(8) 3_466 1_455 ? O1 Cd1 O3 53.45(8) 1_455 1_455 ? O13 Cd1 O3 105.69(10) 2_565 1_455 ? O30 Cd1 O34 86.10(10) . 2_565 ? O4 Cd1 O34 135.54(10) 3_466 2_565 ? O1 Cd1 O34 81.91(9) 1_455 2_565 ? O13 Cd1 O34 52.83(9) 2_565 2_565 ? O3 Cd1 O34 87.88(10) 1_455 2_565 ? O30 Cd1 C9 132.19(11) . 1_455 ? O4 Cd1 C9 105.40(10) 3_466 1_455 ? O1 Cd1 C9 26.57(9) 1_455 1_455 ? O13 Cd1 C9 121.28(10) 2_565 1_455 ? O3 Cd1 C9 26.91(9) 1_455 1_455 ? O34 Cd1 C9 83.30(9) 2_565 1_455 ? O12 Cd2 O18 143.28(10) . 4_655 ? O12 Cd2 O23 117.56(9) . 1_655 ? O18 Cd2 O23 84.82(10) 4_655 1_655 ? O12 Cd2 O2 85.57(9) . 3_565 ? O18 Cd2 O2 98.76(11) 4_655 3_565 ? O23 Cd2 O2 134.91(9) 1_655 3_565 ? O12 Cd2 O26 122.52(9) . 3_565 ? O18 Cd2 O26 87.29(11) 4_655 3_565 ? O23 Cd2 O26 82.03(8) 1_655 3_565 ? O2 Cd2 O26 53.53(8) 3_565 3_565 ? O12 Cd2 O22 91.04(9) . 4_655 ? O18 Cd2 O22 52.77(9) 4_655 4_655 ? O23 Cd2 O22 124.95(9) 1_655 4_655 ? O2 Cd2 O22 89.79(10) 3_565 4_655 ? O26 Cd2 O22 122.56(10) 3_565 4_655 ? O12 Cd2 O8 84.77(9) . 1_655 ? O18 Cd2 O8 87.57(10) 4_655 1_655 ? O23 Cd2 O8 52.98(8) 1_655 1_655 ? O2 Cd2 O8 170.04(8) 3_565 1_655 ? O26 Cd2 O8 135.00(8) 3_565 1_655 ? O22 Cd2 O8 87.95(10) 4_655 1_655 ? O12 Cd2 O15 52.46(8) . . ? O18 Cd2 O15 164.20(9) 4_655 . ? O23 Cd2 O15 83.76(9) 1_655 . ? O2 Cd2 O15 81.81(11) 3_565 . ? O26 Cd2 O15 80.35(10) 3_565 . ? O22 Cd2 O15 142.91(8) 4_655 . ? O8 Cd2 O15 94.20(10) 1_655 . ? O42 P3 O35 121.8(2) . . ? O42 P3 O9 104.32(18) . . ? O35 P3 O9 111.74(17) . . ? O42 P3 O10 110.27(17) . . ? O35 P3 O10 104.79(17) . . ? O9 P3 O10 102.40(12) . . ? C9 O1 Cd1 93.55(19) . 1_655 ? C20 O2 Cd2 93.7(2) . 3_465 ? C9 O3 Cd1 91.5(2) . 1_655 ? C18 O4 Cd1 117.8(2) . 3_566 ? C46 C5 C10 117.7(3) . . ? C46 C5 C7 121.5(3) . . ? C10 C5 C7 120.8(3) . . ? C1C C7 C15 119.2(3) . . ? C1C C7 C5 120.3(3) . . ? C15 C7 C5 120.5(3) . . ? C3 O8 Cd2 86.9(2) . 1_455 ? C46 O9 P3 120.8(2) . . ? C1C O10 P3 121.2(2) . . ? C40 C11 C37 121.0(3) . . ? C40 C11 H11 119.5 . . ? C37 C11 H11 119.5 . . ? C1D O12 Cd2 99.2(2) . . ? C25 O13 Cd1 94.5(2) . 2_564 ? C16 C14 C28 118.2(3) . . ? C16 C14 C25 120.7(3) . . ? C28 C14 C25 121.0(3) . . ? C1D O15 Cd2 83.8(2) . . ? C17 C16 C14 120.9(3) . . ? C17 C16 H16 119.6 . . ? C14 C16 H16 119.6 . . ? C21 C17 C16 119.5(3) . . ? C21 C17 C44 120.5(3) . . ? C16 C17 C44 119.8(3) . . ? C23 O18 Cd2 98.0(2) . 4_645 ? C39 C19 C41 121.9(3) . . ? C39 C19 H19 119.1 . . ? C41 C19 H19 119.1 . . ? O26 C20 O2 121.8(3) . . ? O26 C20 C37 119.3(3) . . ? O2 C20 C37 118.7(3) . . ? C17 C21 C27 122.4(3) . . ? C17 C21 H21 118.8 . . ? C27 C21 H21 118.8 . . ? C23 O22 Cd2 88.7(2) . 4_645 ? C3 O23 Cd2 97.1(2) . 1_455 ? C40 C24 C22 121.9(3) . . ? C40 C24 H24 119.0 . . ? C22 C24 H24 119.0 . . ? O13 C25 O34 120.2(3) . . ? O13 C25 C14 120.7(3) . . ? O34 C25 C14 119.2(4) . . ? C20 O26 Cd2 90.6(2) . 3_465 ? C21 C27 C28 118.8(3) . . ? C21 C27 C1D 121.0(3) . . ? C28 C27 C1D 120.0(3) . . ? C27 C28 C14 120.3(3) . . ? C27 C28 H28 119.9 . . ? C14 C28 H28 119.9 . . ? C50 C29 C31 121.5(3) . . ? C50 C29 H29 119.3 . . ? C31 C29 H29 119.3 . . ? C8 O30 Cd1 102.5(2) . . ? C29 C31 C10 120.3(3) . . ? C29 C31 C48 121.0(3) . . ? C10 C31 C48 118.7(3) . . ? C36 C32 C2 122.3(3) . . ? C36 C32 H32 118.8 . . ? C2 C32 H32 118.8 . . ? C6 C33 C41 121.0(3) . . ? C6 C33 H33 119.5 . . ? C41 C33 H33 119.5 . . ? C25 O34 Cd1 91.2(2) . 2_564 ? C32 C36 C38 117.8(3) . . ? C32 C36 C1E 119.6(3) . . ? C38 C36 C1E 122.5(3) . . ? C1A C37 C11 119.8(3) . . ? C1A C37 C20 120.0(3) . . ? C11 C37 C20 120.2(3) . . ? C1 C38 C36 121.0(3) . . ? C1 C38 H38 119.5 . . ? C36 C38 H38 119.5 . . ? C19 C39 C47 120.0(3) . . ? C19 C39 C9 120.9(3) . . ? C47 C39 C9 119.1(3) . . ? C11 C40 C24 118.7(3) . . ? C11 C40 C3 121.1(3) . . ? C24 C40 C3 120.0(3) . . ? C19 C41 C33 117.4(3) . . ? C19 C41 C50 121.4(3) . . ? C33 C41 C50 121.0(3) . . ? C1 C43 C2 120.6(3) . . ? C1 C43 H43 119.7 . . ? C2 C43 H43 119.7 . . ? C48 C44 C1F 119.6(3) . . ? C48 C44 C17 120.5(3) . . ? C1F C44 C17 119.8(3) . . ? C5 C46 O9 117.0(3) . . ? C5 C46 C50 123.2(3) . . ? O9 C46 C50 119.8(3) . . ? C39 C47 C6 118.7(3) . . ? C39 C47 H47 120.7 . . ? C6 C47 H47 120.7 . . ? C44 C48 C31 120.8(3) . . ? C44 C48 H48 119.6 . . ? C31 C48 H48 119.6 . . ? C1F C49 C10 120.5(3) . . ? C1F C49 H49 119.7 . . ? C10 C49 H49 119.7 . . ? C29 C50 C46 118.0(3) . . ? C29 C50 C41 119.3(3) . . ? C46 C50 C41 122.7(3) . . ? C43 C1 C38 120.2(3) . . ? C43 C1 C23 118.1(3) . . ? C38 C1 C23 121.7(3) . . ? C32 C2 C43 118.0(3) . . ? C32 C2 C8 121.2(3) . . ? C43 C2 C8 120.8(3) . . ? O23 C3 O8 123.0(3) . . ? O23 C3 C40 117.5(3) . . ? O8 C3 C40 119.4(3) . . ? C12 C4 C1B 121.7(3) . . ? C12 C4 C15 119.2(3) . . ? C1B C4 C15 119.0(3) . . ? C33 C6 C47 121.0(3) . . ? C33 C6 C18 120.3(3) . . ? C47 C6 C18 118.7(3) . . ? O6 C8 O30 123.1(3) . . ? O6 C8 C2 119.8(3) . . ? O30 C8 C2 117.0(3) . . ? O1 C9 O3 121.3(3) . . ? O1 C9 C39 118.8(3) . . ? O3 C9 C39 119.9(3) . . ? O1 C9 Cd1 59.88(16) . 1_655 ? O3 C9 Cd1 61.55(17) . 1_655 ? C39 C9 Cd1 176.0(2) . 1_655 ? C31 C10 C49 119.5(3) . . ? C31 C10 C5 119.0(3) . . ? C49 C10 C5 121.5(3) . . ? C1E C12 C4 121.8(3) . . ? C1E C12 H12 119.1 . . ? C4 C12 H12 119.1 . . ? C1H C13 C15 122.5(3) . . ? C1H C13 H13 118.8 . . ? C15 C13 H13 118.8 . . ? C13 C15 C7 124.8(3) . . ? C13 C15 C4 116.5(3) . . ? C7 C15 C4 118.6(3) . . ? O4 C18 O21 123.8(4) . . ? O4 C18 C6 117.8(3) . . ? O21 C18 C6 117.9(4) . . ? C37 C1A C22 121.6(3) . . ? C37 C1A H1A 119.2 . . ? C22 C1A H1A 119.2 . . ? C1G C1B C4 121.5(3) . . ? C1G C1B H1B 119.3 . . ? C4 C1B H1B 119.3 . . ? C7 C1C O10 118.7(3) . . ? C7 C1C C1E 122.6(3) . . ? O10 C1C C1E 118.7(3) . . ? O15 C1D O12 123.8(3) . . ? O15 C1D C27 118.4(4) . . ? O12 C1D C27 117.8(3) . . ? C12 C1E C1C 118.3(3) . . ? C12 C1E C36 120.0(3) . . ? C1C C1E C36 121.6(3) . . ? C49 C1F C44 120.7(3) . . ? C49 C1F H1F 119.6 . . ? C44 C1F H1F 119.6 . . ? C1B C1G C1H 119.2(3) . . ? C1B C1G C22 120.5(3) . . ? C1H C1G C22 120.2(3) . . ? C13 C1H C1G 120.3(3) . . ? C13 C1H H1H 119.8 . . ? C1G C1H H1H 119.8 . . ? C24 C22 C1A 116.6(3) . . ? C24 C22 C1G 123.3(3) . . ? C1A C22 C1G 120.1(3) . . ? O22 C23 O18 120.5(3) . . ? O22 C23 C1 120.9(3) . . ? O18 C23 C1 118.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C46 C5 C7 C1C -54.0(6) . . . . ? C10 C5 C7 C1C 128.7(4) . . . . ? C46 C5 C7 C15 123.3(4) . . . . ? C10 C5 C7 C15 -54.1(6) . . . . ? O42 P3 O9 C46 -166.1(2) . . . . ? O35 P3 O9 C46 60.6(3) . . . . ? O10 P3 O9 C46 -51.1(2) . . . . ? O42 P3 O10 C1C 69.3(3) . . . . ? O35 P3 O10 C1C -158.1(2) . . . . ? O9 P3 O10 C1C -41.3(2) . . . . ? O18 Cd2 O12 C1D 177.3(2) 4_655 . . . ? O23 Cd2 O12 C1D -60.7(2) 1_655 . . . ? O2 Cd2 O12 C1D 78.6(2) 3_565 . . . ? O26 Cd2 O12 C1D 37.7(2) 3_565 . . . ? O22 Cd2 O12 C1D 168.3(2) 4_655 . . . ? O8 Cd2 O12 C1D -103.9(2) 1_655 . . . ? O15 Cd2 O12 C1D -4.5(2) . . . . ? O12 Cd2 O15 C1D 4.5(2) . . . . ? O18 Cd2 O15 C1D -179.4(3) 4_655 . . . ? O23 Cd2 O15 C1D 136.6(2) 1_655 . . . ? O2 Cd2 O15 C1D -86.2(2) 3_565 . . . ? O26 Cd2 O15 C1D -140.4(2) 3_565 . . . ? O22 Cd2 O15 C1D -7.6(3) 4_655 . . . ? O8 Cd2 O15 C1D 84.6(2) 1_655 . . . ? C28 C14 C16 C17 -0.4(5) . . . . ? C25 C14 C16 C17 -179.1(3) . . . . ? C14 C16 C17 C21 1.2(5) . . . . ? C14 C16 C17 C44 175.8(3) . . . . ? Cd2 O2 C20 O26 -6.6(5) 3_465 . . . ? Cd2 O2 C20 C37 178.9(3) 3_465 . . . ? C16 C17 C21 C27 -1.2(5) . . . . ? C44 C17 C21 C27 -175.8(3) . . . . ? Cd1 O13 C25 O34 -11.4(4) 2_564 . . . ? Cd1 O13 C25 C14 168.7(3) 2_564 . . . ? C16 C14 C25 O13 0.6(5) . . . . ? C28 C14 C25 O13 -178.1(3) . . . . ? C16 C14 C25 O34 -179.3(3) . . . . ? C28 C14 C25 O34 2.0(5) . . . . ? O2 C20 O26 Cd2 6.3(4) . . . 3_465 ? C37 C20 O26 Cd2 -179.2(4) . . . 3_465 ? C17 C21 C27 C28 0.3(5) . . . . ? C17 C21 C27 C1D 174.7(3) . . . . ? C21 C27 C28 C14 0.5(5) . . . . ? C1D C27 C28 C14 -173.9(3) . . . . ? C16 C14 C28 C27 -0.5(5) . . . . ? C25 C14 C28 C27 178.2(3) . . . . ? O4 Cd1 O30 C8 -73.0(3) 3_466 . . . ? O1 Cd1 O30 C8 67.5(2) 1_455 . . . ? O13 Cd1 O30 C8 -159.0(2) 2_565 . . . ? O3 Cd1 O30 C8 74.4(4) 1_455 . . . ? O34 Cd1 O30 C8 148.0(2) 2_565 . . . ? C9 Cd1 O30 C8 70.7(3) 1_455 . . . ? C50 C29 C31 C10 -1.5(6) . . . . ? C50 C29 C31 C48 -178.5(3) . . . . ? O13 C25 O34 Cd1 11.2(4) . . . 2_564 ? C14 C25 O34 Cd1 -168.9(3) . . . 2_564 ? C2 C32 C36 C38 2.7(5) . . . . ? C2 C32 C36 C1E 179.2(3) . . . . ? C40 C11 C37 C1A 3.9(7) . . . . ? C40 C11 C37 C20 -177.0(4) . . . . ? O26 C20 C37 C1A -14.0(7) . . . . ? O2 C20 C37 C1A 160.7(4) . . . . ? O26 C20 C37 C11 166.9(4) . . . . ? O2 C20 C37 C11 -18.4(7) . . . . ? C32 C36 C38 C1 -2.3(5) . . . . ? C1E C36 C38 C1 -178.8(3) . . . . ? C41 C19 C39 C47 -1.5(5) . . . . ? C41 C19 C39 C9 179.2(3) . . . . ? C37 C11 C40 C24 -6.3(7) . . . . ? C37 C11 C40 C3 178.3(4) . . . . ? C22 C24 C40 C11 3.4(7) . . . . ? C22 C24 C40 C3 178.8(4) . . . . ? C39 C19 C41 C33 1.0(5) . . . . ? C39 C19 C41 C50 176.7(3) . . . . ? C6 C33 C41 C19 -0.2(5) . . . . ? C6 C33 C41 C50 -175.8(3) . . . . ? C21 C17 C44 C48 -41.0(5) . . . . ? C16 C17 C44 C48 144.4(3) . . . . ? C21 C17 C44 C1F 135.9(4) . . . . ? C16 C17 C44 C1F -38.7(5) . . . . ? C10 C5 C46 O9 -175.3(3) . . . . ? C7 C5 C46 O9 7.3(5) . . . . ? C10 C5 C46 C50 6.7(5) . . . . ? C7 C5 C46 C50 -170.8(3) . . . . ? P3 O9 C46 C5 71.1(4) . . . . ? P3 O9 C46 C50 -110.9(3) . . . . ? C19 C39 C47 C6 1.2(5) . . . . ? C9 C39 C47 C6 -179.5(3) . . . . ? C1F C44 C48 C31 -2.2(5) . . . . ? C17 C44 C48 C31 174.7(3) . . . . ? C29 C31 C48 C44 177.2(3) . . . . ? C10 C31 C48 C44 0.3(5) . . . . ? C31 C29 C50 C46 0.5(5) . . . . ? C31 C29 C50 C41 179.4(3) . . . . ? C5 C46 C50 C29 -3.2(5) . . . . ? O9 C46 C50 C29 178.8(3) . . . . ? C5 C46 C50 C41 177.9(3) . . . . ? O9 C46 C50 C41 -0.1(5) . . . . ? C19 C41 C50 C29 -35.1(5) . . . . ? C33 C41 C50 C29 140.4(3) . . . . ? C19 C41 C50 C46 143.8(3) . . . . ? C33 C41 C50 C46 -40.7(5) . . . . ? C2 C43 C1 C38 1.4(5) . . . . ? C2 C43 C1 C23 -177.3(3) . . . . ? C36 C38 C1 C43 0.3(5) . . . . ? C36 C38 C1 C23 179.1(3) . . . . ? C36 C32 C2 C43 -1.0(5) . . . . ? C36 C32 C2 C8 177.5(3) . . . . ? C1 C43 C2 C32 -1.1(5) . . . . ? C1 C43 C2 C8 -179.6(3) . . . . ? Cd2 O23 C3 O8 3.2(4) 1_455 . . . ? Cd2 O23 C3 C40 -174.3(3) 1_455 . . . ? Cd2 O8 C3 O23 -2.9(4) 1_455 . . . ? Cd2 O8 C3 C40 174.5(3) 1_455 . . . ? C11 C40 C3 O23 6.9(6) . . . . ? C24 C40 C3 O23 -168.4(4) . . . . ? C11 C40 C3 O8 -170.7(4) . . . . ? C24 C40 C3 O8 14.1(6) . . . . ? C41 C33 C6 C47 -0.2(5) . . . . ? C41 C33 C6 C18 178.5(3) . . . . ? C39 C47 C6 C33 -0.3(5) . . . . ? C39 C47 C6 C18 -179.0(3) . . . . ? Cd1 O30 C8 O6 -10.8(5) . . . . ? Cd1 O30 C8 C2 169.7(2) . . . . ? C32 C2 C8 O6 17.3(5) . . . . ? C43 C2 C8 O6 -164.3(4) . . . . ? C32 C2 C8 O30 -163.2(3) . . . . ? C43 C2 C8 O30 15.2(5) . . . . ? Cd1 O1 C9 O3 4.0(4) 1_655 . . . ? Cd1 O1 C9 C39 -175.6(3) 1_655 . . . ? Cd1 O3 C9 O1 -3.9(3) 1_655 . . . ? Cd1 O3 C9 C39 175.7(3) 1_655 . . . ? C19 C39 C9 O1 3.8(5) . . . . ? C47 C39 C9 O1 -175.5(3) . . . . ? C19 C39 C9 O3 -175.9(3) . . . . ? C47 C39 C9 O3 4.8(5) . . . . ? C19 C39 C9 Cd1 -66(4) . . . 1_655 ? C47 C39 C9 Cd1 115(3) . . . 1_655 ? C29 C31 C10 C49 -174.1(4) . . . . ? C48 C31 C10 C49 2.9(5) . . . . ? C29 C31 C10 C5 5.0(5) . . . . ? C48 C31 C10 C5 -178.0(3) . . . . ? C1F C49 C10 C31 -4.2(6) . . . . ? C1F C49 C10 C5 176.7(4) . . . . ? C46 C5 C10 C31 -7.4(5) . . . . ? C7 C5 C10 C31 170.0(3) . . . . ? C46 C5 C10 C49 171.7(3) . . . . ? C7 C5 C10 C49 -10.8(6) . . . . ? C1B C4 C12 C1E 175.0(4) . . . . ? C15 C4 C12 C1E -0.6(6) . . . . ? C1H C13 C15 C7 172.1(4) . . . . ? C1H C13 C15 C4 -9.5(6) . . . . ? C1C C7 C15 C13 172.3(4) . . . . ? C5 C7 C15 C13 -5.0(6) . . . . ? C1C C7 C15 C4 -6.0(5) . . . . ? C5 C7 C15 C4 176.7(3) . . . . ? C12 C4 C15 C13 -173.6(4) . . . . ? C1B C4 C15 C13 10.7(6) . . . . ? C12 C4 C15 C7 4.9(6) . . . . ? C1B C4 C15 C7 -170.8(4) . . . . ? Cd1 O4 C18 O21 -0.3(7) 3_566 . . . ? Cd1 O4 C18 C6 -172.3(3) 3_566 . . . ? C33 C6 C18 O4 22.5(6) . . . . ? C47 C6 C18 O4 -158.8(4) . . . . ? C33 C6 C18 O21 -149.9(5) . . . . ? C47 C6 C18 O21 28.8(7) . . . . ? C11 C37 C1A C22 1.7(7) . . . . ? C20 C37 C1A C22 -177.5(4) . . . . ? C12 C4 C1B C1G -179.6(4) . . . . ? C15 C4 C1B C1G -4.0(7) . . . . ? C15 C7 C1C O10 -177.7(3) . . . . ? C5 C7 C1C O10 -0.4(5) . . . . ? C15 C7 C1C C1E 3.0(6) . . . . ? C5 C7 C1C C1E -179.7(3) . . . . ? P3 O10 C1C C7 71.3(4) . . . . ? P3 O10 C1C C1E -109.4(3) . . . . ? Cd2 O15 C1D O12 -7.9(4) . . . . ? Cd2 O15 C1D C27 169.9(3) . . . . ? Cd2 O12 C1D O15 9.1(4) . . . . ? Cd2 O12 C1D C27 -168.7(3) . . . . ? C21 C27 C1D O15 -176.8(3) . . . . ? C28 C27 C1D O15 -2.5(5) . . . . ? C21 C27 C1D O12 1.2(5) . . . . ? C28 C27 C1D O12 175.4(3) . . . . ? C4 C12 C1E C1C -2.5(6) . . . . ? C4 C12 C1E C36 178.3(3) . . . . ? C7 C1C C1E C12 1.3(5) . . . . ? O10 C1C C1E C12 -177.9(3) . . . . ? C7 C1C C1E C36 -179.5(3) . . . . ? O10 C1C C1E C36 1.2(5) . . . . ? C32 C36 C1E C12 -54.1(5) . . . . ? C38 C36 C1E C12 122.3(4) . . . . ? C32 C36 C1E C1C 126.8(4) . . . . ? C38 C36 C1E C1C -56.8(5) . . . . ? C10 C49 C1F C44 2.3(6) . . . . ? C48 C44 C1F C49 0.9(6) . . . . ? C17 C44 C1F C49 -176.1(4) . . . . ? C4 C1B C1G C1H -4.4(7) . . . . ? C4 C1B C1G C22 172.3(4) . . . . ? C15 C13 C1H C1G 1.3(7) . . . . ? C1B C1G C1H C13 5.9(7) . . . . ? C22 C1G C1H C13 -170.7(4) . . . . ? C40 C24 C22 C1A 1.8(7) . . . . ? C40 C24 C22 C1G -176.7(4) . . . . ? C37 C1A C22 C24 -4.4(7) . . . . ? C37 C1A C22 C1G 174.2(4) . . . . ? C1B C1G C22 C24 31.7(7) . . . . ? C1H C1G C22 C24 -151.7(5) . . . . ? C1B C1G C22 C1A -146.8(5) . . . . ? C1H C1G C22 C1A 29.9(7) . . . . ? Cd2 O22 C23 O18 1.1(4) 4_645 . . . ? Cd2 O22 C23 C1 -176.8(3) 4_645 . . . ? Cd2 O18 C23 O22 -1.2(4) 4_645 . . . ? Cd2 O18 C23 C1 176.7(3) 4_645 . . . ? C43 C1 C23 O22 166.2(3) . . . . ? C38 C1 C23 O22 -12.6(5) . . . . ? C43 C1 C23 O18 -11.8(5) . . . . ? C38 C1 C23 O18 169.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 64.74 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.589 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.033 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.066 0.416 0.036 7921 2594 ' ' _platon_squeeze_details ; the solvent molecules removed by the SQUEEZE process could be regarded as DMF molecules and dimethylammonium cations(DMA+) as counterions. In every single unit cell, there are 16 dimethylammonium cations containing 416 electrons, so the rest of 2594 C 416 = 2178 electrons are belongs to DMF molecules. As a result, there are ~55 DMF molecules per unit cell. The theoretical occupied volume of single DMF molecule and dimethylammonium cations are 75.26 and 55.33 respectively, indicating total volume of free molecules is 75.26*54 + 55.33*16 = 5024.58 per unit cell which is much smaller than 7921 calculated by PLATON. ; _database_code_depnum_ccdc_archive 'CCDC 936188'