#------------------------------------------------------------------------------ #$Date: 2014-09-06 04:49:05 +0300 (Sat, 06 Sep 2014) $ #$Revision: 123085 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/08/41/4084119.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4084119 loop_ _publ_author_name 'Jacquot, L\'ea' 'X\'emard, Mathieu' 'Clavagu\'era, Carine' 'Nocton, Gr\'egory' _publ_section_title ; Multiple One-Electron Transfers in Bipyridine Complexes of Bis(phospholyl) Thulium ; _journal_issue 15 _journal_name_full Organometallics _journal_page_first 4100 _journal_paper_doi 10.1021/om500607r _journal_volume 33 _journal_year 2014 _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'C34 H40 N4 P Tm, C7 H8' _chemical_formula_sum 'C41 H48 N4 P Tm' _chemical_formula_weight 796.73 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _atom_sites_solution_hydrogens geom _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_creation_date 2013-12-18T16:17:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 92.7420(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.7289(3) _cell_length_b 19.5591(4) _cell_length_c 17.0420(5) _cell_measurement_reflns_used 7106 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1 _cell_measurement_wavelength 0.71073 _cell_volume 3572.13(16) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _diffrn_ambient_temperature 150(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_UB_11 -0.026097 _diffrn_orient_matrix_UB_12 -0.007735 _diffrn_orient_matrix_UB_13 0.054847 _diffrn_orient_matrix_UB_21 -0.088487 _diffrn_orient_matrix_UB_22 0.010123 _diffrn_orient_matrix_UB_23 -0.017225 _diffrn_orient_matrix_UB_31 -0.014014 _diffrn_orient_matrix_UB_32 -0.049514 _diffrn_orient_matrix_UB_33 -0.01209 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 22234 _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; _diffrn_reflns_theta_full 25 _diffrn_reflns_theta_max 27.523 _diffrn_reflns_theta_min 1.586 _diffrn_source 'Enraf Nonius FR590' _exptl_absorpt_coefficient_mu 2.563 _exptl_absorpt_correction_T_max 0.632 _exptl_absorpt_correction_T_min 0.607 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1624 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.948 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.146 _refine_ls_extinction_coef 0.00007(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 425 _refine_ls_number_reflns 8132 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0471 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+26.4470P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0876 _refine_ls_wR_factor_ref 0.1027 _reflns_number_gt 5750 _reflns_number_total 8132 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL import in P 21/a CELL 0.71073 10.7289 19.5591 17.0420 90.000 92.742 90.000 ZERR 4.00 0.0003 0.0004 0.0005 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, - Z SFAC C H N P TM UNIT 164 192 16 4 4 MERG 2 FMAP 2 PLAN 20 SIZE 0.180 0.200 0.200 ACTA 50.00 BOND CONF L.S. 20 TEMP -123.00 WGHT 0.000000 26.447001 EXTI 0.000070 FVAR 0.11914 C4 1 0.407137 0.510893 0.302863 11.00000 0.02216 0.01842 = 0.01829 0.00487 -0.00230 0.00125 C2 1 0.286553 0.409111 0.305810 11.00000 0.01722 0.01564 = 0.02573 0.00168 0.00076 0.00099 C14 1 0.536683 0.566831 0.411182 11.00000 0.04749 0.02811 = 0.03898 -0.00137 -0.02344 -0.00034 AFIX 33 H14A 2 0.575753 0.609615 0.429449 11.00000 -1.50000 H14B 2 0.600969 0.531676 0.406432 11.00000 -1.50000 H14C 2 0.476354 0.551795 0.448986 11.00000 -1.50000 AFIX 0 C1 1 0.360906 0.393778 0.242712 11.00000 0.02163 0.01875 = 0.02692 0.00134 -0.00405 0.00133 C3 1 0.312961 0.475018 0.340016 11.00000 0.02605 0.02341 = 0.01803 0.00321 -0.00451 0.00323 C11 1 0.468986 0.578485 0.330434 11.00000 0.03152 0.02034 = 0.02434 -0.00179 -0.00134 -0.00192 C12 1 0.567547 0.600892 0.273769 11.00000 0.03273 0.02863 = 0.04232 0.00063 -0.00709 -0.00897 AFIX 33 H12A 2 0.605568 0.643902 0.292194 11.00000 -1.50000 H12B 2 0.528129 0.607551 0.221259 11.00000 -1.50000 H12C 2 0.632081 0.565578 0.271555 11.00000 -1.50000 AFIX 0 C9 1 0.194837 0.361410 0.341858 11.00000 0.03329 0.02442 = 0.03890 0.00696 0.00421 -0.00579 AFIX 33 H9A 2 0.154302 0.384935 0.384547 11.00000 -1.50000 H9B 2 0.239026 0.320987 0.362742 11.00000 -1.50000 H9C 2 0.131579 0.347308 0.301710 11.00000 -1.50000 AFIX 0 C13 1 0.376471 0.638031 0.336057 11.00000 0.04455 0.02273 = 0.03096 -0.00346 -0.00941 0.00032 AFIX 33 H13A 2 0.421342 0.679201 0.354080 11.00000 -1.50000 H13B 2 0.313190 0.626333 0.373433 11.00000 -1.50000 H13C 2 0.335864 0.646544 0.284244 11.00000 -1.50000 AFIX 0 N1 3 0.221974 0.464602 0.061442 11.00000 0.01872 0.02190 = 0.01897 -0.00082 0.00103 -0.00093 N2 3 0.035005 0.441066 0.156520 11.00000 0.01988 0.02093 = 0.02376 -0.00304 -0.00206 0.00292 C15 1 0.319252 0.471611 0.014457 11.00000 0.02019 0.02663 = 0.03107 0.00156 0.00423 0.00129 AFIX 43 H15 2 0.395411 0.488189 0.038007 11.00000 -1.20000 AFIX 0 C24 1 -0.056288 0.426301 0.205915 11.00000 0.02537 0.02526 = 0.02211 -0.00250 0.00213 0.00221 AFIX 43 H24 2 -0.040291 0.435074 0.260294 11.00000 -1.20000 AFIX 0 C7 1 0.243937 0.300829 0.162779 11.00000 0.03952 0.02103 = 0.04843 -0.00704 -0.00356 0.00107 AFIX 33 H7A 2 0.182478 0.297470 0.203334 11.00000 -1.50000 H7B 2 0.254276 0.255958 0.138341 11.00000 -1.50000 H7C 2 0.214911 0.333876 0.122724 11.00000 -1.50000 AFIX 0 C6 1 0.462275 0.328056 0.134672 11.00000 0.03717 0.03075 = 0.05161 -0.01051 0.01370 -0.00123 AFIX 33 H6A 2 0.465996 0.283470 0.108652 11.00000 -1.50000 H6B 2 0.545205 0.340015 0.157142 11.00000 -1.50000 H6C 2 0.434836 0.362864 0.096254 11.00000 -1.50000 AFIX 0 C5 1 0.369651 0.324642 0.200323 11.00000 0.02819 0.02060 = 0.03519 -0.00658 -0.00590 0.00147 C8 1 0.419655 0.270879 0.260043 11.00000 0.04889 0.02045 = 0.05229 0.00123 -0.00586 0.01084 AFIX 33 H8A 2 0.362534 0.267191 0.303029 11.00000 -1.50000 H8B 2 0.502350 0.284801 0.281171 11.00000 -1.50000 H8C 2 0.425865 0.226471 0.233888 11.00000 -1.50000 AFIX 0 C18 1 0.105834 0.421488 -0.054194 11.00000 0.02551 0.02163 = 0.02806 -0.00166 0.00011 0.00099 AFIX 43 H18 2 0.030618 0.403782 -0.077845 11.00000 -1.20000 AFIX 0 C21 1 -0.101924 0.396091 0.052211 11.00000 0.02725 0.02490 = 0.02379 -0.00206 -0.00776 -0.00326 AFIX 43 H21 2 -0.116037 0.384921 -0.001734 11.00000 -1.20000 AFIX 0 C20 1 0.013470 0.424266 0.078203 11.00000 0.01698 0.02013 = 0.01876 0.00173 -0.00444 0.00246 C16 1 0.317415 0.456903 -0.063955 11.00000 0.02633 0.03436 = 0.02213 -0.00341 0.00202 -0.00042 AFIX 43 H16 2 0.389283 0.463400 -0.093563 11.00000 -1.20000 AFIX 0 C19 1 0.112339 0.436735 0.027712 11.00000 0.02538 0.02057 = 0.02251 -0.00103 -0.00098 0.00436 C23 1 -0.170421 0.399515 0.182807 11.00000 0.02407 0.03352 = 0.02983 0.00320 0.00344 -0.00583 AFIX 43 H23 2 -0.232159 0.391290 0.219821 11.00000 -1.20000 AFIX 0 C17 1 0.206047 0.431945 -0.099144 11.00000 0.03172 0.02853 = 0.02918 -0.00345 -0.00055 0.00128 AFIX 43 H17 2 0.200211 0.422358 -0.153845 11.00000 -1.20000 AFIX 0 C22 1 -0.193199 0.384635 0.102837 11.00000 0.02573 0.02662 = 0.03510 0.00224 -0.00260 -0.00478 AFIX 43 H22 2 -0.271596 0.366765 0.084463 11.00000 -1.20000 AFIX 0 C27 1 0.275328 0.741435 0.075411 11.00000 0.04817 0.02540 = 0.03298 0.00518 -0.00111 -0.01147 AFIX 43 H27 2 0.281936 0.784802 0.050852 11.00000 -1.20000 AFIX 0 C35 1 -0.300128 0.806345 0.513336 11.00000 0.06226 0.04901 = 0.03619 -0.00589 0.00874 -0.02235 C36 1 -0.188677 0.818649 0.557468 11.00000 0.06915 0.03714 = 0.05075 0.00443 0.00500 -0.00448 AFIX 43 H36 2 -0.120714 0.787692 0.555205 11.00000 -1.20000 AFIX 0 C38 1 -0.274229 0.922099 0.609114 11.00000 0.08218 0.04370 = 0.03696 0.00021 0.02625 -0.00559 AFIX 43 H38 2 -0.265653 0.961074 0.642197 11.00000 -1.20000 AFIX 0 C37 1 -0.178638 0.876973 0.604848 11.00000 0.07785 0.04566 = 0.03296 0.00285 -0.00891 -0.01701 AFIX 43 H37 2 -0.103129 0.885206 0.634755 11.00000 -1.20000 AFIX 0 C39 1 -0.382217 0.911349 0.565918 11.00000 0.05569 0.06087 = 0.05704 0.01188 0.01653 -0.00465 AFIX 43 H39 2 -0.448504 0.943383 0.568192 11.00000 -1.20000 AFIX 0 C40 1 -0.396328 0.854059 0.518625 11.00000 0.04349 0.07736 = 0.04576 0.00029 0.00513 -0.02517 AFIX 43 H40 2 -0.472754 0.847054 0.489247 11.00000 -1.20000 AFIX 0 C41 1 -0.314508 0.744198 0.461207 11.00000 0.13237 0.06926 = 0.04944 -0.01559 0.01090 -0.03530 AFIX 33 H41A 2 -0.398088 0.744004 0.435356 11.00000 -1.50000 H41B 2 -0.303092 0.702763 0.493075 11.00000 -1.50000 H41C 2 -0.251683 0.745470 0.421339 11.00000 -1.50000 AFIX 0 MOLE 1 TM1 5 0.217164 0.501860 0.192125 11.00000 0.01880 0.01858 = 0.01842 -0.00096 -0.00173 0.00051 C10 1 0.252042 0.495775 0.415240 11.00000 0.03204 0.03702 = 0.01996 -0.00400 0.00208 0.00147 AFIX 33 H10A 2 0.189878 0.461420 0.428335 11.00000 -1.50000 H10B 2 0.211147 0.540247 0.407656 11.00000 -1.50000 H10C 2 0.315870 0.499025 0.458173 11.00000 -1.50000 AFIX 0 P1 4 0.468281 0.461398 0.225936 11.00000 0.02003 0.02041 = 0.02302 -0.00015 0.00017 0.00000 N3 3 0.251727 0.611116 0.142744 11.00000 0.02845 0.02551 = 0.01916 -0.00101 -0.00415 -0.00231 N4 3 0.083174 0.582421 0.246754 11.00000 0.02188 0.02600 = 0.02221 0.00077 -0.00066 -0.00098 C34 1 0.002808 0.568894 0.302935 11.00000 0.02635 0.03125 = 0.02384 -0.00496 -0.00642 0.00007 AFIX 43 H34 2 0.010647 0.525792 0.328390 11.00000 -1.20000 AFIX 0 C29 1 0.168390 0.663193 0.159476 11.00000 0.02354 0.02310 = 0.02273 -0.00568 -0.01035 0.00006 C30 1 0.077712 0.647272 0.213784 11.00000 0.02666 0.02225 = 0.02226 -0.00623 -0.00744 0.00163 C25 1 0.346505 0.627970 0.096863 11.00000 0.02362 0.02594 = 0.02619 -0.00098 -0.00492 -0.00741 AFIX 43 H25 2 0.406635 0.593548 0.087857 11.00000 -1.20000 AFIX 0 C33 1 -0.089408 0.611581 0.326863 11.00000 0.02465 0.03861 = 0.03407 -0.01003 0.00587 -0.00339 AFIX 43 H33 2 -0.143705 0.598364 0.366598 11.00000 -1.20000 AFIX 0 C28 1 0.181088 0.728354 0.123383 11.00000 0.03937 0.02653 = 0.02717 0.00420 -0.00990 0.00232 AFIX 43 H28 2 0.122336 0.763311 0.133142 11.00000 -1.20000 AFIX 0 C31 1 -0.017404 0.693544 0.234993 11.00000 0.02776 0.02867 = 0.03325 -0.00460 0.00011 0.00699 AFIX 43 H31 2 -0.023073 0.737142 0.210511 11.00000 -1.20000 AFIX 0 C32 1 -0.100180 0.676514 0.289570 11.00000 0.02944 0.03590 = 0.04691 -0.00890 0.00208 0.01329 AFIX 43 H32 2 -0.164224 0.707453 0.302629 11.00000 -1.20000 AFIX 0 C26 1 0.363300 0.689732 0.062543 11.00000 0.03549 0.03328 = 0.03159 -0.00115 0.00239 -0.01445 AFIX 43 H26 2 0.432264 0.697794 0.030840 11.00000 -1.20000 AFIX 0 HKLF 4 REM import in P 21/a REM R1 = 0.0471 for 5750 Fo > 4sig(Fo) and 0.0758 for all 8132 data REM 425 parameters refined using 0 restraints END ; _[local]_cod_data_source_file om500607r_si_002.cif _[local]_cod_data_source_block 4 _[local]_cod_cif_authors_sg_H-M 'P 21/a' _cod_depositor_comments 'Adding full bibliography for 4084117--4084119.cif.' _cod_database_code 4084119 _diffrn_reflns_laue_measured_fraction_full 0.994 _diffrn_reflns_laue_measured_fraction_max 0.99 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.99 _publcif_datablock.id {1c2f0d7e-34cc-4a6d-91a6-484769e617db} loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag C4 C 0.4071(5) 0.5109(3) 0.3029(3) 0.0197(11) Uani 1 d C2 C 0.2866(5) 0.4091(3) 0.3058(3) 0.0195(11) Uani 1 d C14 C 0.5367(7) 0.5668(3) 0.4112(4) 0.0390(17) Uani 1 d H14A H 0.5758 0.6096 0.4294 0.059 Uiso 1 calc H14B H 0.601 0.5317 0.4064 0.059 Uiso 1 calc H14C H 0.4764 0.5518 0.449 0.059 Uiso 1 calc C1 C 0.3609(5) 0.3938(3) 0.2427(3) 0.0226(12) Uani 1 d C3 C 0.3130(6) 0.4750(3) 0.3400(3) 0.0227(12) Uani 1 d C11 C 0.4690(6) 0.5785(3) 0.3304(3) 0.0255(13) Uani 1 d C12 C 0.5675(6) 0.6009(3) 0.2738(4) 0.0348(16) Uani 1 d H12A H 0.6056 0.6439 0.2922 0.052 Uiso 1 calc H12B H 0.5281 0.6076 0.2213 0.052 Uiso 1 calc H12C H 0.6321 0.5656 0.2716 0.052 Uiso 1 calc C9 C 0.1948(6) 0.3614(3) 0.3419(4) 0.0321(15) Uani 1 d H9A H 0.1543 0.3849 0.3845 0.048 Uiso 1 calc H9B H 0.239 0.321 0.3627 0.048 Uiso 1 calc H9C H 0.1316 0.3473 0.3017 0.048 Uiso 1 calc C13 C 0.3765(7) 0.6380(3) 0.3361(4) 0.0331(15) Uani 1 d H13A H 0.4213 0.6792 0.3541 0.05 Uiso 1 calc H13B H 0.3132 0.6263 0.3734 0.05 Uiso 1 calc H13C H 0.3359 0.6465 0.2842 0.05 Uiso 1 calc N1 N 0.2220(4) 0.4646(2) 0.0614(3) 0.0199(10) Uani 1 d N2 N 0.0350(4) 0.4411(2) 0.1565(3) 0.0216(10) Uani 1 d C15 C 0.3193(6) 0.4716(3) 0.0145(4) 0.0259(13) Uani 1 d H15 H 0.3954 0.4882 0.038 0.031 Uiso 1 calc C24 C -0.0563(6) 0.4263(3) 0.2059(3) 0.0242(12) Uani 1 d H24 H -0.0403 0.4351 0.2603 0.029 Uiso 1 calc C7 C 0.2439(7) 0.3008(3) 0.1628(4) 0.0365(16) Uani 1 d H7A H 0.1825 0.2975 0.2033 0.055 Uiso 1 calc H7B H 0.2543 0.256 0.1383 0.055 Uiso 1 calc H7C H 0.2149 0.3339 0.1227 0.055 Uiso 1 calc C6 C 0.4623(7) 0.3281(3) 0.1347(4) 0.0395(17) Uani 1 d H6A H 0.466 0.2835 0.1087 0.059 Uiso 1 calc H6B H 0.5452 0.34 0.1571 0.059 Uiso 1 calc H6C H 0.4348 0.3629 0.0963 0.059 Uiso 1 calc C5 C 0.3697(6) 0.3246(3) 0.2003(4) 0.0282(14) Uani 1 d C8 C 0.4197(7) 0.2709(3) 0.2600(4) 0.0408(18) Uani 1 d H8A H 0.3625 0.2672 0.303 0.061 Uiso 1 calc H8B H 0.5023 0.2848 0.2812 0.061 Uiso 1 calc H8C H 0.4259 0.2265 0.2339 0.061 Uiso 1 calc C18 C 0.1058(6) 0.4215(3) -0.0542(4) 0.0251(13) Uani 1 d H18 H 0.0306 0.4038 -0.0778 0.03 Uiso 1 calc C21 C -0.1019(6) 0.3961(3) 0.0522(4) 0.0256(13) Uani 1 d H21 H -0.116 0.3849 -0.0017 0.031 Uiso 1 calc C20 C 0.0135(5) 0.4243(3) 0.0782(3) 0.0188(11) Uani 1 d C16 C 0.3174(6) 0.4569(3) -0.0640(3) 0.0276(13) Uani 1 d H16 H 0.3893 0.4634 -0.0936 0.033 Uiso 1 calc C19 C 0.1123(6) 0.4367(3) 0.0277(3) 0.0229(12) Uani 1 d C23 C -0.1704(6) 0.3995(3) 0.1828(4) 0.0291(14) Uani 1 d H23 H -0.2322 0.3913 0.2198 0.035 Uiso 1 calc C17 C 0.2060(6) 0.4319(3) -0.0991(4) 0.0299(14) Uani 1 d H17 H 0.2002 0.4224 -0.1538 0.036 Uiso 1 calc C22 C -0.1932(6) 0.3846(3) 0.1028(4) 0.0293(14) Uani 1 d H22 H -0.2716 0.3668 0.0845 0.035 Uiso 1 calc C27 C 0.2753(7) 0.7414(3) 0.0754(4) 0.0356(16) Uani 1 d H27 H 0.2819 0.7848 0.0509 0.043 Uiso 1 calc C35 C -0.3001(9) 0.8063(4) 0.5133(5) 0.049(2) Uani 1 d C36 C -0.1887(9) 0.8186(4) 0.5575(5) 0.052(2) Uani 1 d H36 H -0.1207 0.7877 0.5552 0.063 Uiso 1 calc C38 C -0.2742(9) 0.9221(4) 0.6091(5) 0.054(2) Uani 1 d H38 H -0.2657 0.9611 0.6422 0.064 Uiso 1 calc C37 C -0.1786(9) 0.8770(4) 0.6048(4) 0.053(2) Uani 1 d H37 H -0.1031 0.8852 0.6348 0.063 Uiso 1 calc C39 C -0.3822(9) 0.9113(5) 0.5659(5) 0.057(2) Uani 1 d H39 H -0.4485 0.9434 0.5682 0.069 Uiso 1 calc C40 C -0.3963(8) 0.8541(5) 0.5186(5) 0.055(2) Uani 1 d H40 H -0.4728 0.8471 0.4892 0.067 Uiso 1 calc C41 C -0.3145(12) 0.7442(5) 0.4612(6) 0.083(4) Uani 1 d H41A H -0.3981 0.744 0.4354 0.125 Uiso 1 calc H41B H -0.3031 0.7028 0.4931 0.125 Uiso 1 calc H41C H -0.2517 0.7455 0.4213 0.125 Uiso 1 calc Tm1 Tm 0.21716(2) 0.50186(2) 0.19213(2) 0.01869(8) Uani 1 d C10 C 0.2520(6) 0.4958(4) 0.4152(3) 0.0296(13) Uani 1 d H10A H 0.1899 0.4614 0.4283 0.044 Uiso 1 calc H10B H 0.2111 0.5402 0.4077 0.044 Uiso 1 calc H10C H 0.3159 0.499 0.4582 0.044 Uiso 1 calc P1 P 0.46828(14) 0.46140(7) 0.22594(9) 0.0212(3) Uani 1 d N3 N 0.2517(5) 0.6111(2) 0.1427(3) 0.0245(11) Uani 1 d N4 N 0.0832(5) 0.5824(2) 0.2468(3) 0.0234(11) Uani 1 d C34 C 0.0028(6) 0.5689(3) 0.3029(4) 0.0274(13) Uani 1 d H34 H 0.0106 0.5258 0.3284 0.033 Uiso 1 calc C29 C 0.1684(6) 0.6632(3) 0.1595(3) 0.0235(13) Uani 1 d C30 C 0.0777(6) 0.6473(3) 0.2138(3) 0.0240(13) Uani 1 d C25 C 0.3465(6) 0.6280(3) 0.0969(3) 0.0254(13) Uani 1 d H25 H 0.4066 0.5935 0.0879 0.031 Uiso 1 calc C33 C -0.0894(6) 0.6116(3) 0.3269(4) 0.0323(15) Uani 1 d H33 H -0.1437 0.5984 0.3666 0.039 Uiso 1 calc C28 C 0.1811(7) 0.7284(3) 0.1234(4) 0.0314(15) Uani 1 d H28 H 0.1223 0.7633 0.1331 0.038 Uiso 1 calc C31 C -0.0174(6) 0.6935(3) 0.2350(4) 0.0299(14) Uani 1 d H31 H -0.0231 0.7371 0.2105 0.036 Uiso 1 calc C32 C -0.1002(7) 0.6765(3) 0.2896(4) 0.0374(16) Uani 1 d H32 H -0.1642 0.7075 0.3026 0.045 Uiso 1 calc C26 C 0.3633(7) 0.6897(3) 0.0625(4) 0.0334(15) Uani 1 d H26 H 0.4323 0.6978 0.0308 0.04 Uiso 1 calc 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 C4 0.022(3) 0.018(3) 0.018(3) 0.005(2) -0.002(2) 0.001(2) C2 0.017(3) 0.016(2) 0.026(3) 0.002(2) 0.001(2) 0.001(2) C14 0.047(4) 0.028(3) 0.039(4) -0.001(3) -0.023(3) 0.000(3) C1 0.022(3) 0.019(3) 0.027(3) 0.001(2) -0.004(2) 0.001(2) C3 0.026(3) 0.023(3) 0.018(3) 0.003(2) -0.005(2) 0.003(2) C11 0.032(3) 0.020(3) 0.024(3) -0.002(2) -0.001(3) -0.002(2) C12 0.033(4) 0.029(3) 0.042(4) 0.001(3) -0.007(3) -0.009(3) C9 0.033(4) 0.024(3) 0.039(4) 0.007(3) 0.004(3) -0.006(3) C13 0.045(4) 0.023(3) 0.031(3) -0.003(3) -0.009(3) 0.000(3) N1 0.019(2) 0.022(2) 0.019(2) -0.0008(19) 0.0010(19) -0.001(2) N2 0.020(3) 0.021(2) 0.024(3) -0.0030(19) -0.002(2) 0.0029(19) C15 0.020(3) 0.027(3) 0.031(3) 0.002(2) 0.004(3) 0.001(2) C24 0.025(3) 0.025(3) 0.022(3) -0.002(2) 0.002(2) 0.002(2) C7 0.040(4) 0.021(3) 0.048(4) -0.007(3) -0.004(3) 0.001(3) C6 0.037(4) 0.031(4) 0.052(5) -0.011(3) 0.014(3) -0.001(3) C5 0.028(3) 0.021(3) 0.035(4) -0.007(3) -0.006(3) 0.001(3) C8 0.049(5) 0.020(3) 0.052(5) 0.001(3) -0.006(4) 0.011(3) C18 0.026(3) 0.022(3) 0.028(3) -0.002(2) 0.000(3) 0.001(2) C21 0.027(3) 0.025(3) 0.024(3) -0.002(2) -0.008(3) -0.003(3) C20 0.017(3) 0.020(3) 0.019(3) 0.002(2) -0.004(2) 0.002(2) C16 0.026(3) 0.034(3) 0.022(3) -0.003(3) 0.002(2) 0.000(3) C19 0.025(3) 0.021(3) 0.023(3) -0.001(2) -0.001(2) 0.004(2) C23 0.024(3) 0.034(3) 0.030(3) 0.003(3) 0.003(3) -0.006(3) C17 0.032(4) 0.029(3) 0.029(3) -0.003(3) -0.001(3) 0.001(3) C22 0.026(3) 0.027(3) 0.035(4) 0.002(3) -0.003(3) -0.005(3) C27 0.048(4) 0.025(3) 0.033(4) 0.005(3) -0.001(3) -0.011(3) C35 0.062(6) 0.049(5) 0.036(4) -0.006(3) 0.009(4) -0.022(4) C36 0.069(6) 0.037(4) 0.051(5) 0.004(4) 0.005(4) -0.004(4) C38 0.082(7) 0.044(4) 0.037(4) 0.000(4) 0.026(4) -0.006(5) C37 0.078(6) 0.046(5) 0.033(4) 0.003(3) -0.009(4) -0.017(4) C39 0.056(6) 0.061(6) 0.057(6) 0.012(4) 0.017(5) -0.005(4) C40 0.043(5) 0.077(6) 0.046(5) 0.000(4) 0.005(4) -0.025(5) C41 0.132(11) 0.069(6) 0.049(6) -0.016(5) 0.011(6) -0.035(7) Tm1 0.01880(12) 0.01858(12) 0.01842(12) -0.00096(11) -0.00173(8) 0.00051(12) C10 0.032(3) 0.037(3) 0.020(3) -0.004(3) 0.002(2) 0.001(3) P1 0.0200(7) 0.0204(7) 0.0230(7) -0.0002(6) 0.0002(6) 0.0000(6) N3 0.028(3) 0.026(3) 0.019(2) -0.001(2) -0.004(2) -0.002(2) N4 0.022(3) 0.026(3) 0.022(3) 0.001(2) -0.001(2) -0.001(2) C34 0.026(3) 0.031(3) 0.024(3) -0.005(3) -0.006(3) 0.000(3) C29 0.024(3) 0.023(3) 0.023(3) -0.006(2) -0.010(2) 0.000(2) C30 0.027(3) 0.022(3) 0.022(3) -0.006(2) -0.007(2) 0.002(2) C25 0.024(3) 0.026(3) 0.026(3) -0.001(2) -0.005(2) -0.007(3) C33 0.025(3) 0.039(4) 0.034(4) -0.010(3) 0.006(3) -0.003(3) C28 0.039(4) 0.027(3) 0.027(3) 0.004(3) -0.010(3) 0.002(3) C31 0.028(3) 0.029(3) 0.033(4) -0.005(3) 0.000(3) 0.007(3) C32 0.029(4) 0.036(4) 0.047(4) -0.009(3) 0.002(3) 0.013(3) C26 0.035(4) 0.033(3) 0.032(4) -0.001(3) 0.002(3) -0.014(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C3 C4 C11 126.8(5) C3 C4 P1 111.0(4) C11 C4 P1 121.5(4) C3 C4 Tm1 75.5(3) C11 C4 Tm1 124.4(4) P1 C4 Tm1 75.15(18) C1 C2 C3 113.2(5) C1 C2 C9 125.9(5) C3 C2 C9 120.6(5) C1 C2 Tm1 75.2(3) C3 C2 Tm1 74.6(3) C9 C2 Tm1 122.6(4) C2 C1 C5 126.7(5) C2 C1 P1 111.1(4) C5 C1 P1 121.4(5) C2 C1 Tm1 75.1(3) C5 C1 Tm1 125.3(4) P1 C1 Tm1 74.64(19) C4 C3 C2 113.4(5) C4 C3 C10 126.4(5) C2 C3 C10 119.8(5) C4 C3 Tm1 74.6(3) C2 C3 Tm1 74.9(3) C10 C3 Tm1 124.7(4) C12 C11 C13 106.9(5) C12 C11 C14 107.2(6) C13 C11 C14 109.5(5) C12 C11 C4 110.7(5) C13 C11 C4 113.5(5) C14 C11 C4 108.8(5) C15 N1 C19 117.1(5) C15 N1 Tm1 125.7(4) C19 N1 Tm1 117.1(4) C24 N2 C20 117.2(5) C24 N2 Tm1 124.5(4) C20 N2 Tm1 118.0(4) N1 C15 C16 125.6(6) N2 C24 C23 124.4(6) C6 C5 C7 107.2(6) C6 C5 C1 111.1(5) C7 C5 C1 112.9(5) C6 C5 C8 107.1(6) C7 C5 C8 109.8(5) C1 C5 C8 108.5(5) C17 C18 C19 121.0(6) C22 C21 C20 121.1(6) N2 C20 C21 120.0(5) N2 C20 C19 116.7(5) C21 C20 C19 123.3(5) C15 C16 C17 117.7(6) N1 C19 C20 117.2(5) N1 C19 C18 119.1(5) C20 C19 C18 123.7(6) C24 C23 C22 118.0(6) C18 C17 C16 119.4(6) C21 C22 C23 119.1(6) C28 C27 C26 118.9(6) C40 C35 C36 117.7(7) C40 C35 C41 121.4(9) C36 C35 C41 121.0(9) C37 C36 C35 119.3(9) C37 C38 C39 119.8(8) C38 C37 C36 121.6(9) C38 C39 C40 120.5(9) C39 C40 C35 121.2(8) N3 Tm1 N2 121.10(17) N3 Tm1 N1 86.04(16) N2 Tm1 N1 69.66(16) N3 Tm1 N4 68.91(17) N2 Tm1 N4 85.67(16) N1 Tm1 N4 128.66(16) N3 Tm1 C4 93.68(16) N2 Tm1 C4 143.31(16) N1 Tm1 C4 129.04(16) N4 Tm1 C4 97.69(16) N3 Tm1 C3 116.77(17) N2 Tm1 C3 114.49(17) N1 Tm1 C3 142.47(17) N4 Tm1 C3 88.49(17) C4 Tm1 C3 29.93(17) N3 Tm1 C2 145.25(17) N2 Tm1 C2 92.42(16) N1 Tm1 C2 116.70(16) N4 Tm1 C2 108.35(17) C4 Tm1 C2 51.72(16) C3 Tm1 C2 30.54(16) N3 Tm1 C1 136.52(18) N2 Tm1 C1 98.07(16) N1 Tm1 C1 91.23(17) N4 Tm1 C1 137.66(17) C4 Tm1 C1 55.78(16) C3 Tm1 C1 51.48(17) C2 Tm1 C1 29.73(17) N3 Tm1 P1 99.37(13) N2 Tm1 P1 133.04(12) N1 Tm1 P1 92.42(12) N4 Tm1 P1 134.21(12) C4 Tm1 P1 37.28(12) C3 Tm1 P1 56.43(13) C2 Tm1 P1 56.45(12) C1 Tm1 P1 37.32(13) C4 P1 C1 91.2(3) C4 P1 Tm1 67.57(18) C1 P1 Tm1 68.04(19) C25 N3 C29 116.6(5) C25 N3 Tm1 124.6(4) C29 N3 Tm1 118.8(4) C34 N4 C30 116.9(5) C34 N4 Tm1 125.0(4) C30 N4 Tm1 117.8(4) N4 C34 C33 126.0(6) N3 C29 C30 116.3(5) N3 C29 C28 119.3(6) C30 C29 C28 124.4(6) N4 C30 C29 116.8(5) N4 C30 C31 119.7(6) C29 C30 C31 123.5(6) N3 C25 C26 125.8(6) C34 C33 C32 117.1(6) C27 C28 C29 121.3(6) C32 C31 C30 121.2(6) C31 C32 C33 118.9(6) C25 C26 C27 117.9(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C4 C3 1.405(8) C4 C11 1.542(8) C4 P1 1.780(6) C4 Tm1 2.716(5) C2 C1 1.402(8) C2 C3 1.437(8) C2 C9 1.508(8) C2 Tm1 2.731(5) C14 C11 1.542(8) C1 C5 1.538(8) C1 P1 1.786(6) C1 Tm1 2.732(6) C3 C10 1.522(8) C3 Tm1 2.727(5) C11 C12 1.530(9) C11 C13 1.536(9) N1 C15 1.352(7) N1 C19 1.395(7) N1 Tm1 2.346(5) N2 C24 1.353(7) N2 C20 1.383(7) N2 Tm1 2.343(5) C15 C16 1.366(8) C24 C23 1.372(8) C7 C5 1.537(9) C6 C5 1.533(9) C5 C8 1.542(9) C18 C17 1.365(9) C18 C19 1.426(8) C21 C22 1.354(9) C21 C20 1.407(8) C20 C19 1.419(8) C16 C17 1.399(9) C23 C22 1.404(9) C27 C28 1.355(9) C27 C26 1.408(10) C35 C40 1.398(12) C35 C36 1.403(12) C35 C41 1.509(11) C36 C37 1.399(11) C38 C37 1.358(12) C38 C39 1.359(12) C39 C40 1.384(12) Tm1 N3 2.333(5) Tm1 N4 2.355(5) Tm1 P1 2.8405(15) N3 C25 1.353(8) N3 C29 1.394(8) N4 C34 1.345(8) N4 C30 1.387(7) C34 C33 1.371(9) C29 C30 1.409(9) C29 C28 1.425(8) C30 C31 1.424(8) C25 C26 1.358(8) C33 C32 1.422(10) C31 C32 1.358(9) 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 C3 C2 C1 C5 171.2(5) C9 C2 C1 C5 -3.5(10) Tm1 C2 C1 C5 -123.3(6) C3 C2 C1 P1 1.1(6) C9 C2 C1 P1 -173.6(5) Tm1 C2 C1 P1 66.7(3) C3 C2 C1 Tm1 -65.6(4) C9 C2 C1 Tm1 119.8(6) C11 C4 C3 C2 -172.1(5) P1 C4 C3 C2 -1.9(6) Tm1 C4 C3 C2 65.6(4) C11 C4 C3 C10 0.3(9) P1 C4 C3 C10 170.5(5) Tm1 C4 C3 C10 -122.0(6) C11 C4 C3 Tm1 122.3(5) P1 C4 C3 Tm1 -67.5(3) C1 C2 C3 C4 0.5(7) C9 C2 C3 C4 175.5(5) Tm1 C2 C3 C4 -65.4(4) C1 C2 C3 C10 -172.4(5) C9 C2 C3 C10 2.6(8) Tm1 C2 C3 C10 121.7(5) C1 C2 C3 Tm1 65.9(4) C9 C2 C3 Tm1 -119.1(5) C3 C4 C11 C12 180.0(5) P1 C4 C11 C12 10.7(7) Tm1 C4 C11 C12 -82.5(6) C3 C4 C11 C13 -59.8(8) P1 C4 C11 C13 130.9(5) Tm1 C4 C11 C13 37.7(7) C3 C4 C11 C14 62.4(8) P1 C4 C11 C14 -106.9(5) Tm1 C4 C11 C14 160.0(4) C19 N1 C15 C16 3.4(9) Tm1 N1 C15 C16 -172.2(5) C20 N2 C24 C23 -3.8(8) Tm1 N2 C24 C23 170.2(5) C2 C1 C5 C6 -179.5(6) P1 C1 C5 C6 -10.3(7) Tm1 C1 C5 C6 82.7(6) C2 C1 C5 C7 60.0(8) P1 C1 C5 C7 -130.9(5) Tm1 C1 C5 C7 -37.9(7) C2 C1 C5 C8 -62.0(8) P1 C1 C5 C8 107.2(6) Tm1 C1 C5 C8 -159.8(4) C24 N2 C20 C21 3.0(8) Tm1 N2 C20 C21 -171.4(4) C24 N2 C20 C19 -176.8(5) Tm1 N2 C20 C19 8.8(6) C22 C21 C20 N2 -0.3(9) C22 C21 C20 C19 179.5(6) N1 C15 C16 C17 -0.5(9) C15 N1 C19 C20 175.1(5) Tm1 N1 C19 C20 -8.8(6) C15 N1 C19 C18 -4.0(8) Tm1 N1 C19 C18 172.1(4) N2 C20 C19 N1 0.1(7) C21 C20 C19 N1 -179.7(5) N2 C20 C19 C18 179.1(5) C21 C20 C19 C18 -0.7(9) C17 C18 C19 N1 1.9(8) C17 C18 C19 C20 -177.2(6) N2 C24 C23 C22 1.8(9) C19 C18 C17 C16 1.1(9) C15 C16 C17 C18 -1.8(9) C20 C21 C22 C23 -1.7(9) C24 C23 C22 C21 1.1(9) C40 C35 C36 C37 0.5(12) C41 C35 C36 C37 179.7(8) C39 C38 C37 C36 -0.8(12) C35 C36 C37 C38 -0.1(12) C37 C38 C39 C40 1.2(12) C38 C39 C40 C35 -0.7(13) C36 C35 C40 C39 -0.2(12) C41 C35 C40 C39 -179.3(8) C3 C4 P1 C1 2.1(4) C11 C4 P1 C1 172.9(5) Tm1 C4 P1 C1 -65.6(2) C3 C4 P1 Tm1 67.7(4) C11 C4 P1 Tm1 -121.5(5) C2 C1 P1 C4 -1.8(4) C5 C1 P1 C4 -172.5(5) Tm1 C1 P1 C4 65.15(19) C2 C1 P1 Tm1 -67.0(4) C5 C1 P1 Tm1 122.3(5) C30 N4 C34 C33 4.7(9) Tm1 N4 C34 C33 -169.0(5) C25 N3 C29 C30 -173.6(5) Tm1 N3 C29 C30 7.8(6) C25 N3 C29 C28 4.8(8) Tm1 N3 C29 C28 -173.8(4) C34 N4 C30 C29 175.1(5) Tm1 N4 C30 C29 -10.7(6) C34 N4 C30 C31 -5.5(8) Tm1 N4 C30 C31 168.7(4) N3 C29 C30 N4 2.0(7) C28 C29 C30 N4 -176.3(5) N3 C29 C30 C31 -177.4(5) C28 C29 C30 C31 4.3(9) C29 N3 C25 C26 -3.8(9) Tm1 N3 C25 C26 174.7(5) N4 C34 C33 C32 -0.8(10) C26 C27 C28 C29 -1.2(10) N3 C29 C28 C27 -2.5(9) C30 C29 C28 C27 175.8(6) N4 C30 C31 C32 2.8(9) C29 C30 C31 C32 -177.8(6) C30 C31 C32 C33 1.1(10) C34 C33 C32 C31 -2.1(10) N3 C25 C26 C27 0.2(10) C28 C27 C26 C25 2.4(10)