#------------------------------------------------------------------------------ #$Date: 2019-11-17 11:39:28 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229647 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/80/7048010.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_7048010 loop_ _publ_author_name 'LaPierre, Etienne A.' 'Piers, Warren E.' 'Gendy, Chris' _publ_section_title ; Redox-state dependent activation of silanes and ammonia with reverse polarity (PCcarbeneP)Ni complexes: electrophilic vs. nucleophilic carbenes. ; _journal_issue 46 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 16789 _journal_page_last 16797 _journal_paper_doi 10.1039/c8dt04409k _journal_volume 47 _journal_year 2018 _chemical_formula_moiety 'C28 H40 Br Ni P2' _chemical_formula_sum 'C28 H40 Br Ni P2' _chemical_formula_weight 577.16 _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 ; 2018-08-22 deposited with the CCDC. 2018-11-07 downloaded from the CCDC. ; _cell_angle_alpha 107.237(2) _cell_angle_beta 98.206(2) _cell_angle_gamma 111.768(2) _cell_formula_units_Z 2 _cell_length_a 11.0190(6) _cell_length_b 11.1636(7) _cell_length_c 13.0424(8) _cell_measurement_reflns_used 7192 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.56 _cell_measurement_theta_min 2.93 _cell_volume 1364.11(15) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'LinXTL v. 5.9.1 (Spasyuk, 2009)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_unetI/netI 0.0473 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 13547 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.564 _diffrn_reflns_theta_min 3.040 _exptl_absorpt_coefficient_mu 2.307 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_crystal_colour Blue _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 602 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.26 _refine_diff_density_max 0.509 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.076 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 299 _refine_ls_number_reflns 6218 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.000 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0334 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.0801 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4938 _reflns_number_total 6218 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8dt04409k2.cif _cod_data_source_block CGEL180207017_0m _cod_depositor_comments 'Adding full bibliography for 7048006--7048012.cif.' _cod_original_cell_volume 1364.11(14) _cod_database_code 7048010 _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 ; CGEL180207017_0m_a.res created by SHELXL-2014/7 TITL CGEL180207017_0m_a.res in P-1 CELL 0.71073 11.0190 11.1636 13.0424 107.237 98.206 111.768 ZERR 2.000 0.0006 0.0007 0.0008 0.002 0.002 0.002 LATT 1 SFAC C H BR NI P UNIT 56 80 2 2 4 OMIT -2 -6 12 OMIT 5 -13 3 OMIT -1 4 10 OMIT -4 4 8 OMIT 4 -6 4 OMIT -10 0 7 OMIT -1 -4 3 OMIT 3 2 4 OMIT 1 -2 7 OMIT -1 -1 2 OMIT 2 -10 7 OMIT -9 3 12 OMIT 2 -4 5 OMIT -2 -4 2 OMIT 5 -10 6 OMIT -9 9 5 OMIT -2 0 6 OMIT -11 0 3 OMIT -2 -2 4 OMIT 1 -1 2 OMIT -3 2 2 OMIT -2 -5 6 OMIT 4 -6 2 OMIT 0 0 2 OMIT 3 -5 4 OMIT 4 2 1 OMIT -3 2 1 OMIT 5 -8 3 OMIT 1 4 2 OMIT 4 -5 4 OMIT -5 2 0 OMIT -11 0 9 OMIT -7 1 1 OMIT 2 -3 6 OMIT 8 -1 2 OMIT 0 -9 8 OMIT -1 -5 2 OMIT 3 -4 1 OMIT 0 4 4 OMIT 4 -5 2 OMIT -2 1 0 OMIT 0 -1 1 OMIT 1 -1 1 OMIT -1 1 0 OMIT -1 0 1 OMIT 0 1 0 OMIT 1 0 0 OMIT -1 1 1 OMIT 0 0 1 shel 0.1 8 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 LIST 6 TEMP 0.000 WGHT 0.041000 FVAR 0.45547 BR1 3 0.904901 0.636431 0.311801 11.00000 0.01330 0.02346 = 0.06630 0.01426 0.00748 0.00649 C1 1 0.478492 0.490125 0.245381 11.00000 0.01453 0.01766 = 0.01584 0.00431 0.00428 0.00502 C2 1 0.388220 0.343388 0.208207 11.00000 0.01305 0.01797 = 0.01263 0.00317 0.00216 0.00261 C3 1 0.244766 0.290549 0.178205 11.00000 0.01483 0.02327 = 0.01839 0.00266 0.00507 0.00325 C4 1 0.173216 0.385646 0.188021 11.00000 0.01209 0.02974 = 0.02608 0.00457 0.00529 0.00721 C5 1 0.273123 0.537957 0.226321 11.00000 0.01654 0.02878 = 0.02072 0.00778 0.00715 0.01068 C6 1 0.415263 0.583038 0.252110 11.00000 0.01689 0.02243 = 0.01537 0.00475 0.00480 0.00851 C7 1 0.446958 0.249847 0.201957 11.00000 0.01791 0.01667 = 0.01746 0.00461 0.00421 0.00301 C8 1 0.367469 0.108229 0.168937 11.00000 0.02202 0.01984 = 0.02876 0.00524 0.00592 0.00421 AFIX 43 H8 2 0.407925 0.048162 0.167339 11.00000 -1.20000 AFIX 0 C9 1 0.227052 0.057138 0.138331 11.00000 0.02636 0.01568 = 0.03569 0.00095 0.00570 -0.00332 AFIX 43 H9 2 0.172397 -0.038040 0.114667 11.00000 -1.20000 AFIX 0 C10 1 0.168145 0.147463 0.142934 11.00000 0.01406 0.02557 = 0.03010 0.00163 0.00423 -0.00038 AFIX 43 H10 2 0.073569 0.111200 0.121621 11.00000 -1.20000 AFIX 0 C11 1 0.501347 0.727360 0.285455 11.00000 0.01905 0.02214 = 0.02010 0.00640 0.00561 0.01083 C12 1 0.447886 0.822419 0.293700 11.00000 0.03041 0.02366 = 0.03479 0.01107 0.01244 0.01527 AFIX 43 H12 2 0.505511 0.916318 0.314304 11.00000 -1.20000 AFIX 0 C13 1 0.308873 0.778199 0.271376 11.00000 0.03055 0.03695 = 0.04453 0.01392 0.01571 0.02539 AFIX 43 H13 2 0.272627 0.842417 0.278937 11.00000 -1.20000 AFIX 0 C14 1 0.223146 0.637056 0.237491 11.00000 0.02160 0.03844 = 0.03399 0.01113 0.01140 0.01744 AFIX 43 H14 2 0.129480 0.608177 0.221838 11.00000 -1.20000 AFIX 0 C15 1 0.093245 0.367958 0.274792 11.00000 0.02090 0.03516 = 0.03838 0.00774 0.01370 0.00802 AFIX 137 H15A 2 0.023147 0.274071 0.247369 11.00000 -1.50000 H15B 2 0.052559 0.431652 0.286792 11.00000 -1.50000 H15C 2 0.154310 0.387154 0.344161 11.00000 -1.50000 AFIX 0 C16 1 0.072248 0.341701 0.073939 11.00000 0.02399 0.04642 = 0.02983 0.00292 -0.00186 0.01245 AFIX 137 H16A 2 0.121854 0.357917 0.020772 11.00000 -1.50000 H16B 2 0.020947 0.395433 0.082346 11.00000 -1.50000 H16C 2 0.011143 0.244418 0.047743 11.00000 -1.50000 AFIX 0 C17 1 0.709372 0.266191 0.154757 11.00000 0.01938 0.02034 = 0.02506 0.00472 0.00479 0.01039 AFIX 13 H17 2 0.807856 0.324828 0.185595 11.00000 -1.20000 AFIX 0 C18 1 0.668308 0.278282 0.043688 11.00000 0.04242 0.03873 = 0.02599 0.01369 0.01555 0.02197 AFIX 137 H18A 2 0.716140 0.245363 -0.005295 11.00000 -1.50000 H18B 2 0.690873 0.374055 0.055765 11.00000 -1.50000 H18C 2 0.571892 0.223088 0.010217 11.00000 -1.50000 AFIX 0 C19 1 0.687875 0.119061 0.139668 11.00000 0.04334 0.02334 = 0.03562 0.00441 0.01044 0.01989 AFIX 137 H19A 2 0.593488 0.055854 0.103135 11.00000 -1.50000 H19B 2 0.713887 0.115062 0.211589 11.00000 -1.50000 H19C 2 0.742640 0.093117 0.094727 11.00000 -1.50000 AFIX 0 C20 1 0.669613 0.306937 0.380314 11.00000 0.02462 0.02349 = 0.02345 0.01055 0.00200 0.00531 AFIX 13 H20 2 0.628015 0.205642 0.359430 11.00000 -1.20000 AFIX 0 C21 1 0.822100 0.363096 0.432464 11.00000 0.02989 0.03219 = 0.02825 0.01183 0.00259 0.01506 AFIX 137 H21A 2 0.865584 0.461643 0.449825 11.00000 -1.50000 H21B 2 0.859628 0.317339 0.380575 11.00000 -1.50000 H21C 2 0.837225 0.345710 0.499869 11.00000 -1.50000 AFIX 0 C22 1 0.604598 0.368441 0.463851 11.00000 0.03040 0.06727 = 0.02582 0.01877 0.01045 0.01756 AFIX 137 H22A 2 0.618233 0.344282 0.527931 11.00000 -1.50000 H22B 2 0.508686 0.331763 0.429260 11.00000 -1.50000 H22C 2 0.645865 0.468075 0.487059 11.00000 -1.50000 AFIX 0 C23 1 0.715800 0.820536 0.189883 11.00000 0.02855 0.02847 = 0.03537 0.02139 0.01525 0.01412 AFIX 13 H23 2 0.676128 0.885894 0.189788 11.00000 -1.20000 AFIX 0 C24 1 0.867232 0.896068 0.202285 11.00000 0.03321 0.04697 = 0.05677 0.03283 0.02087 0.00864 AFIX 137 H24A 2 0.909469 0.835413 0.205441 11.00000 -1.50000 H24B 2 0.909023 0.978089 0.269947 11.00000 -1.50000 H24C 2 0.878645 0.922306 0.139284 11.00000 -1.50000 AFIX 0 C25 1 0.644524 0.696438 0.078185 11.00000 0.04026 0.05213 = 0.02519 0.01834 0.01297 0.01991 AFIX 137 H25A 2 0.653616 0.728793 0.017945 11.00000 -1.50000 H25B 2 0.549652 0.649057 0.072328 11.00000 -1.50000 H25C 2 0.685464 0.633394 0.074013 11.00000 -1.50000 AFIX 0 C26 1 0.787709 0.900006 0.435452 11.00000 0.02403 0.02058 = 0.02749 0.00079 -0.00256 0.00439 AFIX 13 H26 2 0.881542 0.916729 0.435515 11.00000 -1.20000 AFIX 0 C27 1 0.761962 0.854112 0.531703 11.00000 0.06033 0.04615 = 0.02682 0.00618 -0.00138 0.00863 AFIX 137 H27A 2 0.823861 0.927280 0.600936 11.00000 -1.50000 H27B 2 0.775829 0.771893 0.521705 11.00000 -1.50000 H27C 2 0.669875 0.834074 0.533475 11.00000 -1.50000 AFIX 0 C28 1 0.780716 1.037918 0.454375 11.00000 0.05382 0.02309 = 0.04472 -0.00789 -0.00872 0.01398 AFIX 137 H28A 2 0.694413 1.029905 0.466017 11.00000 -1.50000 H28B 2 0.790434 1.061426 0.389962 11.00000 -1.50000 H28C 2 0.852881 1.109620 0.519109 11.00000 -1.50000 AFIX 0 NI1 4 0.668922 0.555234 0.279061 11.00000 0.01089 0.01240 = 0.02200 0.00551 0.00306 0.00360 P1 5 0.630205 0.342593 0.253689 11.00000 0.01494 0.01290 = 0.01860 0.00443 0.00278 0.00439 P2 5 0.676404 0.757489 0.301736 11.00000 0.01531 0.01352 = 0.02138 0.00589 0.00441 0.00546 HKLF 4 REM CGEL180207017_0m_a.res in P-1 REM R1 = 0.0334 for 4938 Fo > 4sig(Fo) and 0.0478 for all 6218 data REM 299 parameters refined using 0 restraints END WGHT 0.0432 0.0000 REM Highest difference peak 0.509, deepest hole -0.513, 1-sigma level 0.076 Q1 1 0.7911 0.6025 0.2997 11.00000 0.05 0.51 Q2 1 0.9010 0.7165 0.3456 11.00000 0.05 0.46 Q3 1 0.8609 0.6237 0.3604 11.00000 0.05 0.45 Q4 1 0.8664 0.6195 0.2351 11.00000 0.05 0.43 Q5 1 0.5766 0.5202 0.2640 11.00000 0.05 0.42 Q6 1 0.5428 0.2947 0.2349 11.00000 0.05 0.42 Q7 1 0.2252 0.4536 0.2061 11.00000 0.05 0.41 Q8 1 0.2492 0.5785 0.2177 11.00000 0.05 0.39 Q9 1 0.6563 0.3363 0.3292 11.00000 0.05 0.37 Q10 1 0.6669 0.6315 0.3269 11.00000 0.05 0.37 Q11 1 0.2118 0.3429 0.1889 11.00000 0.05 0.37 Q12 1 0.7082 0.7937 0.2485 11.00000 0.05 0.37 Q13 1 0.3136 0.3209 0.1937 11.00000 0.05 0.36 Q14 1 1.0043 0.6730 0.3474 11.00000 0.05 0.36 Q15 1 0.2621 0.6961 0.2336 11.00000 0.05 0.35 Q16 1 0.6423 0.5437 0.2061 11.00000 0.05 0.35 Q17 1 0.5944 0.7399 0.2992 11.00000 0.05 0.33 Q18 1 0.6806 0.2767 0.1071 11.00000 0.05 0.33 Q19 1 0.1425 0.3872 0.2320 11.00000 0.05 0.33 Q20 1 0.6373 0.2625 0.1948 11.00000 0.05 0.32 ; _shelx_res_checksum 92955 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 0.90490(2) 0.63643(3) 0.31180(2) 0.03600(9) Uani 1 1 d . . C1 C 0.47849(19) 0.4901(2) 0.24538(16) 0.0172(4) Uani 1 1 d . . C2 C 0.38822(19) 0.3434(2) 0.20821(16) 0.0167(4) Uani 1 1 d . . C3 C 0.2448(2) 0.2905(2) 0.17821(17) 0.0218(5) Uani 1 1 d . . C4 C 0.1732(2) 0.3856(2) 0.18802(18) 0.0248(5) Uani 1 1 d . . C5 C 0.2731(2) 0.5380(2) 0.22632(17) 0.0220(5) Uani 1 1 d . . C6 C 0.4153(2) 0.5830(2) 0.25211(16) 0.0188(4) Uani 1 1 d . . C7 C 0.4470(2) 0.2498(2) 0.20196(16) 0.0194(4) Uani 1 1 d . . C8 C 0.3675(2) 0.1082(2) 0.16894(18) 0.0263(5) Uani 1 1 d . . H8 H 0.4079 0.0482 0.1673 0.032 Uiso 1 1 calc R U C9 C 0.2271(2) 0.0571(2) 0.1383(2) 0.0325(6) Uani 1 1 d . . H9 H 0.1724 -0.0380 0.1147 0.039 Uiso 1 1 calc R U C10 C 0.1681(2) 0.1475(2) 0.14293(19) 0.0287(5) Uani 1 1 d . . H10 H 0.0736 0.1112 0.1216 0.034 Uiso 1 1 calc R U C11 C 0.5013(2) 0.7274(2) 0.28546(17) 0.0202(4) Uani 1 1 d . . C12 C 0.4479(2) 0.8224(2) 0.29370(19) 0.0281(5) Uani 1 1 d . . H12 H 0.5055 0.9163 0.3143 0.034 Uiso 1 1 calc R U C13 C 0.3089(2) 0.7782(3) 0.2714(2) 0.0337(6) Uani 1 1 d . . H13 H 0.2726 0.8424 0.2789 0.040 Uiso 1 1 calc R U C14 C 0.2231(2) 0.6371(3) 0.23749(19) 0.0302(5) Uani 1 1 d . . H14 H 0.1295 0.6082 0.2218 0.036 Uiso 1 1 calc R U C15 C 0.0932(2) 0.3680(3) 0.2748(2) 0.0338(6) Uani 1 1 d . . H15A H 0.0231 0.2741 0.2474 0.051 Uiso 1 1 calc R U H15B H 0.0526 0.4317 0.2868 0.051 Uiso 1 1 calc R U H15C H 0.1543 0.3872 0.3442 0.051 Uiso 1 1 calc R U C16 C 0.0722(2) 0.3417(3) 0.07394(19) 0.0384(6) Uani 1 1 d . . H16A H 0.1219 0.3579 0.0208 0.058 Uiso 1 1 calc R U H16B H 0.0209 0.3954 0.0823 0.058 Uiso 1 1 calc R U H16C H 0.0111 0.2444 0.0477 0.058 Uiso 1 1 calc R U C17 C 0.7094(2) 0.2662(2) 0.15476(18) 0.0222(5) Uani 1 1 d . . H17 H 0.8079 0.3248 0.1856 0.027 Uiso 1 1 calc R U C18 C 0.6683(3) 0.2783(3) 0.04369(19) 0.0333(6) Uani 1 1 d . . H18A H 0.7161 0.2454 -0.0053 0.050 Uiso 1 1 calc R U H18B H 0.6909 0.3741 0.0558 0.050 Uiso 1 1 calc R U H18C H 0.5719 0.2231 0.0102 0.050 Uiso 1 1 calc R U C19 C 0.6879(3) 0.1191(2) 0.1397(2) 0.0342(6) Uani 1 1 d . . H19A H 0.5935 0.0559 0.1031 0.051 Uiso 1 1 calc R U H19B H 0.7139 0.1151 0.2116 0.051 Uiso 1 1 calc R U H19C H 0.7426 0.0931 0.0947 0.051 Uiso 1 1 calc R U C20 C 0.6696(2) 0.3069(2) 0.38031(18) 0.0257(5) Uani 1 1 d . . H20 H 0.6280 0.2056 0.3594 0.031 Uiso 1 1 calc R U C21 C 0.8221(2) 0.3631(3) 0.43246(19) 0.0302(5) Uani 1 1 d . . H21A H 0.8656 0.4616 0.4498 0.045 Uiso 1 1 calc R U H21B H 0.8596 0.3173 0.3806 0.045 Uiso 1 1 calc R U H21C H 0.8372 0.3457 0.4999 0.045 Uiso 1 1 calc R U C22 C 0.6046(3) 0.3684(3) 0.4639(2) 0.0418(7) Uani 1 1 d . . H22A H 0.6182 0.3443 0.5279 0.063 Uiso 1 1 calc R U H22B H 0.5087 0.3318 0.4293 0.063 Uiso 1 1 calc R U H22C H 0.6459 0.4681 0.4871 0.063 Uiso 1 1 calc R U C23 C 0.7158(2) 0.8205(2) 0.18988(19) 0.0272(5) Uani 1 1 d . . H23 H 0.6761 0.8859 0.1898 0.033 Uiso 1 1 calc R U C24 C 0.8672(3) 0.8961(3) 0.2023(2) 0.0443(7) Uani 1 1 d . . H24A H 0.9095 0.8354 0.2054 0.066 Uiso 1 1 calc R U H24B H 0.9090 0.9781 0.2699 0.066 Uiso 1 1 calc R U H24C H 0.8786 0.9223 0.1393 0.066 Uiso 1 1 calc R U C25 C 0.6445(3) 0.6964(3) 0.07818(19) 0.0379(6) Uani 1 1 d . . H25A H 0.6536 0.7288 0.0179 0.057 Uiso 1 1 calc R U H25B H 0.5497 0.6491 0.0723 0.057 Uiso 1 1 calc R U H25C H 0.6855 0.6334 0.0740 0.057 Uiso 1 1 calc R U C26 C 0.7877(2) 0.9000(2) 0.43545(18) 0.0290(5) Uani 1 1 d . . H26 H 0.8815 0.9167 0.4355 0.035 Uiso 1 1 calc R U C27 C 0.7620(3) 0.8541(3) 0.5317(2) 0.0527(8) Uani 1 1 d . . H27A H 0.8239 0.9273 0.6009 0.079 Uiso 1 1 calc R U H27B H 0.7758 0.7719 0.5217 0.079 Uiso 1 1 calc R U H27C H 0.6699 0.8341 0.5335 0.079 Uiso 1 1 calc R U C28 C 0.7807(3) 1.0379(3) 0.4544(2) 0.0493(8) Uani 1 1 d . . H28A H 0.6944 1.0299 0.4660 0.074 Uiso 1 1 calc R U H28B H 0.7904 1.0614 0.3900 0.074 Uiso 1 1 calc R U H28C H 0.8529 1.1096 0.5191 0.074 Uiso 1 1 calc R U Ni1 Ni 0.66892(2) 0.55523(3) 0.27906(2) 0.01603(8) Uani 1 1 d . . P1 P 0.63020(5) 0.34259(5) 0.25369(4) 0.01665(12) Uani 1 1 d . . P2 P 0.67640(5) 0.75749(6) 0.30174(4) 0.01729(12) Uani 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.01330(12) 0.02346(13) 0.06630(19) 0.01426(12) 0.00748(11) 0.00649(9) C1 0.0145(10) 0.0177(11) 0.0158(10) 0.0043(8) 0.0043(8) 0.0050(8) C2 0.0131(10) 0.0180(11) 0.0126(9) 0.0032(8) 0.0022(8) 0.0026(8) C3 0.0148(10) 0.0233(12) 0.0184(10) 0.0027(9) 0.0051(8) 0.0032(9) C4 0.0121(10) 0.0297(13) 0.0261(11) 0.0046(10) 0.0053(9) 0.0072(9) C5 0.0165(10) 0.0288(12) 0.0207(11) 0.0078(9) 0.0071(9) 0.0107(9) C6 0.0169(10) 0.0224(11) 0.0154(10) 0.0047(8) 0.0048(8) 0.0085(9) C7 0.0179(10) 0.0167(11) 0.0175(10) 0.0046(8) 0.0042(8) 0.0030(8) C8 0.0220(11) 0.0198(12) 0.0288(12) 0.0052(9) 0.0059(10) 0.0042(9) C9 0.0264(12) 0.0157(11) 0.0357(13) 0.0010(10) 0.0057(11) -0.0033(9) C10 0.0141(11) 0.0256(13) 0.0301(12) 0.0016(10) 0.0042(9) -0.0004(9) C11 0.0191(10) 0.0221(11) 0.0201(10) 0.0064(9) 0.0056(9) 0.0108(9) C12 0.0304(13) 0.0237(12) 0.0348(13) 0.0111(10) 0.0124(11) 0.0153(10) C13 0.0305(13) 0.0370(15) 0.0445(15) 0.0139(12) 0.0157(11) 0.0254(12) C14 0.0216(12) 0.0384(15) 0.0340(13) 0.0111(11) 0.0114(10) 0.0174(11) C15 0.0209(12) 0.0352(15) 0.0384(14) 0.0077(11) 0.0137(11) 0.0080(10) C16 0.0240(13) 0.0464(17) 0.0298(13) 0.0029(12) -0.0019(11) 0.0124(12) C17 0.0194(11) 0.0203(11) 0.0251(11) 0.0047(9) 0.0048(9) 0.0104(9) C18 0.0424(15) 0.0387(15) 0.0260(12) 0.0137(11) 0.0156(11) 0.0220(12) C19 0.0433(15) 0.0233(13) 0.0356(13) 0.0044(10) 0.0104(12) 0.0199(11) C20 0.0246(11) 0.0235(12) 0.0235(11) 0.0105(9) 0.0020(9) 0.0053(9) C21 0.0299(13) 0.0322(14) 0.0283(12) 0.0118(10) 0.0026(10) 0.0151(11) C22 0.0304(14) 0.067(2) 0.0258(13) 0.0188(13) 0.0105(11) 0.0176(13) C23 0.0286(12) 0.0285(13) 0.0354(13) 0.0214(11) 0.0153(10) 0.0141(10) C24 0.0332(14) 0.0470(17) 0.0568(18) 0.0328(14) 0.0209(13) 0.0086(12) C25 0.0403(15) 0.0521(18) 0.0252(12) 0.0183(12) 0.0130(11) 0.0199(13) C26 0.0240(12) 0.0206(12) 0.0275(12) 0.0008(10) -0.0026(10) 0.0044(9) C27 0.060(2) 0.0462(19) 0.0268(14) 0.0062(13) -0.0014(14) 0.0086(15) C28 0.0538(18) 0.0231(14) 0.0447(16) -0.0079(12) -0.0087(14) 0.0140(13) Ni1 0.01089(13) 0.01240(14) 0.02200(14) 0.00551(10) 0.00306(10) 0.00360(10) P1 0.0149(3) 0.0129(3) 0.0186(3) 0.0044(2) 0.0028(2) 0.0044(2) P2 0.0153(3) 0.0135(3) 0.0214(3) 0.0059(2) 0.0044(2) 0.0055(2) 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C6 C1 C2 116.67(18) C6 C1 Ni1 121.78(15) C2 C1 Ni1 121.53(16) C7 C2 C3 118.98(19) C7 C2 C1 118.07(18) C3 C2 C1 123.0(2) C10 C3 C2 117.9(2) C10 C3 C4 119.80(19) C2 C3 C4 122.21(19) C5 C4 C3 112.28(18) C5 C4 C16 109.1(2) C3 C4 C16 109.83(19) C5 C4 C15 108.93(19) C3 C4 C15 107.6(2) C16 C4 C15 109.06(18) C14 C5 C6 118.6(2) C14 C5 C4 119.0(2) C6 C5 C4 122.4(2) C5 C6 C11 118.7(2) C5 C6 C1 123.4(2) C11 C6 C1 117.89(18) C8 C7 C2 121.5(2) C8 C7 P1 127.52(18) C2 C7 P1 110.75(15) C9 C8 C7 119.1(2) C9 C8 H8 120.4 C7 C8 H8 120.4 C10 C9 C8 119.9(2) C10 C9 H9 120.0 C8 C9 H9 120.0 C9 C10 C3 122.5(2) C9 C10 H10 118.8 C3 C10 H10 118.8 C12 C11 C6 121.1(2) C12 C11 P2 128.14(18) C6 C11 P2 110.61(16) C11 C12 C13 119.9(2) C11 C12 H12 120.0 C13 C12 H12 120.0 C12 C13 C14 119.7(2) C12 C13 H13 120.2 C14 C13 H13 120.2 C5 C14 C13 122.0(2) C5 C14 H14 119.0 C13 C14 H14 119.0 C4 C15 H15A 109.5 C4 C15 H15B 109.5 H15A C15 H15B 109.5 C4 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C4 C16 H16A 109.5 C4 C16 H16B 109.5 H16A C16 H16B 109.5 C4 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C18 C17 C19 111.77(19) C18 C17 P1 110.07(16) C19 C17 P1 115.70(17) C18 C17 H17 106.2 C19 C17 H17 106.2 P1 C17 H17 106.2 C17 C18 H18A 109.5 C17 C18 H18B 109.5 H18A C18 H18B 109.5 C17 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C17 C19 H19A 109.5 C17 C19 H19B 109.5 H19A C19 H19B 109.5 C17 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C22 C20 C21 110.88(19) C22 C20 P1 108.58(17) C21 C20 P1 112.79(16) C22 C20 H20 108.2 C21 C20 H20 108.2 P1 C20 H20 108.2 C20 C21 H21A 109.5 C20 C21 H21B 109.5 H21A C21 H21B 109.5 C20 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C20 C22 H22A 109.5 C20 C22 H22B 109.5 H22A C22 H22B 109.5 C20 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C24 C23 C25 110.6(2) C24 C23 P2 114.91(16) C25 C23 P2 108.06(16) C24 C23 H23 107.7 C25 C23 H23 107.7 P2 C23 H23 107.7 C23 C24 H24A 109.5 C23 C24 H24B 109.5 H24A C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C23 C25 H25A 109.5 C23 C25 H25B 109.5 H25A C25 H25B 109.5 C23 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C27 C26 C28 110.9(2) C27 C26 P2 109.97(17) C28 C26 P2 115.36(16) C27 C26 H26 106.7 C28 C26 H26 106.7 P2 C26 H26 106.7 C26 C27 H27A 109.5 C26 C27 H27B 109.5 H27A C27 H27B 109.5 C26 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C26 C28 H28A 109.5 C26 C28 H28B 109.5 H28A C28 H28B 109.5 C26 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C1 Ni1 P2 85.95(7) C1 Ni1 P1 85.80(7) P2 Ni1 P1 171.70(2) C1 Ni1 Br1 177.08(6) P2 Ni1 Br1 93.382(17) P1 Ni1 Br1 94.901(18) C7 P1 C17 110.61(10) C7 P1 C20 103.34(10) C17 P1 C20 107.33(11) C7 P1 Ni1 103.18(7) C17 P1 Ni1 115.10(7) C20 P1 Ni1 116.53(8) C11 P2 C26 111.08(11) C11 P2 C23 102.16(10) C26 P2 C23 107.18(11) C11 P2 Ni1 103.40(7) C26 P2 Ni1 116.29(8) C23 P2 Ni1 115.76(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 Ni1 2.3390(3) C1 C6 1.438(3) C1 C2 1.446(3) C1 Ni1 1.8817(19) C2 C7 1.408(3) C2 C3 1.412(3) C3 C10 1.389(3) C3 C4 1.528(3) C4 C5 1.518(3) C4 C16 1.543(3) C4 C15 1.544(3) C5 C14 1.388(3) C5 C6 1.409(3) C6 C11 1.421(3) C7 C8 1.383(3) C7 P1 1.803(2) C8 C9 1.383(3) C8 H8 0.9300 C9 C10 1.379(4) C9 H9 0.9300 C10 H10 0.9300 C11 C12 1.378(3) C11 P2 1.800(2) C12 C13 1.379(3) C12 H12 0.9300 C13 C14 1.391(3) C13 H13 0.9300 C14 H14 0.9300 C15 H15A 0.9600 C15 H15B 0.9600 C15 H15C 0.9600 C16 H16A 0.9600 C16 H16B 0.9600 C16 H16C 0.9600 C17 C18 1.515(3) C17 C19 1.516(3) C17 P1 1.837(2) C17 H17 0.9800 C18 H18A 0.9600 C18 H18B 0.9600 C18 H18C 0.9600 C19 H19A 0.9600 C19 H19B 0.9600 C19 H19C 0.9600 C20 C22 1.522(4) C20 C21 1.523(3) C20 P1 1.841(2) C20 H20 0.9800 C21 H21A 0.9600 C21 H21B 0.9600 C21 H21C 0.9600 C22 H22A 0.9600 C22 H22B 0.9600 C22 H22C 0.9600 C23 C24 1.523(3) C23 C25 1.526(3) C23 P2 1.837(2) C23 H23 0.9800 C24 H24A 0.9600 C24 H24B 0.9600 C24 H24C 0.9600 C25 H25A 0.9600 C25 H25B 0.9600 C25 H25C 0.9600 C26 C27 1.515(4) C26 C28 1.518(4) C26 P2 1.837(2) C26 H26 0.9800 C27 H27A 0.9600 C27 H27B 0.9600 C27 H27C 0.9600 C28 H28A 0.9600 C28 H28B 0.9600 C28 H28C 0.9600 Ni1 P2 2.1568(6) Ni1 P1 2.1609(6)