#------------------------------------------------------------------------------ #$Date: 2019-11-10 18:53:44 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225959 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/58/4515860.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_4515860 loop_ _publ_author_name 'Mondal, Sandip' 'Bera, Sachinath' 'Maity, Suvendu' 'Ghosh, Prasanta' _publ_section_title ; Orthometalated N-(Benzophenoxazine)-o-aminophenol: Phenolato versus Phenoxyl States. ; _journal_issue 10 _journal_name_full 'ACS omega' _journal_page_first 13323 _journal_page_last 13334 _journal_paper_doi 10.1021/acsomega.8b01983 _journal_volume 3 _journal_year 2018 _chemical_formula_sum 'C41 H29 Br2 Cl2 N2 O2 Os P' _chemical_formula_weight 1033.55 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 97.0910(10) _cell_angle_beta 107.7940(10) _cell_angle_gamma 113.5570(10) _cell_formula_units_Z 2 _cell_length_a 11.7693(4) _cell_length_b 12.6976(4) _cell_length_c 14.8599(5) _cell_measurement_reflns_used 9919 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.70 _cell_measurement_theta_min 2.67 _cell_volume 1859.94(11) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_unetI/netI 0.0309 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 25497 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 2.899 _diffrn_source Mo _exptl_absorpt_coefficient_mu 5.802 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.845 _exptl_crystal_description cubic _exptl_crystal_F_000 1000 _exptl_crystal_size_max 0.162 _exptl_crystal_size_mid 0.065 _exptl_crystal_size_min 0.042 _exptl_transmission_factor_max 0.869 _exptl_transmission_factor_min 0.784 _refine_diff_density_max 1.233 _refine_diff_density_min -1.682 _refine_diff_density_rms 0.125 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 460 _refine_ls_number_reflns 6505 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.023 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0335 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.3404P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1127 _refine_ls_wR_factor_ref 0.1198 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5980 _reflns_number_total 6505 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ao8b01983_si_002.cif _cod_data_source_block 2 _cod_database_code 4515860 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; 2.res created by SHELXL-2014/7 TITL 3.res in P-1 CELL 0.71073 11.7693 12.6976 14.8599 97.091 107.794 113.557 ZERR 2.000 0.0004 0.0004 0.0005 0.001 0.001 0.001 LATT 1 SFAC C H N O P Cl Br Os UNIT 82 58 4 4 2 4 4 2 OMIT -2 50 REM Old TITL 604RKM_0m in P1 REM SHELXT solution in P-1 REM R1 0.100, Rweak 0.007, Alpha 0.076, Orientation as input REM Formula found by SHELXT: C37 N7 O3 P Cl Br2 Os L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 WGHT 0.100000 0.340380 FVAR 0.40326 OS1 8 0.340293 0.639820 0.790053 11.00000 0.02977 0.03237 = 0.02909 0.00781 0.01109 0.01566 BR1 7 0.412870 0.679304 0.970178 11.00000 0.06369 0.05384 = 0.03030 0.01119 0.01761 0.03128 BR2 7 0.100321 0.541283 0.775691 11.00000 0.03510 0.08438 = 0.06212 0.01710 0.02411 0.02153 P1 5 0.568386 0.741003 0.806635 11.00000 0.02814 0.02872 = 0.03222 0.00306 0.00964 0.01255 CL1 6 0.556728 0.136748 0.746190 11.00000 0.10596 0.08510 = 0.19001 0.03943 0.03667 0.04374 O1 4 0.340132 0.790578 0.764916 11.00000 0.06310 0.03918 = 0.03867 0.00775 0.00826 0.02965 N1 3 0.253736 0.592506 0.636371 11.00000 0.02745 0.02698 = 0.04697 0.01240 0.00963 0.01534 C6 1 0.223584 0.678266 0.598356 11.00000 0.03822 0.03910 = 0.03715 0.01501 0.00889 0.02334 C15 1 0.345269 0.483683 0.753872 11.00000 0.02842 0.03594 = 0.02798 0.00971 0.00899 0.01297 CL2 6 0.826926 0.291267 0.782659 11.00000 0.15762 0.21289 = 0.29553 0.08742 0.15102 0.04426 C7 1 0.226697 0.484506 0.588434 11.00000 0.03122 0.02809 = 0.02865 0.00572 0.00877 0.01149 C1 1 0.275046 0.785307 0.673062 11.00000 0.03848 0.03897 = 0.03801 0.01102 0.01121 0.02064 N2 3 0.140482 0.130799 0.474587 11.00000 0.05404 0.04054 = 0.04286 0.00549 0.00865 0.02379 O2 4 0.063363 0.262822 0.351652 11.00000 0.11526 0.05487 = 0.02643 0.00454 0.00355 0.03994 C16 1 0.273731 0.420406 0.652222 11.00000 0.03103 0.03481 = 0.03166 0.01066 0.01067 0.01611 C23 1 0.680922 0.677142 0.853449 11.00000 0.02424 0.02705 = 0.05718 0.00760 0.00717 0.00784 C35 1 0.666789 0.895649 0.884976 11.00000 0.03728 0.03338 = 0.04108 0.00970 0.01132 0.01441 C11 1 0.249428 0.302665 0.614539 11.00000 0.03207 0.03319 = 0.03910 0.00872 0.00886 0.01538 C29 1 0.568273 0.757028 0.686146 11.00000 0.03899 0.04733 = 0.04377 0.00957 0.02548 0.01782 C22 1 0.063417 0.079436 0.373754 11.00000 0.04043 0.04140 = 0.03813 0.00338 0.00750 0.01227 C20 1 -0.059345 -0.093914 0.230474 11.00000 0.08944 0.04549 = 0.03142 -0.00674 0.01012 0.02616 AFIX 43 H20 2 -0.088406 -0.174569 0.202818 11.00000 -1.20000 AFIX 0 C10 1 0.171890 0.241871 0.509823 11.00000 0.03388 0.03856 = 0.03306 0.00637 0.00960 0.01642 C13 1 0.371320 0.308193 0.778611 11.00000 0.05361 0.04464 = 0.03912 0.01126 0.00060 0.02770 AFIX 43 H13 2 0.402756 0.269838 0.821964 11.00000 -1.20000 AFIX 0 C30 1 0.525569 0.654650 0.611340 11.00000 0.05926 0.06112 = 0.05491 -0.00330 0.03565 0.02138 AFIX 43 H30 2 0.508908 0.581804 0.625352 11.00000 -1.20000 AFIX 0 C14 1 0.396661 0.423977 0.815317 11.00000 0.04382 0.03817 = 0.03317 0.00383 0.00538 0.01873 AFIX 43 H14 2 0.448627 0.463221 0.881844 11.00000 -1.20000 AFIX 0 C40 1 0.613084 0.954666 0.929498 11.00000 0.04882 0.04603 = 0.04816 0.00253 0.01590 0.02511 AFIX 43 H40 2 0.524458 0.913425 0.923466 11.00000 -1.20000 AFIX 0 C24 1 0.703156 0.662501 0.946355 11.00000 0.04194 0.04845 = 0.06461 0.01217 0.00570 0.02089 AFIX 43 H24 2 0.659747 0.683680 0.982562 11.00000 -1.20000 AFIX 0 C28 1 0.750062 0.650359 0.801665 11.00000 0.04667 0.06080 = 0.08727 0.01148 0.02759 0.03244 AFIX 43 H28 2 0.738842 0.663066 0.739918 11.00000 -1.20000 AFIX 0 C38 1 0.819598 1.134897 0.991946 11.00000 0.06016 0.03222 = 0.05458 0.00201 0.00650 0.01713 AFIX 43 H38 2 0.871100 1.215380 1.027212 11.00000 -1.20000 AFIX 0 C12 1 0.301537 0.247657 0.680628 11.00000 0.05175 0.03316 = 0.03249 0.00542 0.00336 0.01853 AFIX 43 H12 2 0.288702 0.170519 0.657946 11.00000 -1.20000 AFIX 0 C2 1 0.259816 0.884009 0.648734 11.00000 0.05707 0.04025 = 0.06990 0.01729 0.02164 0.03055 AFIX 43 H2 2 0.293989 0.954417 0.697789 11.00000 -1.20000 AFIX 0 C8 1 0.158877 0.426899 0.484840 11.00000 0.07031 0.05010 = 0.03020 0.01319 0.00765 0.03539 AFIX 43 H8 2 0.133661 0.468301 0.441816 11.00000 -1.20000 AFIX 0 C39 1 0.689453 1.074751 0.983183 11.00000 0.06111 0.03825 = 0.06251 0.00583 0.01950 0.02157 AFIX 43 H39 2 0.652293 1.113635 1.012772 11.00000 -1.20000 AFIX 0 C17 1 0.024717 0.144189 0.314011 11.00000 0.06344 0.04979 = 0.03340 0.00496 0.01177 0.02034 C34 1 0.588039 0.862587 0.663435 11.00000 0.06388 0.07084 = 0.05551 0.02722 0.02830 0.03607 AFIX 43 H34 2 0.613459 0.930428 0.712256 11.00000 -1.20000 AFIX 0 C36 1 0.799563 0.958380 0.896589 11.00000 0.04470 0.04360 = 0.06622 0.00881 0.02310 0.01427 AFIX 43 H36 2 0.838295 0.919746 0.868653 11.00000 -1.20000 AFIX 0 C37 1 0.874851 1.077258 0.949007 11.00000 0.04494 0.04506 = 0.06539 0.00031 0.01344 0.00076 AFIX 43 H37 2 0.963605 1.118823 0.955412 11.00000 -1.20000 AFIX 0 C9 1 0.131708 0.313744 0.449802 11.00000 0.05781 0.04471 = 0.02135 0.00617 0.00528 0.02316 C5 1 0.156169 0.672868 0.501674 11.00000 0.12047 0.05724 = 0.04839 0.01602 0.01897 0.05638 AFIX 43 H5 2 0.121266 0.603262 0.451553 11.00000 -1.20000 AFIX 0 C25 1 0.790620 0.615955 0.987174 11.00000 0.04728 0.05441 = 0.09802 0.02276 -0.00177 0.02330 AFIX 43 H25 2 0.803850 0.605007 1.049598 11.00000 -1.20000 AFIX 0 C3 1 0.195323 0.875786 0.553793 11.00000 0.09627 0.05705 = 0.05959 0.02337 0.01076 0.05347 AFIX 43 H3 2 0.186741 0.941221 0.537081 11.00000 -1.20000 AFIX 0 C19 1 -0.095339 -0.025626 0.174687 11.00000 0.07859 0.06710 = 0.03627 -0.00707 0.01365 0.01508 AFIX 43 H19 2 -0.149247 -0.060967 0.107972 11.00000 -1.20000 AFIX 0 C26 1 0.857098 0.586430 0.933953 11.00000 0.04644 0.04676 = 0.15148 0.02830 0.01085 0.02698 AFIX 43 H26 2 0.914658 0.554995 0.960409 11.00000 -1.20000 AFIX 0 C33 1 0.570040 0.868838 0.566494 11.00000 0.09745 0.12282 = 0.07226 0.05866 0.04569 0.06427 AFIX 43 H33 2 0.585231 0.941068 0.551637 11.00000 -1.20000 AFIX 0 C21 1 0.022111 -0.038640 0.329855 11.00000 0.09596 0.05565 = 0.06315 0.00407 0.01650 0.03716 AFIX 43 H21 2 0.049756 -0.083276 0.368157 11.00000 -1.20000 AFIX 0 C4 1 0.140950 0.767800 0.479942 11.00000 0.14768 0.07697 = 0.04708 0.02589 0.01422 0.07569 AFIX 43 H4 2 0.093749 0.761925 0.415086 11.00000 -1.20000 AFIX 0 C31 1 0.508157 0.662342 0.515932 11.00000 0.08106 0.12312 = 0.05084 0.00645 0.04092 0.04043 AFIX 43 H31 2 0.481268 0.594482 0.466562 11.00000 -1.20000 AFIX 0 C18 1 -0.055195 0.090970 0.213325 11.00000 0.11168 0.06470 = 0.03228 0.00439 0.00057 0.03647 AFIX 43 H18 2 -0.080173 0.135650 0.173705 11.00000 -1.20000 AFIX 0 C27 1 0.838279 0.603340 0.843376 11.00000 0.06883 0.07300 = 0.15344 0.01861 0.04134 0.05068 AFIX 43 H27 2 0.883679 0.583917 0.808142 11.00000 -1.20000 AFIX 0 C41 1 0.676328 0.268819 0.804441 11.00000 0.16030 0.07243 = 0.14114 0.01922 0.10563 0.02477 AFIX 23 H41A 2 0.696381 0.281734 0.874420 11.00000 -1.20000 H41B 2 0.648112 0.326883 0.783387 11.00000 -1.20000 AFIX 0 C32 1 0.529978 0.768096 0.493732 11.00000 0.09002 0.17465 = 0.04653 0.03269 0.03893 0.05878 AFIX 43 H32 2 0.517797 0.772028 0.429611 11.00000 -1.20000 AFIX 0 HKLF 4 REM 2.res in P-1 REM R1 = 0.0335 for 5980 Fo > 4sig(Fo) and 0.0375 for all 6505 data REM 460 parameters refined using 0 restraints END WGHT 0.0515 5.0123 REM Highest difference peak 1.233, deepest hole -1.682, 1-sigma level 0.125 Q1 1 0.8483 0.1969 0.7584 11.00000 0.05 1.23 Q2 1 0.2249 0.6133 0.7100 11.00000 0.05 0.84 Q3 1 0.4577 0.6639 0.8722 11.00000 0.05 0.61 Q4 1 0.2385 0.6173 0.7945 11.00000 0.05 0.60 Q5 1 0.3042 0.6100 0.6782 11.00000 0.05 0.56 Q6 1 0.3916 0.5916 0.7215 11.00000 0.05 0.56 Q7 1 0.3046 0.6617 0.8665 11.00000 0.05 0.52 Q8 1 0.3824 0.5761 0.7953 11.00000 0.05 0.48 Q9 1 0.0649 -0.0439 0.3196 11.00000 0.05 0.47 Q10 1 0.4496 0.6577 0.7879 11.00000 0.05 0.47 Q11 1 0.1363 0.5628 0.8504 11.00000 0.05 0.47 Q12 1 0.1789 0.5437 0.6340 11.00000 0.05 0.45 Q13 1 0.2228 0.6791 0.5013 11.00000 0.05 0.45 Q14 1 0.7162 0.2601 0.7814 11.00000 0.05 0.44 Q15 1 0.1182 0.5971 0.6611 11.00000 0.05 0.44 Q16 1 0.4993 0.7640 0.9669 11.00000 0.05 0.44 Q17 1 -0.0555 -0.1044 0.2816 11.00000 0.05 0.43 Q18 1 0.2508 0.5382 0.7973 11.00000 0.05 0.43 Q19 1 0.1653 0.4422 0.5292 11.00000 0.05 0.42 Q20 1 0.7373 1.2007 1.0800 11.00000 0.05 0.42 ; _shelx_res_checksum 86727 _shelx_hkl_file ; -2 0 0 1012.70 46.40 -2 0 0 955.80 46.30 -2 0 0 919.11 46.40 2 0 0 956.60 46.30 2 0 0 903.11 46.30 2 0 0 910.71 46.40 -3 0 0 709.83 34.20 -3 0 0 721.53 33.10 -3 0 0 651.03 33.30 -3 0 0 684.53 33.10 3 0 0 652.53 33.10 3 0 0 649.34 33.10 3 0 0 643.64 33.30 -4 0 0 3522.25 166.38 -4 0 0 3551.24 165.08 -4 0 0 3513.75 164.98 -4 0 0 3229.88 165.18 4 0 0 3328.47 164.98 4 0 0 3142.99 165.18 4 0 0 3399.76 164.98 -5 0 0 162.08 9.00 -5 0 0 150.68 10.60 5 0 0 141.69 8.90 5 0 0 167.98 8.60 5 0 0 159.88 8.40 -6 0 0 100.29 7.10 -6 0 0 110.19 6.30 -6 0 0 109.59 9.30 6 0 0 108.59 6.40 6 0 0 106.79 6.70 6 0 0 122.39 6.30 -7 0 0 103.09 10.20 -7 0 0 106.49 6.30 -7 0 0 100.49 7.20 7 0 0 102.59 7.00 7 0 0 105.29 6.50 7 0 0 108.19 6.20 -8 0 0 93.79 6.70 -8 0 0 64.39 5.50 -8 0 0 67.69 12.80 8 0 0 79.69 5.70 8 0 0 68.99 6.70 8 0 0 83.69 5.40 -9 0 0 868.01 49.30 -9 0 0 916.51 46.40 -9 0 0 942.11 45.60 9 0 0 901.01 46.30 9 0 0 969.80 45.50 9 0 0 911.01 45.70 -10 0 0 120.89 7.90 -10 0 0 115.89 14.40 10 0 0 143.09 9.60 -11 0 0 -11.10 7.10 -12 0 0 271.07 23.90 -12 1 0 295.27 23.50 -11 1 0 61.59 9.80 -11 1 0 85.59 6.50 10 -1 0 30.00 4.60 -10 1 0 24.10 7.00 -10 1 0 24.70 3.40 9 -1 0 616.04 31.30 9 -1 0 624.04 30.70 9 -1 0 668.43 30.40 -9 1 0 607.64 30.80 -9 1 0 551.34 34.00 -9 1 0 586.54 31.10 8 -1 0 258.97 14.60 8 -1 0 294.27 13.80 8 -1 0 275.47 14.10 -8 1 0 243.18 17.30 -8 1 0 254.07 14.40 -8 1 0 274.57 14.20 7 -1 0 100.69 6.70 7 -1 0 105.59 6.20 7 -1 0 113.39 6.00 -7 1 0 95.29 6.30 -7 1 0 94.69 9.20 -7 1 0 97.59 6.50 6 -1 0 362.86 18.30 6 -1 0 372.16 18.50 -6 1 0 383.46 18.30 -6 1 0 345.97 18.50 -6 1 0 337.97 20.60 5 -1 0 3006.80 155.48 5 -1 0 3197.48 155.48 -5 1 0 3306.17 155.48 -5 1 0 3207.78 156.58 -5 1 0 3000.70 155.48 -5 1 0 3386.06 155.38 4 -1 0 163.88 8.50 4 -1 0 156.48 8.50 4 -1 0 151.48 8.50 -4 1 0 154.38 8.40 -4 1 0 160.58 8.50 -4 1 0 174.88 8.90 3 -1 0 300.57 15.80 3 -1 0 310.17 15.70 3 -1 0 331.07 15.70 -3 1 0 290.07 15.80 -3 1 0 327.97 15.80 -3 1 0 332.67 15.70 -2 -1 0 40.50 2.50 -2 -1 0 43.00 2.60 2 1 0 38.70 2.60 2 1 0 38.90 2.60 -3 -1 0 96.39 5.60 -3 -1 0 108.09 5.50 -3 -1 0 101.89 7.60 -3 -1 0 106.99 5.70 3 1 0 103.39 5.60 3 1 0 102.89 5.70 3 1 0 87.69 6.40 -4 -1 0 2397.06 116.59 -4 -1 0 2484.95 116.49 -4 -1 0 2406.16 118.29 -4 -1 0 2340.67 116.69 4 1 0 2321.97 116.59 4 1 0 2486.85 116.69 4 1 0 2338.87 116.49 4 1 0 2302.57 116.69 -5 -1 0 181.88 13.20 -5 -1 0 203.18 11.00 5 1 0 199.38 10.70 5 1 0 199.48 10.50 5 1 0 184.58 12.30 5 1 0 222.68 10.40 -6 -1 0 8.20 4.10 6 1 0 5.80 2.20 6 1 0 8.10 1.60 6 1 0 9.20 1.80 -7 -1 0 480.75 24.60 -7 -1 0 481.95 23.50 7 1 0 452.85 24.10 7 1 0 478.45 23.60 7 1 0 457.55 23.80 -8 -1 0 530.55 32.80 -8 -1 0 590.74 29.80 -8 -1 0 593.94 28.60 8 1 0 593.24 28.60 8 1 0 553.94 28.90 8 1 0 560.44 29.40 -9 -1 0 196.28 17.30 -9 -1 0 205.38 11.30 9 1 0 203.28 12.00 9 1 0 202.88 13.10 9 1 0 225.88 11.60 -10 -1 0 119.19 15.50 -11 -1 0 127.39 17.90 -12 2 0 17.00 7.80 -12 2 0 18.20 3.60 -11 2 0 111.99 13.90 -11 2 0 137.39 9.10 -10 2 0 723.73 41.70 -10 2 0 805.62 38.70 9 -2 0 1.50 1.90 9 -2 0 4.40 2.00 9 -2 0 -0.50 2.70 -9 2 0 -1.50 2.40 -9 2 0 3.90 4.90 -9 2 0 3.80 3.10 8 -2 0 257.27 13.80 8 -2 0 261.87 14.40 8 -2 0 288.67 13.50 -8 2 0 261.27 13.70 -8 2 0 241.08 16.50 -8 2 0 263.07 14.00 7 -2 0 52.79 3.60 7 -2 0 42.10 4.50 -7 2 0 44.00 6.50 -7 2 0 41.40 4.30 -7 2 0 43.00 3.50 6 -2 0 43.00 3.90 6 -2 0 35.70 3.70 6 -2 0 36.00 3.20 -6 2 0 44.70 3.70 -6 2 0 50.89 5.70 -6 2 0 36.80 3.00 5 -2 0 3132.99 152.68 5 -2 0 3020.00 152.38 5 -2 0 3035.80 152.68 -5 2 0 2969.20 152.38 -5 2 0 3326.47 152.68 -5 2 0 3025.30 152.68 -5 2 0 3385.16 153.58 4 -2 0 871.61 45.40 4 -2 0 905.31 45.60 4 -2 0 920.51 45.50 -4 2 0 1010.20 46.30 -4 2 0 861.01 45.40 -4 2 0 982.20 45.60 -4 2 0 948.01 45.60 3 -2 0 1278.27 63.99 3 -2 0 1331.07 64.09 3 -2 0 1313.77 63.99 -3 2 0 1318.67 64.09 -3 2 0 1292.57 63.99 -3 2 0 1305.37 63.89 2 -2 0 1731.03 88.79 2 -2 0 1754.62 88.99 -2 2 0 1878.91 88.79 -2 2 0 1914.11 88.89 0 -2 0 1693.93 84.89 0 -2 0 1707.33 84.99 0 -2 0 1815.82 84.99 0 2 0 1742.73 84.99 0 2 0 1730.73 84.99 -1 -2 0 550.74 31.70 -1 -2 0 649.74 31.30 1 2 0 642.24 31.30 1 2 0 693.73 31.30 1 2 0 644.14 31.30 -2 -2 0 2389.26 113.29 -2 -2 0 2275.67 113.39 -2 -2 0 2686.53 114.59 2 2 0 2287.67 113.39 2 2 0 2294.67 113.39 2 2 0 2010.70 113.59 -3 -2 0 1825.72 84.59 -3 -2 0 1530.45 83.29 -3 -2 0 1657.33 82.99 -3 -2 0 1713.13 82.89 3 2 0 1823.22 82.89 3 2 0 1624.64 82.99 -4 -2 0 987.70 48.00 -4 -2 0 994.10 50.19 -4 -2 0 940.71 48.20 4 2 0 955.80 48.10 4 2 0 901.21 48.20 4 2 0 987.10 48.30 4 2 0 1067.29 48.00 -5 -2 0 236.58 12.70 5 2 0 226.78 12.40 5 2 0 231.98 12.70 5 2 0 243.18 12.30 -6 -2 0 359.36 23.20 -6 -2 0 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33.90 5.50 9 -7 0 41.40 4.40 -9 7 0 39.90 4.00 -9 7 0 38.30 7.00 8 -7 0 23.80 4.30 8 -7 0 20.70 3.60 -8 7 0 16.90 3.30 -8 7 0 18.70 3.30 -8 7 0 21.80 3.30 7 -7 0 1855.21 93.89 7 -7 0 1944.61 93.39 7 -7 0 1885.11 92.89 -7 7 0 1866.51 93.39 -7 7 0 1886.21 93.79 -7 7 0 1938.71 92.89 6 -7 0 1275.97 65.29 6 -7 0 1351.96 64.79 6 -7 0 1304.27 64.69 -6 7 0 1326.67 64.39 -6 7 0 1313.57 65.19 -6 7 0 1290.47 64.79 5 -7 0 66.99 6.30 5 -7 0 72.19 5.40 -5 7 0 56.89 6.30 -5 7 0 77.79 6.00 -5 7 0 70.69 5.40 4 -7 0 1380.26 67.79 4 -7 0 1357.16 67.79 4 -7 0 1373.86 68.39 4 -7 0 1398.26 67.89 -4 7 0 1321.97 67.69 -4 7 0 1427.16 68.19 -4 7 0 1386.26 67.79 3 -7 0 6246.98 306.17 3 -7 0 6244.08 306.07 3 -7 0 6284.37 306.67 3 -7 0 6258.57 306.17 -3 7 0 6609.84 306.27 -3 7 0 6220.68 306.07 -3 7 0 6287.07 306.37 -3 7 0 6088.09 306.07 2 -7 0 254.27 13.60 2 -7 0 261.77 15.10 2 -7 0 267.07 13.90 2 -7 0 255.37 13.80 -2 7 0 251.67 13.70 -2 7 0 255.57 14.10 -2 7 0 279.57 14.00 -2 7 0 261.37 13.60 1 -7 0 132.79 7.90 1 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21.60 -8 13 -5 99.79 9.60 -8 13 -5 79.69 10.00 8 -13 5 68.99 13.10 -9 13 -5 63.09 10.00 9 -13 5 50.49 8.70 -10 13 -5 322.67 20.40 10 -13 5 323.37 23.50 3 12 -5 10.20 5.40 -3 -12 5 27.00 8.60 2 12 -5 50.29 9.00 -2 -12 5 48.20 8.70 1 12 -5 105.79 10.40 -1 -12 5 111.69 14.20 0 12 -5 4.10 4.20 0 12 -5 0.60 2.80 0 -12 5 1.30 6.30 -1 12 -5 283.37 15.60 -1 12 -5 265.27 16.80 1 -12 5 261.57 19.20 1 -12 5 291.67 14.90 -2 12 -5 159.88 10.40 -2 12 -5 151.68 11.50 2 -12 5 157.18 9.40 2 -12 5 145.09 14.00 -3 12 -5 34.70 5.10 -3 12 -5 39.10 6.60 -3 12 -5 41.10 7.10 3 -12 5 38.50 5.50 3 -12 5 34.10 7.00 -4 12 -5 387.36 22.00 -4 12 -5 372.56 21.50 -4 12 -5 406.26 21.30 4 -12 5 369.46 23.60 4 -12 5 423.76 21.70 -5 12 -5 945.71 47.20 -5 12 -5 928.91 46.70 5 -12 5 885.31 48.30 -6 12 -5 49.50 8.10 -6 12 -5 54.89 8.00 6 -12 5 59.99 10.80 -7 12 -5 135.49 10.60 -7 12 -5 133.99 10.80 7 -12 5 128.49 13.20 -8 12 -5 510.85 26.90 -8 12 -5 445.06 29.70 8 -12 5 508.25 28.90 -9 12 -5 163.18 12.90 9 -12 5 170.98 15.80 -10 12 -5 26.80 5.80 10 -12 5 30.40 7.90 5 11 -5 5.50 5.40 -5 -11 5 8.40 8.90 4 11 -5 300.47 18.80 -4 -11 5 318.17 23.50 3 11 -5 175.48 13.10 -3 -11 5 190.88 17.10 2 11 -5 -5.30 4.00 -2 -11 5 -1.60 6.00 1 11 -5 163.98 12.10 1 11 -5 179.38 9.80 -1 -11 5 150.08 15.00 0 11 -5 376.16 22.50 0 11 -5 424.96 21.40 0 11 -5 428.06 23.20 0 -11 5 420.36 20.90 0 -11 5 401.16 22.20 0 -11 5 411.06 25.00 -1 11 -5 133.29 8.90 -1 11 -5 125.39 10.30 1 -11 5 128.49 10.10 1 -11 5 135.69 13.00 1 -11 5 145.69 8.20 -2 11 -5 10.50 3.20 -2 11 -5 8.60 3.90 2 -11 5 14.80 2.50 2 -11 5 15.80 5.70 -3 11 -5 113.99 9.30 -3 11 -5 111.99 8.40 -3 11 -5 109.89 8.60 3 -11 5 138.69 9.40 3 -11 5 104.79 11.70 3 -11 5 113.99 7.90 -4 11 -5 0.90 2.50 -4 11 -5 0.10 3.20 -4 11 -5 1.50 3.70 4 -11 5 1.60 2.70 4 -11 5 1.90 5.10 -5 11 -5 485.15 27.00 -5 11 -5 481.25 27.50 -5 11 -5 545.75 26.80 5 -11 5 497.55 28.60 5 -11 5 557.94 27.00 -6 11 -5 362.76 21.00 -6 11 -5 369.76 21.00 -6 11 -5 397.06 20.70 6 -11 5 352.46 22.60 6 -11 5 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6 -17 53.99 9.20 2 6 -17 40.10 6.80 1 6 -17 14.40 7.80 1 6 -17 17.20 5.50 0 6 -17 223.88 15.00 0 6 -17 201.58 19.80 6 5 -17 -2.50 6.90 6 5 -17 -3.80 6.00 5 5 -17 56.09 8.10 5 5 -17 85.39 14.00 4 5 -17 27.50 6.70 4 5 -17 27.30 7.80 3 5 -17 19.40 6.10 3 5 -17 37.50 11.00 2 5 -17 180.78 17.60 2 5 -17 177.28 13.90 1 5 -17 12.20 5.20 1 5 -17 8.40 7.80 0 5 -17 30.60 8.70 0 5 -17 20.70 5.20 6 4 -17 0.80 6.70 6 4 -17 0.50 6.00 5 4 -17 36.60 7.80 5 4 -17 38.50 7.20 4 4 -17 293.97 20.10 4 4 -17 329.37 21.90 3 4 -17 17.00 7.40 3 4 -17 7.50 5.40 2 4 -17 130.39 12.10 2 4 -17 152.88 16.00 1 4 -17 280.57 21.40 1 4 -17 279.97 17.70 0 4 -17 148.79 16.40 0 4 -17 124.89 11.20 7 3 -17 21.60 6.90 7 3 -17 22.00 7.30 6 3 -17 18.60 6.50 6 3 -17 16.00 6.80 5 3 -17 7.90 5.80 5 3 -17 12.50 6.60 4 3 -17 223.48 16.50 4 3 -17 242.68 18.40 3 3 -17 225.48 18.60 3 3 -17 244.18 16.30 2 3 -17 -4.20 6.50 2 3 -17 -2.80 4.60 1 3 -17 151.88 16.40 1 3 -17 156.68 12.30 0 3 -17 634.14 33.00 0 3 -17 603.24 36.10 8 2 -17 108.79 14.90 8 2 -17 89.39 13.40 7 2 -17 1.40 5.80 7 2 -17 -1.60 6.60 6 2 -17 25.30 7.00 6 2 -17 38.50 6.50 -6 -2 17 14.80 6.70 5 2 -17 211.78 17.10 5 2 -17 231.98 15.20 -5 -2 17 167.78 15.80 4 2 -17 7.00 6.40 4 2 -17 13.50 5.00 -4 -2 17 -3.80 5.50 3 2 -17 238.68 18.30 3 2 -17 263.87 15.60 -3 -2 17 192.38 16.00 2 2 -17 210.68 13.80 2 2 -17 182.58 17.20 1 2 -17 33.60 8.00 1 2 -17 29.90 5.20 0 2 -17 290.67 22.00 8 1 -17 59.99 9.20 -8 -1 17 55.79 8.40 7 1 -17 5.90 6.50 -7 -1 17 -6.60 7.70 6 1 -17 9.50 6.50 5 1 -17 294.77 19.80 -5 -1 17 245.08 18.10 4 1 -17 167.38 15.20 -4 -1 17 128.99 13.00 3 1 -17 16.30 6.60 -3 -1 17 7.90 5.50 2 1 -17 295.77 22.70 -2 -1 17 231.38 16.70 1 1 -17 487.35 28.10 -1 -1 17 424.56 25.20 8 0 -17 5.50 7.00 -8 0 17 -5.60 6.10 7 0 -17 17.90 7.20 -7 0 17 9.50 6.40 6 0 -17 109.79 14.00 -6 0 17 77.39 11.80 5 0 -17 36.00 7.20 -5 0 17 24.60 6.30 4 0 -17 238.98 17.80 -4 0 17 208.98 15.70 -3 0 17 48.20 6.60 2 0 -17 10.20 6.60 -2 0 17 1.50 5.00 1 0 -17 474.25 28.30 -1 0 17 443.46 25.40 8 -1 -17 -8.50 6.70 -8 1 17 -4.30 5.90 7 -1 -17 33.50 8.20 6 -1 -17 403.96 25.40 -6 1 17 389.36 23.80 -5 1 17 49.40 9.60 4 -1 -17 111.29 13.40 -4 1 17 84.89 11.00 3 -1 -17 321.77 20.90 -3 1 17 276.97 18.50 2 -1 -17 310.27 21.10 -2 1 17 291.57 18.50 8 -2 -17 23.80 7.90 -8 2 17 18.10 6.70 7 -2 -17 2.50 7.20 -7 2 17 -5.60 5.60 6 -2 -17 175.88 17.10 -6 2 17 170.38 14.40 5 -2 -17 199.78 17.00 -5 2 17 171.48 14.40 4 -2 -17 4.30 6.30 -4 2 17 -6.20 4.80 3 -2 -17 115.29 13.80 -3 2 17 83.09 10.90 7 -3 -17 185.28 18.20 -7 3 17 187.28 15.20 6 -3 -17 -2.40 7.20 -6 3 17 -1.30 5.60 5 -3 -17 159.78 16.40 -5 3 17 175.58 14.10 4 3 -18 305.77 21.70 4 3 -18 290.87 19.70 3 3 -18 0.90 7.30 5 2 -18 22.80 7.40 5 2 -18 17.10 6.10 4 2 -18 459.35 25.90 4 2 -18 429.76 27.60 3 2 -18 178.68 17.20 -5 -1 18 112.19 13.30 -4 -1 18 18.00 6.30 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 6702 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Os1 Os 0.34029(2) 0.63982(2) 0.79005(2) 0.03014(11) Uani 1 1 d . . Br1 Br 0.41287(6) 0.67930(5) 0.97018(4) 0.04807(17) Uani 1 1 d . . Br2 Br 0.10032(6) 0.54128(7) 0.77569(5) 0.0617(2) Uani 1 1 d . . P1 P 0.56839(13) 0.74100(11) 0.80663(10) 0.0310(3) Uani 1 1 d . . Cl1 Cl 0.5567(3) 0.1367(2) 0.7462(3) 0.1327(11) Uani 1 1 d . . O1 O 0.3401(4) 0.7906(3) 0.7649(3) 0.0482(9) Uani 1 1 d . . N1 N 0.2537(4) 0.5925(4) 0.6364(3) 0.0339(9) Uani 1 1 d . . C6 C 0.2236(5) 0.6783(5) 0.5984(4) 0.0373(11) Uani 1 1 d . . C15 C 0.3453(4) 0.4837(4) 0.7539(3) 0.0319(10) Uani 1 1 d . . Cl2 Cl 0.8269(5) 0.2913(5) 0.7827(4) 0.219(2) Uani 1 1 d . . C7 C 0.2267(5) 0.4845(4) 0.5884(3) 0.0311(10) Uani 1 1 d . . C1 C 0.2750(5) 0.7853(4) 0.6731(4) 0.0385(11) Uani 1 1 d . . N2 N 0.1405(5) 0.1308(4) 0.4746(3) 0.0485(11) Uani 1 1 d . . O2 O 0.0634(6) 0.2628(4) 0.3517(3) 0.0724(14) Uani 1 1 d . . C16 C 0.2737(5) 0.4204(4) 0.6522(3) 0.0325(10) Uani 1 1 d . . C23 C 0.6809(5) 0.6771(4) 0.8534(4) 0.0403(12) Uani 1 1 d . . C35 C 0.6668(5) 0.8956(4) 0.8850(4) 0.0391(11) Uani 1 1 d . . C11 C 0.2494(5) 0.3027(4) 0.6145(4) 0.0362(11) Uani 1 1 d . . C29 C 0.5683(5) 0.7570(5) 0.6861(4) 0.0420(12) Uani 1 1 d . . C22 C 0.0634(6) 0.0794(5) 0.3738(4) 0.0452(13) Uani 1 1 d . . C20 C -0.0593(8) -0.0939(6) 0.2305(4) 0.0626(18) Uani 1 1 d . . H20 H -0.0884 -0.1746 0.2028 0.075 Uiso 1 1 calc R U C10 C 0.1719(5) 0.2419(4) 0.5098(4) 0.0366(10) Uani 1 1 d . . C13 C 0.3713(6) 0.3082(5) 0.7786(4) 0.0487(13) Uani 1 1 d . . H13 H 0.4028 0.2698 0.8220 0.058 Uiso 1 1 calc R U C30 C 0.5256(6) 0.6546(6) 0.6113(5) 0.0592(16) Uani 1 1 d . . H30 H 0.5089 0.5818 0.6254 0.071 Uiso 1 1 calc R U C14 C 0.3967(5) 0.4240(4) 0.8153(4) 0.0417(12) Uani 1 1 d . . H14 H 0.4486 0.4632 0.8818 0.050 Uiso 1 1 calc R U C40 C 0.6131(6) 0.9547(5) 0.9295(4) 0.0484(13) Uani 1 1 d . . H40 H 0.5245 0.9134 0.9235 0.058 Uiso 1 1 calc R U C24 C 0.7032(6) 0.6625(5) 0.9464(5) 0.0560(15) Uani 1 1 d . . H24 H 0.6597 0.6837 0.9826 0.067 Uiso 1 1 calc R U C28 C 0.7501(6) 0.6504(6) 0.8017(6) 0.0628(17) Uani 1 1 d . . H28 H 0.7388 0.6631 0.7399 0.075 Uiso 1 1 calc R U C38 C 0.8196(6) 1.1349(5) 0.9919(5) 0.0558(15) Uani 1 1 d . . H38 H 0.8711 1.2154 1.0272 0.067 Uiso 1 1 calc R U C12 C 0.3015(6) 0.2477(5) 0.6806(4) 0.0434(12) Uani 1 1 d . . H12 H 0.2887 0.1705 0.6579 0.052 Uiso 1 1 calc R U C2 C 0.2598(6) 0.8840(5) 0.6487(5) 0.0535(15) Uani 1 1 d . . H2 H 0.2940 0.9544 0.6978 0.064 Uiso 1 1 calc R U C8 C 0.1589(6) 0.4269(5) 0.4848(4) 0.0505(14) Uani 1 1 d . . H8 H 0.1337 0.4683 0.4418 0.061 Uiso 1 1 calc R U C39 C 0.6895(6) 1.0748(5) 0.9832(5) 0.0565(15) Uani 1 1 d . . H39 H 0.6523 1.1136 1.0128 0.068 Uiso 1 1 calc R U C17 C 0.0247(6) 0.1442(5) 0.3140(4) 0.0536(14) Uani 1 1 d . . C34 C 0.5880(7) 0.8626(6) 0.6634(5) 0.0594(16) Uani 1 1 d . . H34 H 0.6135 0.9304 0.7123 0.071 Uiso 1 1 calc R U C36 C 0.7996(6) 0.9584(5) 0.8966(5) 0.0540(15) Uani 1 1 d . . H36 H 0.8383 0.9197 0.8687 0.065 Uiso 1 1 calc R U C37 C 0.8749(7) 1.0773(6) 0.9490(5) 0.0627(17) Uani 1 1 d . . H37 H 0.9636 1.1188 0.9554 0.075 Uiso 1 1 calc R U C9 C 0.1317(6) 0.3137(5) 0.4498(4) 0.0445(13) Uani 1 1 d . . C5 C 0.1562(9) 0.6729(6) 0.5017(5) 0.073(2) Uani 1 1 d . . H5 H 0.1213 0.6033 0.4516 0.088 Uiso 1 1 calc R U C25 C 0.7906(7) 0.6160(6) 0.9872(6) 0.074(2) Uani 1 1 d . . H25 H 0.8038 0.6050 1.0496 0.089 Uiso 1 1 calc R U C3 C 0.1953(8) 0.8758(6) 0.5538(5) 0.069(2) Uani 1 1 d . . H3 H 0.1867 0.9412 0.5371 0.083 Uiso 1 1 calc R U C19 C -0.0953(8) -0.0256(7) 0.1747(5) 0.072(2) Uani 1 1 d . . H19 H -0.1492 -0.0610 0.1080 0.086 Uiso 1 1 calc R U C26 C 0.8571(7) 0.5864(6) 0.9340(8) 0.087(3) Uani 1 1 d . . H26 H 0.9147 0.5550 0.9604 0.104 Uiso 1 1 calc R U C33 C 0.5700(9) 0.8688(9) 0.5665(6) 0.086(3) Uani 1 1 d . . H33 H 0.5852 0.9411 0.5516 0.103 Uiso 1 1 calc R U C21 C 0.0221(8) -0.0386(6) 0.3299(6) 0.076(2) Uani 1 1 d . . H21 H 0.0498 -0.0833 0.3682 0.091 Uiso 1 1 calc R U C4 C 0.1410(10) 0.7678(7) 0.4799(5) 0.087(3) Uani 1 1 d . . H4 H 0.0937 0.7619 0.4151 0.105 Uiso 1 1 calc R U C31 C 0.5082(8) 0.6623(9) 0.5159(6) 0.085(3) Uani 1 1 d . . H31 H 0.4813 0.5945 0.4666 0.102 Uiso 1 1 calc R U C18 C -0.0552(9) 0.0910(7) 0.2133(5) 0.079(2) Uani 1 1 d . . H18 H -0.0802 0.1357 0.1737 0.095 Uiso 1 1 calc R U C27 C 0.8383(8) 0.6033(7) 0.8434(9) 0.094(3) Uani 1 1 d . . H27 H 0.8837 0.5839 0.8081 0.113 Uiso 1 1 calc R U C41 C 0.6763(12) 0.2688(8) 0.8044(9) 0.124(4) Uani 1 1 d . . H41A H 0.6964 0.2817 0.8744 0.149 Uiso 1 1 calc R U H41B H 0.6481 0.3269 0.7834 0.149 Uiso 1 1 calc R U C32 C 0.5300(10) 0.7681(12) 0.4937(6) 0.101(3) Uani 1 1 d . . H32 H 0.5178 0.7720 0.4296 0.121 Uiso 1 1 calc R U 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 Os1 0.02977(16) 0.03237(15) 0.02909(16) 0.00781(10) 0.01109(10) 0.01566(11) Br1 0.0637(4) 0.0538(3) 0.0303(3) 0.0112(2) 0.0176(3) 0.0313(3) Br2 0.0351(3) 0.0844(5) 0.0621(4) 0.0171(4) 0.0241(3) 0.0215(3) P1 0.0281(6) 0.0287(6) 0.0322(7) 0.0031(5) 0.0096(5) 0.0125(5) Cl1 0.106(2) 0.0851(16) 0.190(3) 0.0394(18) 0.037(2) 0.0437(15) O1 0.063(3) 0.0392(19) 0.039(2) 0.0078(16) 0.0083(19) 0.0296(19) N1 0.027(2) 0.027(2) 0.047(3) 0.0124(18) 0.0096(18) 0.0153(17) C6 0.038(3) 0.039(3) 0.037(3) 0.015(2) 0.009(2) 0.023(2) C15 0.028(2) 0.036(2) 0.028(2) 0.0097(19) 0.009(2) 0.013(2) Cl2 0.158(4) 0.213(5) 0.296(7) 0.087(4) 0.151(4) 0.044(3) C7 0.031(2) 0.028(2) 0.029(2) 0.0057(18) 0.009(2) 0.0115(19) C1 0.038(3) 0.039(3) 0.038(3) 0.011(2) 0.011(2) 0.021(2) N2 0.054(3) 0.041(2) 0.043(3) 0.005(2) 0.009(2) 0.024(2) O2 0.115(4) 0.055(2) 0.026(2) 0.0045(18) 0.004(2) 0.040(3) C16 0.031(2) 0.035(2) 0.032(3) 0.0107(19) 0.011(2) 0.016(2) C23 0.024(2) 0.027(2) 0.057(3) 0.008(2) 0.007(2) 0.0078(19) C35 0.037(3) 0.033(2) 0.041(3) 0.010(2) 0.011(2) 0.014(2) C11 0.032(2) 0.033(2) 0.039(3) 0.009(2) 0.009(2) 0.015(2) C29 0.039(3) 0.047(3) 0.044(3) 0.010(2) 0.025(2) 0.018(2) C22 0.040(3) 0.041(3) 0.038(3) 0.003(2) 0.007(2) 0.012(2) C20 0.089(5) 0.045(3) 0.031(3) -0.007(3) 0.010(3) 0.026(3) C10 0.034(3) 0.039(3) 0.033(3) 0.006(2) 0.010(2) 0.016(2) C13 0.054(3) 0.045(3) 0.039(3) 0.011(2) 0.001(3) 0.028(3) C30 0.059(4) 0.061(4) 0.055(4) -0.003(3) 0.036(3) 0.021(3) C14 0.044(3) 0.038(3) 0.033(3) 0.004(2) 0.005(2) 0.019(2) C40 0.049(3) 0.046(3) 0.048(3) 0.003(2) 0.016(3) 0.025(3) C24 0.042(3) 0.048(3) 0.065(4) 0.012(3) 0.006(3) 0.021(3) C28 0.047(3) 0.061(4) 0.087(5) 0.011(3) 0.028(3) 0.032(3) C38 0.060(4) 0.032(3) 0.055(4) 0.002(2) 0.007(3) 0.017(3) C12 0.052(3) 0.033(3) 0.032(3) 0.005(2) 0.003(2) 0.019(2) C2 0.057(4) 0.040(3) 0.070(4) 0.017(3) 0.022(3) 0.031(3) C8 0.070(4) 0.050(3) 0.030(3) 0.013(2) 0.008(3) 0.035(3) C39 0.061(4) 0.038(3) 0.063(4) 0.006(3) 0.019(3) 0.022(3) C17 0.063(4) 0.050(3) 0.033(3) 0.005(2) 0.012(3) 0.020(3) C34 0.064(4) 0.071(4) 0.056(4) 0.027(3) 0.028(3) 0.036(3) C36 0.045(3) 0.044(3) 0.066(4) 0.009(3) 0.023(3) 0.014(3) C37 0.045(3) 0.045(3) 0.065(4) 0.000(3) 0.013(3) 0.001(3) C9 0.058(3) 0.045(3) 0.021(2) 0.006(2) 0.005(2) 0.023(3) C5 0.120(6) 0.057(4) 0.048(4) 0.016(3) 0.019(4) 0.056(4) C25 0.047(4) 0.054(4) 0.098(6) 0.023(4) -0.002(4) 0.023(3) C3 0.096(5) 0.057(4) 0.060(4) 0.023(3) 0.011(4) 0.053(4) C19 0.079(5) 0.067(4) 0.036(4) -0.007(3) 0.014(3) 0.015(4) C26 0.046(4) 0.047(4) 0.151(9) 0.028(5) 0.011(5) 0.027(3) C33 0.097(6) 0.123(7) 0.072(5) 0.059(5) 0.046(5) 0.064(6) C21 0.096(6) 0.056(4) 0.063(5) 0.004(3) 0.017(4) 0.037(4) C4 0.148(8) 0.077(5) 0.047(4) 0.026(4) 0.014(5) 0.076(5) C31 0.081(5) 0.123(7) 0.051(4) 0.006(5) 0.041(4) 0.040(5) C18 0.112(6) 0.065(4) 0.032(3) 0.004(3) 0.001(4) 0.036(4) C27 0.069(5) 0.073(5) 0.153(9) 0.019(6) 0.041(6) 0.051(4) C41 0.160(10) 0.072(6) 0.141(10) 0.019(6) 0.106(9) 0.025(6) C32 0.090(6) 0.175(11) 0.047(5) 0.033(6) 0.039(5) 0.059(7) 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 0.0000 0.0000 '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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 '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 O1 Os1 C15 153.33(19) O1 Os1 N1 77.84(15) C15 Os1 N1 78.49(17) O1 Os1 P1 82.54(13) C15 Os1 P1 88.13(13) N1 Os1 P1 96.59(12) O1 Os1 Br1 104.18(11) C15 Os1 Br1 100.86(13) N1 Os1 Br1 172.57(11) P1 Os1 Br1 90.78(3) O1 Os1 Br2 95.49(12) C15 Os1 Br2 94.23(13) N1 Os1 Br2 84.29(12) P1 Os1 Br2 177.61(3) Br1 Os1 Br2 88.39(2) C23 P1 C29 107.3(3) C23 P1 C35 101.8(2) C29 P1 C35 102.8(2) C23 P1 Os1 119.16(16) C29 P1 Os1 108.01(18) C35 P1 Os1 116.29(17) C1 O1 Os1 117.0(3) C7 N1 C6 128.8(5) C7 N1 Os1 117.0(3) C6 N1 Os1 114.1(3) C5 C6 N1 129.8(5) C5 C6 C1 118.4(5) N1 C6 C1 111.8(4) C14 C15 C16 116.1(4) C14 C15 Os1 129.4(4) C16 C15 Os1 114.2(3) N1 C7 C8 128.2(4) N1 C7 C16 113.5(4) C8 C7 C16 118.3(4) O1 C1 C2 121.5(5) O1 C1 C6 118.3(4) C2 C1 C6 120.2(5) C10 N2 C22 116.7(5) C9 O2 C17 119.0(4) C11 C16 C15 122.7(4) C11 C16 C7 121.4(4) C15 C16 C7 115.9(4) C24 C23 C28 119.4(5) C24 C23 P1 118.1(4) C28 C23 P1 122.4(5) C36 C35 C40 118.3(5) C36 C35 P1 118.5(4) C40 C35 P1 123.1(4) C12 C11 C16 118.0(4) C12 C11 C10 122.2(4) C16 C11 C10 119.8(4) C34 C29 C30 119.3(6) C34 C29 P1 121.1(4) C30 C29 P1 118.8(5) C21 C22 C17 117.2(6) C21 C22 N2 121.1(6) C17 C22 N2 121.7(5) C19 C20 C21 117.8(6) C19 C20 H20 121.1 C21 C20 H20 121.1 N2 C10 C11 120.9(5) N2 C10 C9 123.6(5) C11 C10 C9 115.5(4) C12 C13 C14 122.3(5) C12 C13 H13 118.8 C14 C13 H13 118.8 C31 C30 C29 119.7(7) C31 C30 H30 120.2 C29 C30 H30 120.2 C13 C14 C15 121.1(5) C13 C14 H14 119.5 C15 C14 H14 119.5 C35 C40 C39 121.1(6) C35 C40 H40 119.5 C39 C40 H40 119.5 C23 C24 C25 120.8(7) C23 C24 H24 119.6 C25 C24 H24 119.6 C23 C28 C27 119.5(8) C23 C28 H28 120.2 C27 C28 H28 120.2 C39 C38 C37 120.4(5) C39 C38 H38 119.8 C37 C38 H38 119.8 C13 C12 C11 119.6(5) C13 C12 H12 120.2 C11 C12 H12 120.2 C3 C2 C1 119.6(6) C3 C2 H2 120.2 C1 C2 H2 120.2 C9 C8 C7 120.1(5) C9 C8 H8 119.9 C7 C8 H8 119.9 C38 C39 C40 119.3(6) C38 C39 H39 120.4 C40 C39 H39 120.4 O2 C17 C22 120.8(5) O2 C17 C18 118.0(6) C22 C17 C18 121.2(6) C29 C34 C33 120.3(7) C29 C34 H34 119.9 C33 C34 H34 119.9 C37 C36 C35 120.7(6) C37 C36 H36 119.7 C35 C36 H36 119.7 C38 C37 C36 120.3(6) C38 C37 H37 119.9 C36 C37 H37 119.9 C8 C9 O2 117.4(5) C8 C9 C10 124.7(5) O2 C9 C10 117.9(5) C4 C5 C6 120.6(6) C4 C5 H5 119.7 C6 C5 H5 119.7 C26 C25 C24 119.6(8) C26 C25 H25 120.2 C24 C25 H25 120.2 C2 C3 C4 119.9(5) C2 C3 H3 120.0 C4 C3 H3 120.0 C18 C19 C20 122.1(6) C18 C19 H19 119.0 C20 C19 H19 119.0 C27 C26 C25 120.0(7) C27 C26 H26 120.0 C25 C26 H26 120.0 C32 C33 C34 120.0(8) C32 C33 H33 120.0 C34 C33 H33 120.0 C22 C21 C20 122.6(7) C22 C21 H21 118.7 C20 C21 H21 118.7 C5 C4 C3 121.2(6) C5 C4 H4 119.4 C3 C4 H4 119.4 C32 C31 C30 120.9(8) C32 C31 H31 119.5 C30 C31 H31 119.5 C19 C18 C17 119.1(7) C19 C18 H18 120.4 C17 C18 H18 120.4 C26 C27 C28 120.7(8) C26 C27 H27 119.6 C28 C27 H27 119.6 Cl1 C41 Cl2 111.2(6) Cl1 C41 H41A 109.4 Cl2 C41 H41A 109.4 Cl1 C41 H41B 109.4 Cl2 C41 H41B 109.4 H41A C41 H41B 108.0 C31 C32 C33 119.8(8) C31 C32 H32 120.1 C33 C32 H32 120.1 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Os1 O1 1.996(4) Os1 C15 2.018(5) Os1 N1 2.089(5) Os1 P1 2.3830(13) Os1 Br1 2.4646(6) Os1 Br2 2.5157(6) P1 C23 1.825(5) P1 C29 1.826(5) P1 C35 1.829(5) Cl1 C41 1.598(10) O1 C1 1.324(6) N1 C7 1.327(6) N1 C6 1.403(6) C6 C5 1.391(8) C6 C1 1.416(7) C15 C14 1.405(7) C15 C16 1.421(7) Cl2 C41 1.816(11) C7 C8 1.430(7) C7 C16 1.448(6) C1 C2 1.409(7) N2 C10 1.297(7) N2 C22 1.396(7) O2 C9 1.352(6) O2 C17 1.370(7) C16 C11 1.409(7) C23 C24 1.375(8) C23 C28 1.382(8) C35 C36 1.383(8) C35 C40 1.382(7) C11 C12 1.404(7) C11 C10 1.457(7) C29 C34 1.369(8) C29 C30 1.399(8) C22 C21 1.375(9) C22 C17 1.380(8) C20 C19 1.369(10) C20 C21 1.391(9) C20 H20 0.9300 C10 C9 1.463(7) C13 C12 1.369(7) C13 C14 1.378(7) C13 H13 0.9300 C30 C31 1.391(10) C30 H30 0.9300 C14 H14 0.9300 C40 C39 1.391(8) C40 H40 0.9300 C24 C25 1.404(8) C24 H24 0.9300 C28 C27 1.418(10) C28 H28 0.9300 C38 C39 1.366(9) C38 C37 1.373(9) C38 H38 0.9300 C12 H12 0.9300 C2 C3 1.350(9) C2 H2 0.9300 C8 C9 1.336(8) C8 H8 0.9300 C39 H39 0.9300 C17 C18 1.401(8) C34 C33 1.408(10) C34 H34 0.9300 C36 C37 1.374(9) C36 H36 0.9300 C37 H37 0.9300 C5 C4 1.350(8) C5 H5 0.9300 C25 C26 1.385(13) C25 H25 0.9300 C3 C4 1.411(9) C3 H3 0.9300 C19 C18 1.345(10) C19 H19 0.9300 C26 C27 1.354(14) C26 H26 0.9300 C33 C32 1.376(14) C33 H33 0.9300 C21 H21 0.9300 C4 H4 0.9300 C31 C32 1.365(14) C31 H31 0.9300 C18 H18 0.9300 C27 H27 0.9300 C41 H41A 0.9700 C41 H41B 0.9700 C32 H32 0.9300