#=============================================================================== data_global #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author #Name and address of author for correspondence ; ? ; _publ_contact_author_phone ? _publ_contact_author_fax ? _publ_contact_author_email ? _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_letter ; ? #Insert text if wanted ; #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? #Insert chemical title here ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address ' ?' #<--'Last name, first name ' ?' #=============================================================================== # 4. TEXT _publ_section_abstract ; ? #Insert appropriate text here if wanted. ; _publ_section_comment ; ? #Insert appropriate text here if wanted. ; _publ_section_experimental ; ? #Insert appropriate text here if wanted. ; _publ_section_references ; Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. and White, P.S. (1989) J. Appl. Cryst., 22, 384-387. Flack, H., (1983) Acta Cryst., A39, 876-881. International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Larson, A.C., (1970) p.293, Crystallographic Computing, Munksgaard, Copenhagen. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. Rogers, D., (1981) Acta Cryst., A37, 734-741. ? #Insert any other references here ; _publ_section_figure_captions ; ? #Insert figure captions here if wanted ; _publ_section_acknowledgements ; ? #Insert any acknowledgements here. ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_c03066 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common ? _chemical_formula_moiety 'W2 P2 C42 H68 B2 N12 O4 ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'W2 P2 C42 H68 B2 N12 O4 ' _chemical_formula_weight 1256.33 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source W ? -0.849 6.872 'International Tables Vol. IV Table 2.2B' P ? 0.102 0.094 'International Tables Vol. IV Table 2.2B' C ? 0.003 0.002 'International Tables Vol. IV Table 2.2B' H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B' B ? 0.001 0.001 'International Tables Vol. IV Table 2.2B' N ? 0.006 0.003 'International Tables Vol. IV Table 2.2B' O ? 0.011 0.006 'International Tables Vol. IV Table 2.2B' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 _cell_length_a 18.2841(4) _cell_length_b 18.5662(4) _cell_length_c 16.1972(4) _cell_angle_alpha 90.0 _cell_angle_beta 111.822(1) _cell_angle_gamma 90.0 _cell_volume 5104.40(20) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 6140 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.00 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method ? _exptl_crystal_F_000 2493.63 _exptl_absorpt_coefficient_mu 4.62 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1K' _diffrn_measurement_method 'Omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 39461 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 28.00 _diffrn_reflns_reduction_process ? _reflns_number_total 12258 _reflns_number_observed 9208 _reflns_observed_criterion 'Inet > 2.5\s(Inet)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT/NRCVAX DATRD2' _computing_structure_solution 'NRCVAX SOLVER' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_molecular_graphics 'NRCVAX' _computing_publication_material 'NRCVAX TABLES Jan 94 Version' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; ? #Insert any special details here. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 1/(\s^2^(F)+0.0000F^2^) _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 9207 _refine_ls_number_parameters 577 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.054 _refine_ls_R_factor_obs 0.034 _refine_ls_wR_factor_all 0.037 _refine_ls_wR_factor_obs 0.036 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.70 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean ? _refine_diff_density_max 4.71 _refine_diff_density_min -1.99 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol W1 0.572231(12) 0.685965(10) 0.677640(13) 0.01711(10) Uani ? . W P1 0.63446(8) 0.71979(7) 0.83806(9) 0.0230(7) Uani ? . P O1 0.52093(21) 0.77524(19) 0.5841(3) 0.0292(23) Uani ? . O C2 0.5387(3) 0.7880(3) 0.6674(4) 0.028(3) Uani ? . C C3 0.5139(4) 0.8582(3) 0.6948(4) 0.044(4) Uani ? . C C4 0.4742(3) 0.6669(3) 0.6888(3) 0.022(3) Uani ? . C O5 0.41213(22) 0.65757(21) 0.6956(3) 0.035(3) Uani ? . O C6 0.7046(3) 0.6555(3) 0.9112(4) 0.033(3) Uani ? . C C7 0.5708(4) 0.7419(3) 0.8990(4) 0.039(4) Uani ? . C C8 0.6975(4) 0.7997(3) 0.8634(4) 0.040(4) Uani ? . C B9 0.6935(3) 0.5785(3) 0.6283(4) 0.019(3) Uani ? . B N10 0.62040(23) 0.57973(21) 0.7343(3) 0.0183(22) Uani ? . N N11 0.67911(23) 0.54936(21) 0.7105(3) 0.0178(23) Uani ? . N C12 0.7001(3) 0.4845(3) 0.7515(3) 0.022(3) Uani ? . C C13 0.6553(3) 0.4733(3) 0.8023(3) 0.024(3) Uani ? . C C14 0.6057(3) 0.5324(3) 0.7893(3) 0.021(3) Uani ? . C C15 0.7617(3) 0.4373(3) 0.7409(4) 0.029(3) Uani ? . C C16 0.5437(3) 0.5434(3) 0.8278(4) 0.028(3) Uani ? . C N17 0.68640(24) 0.71185(21) 0.6545(3) 0.0188(23) Uani ? . N N18 0.73022(24) 0.65414(21) 0.6448(3) 0.0193(24) Uani ? . N C19 0.7961(3) 0.6779(3) 0.6326(3) 0.023(3) Uani ? . C C20 0.7939(3) 0.7516(3) 0.6341(3) 0.026(3) Uani ? . C C21 0.7256(3) 0.7710(3) 0.6477(3) 0.023(3) Uani ? . C C22 0.8564(3) 0.6298(3) 0.6205(4) 0.034(4) Uani ? . C C23 0.6965(4) 0.8467(3) 0.6485(4) 0.034(3) Uani ? . C N24 0.55278(23) 0.62309(21) 0.5561(3) 0.0174(22) Uani ? . N N25 0.61387(23) 0.58252(20) 0.5495(3) 0.0177(23) Uani ? . N C26 0.5891(3) 0.5500(3) 0.4697(3) 0.022(3) Uani ? . C C27 0.5117(3) 0.5692(3) 0.4228(3) 0.024(3) Uani ? . C C28 0.4909(3) 0.6148(3) 0.4787(3) 0.021(3) Uani ? . C C29 0.6415(3) 0.5028(3) 0.4393(4) 0.034(3) Uani ? . C C30 0.4152(3) 0.6537(3) 0.4599(4) 0.033(3) Uani ? . C W2 0.862799(14) 0.377439(11) 0.141232(15) 0.02486(13) Uani ? . W P2 0.74903(9) 0.36660(7) 0.19125(10) 0.0274(8) Uani ? . P C31 0.8592(4) 0.4004(3) 0.0007(4) 0.035(4) Uani ? . C C32 0.7857(4) 0.4503(3) 0.0766(4) 0.040(4) Uani ? . C O32 0.7436(3) 0.49925(25) 0.0431(3) 0.066(4) Uani ? . O C34 0.9079(4) 0.4659(3) 0.1980(4) 0.044(4) Uani ? . C O35 0.9324(4) 0.5233(3) 0.2279(4) 0.082(4) Uani ? . O C36 0.6492(4) 0.3655(4) 0.1072(4) 0.048(4) Uani ? . C C37 0.7367(4) 0.4372(4) 0.2629(5) 0.052(4) Uani ? . C C38 0.7480(4) 0.2837(3) 0.2510(4) 0.040(4) Uani ? . C B39 0.9404(4) 0.2120(3) 0.1867(4) 0.024(3) Uani ? . B N40 0.9198(3) 0.31919(24) 0.2729(3) 0.028(3) Uani ? . N N41 0.9346(3) 0.24659(24) 0.2707(3) 0.026(3) Uani ? . N C42 0.9634(3) 0.2196(3) 0.3545(4) 0.031(3) Uani ? . C C43 0.9660(3) 0.2753(4) 0.4112(4) 0.039(4) Uani ? . C C44 0.9398(3) 0.3370(3) 0.3592(4) 0.032(3) Uani ? . C C45 0.9878(4) 0.1426(4) 0.3750(4) 0.043(4) Uani ? . C C46 0.9400(4) 0.4110(4) 0.3929(4) 0.051(4) Uani ? . C N47 0.8181(3) 0.26847(21) 0.0752(3) 0.0220(25) Uani ? . N N48 0.85931(24) 0.20690(21) 0.1104(3) 0.0198(23) Uani ? . N C49 0.8273(3) 0.1496(3) 0.0586(3) 0.023(3) Uani ? . C C50 0.7622(3) 0.1743(3) -0.0124(3) 0.022(3) Uani ? . C C51 0.7585(3) 0.2479(3) 0.0001(3) 0.023(3) Uani ? . C C52 0.8606(3) 0.0752(3) 0.0778(4) 0.028(3) Uani ? . C C53 0.6990(4) 0.2990(3) -0.0612(4) 0.038(4) Uani ? . C N54 0.9798(3) 0.33440(23) 0.1444(3) 0.027(3) Uani ? . N N55 0.99397(25) 0.26129(23) 0.1557(3) 0.0240(25) Uani ? . N C56 1.0635(3) 0.2443(3) 0.1493(3) 0.029(3) Uani ? . C C57 1.0953(3) 0.3079(4) 0.1341(4) 0.038(4) Uani ? . C C58 1.0428(3) 0.3624(3) 0.1329(4) 0.032(3) Uani ? . C C59 1.0931(3) 0.1697(3) 0.1550(4) 0.040(4) Uani ? . C C60 1.0531(4) 0.4421(3) 0.1229(4) 0.045(4) Uani ? . C H3a 0.531 0.860 0.759 0.0531 Uiso ? . H H3b 0.538 0.897 0.675 0.0531 Uiso ? . H H3c 0.458 0.863 0.669 0.0531 Uiso ? . H H6a 0.741 0.641 0.885 0.0415 Uiso ? . H H6b 0.733 0.678 0.968 0.0415 Uiso ? . H H6c 0.676 0.614 0.920 0.0415 Uiso ? . H H7a 0.534 0.704 0.892 0.0515 Uiso ? . H H7b 0.602 0.748 0.961 0.0515 Uiso ? . H H7c 0.543 0.786 0.876 0.0515 Uiso ? . H H8a 0.669 0.840 0.829 0.0485 Uiso ? . H H8b 0.714 0.811 0.926 0.0485 Uiso ? . H H8c 0.743 0.791 0.849 0.0485 Uiso ? . H H9 0.728 0.546 0.614 0.0294 Uiso ? . H H13 0.658 0.433 0.840 0.0325 Uiso ? . H H15a 0.767 0.394 0.776 0.0381 Uiso ? . H H15b 0.747 0.424 0.679 0.0381 Uiso ? . H H15c 0.811 0.462 0.760 0.0381 Uiso ? . H H16a 0.544 0.503 0.865 0.0400 Uiso ? . H H16b 0.555 0.587 0.863 0.0400 Uiso ? . H H16c 0.493 0.547 0.781 0.0400 Uiso ? . H H20 0.832 0.784 0.627 0.0357 Uiso ? . H H22a 0.897 0.658 0.613 0.0456 Uiso ? . H H22b 0.879 0.600 0.672 0.0456 Uiso ? . H H22c 0.832 0.600 0.569 0.0456 Uiso ? . H H23a 0.734 0.880 0.642 0.0452 Uiso ? . H H23b 0.647 0.853 0.600 0.0452 Uiso ? . H H23c 0.690 0.855 0.704 0.0452 Uiso ? . H H27 0.479 0.554 0.364 0.0333 Uiso ? . H H29a 0.613 0.485 0.380 0.0448 Uiso ? . H H29b 0.686 0.530 0.439 0.0448 Uiso ? . H H29c 0.660 0.463 0.480 0.0448 Uiso ? . H H30a 0.379 0.641 0.402 0.0409 Uiso ? . H H30b 0.394 0.641 0.504 0.0409 Uiso ? . H H30c 0.424 0.705 0.462 0.0409 Uiso ? . H H31a 0.838 0.360 -0.037 0.0495 Uiso ? . H H31b 0.827 0.442 -0.023 0.0495 Uiso ? . H H31c 0.912 0.409 0.003 0.0495 Uiso ? . H H36a 0.646 0.329 0.063 0.0586 Uiso ? . H H36b 0.613 0.354 0.135 0.0586 Uiso ? . H H36c 0.637 0.412 0.079 0.0586 Uiso ? . H H37a 0.737 0.483 0.236 0.0661 Uiso ? . H H37b 0.687 0.431 0.271 0.0661 Uiso ? . H H37c 0.779 0.435 0.320 0.0661 Uiso ? . H H38a 0.798 0.277 0.298 0.0529 Uiso ? . H H38b 0.707 0.286 0.275 0.0529 Uiso ? . H H38c 0.738 0.244 0.210 0.0529 Uiso ? . H H39 0.963 0.165 0.201 0.0347 Uiso ? . H H43 0.983 0.273 0.475 0.0492 Uiso ? . H H45a 1.006 0.135 0.438 0.0524 Uiso ? . H H45b 0.943 0.112 0.346 0.0524 Uiso ? . H H45c 1.029 0.131 0.354 0.0524 Uiso ? . H H46a 0.956 0.410 0.456 0.0611 Uiso ? . H H46b 0.976 0.440 0.377 0.0611 Uiso ? . H H46c 0.888 0.431 0.367 0.0611 Uiso ? . H H50 0.727 0.146 -0.060 0.0325 Uiso ? . H H52a 0.829 0.043 0.032 0.0396 Uiso ? . H H52b 0.914 0.075 0.079 0.0396 Uiso ? . H H52c 0.861 0.060 0.134 0.0396 Uiso ? . H H53a 0.662 0.272 -0.110 0.0459 Uiso ? . H H53b 0.671 0.323 -0.029 0.0459 Uiso ? . H H53c 0.725 0.334 -0.084 0.0459 Uiso ? . H H57 1.144 0.314 0.126 0.0487 Uiso ? . H H59a 1.143 0.169 0.149 0.0492 Uiso ? . H H59b 1.098 0.150 0.212 0.0492 Uiso ? . H H59c 1.056 0.141 0.108 0.0492 Uiso ? . H H60a 1.102 0.451 0.115 0.0544 Uiso ? . H H60b 1.010 0.460 0.072 0.0544 Uiso ? . H H60c 1.054 0.467 0.175 0.0544 Uiso ? . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol W1 0.01753(10) 0.01804(10) 0.01724(11) 0.00074(9) 0.00817(8) -0.00092(9) W P1 0.0258(7) 0.0242(7) 0.0210(8) -0.0020(6) 0.0109(6) -0.0046(6) P O1 0.0288(21) 0.0279(20) 0.0309(24) 0.0037(17) 0.0110(18) 0.0058(18) O C2 0.021(3) 0.022(3) 0.043(4) 0.0019(24) 0.013(3) -0.001(3) C C3 0.043(4) 0.031(3) 0.055(4) 0.014(3) 0.016(3) -0.008(3) C C4 0.018(3) 0.023(3) 0.021(3) 0.0071(22) 0.0049(23) 0.0040(22) C O5 0.0230(21) 0.0453(24) 0.041(3) 0.0002(19) 0.0166(20) 0.0029(20) O C6 0.034(3) 0.037(3) 0.024(3) 0.000(3) 0.005(3) -0.002(3) C C7 0.051(4) 0.040(3) 0.033(4) 0.004(3) 0.025(3) -0.006(3) C C8 0.042(4) 0.037(3) 0.036(4) -0.013(3) 0.010(3) -0.010(3) C B9 0.023(3) 0.017(3) 0.019(3) 0.0004(25) 0.010(3) -0.0023(24) B N10 0.0193(22) 0.0199(21) 0.0168(23) -0.0010(18) 0.0079(19) -0.0027(18) N N11 0.0166(21) 0.0197(21) 0.0187(23) 0.0013(18) 0.0086(18) -0.0005(18) N C12 0.024(3) 0.020(3) 0.020(3) -0.0022(22) 0.0049(23) 0.0011(22) C C13 0.025(3) 0.023(3) 0.020(3) -0.0015(23) 0.0048(24) 0.0048(22) C C14 0.023(3) 0.025(3) 0.017(3) -0.0021(23) 0.0078(23) 0.0020(22) C C15 0.029(3) 0.024(3) 0.031(3) 0.005(3) 0.008(3) 0.0027(25) C C16 0.034(3) 0.027(3) 0.029(3) -0.001(3) 0.017(3) 0.0062(24) C N17 0.0204(22) 0.0199(21) 0.0169(23) 0.0016(19) 0.0077(19) 0.0008(18) N N18 0.0194(22) 0.0197(21) 0.0207(24) 0.0008(19) 0.0097(19) -0.0007(18) N C19 0.019(3) 0.033(3) 0.015(3) -0.0061(24) 0.0048(22) 0.0007(23) C C20 0.024(3) 0.030(3) 0.023(3) -0.006(3) 0.0090(24) 0.0044(24) C C21 0.032(3) 0.021(3) 0.015(3) -0.0042(24) 0.0081(24) 0.0000(22) C C22 0.020(3) 0.040(3) 0.047(4) 0.003(3) 0.017(3) 0.006(3) C C23 0.041(4) 0.026(3) 0.038(4) -0.008(3) 0.020(3) -0.001(3) C N24 0.0161(21) 0.0213(21) 0.0162(23) -0.0020(18) 0.0077(18) -0.0022(18) N N25 0.0217(23) 0.0184(21) 0.0132(22) 0.0013(18) 0.0067(18) -0.0002(17) N C26 0.034(3) 0.0171(24) 0.019(3) -0.0026(23) 0.0136(25) -0.0038(21) C C27 0.024(3) 0.022(3) 0.024(3) -0.0049(24) 0.0057(24) -0.0022(23) C C28 0.020(3) 0.022(3) 0.021(3) -0.0059(22) 0.0090(23) 0.0047(22) C C29 0.044(4) 0.033(3) 0.027(3) 0.003(3) 0.016(3) -0.011(3) C C30 0.019(3) 0.044(3) 0.029(3) -0.004(3) 0.003(3) -0.003(3) C W2 0.03935(14) 0.01951(11) 0.02334(13) -0.00699(10) 0.02050(11) -0.00400(9) W P2 0.0348(8) 0.0250(7) 0.0278(9) 0.0013(7) 0.0180(7) 0.0006(6) P C31 0.049(4) 0.030(3) 0.039(4) 0.003(3) 0.031(3) 0.005(3) C C32 0.069(5) 0.027(3) 0.040(4) 0.005(3) 0.039(4) 0.003(3) C O32 0.109(4) 0.041(3) 0.066(3) 0.036(3) 0.054(3) 0.023(3) O C34 0.071(5) 0.041(4) 0.037(4) -0.027(4) 0.040(4) -0.012(3) C O35 0.147(6) 0.052(3) 0.086(4) -0.055(3) 0.089(4) -0.044(3) O C36 0.041(4) 0.064(5) 0.042(4) -0.001(3) 0.019(3) 0.003(3) C C37 0.050(4) 0.058(4) 0.060(5) -0.007(4) 0.035(4) -0.027(4) C C38 0.036(4) 0.041(3) 0.051(4) 0.003(3) 0.025(3) 0.016(3) C B39 0.028(3) 0.023(3) 0.023(4) 0.003(3) 0.012(3) 0.005(3) B N40 0.030(3) 0.036(3) 0.022(3) -0.0104(22) 0.0134(21) -0.0062(21) N N41 0.032(3) 0.032(3) 0.0180(25) -0.0060(22) 0.0137(21) 0.0013(20) N C42 0.025(3) 0.048(4) 0.019(3) -0.007(3) 0.007(3) 0.005(3) C C43 0.031(3) 0.070(5) 0.017(3) -0.009(3) 0.009(3) -0.006(3) C C44 0.027(3) 0.053(4) 0.020(3) -0.008(3) 0.013(3) -0.011(3) C C45 0.050(4) 0.057(4) 0.021(3) 0.003(3) 0.010(3) 0.011(3) C C46 0.055(4) 0.062(5) 0.037(4) 0.001(4) 0.018(3) -0.022(3) C N47 0.033(3) 0.0190(21) 0.0198(25) 0.0019(20) 0.0159(21) 0.0028(18) N N48 0.0236(23) 0.0214(21) 0.0150(23) -0.0010(19) 0.0080(19) 0.0034(18) N C49 0.030(3) 0.020(3) 0.025(3) -0.0069(24) 0.019(3) 0.0002(23) C C50 0.021(3) 0.025(3) 0.021(3) -0.0054(23) 0.0086(23) -0.0029(23) C C51 0.027(3) 0.025(3) 0.017(3) -0.0017(24) 0.0080(24) -0.0015(23) C C52 0.032(3) 0.022(3) 0.036(3) -0.0021(25) 0.018(3) 0.0001(25) C C53 0.049(4) 0.033(3) 0.025(3) 0.006(3) 0.006(3) 0.000(3) C N54 0.035(3) 0.0312(25) 0.0178(25) -0.0175(22) 0.0129(21) -0.0063(20) N N55 0.0251(24) 0.0323(25) 0.0167(24) -0.0068(21) 0.0102(20) -0.0024(20) N C56 0.020(3) 0.048(4) 0.016(3) -0.008(3) 0.0037(24) 0.000(3) C C57 0.022(3) 0.062(4) 0.032(4) -0.017(3) 0.012(3) 0.000(3) C C58 0.033(3) 0.043(4) 0.022(3) -0.017(3) 0.013(3) -0.006(3) C C59 0.023(3) 0.055(4) 0.039(4) -0.003(3) 0.011(3) 0.001(3) C C60 0.050(4) 0.042(4) 0.041(4) -0.029(3) 0.016(3) -0.004(3) C #=============================================================================== # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W(1) P(1) 2.4985(14) ? ? ? W(1) O(1) 2.206(3) ? ? ? W(1) C(2) 1.979(5) ? ? ? W(1) C(4) 1.901(5) ? ? ? W(1) N(10) 2.215(4) ? ? ? W(1) N(17) 2.304(4) ? ? ? W(1) N(24) 2.201(4) ? ? ? P(1) C(6) 1.828(6) ? ? ? P(1) C(7) 1.830(6) ? ? ? P(1) C(8) 1.829(6) ? ? ? O(1) C(2) 1.288(7) ? ? ? C(2) C(3) 1.501(8) ? ? ? C(4) O(5) 1.192(6) ? ? ? B(9) N(11) 1.547(7) ? ? ? B(9) N(18) 1.537(7) ? ? ? B(9) N(25) 1.541(7) ? ? ? N(10) N(11) 1.388(6) ? ? ? N(10) C(14) 1.348(6) ? ? ? N(11) C(12) 1.360(6) ? ? ? C(12) C(13) 1.376(8) ? ? ? C(12) C(15) 1.486(7) ? ? ? C(13) C(14) 1.390(7) ? ? ? C(14) C(16) 1.496(8) ? ? ? N(17) N(18) 1.381(6) ? ? ? N(17) C(21) 1.339(6) ? ? ? N(18) C(19) 1.364(7) ? ? ? C(19) C(20) 1.369(7) ? ? ? C(19) C(22) 1.489(8) ? ? ? C(20) C(21) 1.395(8) ? ? ? C(21) C(23) 1.503(8) ? ? ? N(24) N(25) 1.384(6) ? ? ? N(24) C(28) 1.350(6) ? ? ? N(25) C(26) 1.343(6) ? ? ? C(26) C(27) 1.381(7) ? ? ? C(26) C(29) 1.509(7) ? ? ? C(27) C(28) 1.391(7) ? ? ? C(28) C(30) 1.489(8) ? ? ? W(2) P(2) 2.5053(15) ? ? ? W(2) C(31) 2.293(6) ? ? ? W(2) C(32) 1.953(6) ? ? ? W(2) C(34) 1.914(6) ? ? ? W(2) N(40) 2.269(5) ? ? ? W(2) N(47) 2.292(4) ? ? ? W(2) N(54) 2.267(5) ? ? ? P(2) C(36) 1.827(7) ? ? ? P(2) C(37) 1.820(6) ? ? ? P(2) C(38) 1.822(6) ? ? ? C(32) O(32) 1.184(8) ? ? ? C(34) O(35) 1.186(7) ? ? ? B(39) N(41) 1.545(8) ? ? ? B(39) N(48) 1.540(7) ? ? ? B(39) N(55) 1.554(7) ? ? ? N(40) N(41) 1.378(6) ? ? ? N(40) C(44) 1.348(7) ? ? ? N(41) C(42) 1.355(7) ? ? ? C(42) C(43) 1.372(9) ? ? ? C(42) C(45) 1.499(9) ? ? ? C(43) C(44) 1.395(9) ? ? ? C(44) C(46) 1.479(9) ? ? ? N(47) N(48) 1.371(6) ? ? ? N(47) C(51) 1.352(7) ? ? ? N(48) C(49) 1.347(6) ? ? ? C(49) C(50) 1.390(7) ? ? ? C(49) C(52) 1.496(7) ? ? ? C(50) C(51) 1.387(7) ? ? ? C(51) C(53) 1.505(8) ? ? ? N(54) N(55) 1.381(6) ? ? ? N(54) C(58) 1.338(7) ? ? ? N(55) C(56) 1.351(7) ? ? ? C(56) C(57) 1.378(8) ? ? ? C(56) C(59) 1.478(9) ? ? ? C(57) C(58) 1.389(9) ? ? ? C(58) C(60) 1.508(8) ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) W(1) O(1) 116.02(10) ? ? ? ? P(1) W(1) C(2) 81.57(18) ? ? ? ? P(1) W(1) C(4) 91.66(16) ? ? ? ? P(1) W(1) N(10) 80.55(10) ? ? ? ? P(1) W(1) N(17) 91.54(10) ? ? ? ? P(1) W(1) N(24) 157.40(11) ? ? ? ? O(1) W(1) C(2) 35.33(20) ? ? ? ? O(1) W(1) C(4) 91.72(17) ? ? ? ? O(1) W(1) N(10) 162.85(14) ? ? ? ? O(1) W(1) N(17) 84.89(14) ? ? ? ? O(1) W(1) N(24) 84.14(14) ? ? ? ? C(2) W(1) C(4) 84.98(21) ? ? ? ? C(2) W(1) N(10) 161.80(20) ? ? ? ? C(2) W(1) N(17) 93.31(19) ? ? ? ? C(2) W(1) N(24) 119.41(20) ? ? ? ? C(4) W(1) N(10) 92.22(18) ? ? ? ? C(4) W(1) N(17) 176.12(18) ? ? ? ? C(4) W(1) N(24) 98.15(19) ? ? ? ? N(10) W(1) N(17) 90.48(14) ? ? ? ? N(10) W(1) N(24) 78.78(14) ? ? ? ? N(17) W(1) N(24) 79.63(14) ? ? ? ? W(1) P(1) C(6) 116.66(19) ? ? ? ? W(1) P(1) C(7) 118.82(20) ? ? ? ? W(1) P(1) C(8) 116.27(21) ? ? ? ? C(6) P(1) C(7) 103.3(3) ? ? ? ? C(6) P(1) C(8) 98.7(3) ? ? ? ? C(7) P(1) C(8) 99.8(3) ? ? ? ? W(1) O(1) C(2) 62.7(3) ? ? ? ? W(1) C(2) O(1) 82.0(3) ? ? ? ? W(1) C(2) C(3) 157.7(5) ? ? ? ? O(1) C(2) C(3) 118.9(5) ? ? ? ? W(1) C(4) O(5) 177.6(4) ? ? ? ? N(11) B(9) N(18) 111.9(4) ? ? ? ? N(11) B(9) N(25) 108.6(4) ? ? ? ? N(18) B(9) N(25) 108.4(4) ? ? ? ? W(1) N(10) N(11) 118.4(3) ? ? ? ? W(1) N(10) C(14) 135.1(3) ? ? ? ? N(11) N(10) C(14) 106.5(4) ? ? ? ? B(9) N(11) N(10) 119.6(4) ? ? ? ? B(9) N(11) C(12) 128.4(4) ? ? ? ? N(10) N(11) C(12) 109.4(4) ? ? ? ? N(11) C(12) C(13) 107.6(4) ? ? ? ? N(11) C(12) C(15) 123.7(5) ? ? ? ? C(13) C(12) C(15) 128.7(5) ? ? ? ? C(12) C(13) C(14) 106.9(4) ? ? ? ? N(10) C(14) C(13) 109.6(4) ? ? ? ? N(10) C(14) C(16) 123.7(4) ? ? ? ? C(13) C(14) C(16) 126.7(5) ? ? ? ? W(1) N(17) N(18) 117.1(3) ? ? ? ? W(1) N(17) C(21) 136.8(3) ? ? ? ? N(18) N(17) C(21) 106.1(4) ? ? ? ? B(9) N(18) N(17) 119.6(4) ? ? ? ? B(9) N(18) C(19) 128.5(4) ? ? ? ? N(17) N(18) C(19) 110.2(4) ? ? ? ? N(18) C(19) C(20) 106.8(5) ? ? ? ? N(18) C(19) C(22) 124.2(5) ? ? ? ? C(20) C(19) C(22) 129.0(5) ? ? ? ? C(19) C(20) C(21) 107.1(4) ? ? ? ? N(17) C(21) C(20) 109.8(4) ? ? ? ? N(17) C(21) C(23) 124.4(5) ? ? ? ? C(20) C(21) C(23) 125.7(5) ? ? ? ? W(1) N(24) N(25) 119.4(3) ? ? ? ? W(1) N(24) C(28) 133.8(3) ? ? ? ? N(25) N(24) C(28) 106.7(4) ? ? ? ? B(9) N(25) N(24) 120.2(4) ? ? ? ? B(9) N(25) C(26) 130.7(4) ? ? ? ? N(24) N(25) C(26) 109.0(4) ? ? ? ? N(25) C(26) C(27) 108.9(4) ? ? ? ? N(25) C(26) C(29) 123.2(5) ? ? ? ? C(27) C(26) C(29) 127.9(5) ? ? ? ? C(26) C(27) C(28) 105.7(4) ? ? ? ? N(24) C(28) C(27) 109.7(4) ? ? ? ? N(24) C(28) C(30) 121.9(5) ? ? ? ? C(27) C(28) C(30) 128.4(5) ? ? ? ? P(2) W(2) C(31) 127.95(16) ? ? ? ? P(2) W(2) C(32) 73.03(18) ? ? ? ? P(2) W(2) C(34) 100.09(19) ? ? ? ? P(2) W(2) N(40) 78.72(12) ? ? ? ? P(2) W(2) N(47) 83.42(11) ? ? ? ? P(2) W(2) N(54) 148.73(11) ? ? ? ? C(31) W(2) C(32) 65.82(22) ? ? ? ? C(31) W(2) C(34) 99.54(23) ? ? ? ? C(31) W(2) N(40) 148.79(19) ? ? ? ? C(31) W(2) N(47) 80.03(17) ? ? ? ? C(31) W(2) N(54) 76.49(19) ? ? ? ? C(32) W(2) C(34) 76.1(3) ? ? ? ? C(32) W(2) N(40) 145.22(20) ? ? ? ? C(32) W(2) N(47) 107.44(21) ? ? ? ? C(32) W(2) N(54) 138.02(20) ? ? ? ? C(34) W(2) N(40) 89.54(22) ? ? ? ? C(34) W(2) N(47) 175.70(24) ? ? ? ? C(34) W(2) N(54) 93.27(23) ? ? ? ? N(40) W(2) N(47) 88.71(15) ? ? ? ? N(40) W(2) N(54) 73.20(16) ? ? ? ? N(47) W(2) N(54) 82.46(15) ? ? ? ? W(2) P(2) C(36) 118.63(22) ? ? ? ? W(2) P(2) C(37) 117.59(22) ? ? ? ? W(2) P(2) C(38) 114.43(20) ? ? ? ? C(36) P(2) C(37) 99.0(3) ? ? ? ? C(36) P(2) C(38) 100.5(3) ? ? ? ? C(37) P(2) C(38) 104.0(3) ? ? ? ? W(2) C(32) O(32) 173.5(6) ? ? ? ? W(2) C(34) O(35) 175.3(6) ? ? ? ? N(41) B(39) N(48) 111.8(4) ? ? ? ? N(41) B(39) N(55) 107.3(4) ? ? ? ? N(48) B(39) N(55) 108.2(4) ? ? ? ? W(2) N(40) N(41) 117.9(3) ? ? ? ? W(2) N(40) C(44) 135.3(4) ? ? ? ? N(41) N(40) C(44) 106.6(4) ? ? ? ? B(39) N(41) N(40) 120.5(4) ? ? ? ? B(39) N(41) C(42) 126.9(5) ? ? ? ? N(40) N(41) C(42) 110.1(4) ? ? ? ? N(41) C(42) C(43) 107.2(5) ? ? ? ? N(41) C(42) C(45) 123.2(5) ? ? ? ? C(43) C(42) C(45) 129.7(5) ? ? ? ? C(42) C(43) C(44) 107.2(5) ? ? ? ? N(40) C(44) C(43) 109.0(5) ? ? ? ? N(40) C(44) C(46) 125.0(6) ? ? ? ? C(43) C(44) C(46) 125.9(5) ? ? ? ? W(2) N(47) N(48) 119.8(3) ? ? ? ? W(2) N(47) C(51) 134.2(3) ? ? ? ? N(48) N(47) C(51) 105.9(4) ? ? ? ? B(39) N(48) N(47) 119.9(4) ? ? ? ? B(39) N(48) C(49) 127.9(4) ? ? ? ? N(47) N(48) C(49) 110.8(4) ? ? ? ? N(48) C(49) C(50) 107.2(4) ? ? ? ? N(48) C(49) C(52) 123.4(5) ? ? ? ? C(50) C(49) C(52) 129.4(5) ? ? ? ? C(49) C(50) C(51) 106.1(4) ? ? ? ? N(47) C(51) C(50) 110.1(4) ? ? ? ? N(47) C(51) C(53) 124.0(5) ? ? ? ? C(50) C(51) C(53) 125.9(5) ? ? ? ? W(2) N(54) N(55) 118.6(3) ? ? ? ? W(2) N(54) C(58) 135.6(4) ? ? ? ? N(55) N(54) C(58) 105.8(5) ? ? ? ? B(39) N(55) N(54) 120.8(4) ? ? ? ? B(39) N(55) C(56) 127.7(5) ? ? ? ? N(54) N(55) C(56) 110.7(4) ? ? ? ? N(55) C(56) C(57) 106.6(5) ? ? ? ? N(55) C(56) C(59) 123.2(5) ? ? ? ? C(57) C(56) C(59) 130.2(5) ? ? ? ? C(56) C(57) C(58) 106.9(5) ? ? ? ? N(54) C(58) C(57) 109.9(5) ? ? ? ? N(54) C(58) C(60) 123.0(6) ? ? ? ? C(57) C(58) C(60) 127.1(5) ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? #=============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #=============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./