#------------------------------------------------------------------------------ #$Date: 2019-10-12 03:58:44 +0300 (Sat, 12 Oct 2019) $ #$Revision: 219307 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/13/7701358.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_7701358 loop_ _publ_author_name 'Artem'ev, Alexander' 'Davydova, Maria' 'Berezin, Alexey S.' 'Brel, Valery K.' 'Morgalyuk, Vasilii' 'Bagryanskaya, Irina Yu.' 'Samsonenko, Denis G.' _publ_section_title ; Luminescence of Mn2+ ion in non-Oh and Td coordination environments: the missing case of square-pyramid ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT03283E _journal_year 2019 _chemical_formula_moiety 'C54 H54 Br2 Mn N2 O4 P4' _chemical_formula_sum 'C54 H54 Br2 Mn N2 O4 P4' _chemical_formula_weight 1133.63 _chemical_name_systematic 'Complex of manganese(II) bromide with [(dimethylamino)methylene] bis(diphenylphosphine oxide)' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-06-10 deposited with the CCDC. 2019-10-11 downloaded from the CCDC. ; _cell_angle_alpha 63.853(3) _cell_angle_beta 86.986(4) _cell_angle_gamma 84.516(4) _cell_formula_units_Z 2 _cell_length_a 14.1360(13) _cell_length_b 14.4046(10) _cell_length_c 14.9017(13) _cell_measurement_reflns_used 9895 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 24.73 _cell_measurement_theta_min 2.75 _cell_volume 2711.2(4) _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-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _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 0.0578 _diffrn_reflns_av_unetI/netI 0.1384 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 40988 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.026 _diffrn_reflns_theta_max 25.026 _diffrn_reflns_theta_min 2.632 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 1.880 _exptl_absorpt_correction_T_max 0.9281 _exptl_absorpt_correction_T_min 0.7939 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1158 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _refine_diff_density_max 1.419 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.119 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 607 _refine_ls_number_reflns 9502 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0777 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+13.1553P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2297 _refine_ls_wR_factor_ref 0.2378 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5727 _reflns_number_total 9502 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt03283e2.cif _cod_data_source_block md236 _cod_database_code 7701358 _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_estimated_absorpt_t_min 0.520 _shelx_estimated_absorpt_t_max 0.705 _shelx_res_file ; md236.res created by SHELXL-2014/7 TITL 236 in P-1 CELL 0.71073 14.1360 14.4046 14.9017 63.853 86.986 84.516 ZERR 2.00 0.0013 0.0010 0.0013 0.003 0.004 0.004 LATT 1 SFAC C H O P MN BR N UNIT 108 108 8 8 2 4 4 TEMP 23.000 SIZE 0.200 0.400 0.400 ACTA shel 8.90 0.84 L.S. 4 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF omit 6 6 1 omit 6 9 4 omit 7 -1 5 omit 1 6 5 omit -3 6 9 omit -2 6 8 omit -1 -5 3 omit 2 3 1 omit 5 4 7 omit 3 6 4 omit -1 6 9 WGHT 0.062800 13.155302 FVAR 0.09291 BR1 6 0.119964 0.206851 0.427158 11.00000 0.06276 0.04880 = 0.06132 -0.01126 0.02237 -0.00395 MN1 5 0.235514 0.250249 0.282079 11.00000 0.03565 0.02481 = 0.03405 -0.01278 -0.00040 -0.00523 P4 4 0.371626 0.440258 0.269754 11.00000 0.03063 0.03314 = 0.03538 -0.01829 -0.00474 -0.00391 P1 4 0.185996 0.512021 0.157712 11.00000 0.02840 0.02674 = 0.03007 -0.00990 -0.00446 -0.00195 P2 4 0.207608 0.114837 0.146864 11.00000 0.04200 0.02912 = 0.03343 -0.01325 -0.01095 -0.00334 P3 4 0.341361 0.013950 0.321385 11.00000 0.03405 0.03017 = 0.03354 -0.01447 -0.00679 0.00107 BR1S 6 0.336466 -0.196945 0.144921 11.00000 0.09110 0.05176 = 0.08707 -0.04480 0.02218 -0.02772 O1 3 0.175933 0.401253 0.181046 11.00000 0.03607 0.02896 = 0.03771 -0.01248 -0.00475 -0.00618 C56 1 0.339403 0.469325 0.374591 11.00000 0.02738 0.02778 = 0.02204 -0.00856 -0.00968 0.00784 O3 3 0.191749 0.201930 0.177312 11.00000 0.05417 0.02972 = 0.05544 -0.02248 -0.01991 0.00929 O4 3 0.328703 0.111395 0.334556 11.00000 0.04455 0.03383 = 0.03950 -0.01725 -0.01207 -0.00118 C1 1 0.138339 0.596059 0.035888 11.00000 0.02533 0.04143 = 0.03322 -0.01012 -0.00316 0.00404 C2 1 0.113229 0.550542 -0.023025 11.00000 0.05288 0.06041 = 0.03761 -0.01836 -0.01112 -0.00398 AFIX 43 H5 2 0.122467 0.478998 -0.000228 11.00000 -1.20000 AFIX 0 C3 1 0.073807 0.612713 -0.117218 11.00000 0.06373 0.10500 = 0.04990 -0.03336 -0.01033 -0.01606 AFIX 43 H4 2 0.054940 0.582279 -0.156245 11.00000 -1.20000 AFIX 0 C4 1 0.063010 0.718628 -0.151956 11.00000 0.06193 0.08901 = 0.06158 -0.01010 -0.01434 0.01653 AFIX 43 H3 2 0.037921 0.760002 -0.215009 11.00000 -1.20000 AFIX 0 C5 1 0.088801 0.762607 -0.094602 11.00000 0.09816 0.05611 = 0.05239 0.00009 -0.01021 0.02782 AFIX 43 H2 2 0.081729 0.834417 -0.118944 11.00000 -1.20000 AFIX 0 C6 1 0.125694 0.702669 0.000061 11.00000 0.07904 0.04501 = 0.05106 -0.01353 -0.00840 0.01787 AFIX 43 H1 2 0.141847 0.734103 0.039245 11.00000 -1.20000 AFIX 0 C7 1 0.120141 0.549796 0.244124 11.00000 0.03386 0.03961 = 0.02561 -0.00933 -0.01034 0.00543 C8 1 0.048641 0.485515 0.301365 11.00000 0.03971 0.03989 = 0.03319 -0.00634 0.00215 -0.00294 AFIX 43 H10 2 0.038775 0.425205 0.296086 11.00000 -1.20000 AFIX 0 C9 1 -0.005868 0.514964 0.365104 11.00000 0.04597 0.09246 = 0.03967 -0.01933 -0.00519 0.00788 AFIX 43 H9 2 -0.053782 0.474884 0.403809 11.00000 -1.20000 AFIX 0 C10 1 0.011607 0.605058 0.370805 11.00000 0.10861 0.07150 = 0.03441 -0.01934 -0.01221 0.00329 AFIX 43 H8 2 -0.024595 0.622699 0.415784 11.00000 -1.20000 AFIX 0 C11 1 0.075678 0.666917 0.317078 11.00000 0.08051 0.05628 = 0.05746 -0.03934 -0.01359 0.02250 AFIX 43 H7 2 0.081385 0.728425 0.321745 11.00000 -1.20000 AFIX 0 C12 1 0.137516 0.640238 0.250643 11.00000 0.09171 0.02572 = 0.04939 -0.01515 -0.03372 -0.00334 AFIX 43 H6 2 0.186068 0.680850 0.214312 11.00000 -1.20000 AFIX 0 C13 1 0.312064 0.539447 0.155557 11.00000 0.03492 0.02621 = 0.03073 -0.01679 0.00338 -0.00803 AFIX 13 H13A 2 0.312029 0.606343 0.157979 11.00000 -1.20000 AFIX 0 C14 1 0.385113 0.542386 0.388707 11.00000 0.07560 0.08178 = 0.06432 -0.05557 0.01170 -0.01524 AFIX 43 H15 2 0.428484 0.582575 0.341870 11.00000 -1.20000 AFIX 0 C15 1 0.363312 0.553478 0.476950 11.00000 0.10606 0.11103 = 0.08250 -0.07736 -0.01554 0.00392 AFIX 43 H11 2 0.395109 0.599400 0.490528 11.00000 -1.20000 AFIX 0 C16 1 0.296822 0.498305 0.542155 11.00000 0.12238 0.11899 = 0.04697 -0.04919 -0.01090 0.04222 AFIX 43 H12 2 0.284303 0.506500 0.600258 11.00000 -1.20000 AFIX 0 C17 1 0.246361 0.429218 0.524527 11.00000 0.12437 0.07954 = 0.02801 -0.01170 0.01518 0.03002 AFIX 43 H13 2 0.197353 0.395267 0.566942 11.00000 -1.20000 AFIX 0 C18 1 0.272738 0.413557 0.440747 11.00000 0.06704 0.05268 = 0.04851 -0.01707 -0.00068 0.01065 AFIX 43 H14 2 0.244284 0.363990 0.429647 11.00000 -1.20000 AFIX 0 C19 1 0.496887 0.454513 0.246117 11.00000 0.02986 0.06907 = 0.05458 -0.04700 -0.00508 0.00053 C20 1 0.557018 0.365141 0.281176 11.00000 0.05457 0.10597 = 0.09368 -0.06910 -0.03014 0.02389 AFIX 43 H20A 2 0.533499 0.300070 0.312750 11.00000 -1.20000 AFIX 0 C21 1 0.657496 0.376118 0.267176 11.00000 0.04705 0.18015 = 0.12348 -0.11283 -0.02617 0.02904 AFIX 43 H18 2 0.700125 0.317415 0.288742 11.00000 -1.20000 AFIX 0 C22 1 0.690137 0.471531 0.222757 11.00000 0.03576 0.24017 = 0.11353 -0.13537 -0.00132 -0.01526 AFIX 43 H22A 2 0.755304 0.477537 0.214761 11.00000 -1.20000 AFIX 0 C23 1 0.630288 0.558071 0.189840 11.00000 0.04565 0.16240 = 0.07083 -0.07180 0.01164 -0.04362 AFIX 43 H17 2 0.654812 0.622687 0.160030 11.00000 -1.20000 AFIX 0 C24 1 0.532195 0.552301 0.199753 11.00000 0.04805 0.09550 = 0.05326 -0.04729 0.00039 -0.02474 AFIX 43 H16 2 0.491113 0.612265 0.176011 11.00000 -1.20000 AFIX 0 N1 7 0.366641 0.547425 0.067102 11.00000 0.03900 0.03963 = 0.03124 -0.01956 0.00990 -0.00962 C26 1 0.369502 0.460038 0.043042 11.00000 0.05290 0.05491 = 0.04938 -0.03188 0.00209 -0.00748 AFIX 137 H22 2 0.309263 0.458870 0.016820 11.00000 -1.50000 H23 2 0.382619 0.396764 0.102378 11.00000 -1.50000 H24 2 0.418517 0.466607 -0.006008 11.00000 -1.50000 AFIX 0 C27 1 0.364598 0.647461 -0.017801 11.00000 0.06127 0.05249 = 0.05008 -0.01911 0.01000 -0.01263 AFIX 137 H27 2 0.419234 0.650075 -0.059683 11.00000 -1.50000 H26 2 0.365336 0.700401 0.004715 11.00000 -1.50000 H25 2 0.307859 0.658705 -0.055127 11.00000 -1.50000 AFIX 0 C28 1 0.323949 0.040480 0.189268 11.00000 0.03498 0.02424 = 0.03387 -0.01375 -0.00037 -0.00799 AFIX 13 H40 2 0.321492 -0.026392 0.187370 11.00000 -1.20000 AFIX 0 C29 1 0.261990 -0.079946 0.403600 11.00000 0.03799 0.03337 = 0.03731 -0.01013 -0.00912 0.00745 C30 1 0.250485 -0.170221 0.392734 11.00000 0.05312 0.04731 = 0.08076 -0.04262 -0.02794 0.01448 AFIX 43 H32 2 0.281282 -0.183689 0.342509 11.00000 -1.20000 AFIX 0 C31 1 0.189053 -0.239112 0.463149 11.00000 0.07068 0.05470 = 0.05720 -0.01401 -0.00416 -0.03569 AFIX 43 H31 2 0.178268 -0.299731 0.458900 11.00000 -1.20000 AFIX 0 C32 1 0.146274 -0.219836 0.535205 11.00000 0.04630 0.05765 = 0.09806 -0.03017 -0.00881 -0.00599 AFIX 43 H30 2 0.108392 -0.268798 0.581527 11.00000 -1.20000 AFIX 0 C33 1 0.155756 -0.131388 0.543786 11.00000 0.06803 0.06117 = 0.04627 -0.02003 0.01472 -0.00227 AFIX 43 H29 2 0.123334 -0.118451 0.593569 11.00000 -1.20000 AFIX 0 C34 1 0.214501 -0.061347 0.477036 11.00000 0.05491 0.03703 = 0.04286 -0.02087 -0.00409 0.00277 AFIX 43 H28 2 0.222079 -0.000300 0.481892 11.00000 -1.20000 AFIX 0 C35 1 0.460048 -0.046529 0.352482 11.00000 0.04281 0.06350 = 0.04640 -0.02474 -0.00806 0.00841 C36 1 0.487191 -0.142040 0.352037 11.00000 0.04824 0.06322 = 0.15216 -0.03794 -0.00388 0.01845 AFIX 43 H33 2 0.443732 -0.175589 0.334454 11.00000 -1.20000 AFIX 0 C37 1 0.578647 -0.186738 0.377727 11.00000 0.07926 0.10117 = 0.16013 -0.04142 -0.01698 0.04788 AFIX 43 H37A 2 0.597337 -0.249734 0.376249 11.00000 -1.20000 AFIX 0 C38 1 0.522740 0.002907 0.377499 11.00000 0.04450 0.15837 = 0.11190 -0.09587 -0.03007 0.01545 AFIX 43 H38A 2 0.505081 0.066668 0.377743 11.00000 -1.20000 AFIX 0 N2 7 0.398861 0.093029 0.122778 11.00000 0.04537 0.04435 = 0.04804 -0.02340 0.01326 -0.02103 C40 1 0.417682 0.193939 0.109790 11.00000 0.06511 0.06435 = 0.06320 -0.02665 0.02660 -0.03502 AFIX 137 H35 2 0.456857 0.187532 0.163249 11.00000 -1.50000 H36 2 0.358809 0.232898 0.110327 11.00000 -1.50000 H37 2 0.450028 0.229185 0.047069 11.00000 -1.50000 AFIX 0 C41 1 0.477978 0.034224 0.103571 11.00000 0.07819 0.09072 = 0.10806 -0.07258 0.06013 -0.03986 AFIX 33 H41A 2 0.458946 -0.032069 0.114085 11.00000 -1.50000 H41B 2 0.499341 0.070966 0.035669 11.00000 -1.50000 H41C 2 0.528704 0.024338 0.148079 11.00000 -1.50000 AFIX 0 C42 1 0.113483 0.030861 0.192224 11.00000 0.03653 0.02046 = 0.03676 -0.00558 -0.01852 0.00232 C43 1 0.062410 0.026835 0.278494 11.00000 0.04856 0.04501 = 0.04210 -0.00948 -0.00771 0.00057 AFIX 43 H45 2 0.080220 0.064585 0.311001 11.00000 -1.20000 AFIX 0 C44 1 -0.011257 -0.031440 0.312573 11.00000 0.04865 0.03874 = 0.05931 -0.00543 0.01685 0.00676 AFIX 43 H41 2 -0.042258 -0.036385 0.370940 11.00000 -1.20000 AFIX 0 C45 1 -0.042646 -0.084433 0.263767 11.00000 0.03995 0.05825 = 0.10081 -0.01463 0.02027 -0.01596 AFIX 43 H42 2 -0.094479 -0.123942 0.289241 11.00000 -1.20000 AFIX 0 C46 1 0.001406 -0.079493 0.178832 11.00000 0.06538 0.06217 = 0.11597 -0.04263 -0.01051 -0.02395 AFIX 43 H43 2 -0.021291 -0.112934 0.144310 11.00000 -1.20000 AFIX 0 C47 1 0.083561 -0.021761 0.143369 11.00000 0.05472 0.04391 = 0.06169 -0.02210 -0.00159 -0.01384 AFIX 43 H44 2 0.116505 -0.020132 0.087071 11.00000 -1.20000 AFIX 0 C48 1 0.206989 0.164531 0.013627 11.00000 0.05273 0.04589 = 0.02751 -0.00668 -0.00925 -0.02001 C49 1 0.155135 0.256534 -0.039685 11.00000 0.07622 0.05585 = 0.04818 0.00321 -0.02120 -0.02399 AFIX 43 H50 2 0.124048 0.292960 -0.006971 11.00000 -1.20000 AFIX 0 C50 1 0.149090 0.295274 -0.142631 11.00000 0.09266 0.08231 = 0.05575 0.00895 -0.02953 -0.03199 AFIX 43 H49 2 0.112649 0.356874 -0.179061 11.00000 -1.20000 AFIX 0 C51 1 0.196367 0.243132 -0.189727 11.00000 0.13044 0.15261 = 0.02694 -0.01299 -0.00800 -0.08432 AFIX 43 H48 2 0.192494 0.270246 -0.258892 11.00000 -1.20000 AFIX 0 C52 1 0.249902 0.151459 -0.138743 11.00000 0.11702 0.15662 = 0.04230 -0.04784 0.00279 -0.04864 AFIX 43 H47 2 0.282380 0.117270 -0.172871 11.00000 -1.20000 AFIX 0 C53 1 0.254869 0.110757 -0.036254 11.00000 0.09868 0.08636 = 0.04495 -0.03067 -0.01351 -0.01188 AFIX 43 H46 2 0.289800 0.047930 -0.000312 11.00000 -1.20000 AFIX 0 O2 3 0.347596 0.332573 0.293307 11.00000 0.04158 0.02945 = 0.05608 -0.01497 -0.01620 -0.00208 C55 1 0.639879 -0.139121 0.404611 11.00000 0.06539 0.18784 = 0.13258 -0.06958 -0.04340 0.05350 AFIX 43 H55A 2 0.700600 -0.170541 0.424774 11.00000 -1.20000 AFIX 0 C54 1 0.613936 -0.043516 0.402787 11.00000 0.06790 0.27526 = 0.16567 -0.15959 -0.06128 0.02868 AFIX 43 H54A 2 0.658401 -0.009754 0.418792 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM 236 in P-1 REM R1 = 0.0777 for 5727 Fo > 4sig(Fo) and 0.1104 for all 9502 data REM 607 parameters refined using 0 restraints END WGHT 0.0701 11.7426 REM Instructions for potential hydrogen bonds HTAB C8 Br1 EQIV $1 x, y+1, z HTAB C12 Br1S_$1 HTAB C13 Br1S_$1 HTAB C18 Br1 HTAB C26 O2 HTAB C27 Br1S_$1 HTAB C28 Br1S HTAB C30 Br1S HTAB C34 Br1 HTAB C40 O3 HTAB C41 Br1S REM Highest difference peak 1.419, deepest hole -0.540, 1-sigma level 0.119 Q1 1 0.2836 -0.1378 0.3240 11.00000 0.05 1.42 Q2 1 0.2939 0.1892 0.0987 11.00000 0.05 1.38 Q3 1 0.3971 0.4060 0.2105 11.00000 0.05 1.28 Q4 1 0.1589 -0.1850 0.4654 11.00000 0.05 0.96 Q5 1 0.1882 0.6409 0.2253 11.00000 0.05 0.88 ; _shelx_res_checksum 90634 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 Br1 Br 0.11996(8) 0.20685(8) 0.42716(8) 0.0633(3) Uani 1 1 d . . Mn1 Mn 0.23551(8) 0.25025(8) 0.28208(9) 0.0313(3) Uani 1 1 d . . P4 P 0.37163(15) 0.44026(15) 0.26975(15) 0.0316(5) Uani 1 1 d . . P1 P 0.18600(14) 0.51202(14) 0.15771(14) 0.0292(5) Uani 1 1 d . . P2 P 0.20761(16) 0.11484(15) 0.14686(15) 0.0346(5) Uani 1 1 d . . P3 P 0.34136(15) 0.01395(15) 0.32138(15) 0.0324(5) Uani 1 1 d . . Br1S Br 0.33647(9) -0.19694(8) 0.14492(9) 0.0707(4) Uani 1 1 d . . O1 O 0.1759(4) 0.4013(4) 0.1810(4) 0.0346(12) Uani 1 1 d . . C56 C 0.3394(5) 0.4693(5) 0.3746(5) 0.0269(16) Uani 1 1 d . . O3 O 0.1917(4) 0.2019(4) 0.1773(4) 0.0452(15) Uani 1 1 d . . O4 O 0.3287(4) 0.1114(4) 0.3346(4) 0.0385(13) Uani 1 1 d . . C1 C 0.1383(5) 0.5961(6) 0.0359(6) 0.0360(19) Uani 1 1 d . . C2 C 0.1132(7) 0.5505(8) -0.0230(6) 0.051(2) Uani 1 1 d . . H5 H 0.1225 0.4790 -0.0002 0.061 Uiso 1 1 calc R U C3 C 0.0738(8) 0.6127(10) -0.1172(8) 0.072(3) Uani 1 1 d . . H4 H 0.0549 0.5823 -0.1562 0.086 Uiso 1 1 calc R U C4 C 0.0630(8) 0.7186(11) -0.1520(9) 0.080(4) Uani 1 1 d . . H3 H 0.0379 0.7600 -0.2150 0.096 Uiso 1 1 calc R U C5 C 0.0888(9) 0.7626(9) -0.0946(8) 0.080(4) Uani 1 1 d . . H2 H 0.0817 0.8344 -0.1189 0.096 Uiso 1 1 calc R U C6 C 0.1257(8) 0.7027(7) 0.0001(7) 0.062(3) Uani 1 1 d . . H1 H 0.1418 0.7341 0.0392 0.075 Uiso 1 1 calc R U C7 C 0.1201(6) 0.5498(6) 0.2441(5) 0.0351(19) Uani 1 1 d . . C8 C 0.0486(6) 0.4855(6) 0.3014(6) 0.041(2) Uani 1 1 d . . H10 H 0.0388 0.4252 0.2961 0.050 Uiso 1 1 calc R U C9 C -0.0059(7) 0.5150(9) 0.3651(7) 0.064(3) Uani 1 1 d . . H9 H -0.0538 0.4749 0.4038 0.076 Uiso 1 1 calc R U C10 C 0.0116(10) 0.6051(9) 0.3708(8) 0.073(3) Uani 1 1 d . . H8 H -0.0246 0.6227 0.4158 0.088 Uiso 1 1 calc R U C11 C 0.0757(8) 0.6669(8) 0.3171(8) 0.061(3) Uani 1 1 d . . H7 H 0.0814 0.7284 0.3217 0.073 Uiso 1 1 calc R U C12 C 0.1375(8) 0.6402(6) 0.2506(7) 0.055(3) Uani 1 1 d . . H6 H 0.1861 0.6808 0.2143 0.066 Uiso 1 1 calc R U C13 C 0.3121(5) 0.5394(5) 0.1556(5) 0.0288(17) Uani 1 1 d . . H13A H 0.3120 0.6063 0.1580 0.035 Uiso 1 1 calc R U C14 C 0.3851(8) 0.5424(8) 0.3887(8) 0.065(3) Uani 1 1 d . . H15 H 0.4285 0.5826 0.3419 0.078 Uiso 1 1 calc R U C15 C 0.3633(10) 0.5535(11) 0.4769(10) 0.087(4) Uani 1 1 d . . H11 H 0.3951 0.5994 0.4905 0.105 Uiso 1 1 calc R U C16 C 0.2968(12) 0.4983(12) 0.5422(9) 0.095(5) Uani 1 1 d . . H12 H 0.2843 0.5065 0.6003 0.114 Uiso 1 1 calc R U C17 C 0.2464(10) 0.4292(10) 0.5245(7) 0.085(4) Uani 1 1 d . . H13 H 0.1974 0.3953 0.5669 0.102 Uiso 1 1 calc R U C18 C 0.2727(7) 0.4136(8) 0.4407(7) 0.059(3) Uani 1 1 d . . H14 H 0.2443 0.3640 0.4296 0.071 Uiso 1 1 calc R U C19 C 0.4969(6) 0.4545(7) 0.2461(7) 0.044(2) Uani 1 1 d . . C20 C 0.5570(8) 0.3651(10) 0.2812(9) 0.076(3) Uani 1 1 d . . H20A H 0.5335 0.3001 0.3127 0.092 Uiso 1 1 calc R U C21 C 0.6575(10) 0.3761(15) 0.2672(12) 0.102(5) Uani 1 1 d . . H18 H 0.7001 0.3174 0.2887 0.122 Uiso 1 1 calc R U C22 C 0.6901(9) 0.4715(18) 0.2228(12) 0.108(6) Uani 1 1 d . . H22A H 0.7553 0.4775 0.2148 0.130 Uiso 1 1 calc R U C23 C 0.6303(9) 0.5581(13) 0.1898(9) 0.083(4) Uani 1 1 d . . H17 H 0.6548 0.6227 0.1600 0.100 Uiso 1 1 calc R U C24 C 0.5322(7) 0.5523(9) 0.1998(7) 0.059(3) Uani 1 1 d . . H16 H 0.4911 0.6123 0.1760 0.071 Uiso 1 1 calc R U N1 N 0.3666(5) 0.5474(5) 0.0671(5) 0.0351(15) Uani 1 1 d . . C26 C 0.3695(7) 0.4600(7) 0.0430(7) 0.049(2) Uani 1 1 d . . H22 H 0.3093 0.4589 0.0168 0.073 Uiso 1 1 calc R U H23 H 0.3826 0.3968 0.1024 0.073 Uiso 1 1 calc R U H24 H 0.4185 0.4666 -0.0060 0.073 Uiso 1 1 calc R U C27 C 0.3646(7) 0.6475(7) -0.0178(7) 0.056(2) Uani 1 1 d . . H27 H 0.4192 0.6501 -0.0597 0.084 Uiso 1 1 calc R U H26 H 0.3653 0.7004 0.0047 0.084 Uiso 1 1 calc R U H25 H 0.3079 0.6587 -0.0551 0.084 Uiso 1 1 calc R U C28 C 0.3239(5) 0.0405(5) 0.1893(5) 0.0303(17) Uani 1 1 d . . H40 H 0.3215 -0.0264 0.1874 0.036 Uiso 1 1 calc R U C29 C 0.2620(6) -0.0799(6) 0.4036(6) 0.039(2) Uani 1 1 d . . C30 C 0.2505(7) -0.1702(7) 0.3927(8) 0.055(3) Uani 1 1 d . . H32 H 0.2813 -0.1837 0.3425 0.066 Uiso 1 1 calc R U C31 C 0.1891(8) -0.2391(8) 0.4631(8) 0.062(3) Uani 1 1 d . . H31 H 0.1783 -0.2997 0.4589 0.075 Uiso 1 1 calc R U C32 C 0.1463(7) -0.2198(8) 0.5352(10) 0.068(3) Uani 1 1 d . . H30 H 0.1084 -0.2688 0.5815 0.082 Uiso 1 1 calc R U C33 C 0.1558(8) -0.1314(8) 0.5438(7) 0.061(3) Uani 1 1 d . . H29 H 0.1233 -0.1185 0.5936 0.073 Uiso 1 1 calc R U C34 C 0.2145(6) -0.0613(6) 0.4770(6) 0.044(2) Uani 1 1 d . . H28 H 0.2221 -0.0003 0.4819 0.053 Uiso 1 1 calc R U C35 C 0.4600(7) -0.0465(8) 0.3525(7) 0.051(2) Uani 1 1 d . . C36 C 0.4872(8) -0.1420(9) 0.3520(11) 0.093(4) Uani 1 1 d . . H33 H 0.4437 -0.1756 0.3345 0.111 Uiso 1 1 calc R U C37 C 0.5786(12) -0.1867(13) 0.3777(14) 0.123(6) Uani 1 1 d . . H37A H 0.5973 -0.2497 0.3762 0.147 Uiso 1 1 calc R U C38 C 0.5227(8) 0.0029(12) 0.3775(10) 0.092(4) Uani 1 1 d . . H38A H 0.5051 0.0667 0.3777 0.110 Uiso 1 1 calc R U N2 N 0.3989(5) 0.0930(5) 0.1228(5) 0.0441(18) Uani 1 1 d . . C40 C 0.4177(8) 0.1939(8) 0.1098(8) 0.064(3) Uani 1 1 d . . H35 H 0.4569 0.1875 0.1632 0.095 Uiso 1 1 calc R U H36 H 0.3588 0.2329 0.1103 0.095 Uiso 1 1 calc R U H37 H 0.4500 0.2292 0.0471 0.095 Uiso 1 1 calc R U C41 C 0.4780(8) 0.0342(9) 0.1036(9) 0.082(4) Uani 1 1 d . . H41A H 0.4589 -0.0321 0.1141 0.123 Uiso 1 1 calc R U H41B H 0.4993 0.0710 0.0357 0.123 Uiso 1 1 calc R U H41C H 0.5287 0.0243 0.1481 0.123 Uiso 1 1 calc R U C42 C 0.1135(6) 0.0309(5) 0.1922(6) 0.0334(19) Uani 1 1 d . . C43 C 0.0624(7) 0.0268(7) 0.2785(7) 0.049(2) Uani 1 1 d . . H45 H 0.0802 0.0646 0.3110 0.059 Uiso 1 1 calc R U C44 C -0.0113(7) -0.0314(7) 0.3126(8) 0.056(3) Uani 1 1 d . . H41 H -0.0423 -0.0364 0.3709 0.067 Uiso 1 1 calc R U C45 C -0.0426(7) -0.0844(8) 0.2638(10) 0.074(3) Uani 1 1 d . . H42 H -0.0945 -0.1239 0.2892 0.088 Uiso 1 1 calc R U C46 C 0.0014(8) -0.0795(8) 0.1788(10) 0.078(4) Uani 1 1 d . . H43 H -0.0213 -0.1129 0.1443 0.094 Uiso 1 1 calc R U C47 C 0.0836(7) -0.0218(7) 0.1434(7) 0.053(2) Uani 1 1 d . . H44 H 0.1165 -0.0201 0.0871 0.064 Uiso 1 1 calc R U C48 C 0.2070(6) 0.1645(7) 0.0136(6) 0.044(2) Uani 1 1 d . . C49 C 0.1551(8) 0.2565(8) -0.0397(7) 0.067(3) Uani 1 1 d . . H50 H 0.1240 0.2930 -0.0070 0.081 Uiso 1 1 calc R U C50 C 0.1491(10) 0.2953(10) -0.1426(10) 0.088(4) Uani 1 1 d . . H49 H 0.1126 0.3569 -0.1791 0.106 Uiso 1 1 calc R U C51 C 0.1964(13) 0.2431(15) -0.1897(9) 0.107(6) Uani 1 1 d . . H48 H 0.1925 0.2702 -0.2589 0.129 Uiso 1 1 calc R U C52 C 0.2499(11) 0.1515(14) -0.1387(9) 0.101(5) Uani 1 1 d . . H47 H 0.2824 0.1173 -0.1729 0.121 Uiso 1 1 calc R U C53 C 0.2549(9) 0.1108(9) -0.0363(8) 0.075(3) Uani 1 1 d . . H46 H 0.2898 0.0479 -0.0003 0.090 Uiso 1 1 calc R U O2 O 0.3476(4) 0.3326(4) 0.2933(4) 0.0432(14) Uani 1 1 d . . C55 C 0.6399(12) -0.1391(18) 0.4046(13) 0.132(7) Uani 1 1 d . . H55A H 0.7006 -0.1705 0.4248 0.158 Uiso 1 1 calc R U C54 C 0.6139(11) -0.0435(19) 0.4028(14) 0.147(8) Uani 1 1 d . . H54A H 0.6584 -0.0098 0.4188 0.177 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 Br1 0.0628(7) 0.0488(6) 0.0613(7) -0.0113(5) 0.0224(5) -0.0039(5) Mn1 0.0357(7) 0.0248(6) 0.0340(7) -0.0128(5) -0.0004(5) -0.0052(5) P4 0.0306(12) 0.0331(11) 0.0354(11) -0.0183(9) -0.0047(9) -0.0039(9) P1 0.0284(11) 0.0267(10) 0.0301(11) -0.0099(9) -0.0045(8) -0.0020(8) P2 0.0420(13) 0.0291(11) 0.0334(12) -0.0132(9) -0.0110(10) -0.0033(9) P3 0.0340(12) 0.0302(11) 0.0335(11) -0.0145(9) -0.0068(9) 0.0011(9) Br1S 0.0911(9) 0.0518(6) 0.0871(8) -0.0448(6) 0.0222(7) -0.0277(6) O1 0.036(3) 0.029(3) 0.038(3) -0.012(2) -0.005(2) -0.006(2) C56 0.027(4) 0.028(4) 0.022(4) -0.009(3) -0.010(3) 0.008(3) O3 0.054(4) 0.030(3) 0.055(4) -0.022(3) -0.020(3) 0.009(3) O4 0.045(3) 0.034(3) 0.039(3) -0.017(3) -0.012(3) -0.001(2) C1 0.025(4) 0.041(5) 0.033(4) -0.010(4) -0.003(3) 0.004(3) C2 0.053(6) 0.060(6) 0.038(5) -0.018(5) -0.011(4) -0.004(5) C3 0.064(7) 0.105(10) 0.050(6) -0.033(7) -0.010(5) -0.016(7) C4 0.062(8) 0.089(9) 0.062(8) -0.010(7) -0.014(6) 0.017(7) C5 0.098(10) 0.056(7) 0.052(7) 0.000(6) -0.010(7) 0.028(6) C6 0.079(8) 0.045(6) 0.051(6) -0.014(5) -0.008(5) 0.018(5) C7 0.034(5) 0.040(5) 0.026(4) -0.009(4) -0.010(3) 0.005(4) C8 0.040(5) 0.040(5) 0.033(5) -0.006(4) 0.002(4) -0.003(4) C9 0.046(6) 0.092(8) 0.040(6) -0.019(6) -0.005(5) 0.008(6) C10 0.109(10) 0.071(8) 0.034(6) -0.019(6) -0.012(6) 0.003(7) C11 0.081(8) 0.056(6) 0.057(7) -0.039(6) -0.014(6) 0.023(6) C12 0.092(8) 0.026(4) 0.049(6) -0.015(4) -0.034(5) -0.003(5) C13 0.035(4) 0.026(4) 0.031(4) -0.017(3) 0.003(3) -0.008(3) C14 0.076(8) 0.082(7) 0.064(7) -0.056(6) 0.012(6) -0.015(6) C15 0.106(11) 0.111(10) 0.083(9) -0.077(9) -0.016(8) 0.004(9) C16 0.122(13) 0.119(12) 0.047(7) -0.049(8) -0.011(8) 0.042(10) C17 0.124(11) 0.080(8) 0.028(6) -0.012(6) 0.015(6) 0.030(8) C18 0.067(7) 0.053(6) 0.049(6) -0.017(5) -0.001(5) 0.011(5) C19 0.030(5) 0.069(6) 0.055(6) -0.047(5) -0.005(4) 0.001(4) C20 0.055(7) 0.106(9) 0.094(9) -0.069(8) -0.030(6) 0.024(6) C21 0.047(8) 0.180(17) 0.123(12) -0.113(13) -0.026(8) 0.029(9) C22 0.036(8) 0.24(2) 0.114(12) -0.135(15) -0.001(8) -0.015(11) C23 0.046(7) 0.162(13) 0.071(8) -0.072(9) 0.012(6) -0.044(8) C24 0.048(6) 0.096(8) 0.053(6) -0.047(6) 0.000(5) -0.025(6) N1 0.039(4) 0.040(4) 0.031(4) -0.020(3) 0.010(3) -0.010(3) C26 0.053(6) 0.055(6) 0.049(6) -0.032(5) 0.002(4) -0.007(5) C27 0.061(7) 0.052(6) 0.050(6) -0.019(5) 0.010(5) -0.013(5) C28 0.035(5) 0.024(4) 0.034(4) -0.014(3) 0.000(3) -0.008(3) C29 0.038(5) 0.033(4) 0.037(5) -0.010(4) -0.009(4) 0.007(4) C30 0.053(6) 0.047(5) 0.081(7) -0.043(5) -0.028(5) 0.014(5) C31 0.071(7) 0.055(6) 0.057(6) -0.014(5) -0.004(6) -0.036(6) C32 0.046(6) 0.058(7) 0.098(9) -0.030(6) -0.009(6) -0.006(5) C33 0.068(7) 0.061(7) 0.046(6) -0.020(5) 0.015(5) -0.002(5) C34 0.055(6) 0.037(5) 0.043(5) -0.021(4) -0.004(4) 0.003(4) C35 0.043(6) 0.064(6) 0.046(5) -0.025(5) -0.008(4) 0.008(5) C36 0.048(7) 0.063(7) 0.152(13) -0.038(8) -0.004(7) 0.018(6) C37 0.079(11) 0.101(11) 0.160(16) -0.041(11) -0.017(11) 0.048(9) C38 0.044(7) 0.158(13) 0.112(10) -0.096(10) -0.030(7) 0.015(7) N2 0.045(4) 0.044(4) 0.048(4) -0.023(4) 0.013(4) -0.021(3) C40 0.065(7) 0.064(7) 0.063(7) -0.027(5) 0.027(6) -0.035(6) C41 0.078(8) 0.091(8) 0.108(9) -0.073(8) 0.060(7) -0.040(7) C42 0.037(5) 0.020(4) 0.037(5) -0.006(3) -0.019(4) 0.002(3) C43 0.049(6) 0.045(5) 0.042(5) -0.009(4) -0.008(5) 0.001(4) C44 0.049(6) 0.039(5) 0.059(6) -0.005(5) 0.017(5) 0.007(5) C45 0.040(6) 0.058(7) 0.101(10) -0.015(7) 0.020(6) -0.016(5) C46 0.065(8) 0.062(7) 0.116(10) -0.043(7) -0.011(7) -0.024(6) C47 0.055(6) 0.044(5) 0.062(6) -0.022(5) -0.002(5) -0.014(5) C48 0.053(6) 0.046(5) 0.028(4) -0.007(4) -0.009(4) -0.020(4) C49 0.076(8) 0.056(6) 0.048(6) 0.003(5) -0.021(5) -0.024(6) C50 0.093(10) 0.082(9) 0.056(8) 0.009(7) -0.030(7) -0.032(7) C51 0.130(14) 0.153(15) 0.027(7) -0.013(8) -0.008(8) -0.084(12) C52 0.117(12) 0.157(14) 0.042(7) -0.048(9) 0.003(7) -0.049(11) C53 0.099(9) 0.086(8) 0.045(6) -0.031(6) -0.014(6) -0.012(7) O2 0.042(3) 0.029(3) 0.056(4) -0.015(3) -0.016(3) -0.002(2) C55 0.065(11) 0.19(2) 0.133(14) -0.070(14) -0.043(10) 0.053(12) C54 0.068(10) 0.28(3) 0.166(17) -0.160(18) -0.061(11) 0.029(13) 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' 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' Mn Mn 0.3368 0.7283 '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' N N 0.0061 0.0033 '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 O3 Mn1 O2 136.5(2) O3 Mn1 O4 85.0(2) O2 Mn1 O4 89.6(2) O3 Mn1 O1 85.33(19) O2 Mn1 O1 84.11(19) O4 Mn1 O1 158.3(2) O3 Mn1 Br1 111.54(18) O2 Mn1 Br1 111.90(17) O4 Mn1 Br1 100.85(16) O1 Mn1 Br1 100.73(15) O2 P4 C19 111.7(4) O2 P4 C56 110.0(3) C19 P4 C56 107.4(4) O2 P4 C13 112.2(3) C19 P4 C13 105.5(4) C56 P4 C13 109.7(3) O1 P1 C7 111.9(3) O1 P1 C1 109.9(3) C7 P1 C1 106.2(4) O1 P1 C13 112.3(3) C7 P1 C13 109.1(3) C1 P1 C13 107.1(3) O3 P2 C42 110.8(4) O3 P2 C48 110.6(4) C42 P2 C48 105.9(4) O3 P2 C28 111.9(3) C42 P2 C28 110.6(3) C48 P2 C28 106.8(4) O4 P3 C35 111.1(4) O4 P3 C29 111.0(4) C35 P3 C29 106.5(4) O4 P3 C28 111.4(3) C35 P3 C28 106.0(4) C29 P3 C28 110.6(4) P1 O1 Mn1 138.1(3) C18 C56 C14 121.6(8) C18 C56 P4 118.0(6) C14 C56 P4 120.4(6) P2 O3 Mn1 142.0(3) P3 O4 Mn1 137.7(3) C2 C1 C6 119.4(8) C2 C1 P1 117.8(6) C6 C1 P1 122.8(7) C1 C2 C3 119.7(9) C1 C2 H5 120.2 C3 C2 H5 120.2 C4 C3 C2 120.0(10) C4 C3 H4 120.0 C2 C3 H4 120.0 C5 C4 C3 120.0(11) C5 C4 H3 120.0 C3 C4 H3 120.0 C4 C5 C6 121.2(11) C4 C5 H2 119.4 C6 C5 H2 119.4 C1 C6 C5 119.7(10) C1 C6 H1 120.1 C5 C6 H1 120.1 C12 C7 C8 122.7(8) C12 C7 P1 120.7(7) C8 C7 P1 116.6(6) C9 C8 C7 117.9(9) C9 C8 H10 121.0 C7 C8 H10 121.0 C8 C9 C10 119.0(10) C8 C9 H9 120.5 C10 C9 H9 120.5 C11 C10 C9 124.2(11) C11 C10 H8 117.9 C9 C10 H8 117.9 C10 C11 C12 120.2(10) C10 C11 H7 119.9 C12 C11 H7 119.9 C7 C12 C11 115.9(9) C7 C12 H6 122.1 C11 C12 H6 122.1 N1 C13 P4 110.1(5) N1 C13 P1 115.3(5) P4 C13 P1 109.4(4) N1 C13 H13A 107.2 P4 C13 H13A 107.2 P1 C13 H13A 107.2 C56 C14 C15 117.2(10) C56 C14 H15 121.4 C15 C14 H15 121.4 C16 C15 C14 120.9(12) C16 C15 H11 119.6 C14 C15 H11 119.6 C15 C16 C17 121.7(11) C15 C16 H12 119.2 C17 C16 H12 119.2 C18 C17 C16 117.0(12) C18 C17 H13 121.5 C16 C17 H13 121.5 C56 C18 C17 121.3(11) C56 C18 H14 119.3 C17 C18 H14 119.3 C20 C19 C24 121.2(10) C20 C19 P4 117.2(8) C24 C19 P4 121.4(7) C19 C20 C21 117.6(13) C19 C20 H20A 121.2 C21 C20 H20A 121.2 C22 C21 C20 120.2(14) C22 C21 H18 119.9 C20 C21 H18 119.9 C23 C22 C21 121.4(13) C23 C22 H22A 119.3 C21 C22 H22A 119.3 C22 C23 C24 121.0(14) C22 C23 H17 119.5 C24 C23 H17 119.5 C23 C24 C19 118.6(12) C23 C24 H16 120.7 C19 C24 H16 120.7 C27 N1 C26 115.0(7) C27 N1 C13 117.5(7) C26 N1 C13 117.1(6) N1 C26 H22 109.5 N1 C26 H23 109.5 H22 C26 H23 109.5 N1 C26 H24 109.5 H22 C26 H24 109.5 H23 C26 H24 109.5 N1 C27 H27 109.5 N1 C27 H26 109.5 H27 C27 H26 109.5 N1 C27 H25 109.5 H27 C27 H25 109.5 H26 C27 H25 109.5 N2 C28 P2 110.8(5) N2 C28 P3 113.9(5) P2 C28 P3 108.9(4) N2 C28 H40 107.7 P2 C28 H40 107.7 P3 C28 H40 107.7 C34 C29 C30 121.0(9) C34 C29 P3 118.4(6) C30 C29 P3 120.7(7) C29 C30 C31 115.5(10) C29 C30 H32 122.3 C31 C30 H32 122.2 C32 C31 C30 121.8(10) C32 C31 H31 119.1 C30 C31 H31 119.1 C31 C32 C33 122.4(11) C31 C32 H30 118.8 C33 C32 H30 118.8 C32 C33 C34 118.2(10) C32 C33 H29 120.9 C34 C33 H29 120.9 C29 C34 C33 121.0(8) C29 C34 H28 119.5 C33 C34 H28 119.5 C38 C35 C36 120.4(10) C38 C35 P3 117.9(8) C36 C35 P3 121.7(8) C37 C36 C35 120.0(14) C37 C36 H33 120.0 C35 C36 H33 120.0 C55 C37 C36 119.6(16) C55 C37 H37A 120.2 C36 C37 H37A 120.2 C35 C38 C54 118.4(14) C35 C38 H38A 120.8 C54 C38 H38A 120.8 C40 N2 C41 115.2(8) C40 N2 C28 119.7(7) C41 N2 C28 119.8(7) N2 C40 H35 109.5 N2 C40 H36 109.5 H35 C40 H36 109.5 N2 C40 H37 109.5 H35 C40 H37 109.5 H36 C40 H37 109.5 N2 C41 H41A 109.5 N2 C41 H41B 109.5 H41A C41 H41B 109.5 N2 C41 H41C 109.5 H41A C41 H41C 109.5 H41B C41 H41C 109.5 C47 C42 C43 119.1(8) C47 C42 P2 123.1(7) C43 C42 P2 117.5(6) C44 C43 C42 119.6(9) C44 C43 H45 120.2 C42 C43 H45 120.2 C43 C44 C45 121.9(10) C43 C44 H41 119.1 C45 C44 H41 119.1 C46 C45 C44 120.6(10) C46 C45 H42 119.7 C44 C45 H42 119.7 C45 C46 C47 118.7(10) C45 C46 H43 120.6 C47 C46 H43 120.6 C42 C47 C46 120.0(10) C42 C47 H44 120.0 C46 C47 H44 120.0 C49 C48 C53 119.8(9) C49 C48 P2 118.0(8) C53 C48 P2 122.2(7) C48 C49 C50 119.8(12) C48 C49 H50 120.1 C50 C49 H50 120.1 C51 C50 C49 119.7(13) C51 C50 H49 120.2 C49 C50 H49 120.2 C50 C51 C52 122.0(12) C50 C51 H48 119.0 C52 C51 H48 119.0 C51 C52 C53 119.0(14) C51 C52 H47 120.5 C53 C52 H47 120.5 C52 C53 C48 119.6(12) C52 C53 H46 120.2 C48 C53 H46 120.2 P4 O2 Mn1 141.6(3) C37 C55 C54 120.5(14) C37 C55 H55A 119.8 C54 C55 H55A 119.8 C55 C54 C38 121.0(15) C55 C54 H54A 119.5 C38 C54 H54A 119.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 Mn1 2.5230(15) Mn1 O3 2.109(5) Mn1 O2 2.123(5) Mn1 O4 2.139(5) Mn1 O1 2.146(5) P4 O2 1.501(5) P4 C19 1.800(9) P4 C56 1.813(7) P4 C13 1.850(8) P1 O1 1.495(5) P1 C7 1.793(8) P1 C1 1.803(8) P1 C13 1.858(8) P2 O3 1.506(6) P2 C42 1.784(8) P2 C48 1.790(8) P2 C28 1.851(8) P3 O4 1.494(5) P3 C35 1.799(9) P3 C29 1.809(9) P3 C28 1.858(7) C56 C18 1.362(12) C56 C14 1.382(12) C1 C2 1.382(12) C1 C6 1.382(12) C2 C3 1.401(13) C2 H5 0.9300 C3 C4 1.374(16) C3 H4 0.9300 C4 C5 1.349(17) C4 H3 0.9300 C5 C6 1.388(14) C5 H2 0.9300 C6 H1 0.9300 C7 C12 1.394(11) C7 C8 1.414(11) C8 C9 1.375(13) C8 H10 0.9300 C9 C10 1.383(15) C9 H9 0.9300 C10 C11 1.306(15) C10 H8 0.9300 C11 C12 1.439(14) C11 H7 0.9300 C12 H6 0.9300 C13 N1 1.457(9) C13 H13A 0.9800 C14 C15 1.408(14) C14 H15 0.9300 C15 C16 1.351(19) C15 H11 0.9300 C16 C17 1.398(19) C16 H12 0.9300 C17 C18 1.390(14) C17 H13 0.9300 C18 H14 0.9300 C19 C20 1.378(13) C19 C24 1.397(13) C20 C21 1.438(18) C20 H20A 0.9300 C21 C22 1.35(2) C21 H18 0.9300 C22 C23 1.35(2) C22 H22A 0.9300 C23 C24 1.393(14) C23 H17 0.9300 C24 H16 0.9300 N1 C27 1.438(11) N1 C26 1.450(10) C26 H22 0.9600 C26 H23 0.9600 C26 H24 0.9600 C27 H27 0.9600 C27 H26 0.9600 C27 H25 0.9600 C28 N2 1.435(10) C28 H40 0.9800 C29 C34 1.366(12) C29 C30 1.404(12) C30 C31 1.411(14) C30 H32 0.9300 C31 C32 1.326(15) C31 H31 0.9300 C32 C33 1.355(14) C32 H30 0.9300 C33 C34 1.373(13) C33 H29 0.9300 C34 H28 0.9300 C35 C38 1.349(14) C35 C36 1.395(14) C36 C37 1.381(18) C36 H33 0.9300 C37 C55 1.33(2) C37 H37A 0.9300 C38 C54 1.384(19) C38 H38A 0.9300 N2 C40 1.429(11) N2 C41 1.432(12) C40 H35 0.9600 C40 H36 0.9600 C40 H37 0.9600 C41 H41A 0.9600 C41 H41B 0.9600 C41 H41C 0.9600 C42 C47 1.365(11) C42 C43 1.422(12) C43 C44 1.335(13) C43 H45 0.9300 C44 C45 1.377(16) C44 H41 0.9300 C45 C46 1.357(16) C45 H42 0.9300 C46 C47 1.433(14) C46 H43 0.9300 C47 H44 0.9300 C48 C49 1.368(13) C48 C53 1.402(14) C49 C50 1.386(16) C49 H50 0.9300 C50 C51 1.35(2) C50 H49 0.9300 C51 C52 1.37(2) C51 H48 0.9300 C52 C53 1.377(15) C52 H47 0.9300 C53 H46 0.9300 C55 C54 1.38(2) C55 H55A 0.9300 C54 H54A 0.9300 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 C7 P1 O1 Mn1 -80.6(5) C1 P1 O1 Mn1 161.7(5) C13 P1 O1 Mn1 42.5(6) O2 P4 C56 C18 -22.0(7) C19 P4 C56 C18 -143.8(7) C13 P4 C56 C18 101.9(7) O2 P4 C56 C14 154.9(7) C19 P4 C56 C14 33.0(8) C13 P4 C56 C14 -81.2(8) C42 P2 O3 Mn1 101.4(6) C48 P2 O3 Mn1 -141.4(6) C28 P2 O3 Mn1 -22.5(7) C35 P3 O4 Mn1 158.8(5) C29 P3 O4 Mn1 -82.9(6) C28 P3 O4 Mn1 40.8(6) O1 P1 C1 C2 -8.9(8) C7 P1 C1 C2 -130.2(7) C13 P1 C1 C2 113.4(7) O1 P1 C1 C6 170.7(7) C7 P1 C1 C6 49.4(9) C13 P1 C1 C6 -67.0(8) C6 C1 C2 C3 -1.2(14) P1 C1 C2 C3 178.5(8) C1 C2 C3 C4 2.0(16) C2 C3 C4 C5 -1.2(18) C3 C4 C5 C6 -1(2) C2 C1 C6 C5 -0.5(15) P1 C1 C6 C5 179.9(8) C4 C5 C6 C1 1.4(18) O1 P1 C7 C12 164.6(6) C1 P1 C7 C12 -75.5(7) C13 P1 C7 C12 39.6(7) O1 P1 C7 C8 -17.6(7) C1 P1 C7 C8 102.3(6) C13 P1 C7 C8 -142.6(6) C12 C7 C8 C9 0.5(12) P1 C7 C8 C9 -177.2(6) C7 C8 C9 C10 -0.3(13) C8 C9 C10 C11 1.9(16) C9 C10 C11 C12 -3.7(17) C8 C7 C12 C11 -2.1(12) P1 C7 C12 C11 175.5(6) C10 C11 C12 C7 3.7(14) O2 P4 C13 N1 -83.4(6) C19 P4 C13 N1 38.6(6) C56 P4 C13 N1 154.0(5) O2 P4 C13 P1 44.3(5) C19 P4 C13 P1 166.3(4) C56 P4 C13 P1 -78.3(4) O1 P1 C13 N1 75.7(6) C7 P1 C13 N1 -159.6(5) C1 P1 C13 N1 -45.1(6) O1 P1 C13 P4 -49.1(4) C7 P1 C13 P4 75.6(4) C1 P1 C13 P4 -169.9(4) C18 C56 C14 C15 3.0(15) P4 C56 C14 C15 -173.7(8) C56 C14 C15 C16 -3.2(18) C14 C15 C16 C17 -1(2) C15 C16 C17 C18 4.9(19) C14 C56 C18 C17 1.3(14) P4 C56 C18 C17 178.1(8) C16 C17 C18 C56 -5.2(16) O2 P4 C19 C20 -19.6(8) C56 P4 C19 C20 101.2(7) C13 P4 C19 C20 -141.8(7) O2 P4 C19 C24 164.3(6) C56 P4 C19 C24 -74.9(8) C13 P4 C19 C24 42.1(8) C24 C19 C20 C21 -0.8(14) P4 C19 C20 C21 -176.8(8) C19 C20 C21 C22 1.2(17) C20 C21 C22 C23 -1(2) C21 C22 C23 C24 -0.5(19) C22 C23 C24 C19 1.0(15) C20 C19 C24 C23 -0.3(13) P4 C19 C24 C23 175.6(7) P4 C13 N1 C27 -147.8(6) P1 C13 N1 C27 87.8(8) P4 C13 N1 C26 68.9(8) P1 C13 N1 C26 -55.5(8) O3 P2 C28 N2 -80.8(6) C42 P2 C28 N2 155.2(5) C48 P2 C28 N2 40.4(6) O3 P2 C28 P3 45.2(5) C42 P2 C28 P3 -78.8(4) C48 P2 C28 P3 166.4(4) O4 P3 C28 N2 70.9(6) C35 P3 C28 N2 -50.1(7) C29 P3 C28 N2 -165.2(5) O4 P3 C28 P2 -53.4(5) C35 P3 C28 P2 -174.4(4) C29 P3 C28 P2 70.5(4) O4 P3 C29 C34 -11.1(8) C35 P3 C29 C34 109.9(7) C28 P3 C29 C34 -135.3(7) O4 P3 C29 C30 169.6(6) C35 P3 C29 C30 -69.3(8) C28 P3 C29 C30 45.4(8) C34 C29 C30 C31 -1.2(12) P3 C29 C30 C31 178.1(7) C29 C30 C31 C32 -0.8(15) C30 C31 C32 C33 2.5(17) C31 C32 C33 C34 -2.2(16) C30 C29 C34 C33 1.5(13) P3 C29 C34 C33 -177.8(7) C32 C33 C34 C29 0.2(15) O4 P3 C35 C38 -3.5(10) C29 P3 C35 C38 -124.4(9) C28 P3 C35 C38 117.8(9) O4 P3 C35 C36 175.9(9) C29 P3 C35 C36 55.0(10) C28 P3 C35 C36 -62.9(10) C38 C35 C36 C37 0(2) P3 C35 C36 C37 -179.1(11) C35 C36 C37 C55 1(3) C36 C35 C38 C54 0(2) P3 C35 C38 C54 179.2(12) P2 C28 N2 C40 61.7(9) P3 C28 N2 C40 -61.5(9) P2 C28 N2 C41 -145.1(8) P3 C28 N2 C41 91.7(9) O3 P2 C42 C47 148.9(7) C48 P2 C42 C47 28.9(8) C28 P2 C42 C47 -86.5(7) O3 P2 C42 C43 -25.3(7) C48 P2 C42 C43 -145.3(6) C28 P2 C42 C43 99.4(6) C47 C42 C43 C44 2.7(12) P2 C42 C43 C44 177.1(7) C42 C43 C44 C45 -3.2(14) C43 C44 C45 C46 0.5(17) C44 C45 C46 C47 2.6(17) C43 C42 C47 C46 0.4(13) P2 C42 C47 C46 -173.7(7) C45 C46 C47 C42 -3.0(16) O3 P2 C48 C49 -27.7(8) C42 P2 C48 C49 92.4(7) C28 P2 C48 C49 -149.7(7) O3 P2 C48 C53 154.4(8) C42 P2 C48 C53 -85.5(9) C28 P2 C48 C53 32.4(9) C53 C48 C49 C50 1.0(14) P2 C48 C49 C50 -176.9(8) C48 C49 C50 C51 -1.6(17) C49 C50 C51 C52 1(2) C50 C51 C52 C53 1(2) C51 C52 C53 C48 -1.3(18) C49 C48 C53 C52 0.5(16) P2 C48 C53 C52 178.3(9) C19 P4 O2 Mn1 -151.0(6) C56 P4 O2 Mn1 89.7(6) C13 P4 O2 Mn1 -32.7(7) C36 C37 C55 C54 -3(3) C37 C55 C54 C38 3(3) C35 C38 C54 C55 -1(3)