data_Compound6 
 
_audit_creation_method            SHELXL-97 
_audit_update_record 
; 
? 
; 
 
_chemical_name_systematic 
; 
? 
; 
 
_chemical_name_common            ? 
_chemical_melting_point          ? 
_chemical_formula_moiety         'C88 H64 Br2 Ni2 P4' 
_chemical_formula_sum 
 'C88 H64 Br2 Ni2 P4' 
_chemical_formula_structural     ? 
_chemical_formula_weight          1522.51 
 
_chemical_absolute_configuration ad 
_chemical_formula_iupac          ? 
_chemical_formula_analytical     ? 
_chemical_compound_source        ? 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 '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' 
 'P'  'P'   0.2955   0.4335 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ni'  'Ni'  -3.0029   0.5091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Br'  'Br'  -0.6763   1.2805 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting           'Tetragonal' 
_symmetry_space_group_name_H-M   'P4(3)2(1)2 ' 
_symmetry_space_group_name_Hall  'P 4nw 2abw ' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z+1/2' 
 '-y+1/2, x+1/2, z+3/4' 
 'y+1/2, -x+1/2, z+1/4' 
 '-x+1/2, y+1/2, -z+3/4' 
 'x+1/2, -y+1/2, -z+1/4' 
 'y, x, -z' 
 '-y, -x, -z+1/2' 
 
_cell_length_a                    13.9150(2) 
_cell_length_b                    13.9150(2) 
_cell_length_c                    35.8750(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      6946.4(2) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used    9973 
_cell_measurement_theta_min        3.41 
_cell_measurement_theta_max       67.23 
_exptl_crystal_description       'block' 
_exptl_crystal_colour            'red' 
_exptl_crystal_size_max          0.296 
_exptl_crystal_size_mid          0.268 
_exptl_crystal_size_min          0.209 
_exptl_crystal_density_meas      ? 
_exptl_crystal_density_diffrn     1.456 
_exptl_crystal_density_method    'not measured' 
_exptl_crystal_F_000              3112 
_exptl_crystal_id                Compound6
 
_exptl_crystal_preparation 
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 -1 2) scattering 
planes roughly normal to the spindle axis. 
; 
_exptl_absorpt_coefficient_mu     3.259 
_exptl_absorpt_correction_type   'integration' 
_exptl_absorpt_correction_T_min  0.5357 
_exptl_absorpt_correction_T_max  0.6541 
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)' 
 
_exptl_special_details 
; 
One distinct cell was identified using APEX2 (Bruker, 2010).  Six 
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2005) then corrected for absorption by 
integration using SHELXTL/XPREP V2005/2 (Bruker, 2005) before using 
SADABS (Bruker, 2005) to sort, merge, and scale 
the combined data.  No decay correction was applied. 
; 
 
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_wavelength_id  Compound6
_diffrn_radiation_type           'CuK\a' 
_diffrn_radiation_source         'fine-focus sealed tube' 
_diffrn_radiation_monochromator  'graphite' 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD' 
_diffrn_measurement_method       'profile data from \f and \w scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number            25322 
 
_diffrn_reflns_av_R_equivalents   0.0356 
_diffrn_reflns_av_sigmaI/netI     0.0299 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -42 
_diffrn_reflns_limit_l_max        41 
_diffrn_reflns_theta_min          3.41 
_diffrn_reflns_theta_max          67.77 
_reflns_number_total              6205 
_reflns_number_gt                 5930 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)' 
 
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)' 
_computing_data_reduction 
; 
SAINT V7.68A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
; 
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)' 
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)' 
_computing_molecular_graphics 
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
; 
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)' 
 
_refine_special_details 
; 
Structure was phased by direct methods (Sheldrick, 2008).  Systematic 
conditions suggested the ambiguous space group.  The space group 
choice was confirmed by successful convergence of the 
full-matrix least-squares refinement on F^2^.  The highest peaks in 
the final difference Fourier map were in the vicinity of atoms Br1 and Ni1; 
the final map had no other significant features.  A final analysis of 
variance between observed and calculated structure factors showed little 
dependence on amplitude and resolution. 
; 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+1.0960P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment    noref 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 'Flack (1983),  2575 Friedels' 
_refine_ls_abs_structure_Flack    0.012(18) 
_refine_ls_number_reflns          6205 
_refine_ls_number_parameters      464 
_refine_ls_number_restraints      181 
_refine_ls_R_factor_all           0.0356 
_refine_ls_R_factor_gt            0.0340 
_refine_ls_wR_factor_ref          0.0923 
_refine_ls_wR_factor_gt           0.0911 
_refine_ls_goodness_of_fit_ref    1.063 
_refine_ls_restrained_S_all       1.068 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ni1 Ni -0.07508(3) 1.09143(3) 0.000285(12) 0.02991(12) Uani 1 1 d . A . 
Br1 Br -0.00883(3) 0.98766(2) 0.050875(8) 0.04735(11) Uani 1 1 d . . . 
P1 P -0.04589(4) 1.24702(4) 0.001067(19) 0.02918(14) Uani 1 1 d . . . 
P2 P -0.23318(4) 1.10465(4) 0.002115(18) 0.02752(13) Uani 1 1 d D . . 
C1 C 0.0707(2) 1.2857(2) -0.01897(8) 0.0354(6) Uani 1 1 d . . . 
C2 C 0.1261(2) 1.2166(3) -0.03730(8) 0.0451(7) Uani 1 1 d . . . 
H2 H 0.1015 1.1533 -0.0402 0.054 Uiso 1 1 calc R . . 
C3 C 0.2157(2) 1.2386(3) -0.05121(9) 0.0502(8) Uani 1 1 d . . . 
H3 H 0.2528 1.1904 -0.0632 0.060 Uiso 1 1 calc R . . 
C4 C 0.2512(3) 1.3298(3) -0.04781(9) 0.0553(9) Uani 1 1 d . . . 
H4 H 0.3123 1.3456 -0.0579 0.066 Uiso 1 1 calc R . . 
C5 C 0.1989(3) 1.3972(3) -0.02996(13) 0.0684(11) Uani 1 1 d . . . 
H5 H 0.2239 1.4604 -0.0274 0.082 Uiso 1 1 calc R . . 
C6 C 0.1083(3) 1.3756(3) -0.01509(11) 0.0574(9) Uani 1 1 d . . . 
H6 H 0.0729 1.4238 -0.0023 0.069 Uiso 1 1 calc R . . 
C7 C -0.0488(2) 1.3097(2) 0.04608(8) 0.0342(6) Uani 1 1 d . . . 
C8 C -0.0410(2) 1.2541(3) 0.07787(8) 0.0433(7) Uani 1 1 d . . . 
H8 H -0.0354 1.1863 0.0759 0.052 Uiso 1 1 calc R . . 
C9 C -0.0413(3) 1.2974(4) 0.11275(9) 0.0604(10) Uani 1 1 d . . . 
H9 H -0.0362 1.2590 0.1346 0.073 Uiso 1 1 calc R . . 
C10 C -0.0489(3) 1.3956(4) 0.11588(10) 0.0622(11) Uani 1 1 d . . . 
H10 H -0.0480 1.4251 0.1398 0.075 Uiso 1 1 calc R . . 
C11 C -0.0578(3) 1.4509(3) 0.08453(11) 0.0538(9) Uani 1 1 d . . . 
H11 H -0.0643 1.5186 0.0868 0.065 Uiso 1 1 calc R . . 
C12 C -0.0575(2) 1.4088(2) 0.04944(9) 0.0416(7) Uani 1 1 d . . . 
H12 H -0.0631 1.4477 0.0278 0.050 Uiso 1 1 calc R . . 
C13 C -0.1361(2) 1.30560(19) -0.02886(7) 0.0296(5) Uani 1 1 d . . . 
C14 C -0.1105(2) 1.3177(2) -0.06697(8) 0.0385(6) Uani 1 1 d . . . 
H14 H -0.0469 1.3034 -0.0748 0.046 Uiso 1 1 calc R . . 
C15 C -0.1760(2) 1.3494(2) -0.09231(8) 0.0423(7) Uani 1 1 d . . . 
H15 H -0.1578 1.3557 -0.1177 0.051 Uiso 1 1 calc R . . 
C16 C -0.2710(3) 1.3731(2) -0.08145(8) 0.0399(7) Uani 1 1 d . . . 
C17 C -0.3408(3) 1.4070(2) -0.10734(9) 0.0493(8) Uani 1 1 d . . . 
H17 H -0.3240 1.4129 -0.1329 0.059 Uiso 1 1 calc R . . 
C18 C -0.4304(3) 1.4307(3) -0.09616(10) 0.0537(8) Uani 1 1 d . . . 
H18 H -0.4758 1.4533 -0.1139 0.064 Uiso 1 1 calc R . . 
C19 C -0.4567(3) 1.4224(2) -0.05896(10) 0.0529(9) Uani 1 1 d . . . 
H19 H -0.5195 1.4407 -0.0514 0.063 Uiso 1 1 calc R . . 
C20 C -0.3925(2) 1.3880(2) -0.03290(8) 0.0426(6) Uani 1 1 d . . . 
H20 H -0.4121 1.3815 -0.0077 0.051 Uiso 1 1 calc R . . 
C21 C -0.2978(2) 1.3622(2) -0.04333(8) 0.0349(6) Uani 1 1 d . . . 
C22 C -0.2295(2) 1.32364(19) -0.01738(7) 0.0299(5) Uani 1 1 d . A . 
C23 C -0.26222(18) 1.29923(19) 0.02166(7) 0.0291(5) Uani 1 1 d . . . 
C24 C -0.2838(2) 1.3747(2) 0.04759(7) 0.0340(6) Uani 1 1 d . A . 
C25 C -0.2773(2) 1.4736(2) 0.03799(9) 0.0447(7) Uani 1 1 d . . . 
H25 H -0.2585 1.4913 0.0135 0.054 Uiso 1 1 calc R A . 
C26 C -0.2976(3) 1.5433(3) 0.06349(10) 0.0527(8) Uani 1 1 d . A . 
H26 H -0.2925 1.6090 0.0565 0.063 Uiso 1 1 calc R . . 
C27 C -0.3256(3) 1.5195(3) 0.09971(11) 0.0597(10) Uani 1 1 d . . . 
H27 H -0.3402 1.5688 0.1171 0.072 Uiso 1 1 calc R A . 
C28 C -0.3322(3) 1.4261(3) 0.11010(9) 0.0562(10) Uani 1 1 d . A . 
H28 H -0.3510 1.4107 0.1348 0.067 Uiso 1 1 calc R . . 
C29 C -0.3113(2) 1.3507(3) 0.08453(8) 0.0421(7) Uani 1 1 d . . . 
C30 C -0.3152(3) 1.2542(3) 0.09491(8) 0.0489(8) Uani 1 1 d . A . 
H30 H -0.3325 1.2378 0.1197 0.059 Uiso 1 1 calc R . . 
C31 C -0.2946(2) 1.1828(3) 0.07004(8) 0.0408(7) Uani 1 1 d . . . 
H31 H -0.2968 1.1177 0.0779 0.049 Uiso 1 1 calc R A . 
C32 C -0.27013(19) 1.2044(2) 0.03258(7) 0.0296(5) Uani 1 1 d . A . 
C33 C -0.2998(2) 1.12374(19) -0.04135(7) 0.0304(6) Uani 1 1 d . A . 
C34 C -0.3949(2) 1.1546(2) -0.04204(8) 0.0371(6) Uani 1 1 d . . . 
H34 H -0.4269 1.1680 -0.0192 0.045 Uiso 1 1 calc R A . 
C35 C -0.4431(2) 1.1659(2) -0.07507(9) 0.0429(7) Uani 1 1 d . A . 
H35 H -0.5078 1.1877 -0.0751 0.052 Uiso 1 1 calc R . . 
C36 C -0.3975(3) 1.1455(3) -0.10829(9) 0.0489(8) Uani 1 1 d . . . 
H36 H -0.4308 1.1530 -0.1312 0.059 Uiso 1 1 calc R A . 
C37 C -0.3037(3) 1.1142(3) -0.10815(9) 0.0534(9) Uani 1 1 d . A . 
H37 H -0.2726 1.0998 -0.1310 0.064 Uiso 1 1 calc R . . 
C38 C -0.2543(2) 1.1035(2) -0.07482(7) 0.0410(7) Uani 1 1 d . . . 
H38 H -0.1894 1.0823 -0.0749 0.049 Uiso 1 1 calc R A . 
C39 C -0.2972(2) 0.99974(18) 0.02094(9) 0.0353(10) Uani 0.767(7) 1 d PGDU A 1 
C40 C -0.3917(2) 1.0020(2) 0.03351(11) 0.0478(11) Uani 0.767(7) 1 d PGU A 1 
H40 H -0.4254 1.0613 0.0346 0.057 Uiso 0.767(7) 1 calc PR A 1 
C41 C -0.43687(19) 0.9175(3) 0.04446(11) 0.0580(13) Uani 0.767(7) 1 d PGU A 1 
H41 H -0.5014 0.9191 0.0530 0.070 Uiso 0.767(7) 1 calc PR A 1 
C42 C -0.3876(3) 0.8307(2) 0.04285(10) 0.0581(13) Uani 0.767(7) 1 d PGU A 1 
H42 H -0.4184 0.7730 0.0503 0.070 Uiso 0.767(7) 1 calc PR A 1 
C43 C -0.2931(3) 0.82845(17) 0.03029(14) 0.0689(14) Uani 0.767(7) 1 d PGU A 1 
H43 H -0.2594 0.7691 0.0292 0.083 Uiso 0.767(7) 1 calc PR A 1 
C44 C -0.2479(2) 0.9130(2) 0.01933(13) 0.0574(12) Uani 0.767(7) 1 d PGU A 1 
H44 H -0.1834 0.9114 0.0107 0.069 Uiso 0.767(7) 1 calc PR A 1 
C39B C -0.2910(8) 0.9940(6) 0.0213(3) 0.044(3) Uani 0.233(7) 1 d PGDU A 2 
C40B C -0.3890(8) 0.9776(9) 0.0171(4) 0.054(2) Uani 0.233(7) 1 d PGU A 2 
H40A H -0.4284 1.0246 0.0055 0.065 Uiso 0.233(7) 1 calc PR A 2 
C41B C -0.4292(7) 0.8923(10) 0.0299(4) 0.056(2) Uani 0.233(7) 1 d PGU A 2 
H41A H -0.4961 0.8810 0.0270 0.068 Uiso 0.233(7) 1 calc PR A 2 
C42B C -0.3715(9) 0.8235(7) 0.0469(4) 0.057(2) Uani 0.233(7) 1 d PGU A 2 
H42A H -0.3990 0.7652 0.0556 0.068 Uiso 0.233(7) 1 calc PR A 2 
C43B C -0.2736(8) 0.8400(7) 0.0511(4) 0.057(2) Uani 0.233(7) 1 d PGU A 2 
H43A H -0.2342 0.7929 0.0627 0.068 Uiso 0.233(7) 1 calc PR A 2 
C44B C -0.2334(6) 0.9252(8) 0.0383(4) 0.050(2) Uani 0.233(7) 1 d PGU A 2 
H44A H -0.1664 0.9365 0.0412 0.060 Uiso 0.233(7) 1 calc PR A 2 
 
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 
Ni1 0.0278(2) 0.0301(2) 0.0318(2) 0.0007(2) 0.00119(19) 0.00009(15) 
Br1 0.0621(2) 0.0485(2) 0.03151(16) 0.01051(12) 0.01311(12) 0.02113(14) 
P1 0.0276(3) 0.0309(3) 0.0291(3) -0.0003(3) 0.0021(3) -0.0032(2) 
P2 0.0270(3) 0.0290(3) 0.0266(3) 0.0029(3) -0.0002(3) -0.0030(2) 
C1 0.0287(13) 0.0428(16) 0.0346(14) 0.0023(12) 0.0000(11) -0.0045(11) 
C2 0.0439(18) 0.0498(19) 0.0418(16) -0.0040(13) 0.0088(13) -0.0060(14) 
C3 0.0421(18) 0.066(2) 0.0427(15) 0.0018(15) 0.0120(13) 0.0025(15) 
C4 0.0384(17) 0.079(3) 0.0483(17) 0.0024(17) 0.0104(14) -0.0123(17) 
C5 0.049(2) 0.064(2) 0.092(3) -0.013(2) 0.021(2) -0.0224(19) 
C6 0.0483(19) 0.045(2) 0.079(2) -0.0114(17) 0.0248(18) -0.0119(15) 
C7 0.0251(13) 0.0441(16) 0.0334(14) -0.0067(12) -0.0001(10) -0.0028(11) 
C8 0.0368(16) 0.058(2) 0.0352(14) -0.0003(14) -0.0028(12) 0.0026(14) 
C9 0.056(2) 0.095(3) 0.0302(15) -0.0036(17) -0.0062(15) 0.007(2) 
C10 0.048(2) 0.092(3) 0.0465(19) -0.033(2) -0.0057(15) -0.0004(19) 
C11 0.0400(17) 0.057(2) 0.064(2) -0.0264(18) -0.0010(15) -0.0022(15) 
C12 0.0347(16) 0.0446(17) 0.0455(16) -0.0098(14) -0.0003(13) -0.0059(12) 
C13 0.0341(14) 0.0270(13) 0.0275(12) 0.0014(9) -0.0001(10) -0.0063(10) 
C14 0.0420(16) 0.0391(16) 0.0345(14) 0.0004(12) 0.0031(12) -0.0078(13) 
C15 0.0568(19) 0.0430(17) 0.0271(13) 0.0059(12) -0.0004(12) -0.0113(14) 
C16 0.0539(19) 0.0331(15) 0.0327(13) 0.0093(11) -0.0083(13) -0.0079(13) 
C17 0.067(2) 0.0408(18) 0.0403(16) 0.0114(13) -0.0126(16) -0.0068(16) 
C18 0.066(2) 0.0432(19) 0.0524(18) 0.0087(15) -0.0239(17) 0.0043(14) 
C19 0.049(2) 0.0449(19) 0.065(2) 0.0006(15) -0.0145(16) 0.0089(15) 
C20 0.0460(18) 0.0397(17) 0.0422(14) -0.0014(13) -0.0089(13) 0.0062(12) 
C21 0.0415(16) 0.0261(14) 0.0370(14) 0.0030(11) -0.0038(12) -0.0040(11) 
C22 0.0352(14) 0.0245(12) 0.0300(12) -0.0005(10) -0.0025(11) -0.0049(10) 
C23 0.0231(12) 0.0346(14) 0.0296(12) 0.0003(10) -0.0015(10) -0.0001(10) 
C24 0.0265(13) 0.0420(16) 0.0336(13) -0.0051(12) -0.0011(11) 0.0038(11) 
C25 0.0433(17) 0.0404(17) 0.0503(17) -0.0080(14) -0.0043(14) 0.0045(13) 
C26 0.053(2) 0.0435(19) 0.062(2) -0.0147(16) -0.0057(16) 0.0108(15) 
C27 0.052(2) 0.063(2) 0.064(2) -0.0300(19) -0.0094(17) 0.0201(17) 
C28 0.052(2) 0.080(3) 0.0364(16) -0.0160(16) 0.0051(14) 0.0148(19) 
C29 0.0356(15) 0.0559(19) 0.0347(14) -0.0083(13) -0.0006(11) 0.0081(14) 
C30 0.0504(19) 0.071(2) 0.0254(13) -0.0015(14) 0.0077(12) 0.0016(16) 
C31 0.0426(17) 0.0490(18) 0.0307(14) 0.0049(12) 0.0042(12) 0.0010(13) 
C32 0.0225(12) 0.0391(14) 0.0274(12) -0.0007(10) 0.0015(10) 0.0004(10) 
C33 0.0360(14) 0.0254(13) 0.0298(13) 0.0013(10) -0.0054(10) -0.0041(10) 
C34 0.0336(14) 0.0378(16) 0.0399(15) -0.0015(12) 0.0006(11) -0.0042(12) 
C35 0.0397(16) 0.0411(17) 0.0480(17) 0.0028(14) -0.0140(13) -0.0018(13) 
C36 0.055(2) 0.0514(19) 0.0400(16) 0.0011(14) -0.0188(14) 0.0040(16) 
C37 0.061(2) 0.067(2) 0.0324(15) -0.0074(15) -0.0085(14) 0.0122(18) 
C38 0.0435(17) 0.0497(18) 0.0298(13) -0.0025(12) -0.0022(12) 0.0085(14) 
C39 0.036(2) 0.036(2) 0.0335(18) 0.0077(17) -0.0048(16) -0.0088(17) 
C40 0.0384(19) 0.065(3) 0.040(2) 0.013(2) -0.0025(18) -0.0138(19) 
C41 0.054(2) 0.083(3) 0.038(2) 0.015(2) -0.0022(19) -0.032(2) 
C42 0.070(3) 0.060(3) 0.044(2) 0.013(2) -0.009(2) -0.034(2) 
C43 0.076(3) 0.046(2) 0.085(3) 0.017(2) -0.008(3) -0.018(2) 
C44 0.053(2) 0.040(2) 0.079(3) 0.009(2) 0.001(2) -0.0071(19) 
C39B 0.039(4) 0.045(4) 0.047(5) 0.011(4) -0.004(4) -0.012(4) 
C40B 0.048(4) 0.063(5) 0.052(5) 0.018(4) -0.007(4) -0.016(4) 
C41B 0.055(4) 0.066(5) 0.049(5) 0.014(4) -0.012(4) -0.024(4) 
C42B 0.062(5) 0.056(4) 0.053(4) 0.014(4) -0.006(4) -0.018(4) 
C43B 0.059(5) 0.048(4) 0.064(5) 0.021(4) -0.007(4) -0.015(4) 
C44B 0.046(4) 0.042(4) 0.061(5) 0.018(4) -0.004(4) -0.013(4) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Ni1 P1 2.2030(7) . ? 
Ni1 P2 2.2087(7) . ? 
Ni1 Br1 2.4651(5) 7_465 ? 
Ni1 Br1 2.4958(5) . ? 
Br1 Ni1 2.4652(5) 7_465 ? 
P1 C7 1.836(3) . ? 
P1 C13 1.842(3) . ? 
P1 C1 1.854(3) . ? 
P2 C33 1.834(3) . ? 
P2 C32 1.840(3) . ? 
P2 C39 1.839(2) . ? 
P2 C39B 1.869(6) . ? 
C1 C6 1.363(5) . ? 
C1 C2 1.397(5) . ? 
C2 C3 1.378(5) . ? 
C2 H2 0.9500 . ? 
C3 C4 1.368(5) . ? 
C3 H3 0.9500 . ? 
C4 C5 1.348(6) . ? 
C4 H4 0.9500 . ? 
C5 C6 1.402(5) . ? 
C5 H5 0.9500 . ? 
C6 H6 0.9500 . ? 
C7 C8 1.382(4) . ? 
C7 C12 1.389(5) . ? 
C8 C9 1.389(5) . ? 
C8 H8 0.9500 . ? 
C9 C10 1.376(7) . ? 
C9 H9 0.9500 . ? 
C10 C11 1.368(6) . ? 
C10 H10 0.9500 . ? 
C11 C12 1.389(5) . ? 
C11 H11 0.9500 . ? 
C12 H12 0.9500 . ? 
C13 C22 1.386(4) . ? 
C13 C14 1.423(4) . ? 
C14 C15 1.361(5) . ? 
C14 H14 0.9500 . ? 
C15 C16 1.416(5) . ? 
C15 H15 0.9500 . ? 
C16 C21 1.426(4) . ? 
C16 C17 1.424(5) . ? 
C17 C18 1.352(6) . ? 
C17 H17 0.9500 . ? 
C18 C19 1.389(5) . ? 
C18 H18 0.9500 . ? 
C19 C20 1.379(4) . ? 
C19 H19 0.9500 . ? 
C20 C21 1.416(4) . ? 
C20 H20 0.9500 . ? 
C21 C22 1.435(4) . ? 
C22 C23 1.511(4) . ? 
C23 C32 1.381(4) . ? 
C23 C24 1.435(4) . ? 
C24 C29 1.419(4) . ? 
C24 C25 1.421(5) . ? 
C25 C26 1.364(5) . ? 
C25 H25 0.9500 . ? 
C26 C27 1.397(6) . ? 
C26 H26 0.9500 . ? 
C27 C28 1.354(6) . ? 
C27 H27 0.9500 . ? 
C28 C29 1.424(5) . ? 
C28 H28 0.9500 . ? 
C29 C30 1.395(5) . ? 
C30 C31 1.366(5) . ? 
C30 H30 0.9500 . ? 
C31 C32 1.419(4) . ? 
C31 H31 0.9500 . ? 
C33 C34 1.390(4) . ? 
C33 C38 1.387(4) . ? 
C34 C35 1.371(4) . ? 
C34 H34 0.9500 . ? 
C35 C36 1.380(5) . ? 
C35 H35 0.9500 . ? 
C36 C37 1.375(5) . ? 
C36 H36 0.9500 . ? 
C37 C38 1.387(4) . ? 
C37 H37 0.9500 . ? 
C38 H38 0.9500 . ? 
C39 C40 1.3900 . ? 
C39 C44 1.3900 . ? 
C40 C41 1.3900 . ? 
C40 H40 0.9500 . ? 
C41 C42 1.3900 . ? 
C41 H41 0.9500 . ? 
C42 C43 1.3900 . ? 
C42 H42 0.9500 . ? 
C43 C44 1.3900 . ? 
C43 H43 0.9500 . ? 
C44 H44 0.9500 . ? 
C39B C40B 1.3900 . ? 
C39B C44B 1.3900 . ? 
C40B C41B 1.3900 . ? 
C40B H40A 0.9500 . ? 
C41B C42B 1.3900 . ? 
C41B H41A 0.9500 . ? 
C42B C43B 1.3900 . ? 
C42B H42A 0.9500 . ? 
C43B C44B 1.3900 . ? 
C43B H43A 0.9500 . ? 
C44B H44A 0.9500 . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
P1 Ni1 P2 95.82(3) . . ? 
P1 Ni1 Br1 120.02(3) . 7_465 ? 
P2 Ni1 Br1 114.96(3) . 7_465 ? 
P1 Ni1 Br1 119.42(3) . . ? 
P2 Ni1 Br1 113.24(3) . . ? 
Br1 Ni1 Br1 94.770(17) 7_465 . ? 
Ni1 Br1 Ni1 82.675(16) 7_465 . ? 
C7 P1 C13 106.69(13) . . ? 
C7 P1 C1 102.84(13) . . ? 
C13 P1 C1 104.01(12) . . ? 
C7 P1 Ni1 118.31(10) . . ? 
C13 P1 Ni1 107.56(9) . . ? 
C1 P1 Ni1 116.20(10) . . ? 
C33 P2 C32 104.74(12) . . ? 
C33 P2 C39 100.50(13) . . ? 
C32 P2 C39 104.20(14) . . ? 
C33 P2 C39B 102.4(4) . . ? 
C32 P2 C39B 106.4(4) . . ? 
C33 P2 Ni1 119.39(10) . . ? 
C32 P2 Ni1 111.03(9) . . ? 
C39 P2 Ni1 115.31(11) . . ? 
C39B P2 Ni1 111.8(4) . . ? 
C6 C1 C2 117.9(3) . . ? 
C6 C1 P1 124.2(2) . . ? 
C2 C1 P1 117.7(2) . . ? 
C3 C2 C1 121.1(3) . . ? 
C3 C2 H2 119.4 . . ? 
C1 C2 H2 119.4 . . ? 
C4 C3 C2 120.1(3) . . ? 
C4 C3 H3 119.9 . . ? 
C2 C3 H3 119.9 . . ? 
C5 C4 C3 119.5(3) . . ? 
C5 C4 H4 120.3 . . ? 
C3 C4 H4 120.3 . . ? 
C4 C5 C6 121.2(4) . . ? 
C4 C5 H5 119.4 . . ? 
C6 C5 H5 119.4 . . ? 
C1 C6 C5 120.2(4) . . ? 
C1 C6 H6 119.9 . . ? 
C5 C6 H6 119.9 . . ? 
C8 C7 C12 119.4(3) . . ? 
C8 C7 P1 117.2(2) . . ? 
C12 C7 P1 123.4(2) . . ? 
C7 C8 C9 120.0(3) . . ? 
C7 C8 H8 120.0 . . ? 
C9 C8 H8 120.0 . . ? 
C10 C9 C8 120.3(4) . . ? 
C10 C9 H9 119.8 . . ? 
C8 C9 H9 119.8 . . ? 
C11 C10 C9 119.9(3) . . ? 
C11 C10 H10 120.1 . . ? 
C9 C10 H10 120.1 . . ? 
C10 C11 C12 120.5(4) . . ? 
C10 C11 H11 119.7 . . ? 
C12 C11 H11 119.7 . . ? 
C7 C12 C11 119.8(3) . . ? 
C7 C12 H12 120.1 . . ? 
C11 C12 H12 120.1 . . ? 
C22 C13 C14 119.9(3) . . ? 
C22 C13 P1 123.1(2) . . ? 
C14 C13 P1 116.2(2) . . ? 
C15 C14 C13 120.8(3) . . ? 
C15 C14 H14 119.6 . . ? 
C13 C14 H14 119.6 . . ? 
C14 C15 C16 121.1(3) . . ? 
C14 C15 H15 119.5 . . ? 
C16 C15 H15 119.5 . . ? 
C15 C16 C21 118.9(3) . . ? 
C15 C16 C17 122.3(3) . . ? 
C21 C16 C17 118.8(3) . . ? 
C18 C17 C16 121.1(3) . . ? 
C18 C17 H17 119.4 . . ? 
C16 C17 H17 119.4 . . ? 
C17 C18 C19 120.5(3) . . ? 
C17 C18 H18 119.7 . . ? 
C19 C18 H18 119.7 . . ? 
C20 C19 C18 120.7(3) . . ? 
C20 C19 H19 119.7 . . ? 
C18 C19 H19 119.7 . . ? 
C19 C20 C21 120.8(3) . . ? 
C19 C20 H20 119.6 . . ? 
C21 C20 H20 119.6 . . ? 
C20 C21 C16 118.1(3) . . ? 
C20 C21 C22 122.7(3) . . ? 
C16 C21 C22 119.2(3) . . ? 
C13 C22 C21 119.7(2) . . ? 
C13 C22 C23 121.1(2) . . ? 
C21 C22 C23 119.1(2) . . ? 
C32 C23 C24 119.9(2) . . ? 
C32 C23 C22 120.1(2) . . ? 
C24 C23 C22 119.9(2) . . ? 
C29 C24 C25 118.1(3) . . ? 
C29 C24 C23 119.3(3) . . ? 
C25 C24 C23 122.6(3) . . ? 
C26 C25 C24 120.9(3) . . ? 
C26 C25 H25 119.6 . . ? 
C24 C25 H25 119.6 . . ? 
C25 C26 C27 120.8(4) . . ? 
C25 C26 H26 119.6 . . ? 
C27 C26 H26 119.6 . . ? 
C28 C27 C26 120.2(3) . . ? 
C28 C27 H27 119.9 . . ? 
C26 C27 H27 119.9 . . ? 
C27 C28 C29 121.1(3) . . ? 
C27 C28 H28 119.5 . . ? 
C29 C28 H28 119.5 . . ? 
C30 C29 C24 119.1(3) . . ? 
C30 C29 C28 122.0(3) . . ? 
C24 C29 C28 118.9(3) . . ? 
C31 C30 C29 121.2(3) . . ? 
C31 C30 H30 119.4 . . ? 
C29 C30 H30 119.4 . . ? 
C30 C31 C32 121.0(3) . . ? 
C30 C31 H31 119.5 . . ? 
C32 C31 H31 119.5 . . ? 
C23 C32 C31 119.4(3) . . ? 
C23 C32 P2 122.01(19) . . ? 
C31 C32 P2 118.0(2) . . ? 
C34 C33 C38 118.8(3) . . ? 
C34 C33 P2 122.7(2) . . ? 
C38 C33 P2 118.4(2) . . ? 
C35 C34 C33 121.1(3) . . ? 
C35 C34 H34 119.4 . . ? 
C33 C34 H34 119.4 . . ? 
C34 C35 C36 119.8(3) . . ? 
C34 C35 H35 120.1 . . ? 
C36 C35 H35 120.1 . . ? 
C35 C36 C37 119.9(3) . . ? 
C35 C36 H36 120.1 . . ? 
C37 C36 H36 120.1 . . ? 
C36 C37 C38 120.5(3) . . ? 
C36 C37 H37 119.8 . . ? 
C38 C37 H37 119.8 . . ? 
C37 C38 C33 119.9(3) . . ? 
C37 C38 H38 120.1 . . ? 
C33 C38 H38 120.1 . . ? 
C40 C39 C44 120.0 . . ? 
C40 C39 P2 124.01(18) . . ? 
C44 C39 P2 115.80(18) . . ? 
C41 C40 C39 120.0 . . ? 
C41 C40 H40 120.0 . . ? 
C39 C40 H40 120.0 . . ? 
C42 C41 C40 120.0 . . ? 
C42 C41 H41 120.0 . . ? 
C40 C41 H41 120.0 . . ? 
C41 C42 C43 120.0 . . ? 
C41 C42 H42 120.0 . . ? 
C43 C42 H42 120.0 . . ? 
C42 C43 C44 120.0 . . ? 
C42 C43 H43 120.0 . . ? 
C44 C43 H43 120.0 . . ? 
C43 C44 C39 120.0 . . ? 
C43 C44 H44 120.0 . . ? 
C39 C44 H44 120.0 . . ? 
C40B C39B C44B 120.0 . . ? 
C40B C39B P2 121.2(6) . . ? 
C44B C39B P2 118.7(6) . . ? 
C39B C40B C41B 120.0 . . ? 
C39B C40B H40A 120.0 . . ? 
C41B C40B H40A 120.0 . . ? 
C42B C41B C40B 120.0 . . ? 
C42B C41B H41A 120.0 . . ? 
C40B C41B H41A 120.0 . . ? 
C43B C42B C41B 120.0 . . ? 
C43B C42B H42A 120.0 . . ? 
C41B C42B H42A 120.0 . . ? 
C44B C43B C42B 120.0 . . ? 
C44B C43B H43A 120.0 . . ? 
C42B C43B H43A 120.0 . . ? 
C43B C44B C39B 120.0 . . ? 
C43B C44B H44A 120.0 . . ? 
C39B C44B H44A 120.0 . . ? 
 
_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              67.77 
_diffrn_measured_fraction_theta_full   0.990 
_diffrn_standards_number         ? 
_diffrn_standards_decay_%        ? 
_diffrn_standards_interval_time  ? 
 
_refine_diff_density_max    0.536 
_refine_diff_density_min   -0.363 
_refine_diff_density_rms    0.060 
_publ_requested_category         FM 
 
_publ_section_references 
; 
 
Bruker (2010). APEX2. Bruker AXS, Inc., Madison, Wisconsin, USA. 
 
Bruker (2005). SAINT, SHELXTL, XCIF, XPREP.  Bruker AXS, Inc., Madison, 
Wisconsin, USA. 
 
Bruker (2007).  SADABS, TWINABS. Bruker AXS, Inc., Madison, Wisconsin, USA. 
 
CrystalMaker (1994).  CrystalMaker, a crystal and molecular structures 
program for Mac and Windows. CrystalMaker Software Ltd., Oxford, England 
(www.crystalmaker.com). 
 
Flack, H. D. (1983), Acta Cryst. A39, 876-881. 
Flack, H. D. (2000), J. Appl. Cryst., 33, 1143-1148. 
 
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 
; 
 
_publ_section_figure_captions 
; 
Figure 1.  SHELXTL (Bruker, 2005) plot showing 35% probability ellipsoids 
for non-H atoms and circles of arbitrary size for H atoms.  The unlabeled 
atoms are related by the symmetry operator (y-1, x-1, -z). 
; 
 
_publ_section_exptl_prep 
; 
Crystals were grown from a solution of tetrahydrofuran and pentane. 
; 
 
_publ_section_exptl_refinement 
; 
A structural model consisting of one half of the molecule per assymetric 
unitwas developed.  One of the phenyl groups was disordered over 2 sites. 
The disordered phenyl rings were restrained to be perfect hexagons (C-C 
bond distance 1.39 /%A).  Like C-P bond distances were also restrained 
to be similar (esd 0.01). Similar 
displacement amplitudes (esd 0.01) were imposed on disordered sites 
overlapping by less than the sum of van der Waals radii. 
 
H atoms were included as riding idealized contributors, and their U's were 
assigned as 1.2 times carrier U~eq~.  On the basis of 2575 unmerged 
Friedel opposites, the fractional contribution of the racemic twin was 
negligible (Flack, 1983 & 2000). 
; 
 
_publ_contact_author 
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
; 
_publ_contact_author_phone        '1  217 244 1708' 
_publ_contact_author_fax          '1  217 244 8068' 
_publ_contact_author_email        dgray@illinois.edu 
_publ_contact_letter 
; 
Please consider this CIF submission for publication as a structural paper 
in Journal of the American Chemical Society. 
; 
_publ_requested_journal           'Journal of the American Chemical Society' 
_publ_requested_coeditor_name     ? 
 
_publ_section_title 
; 
 ? 
; 
 
_publ_section_abstract 
; 
 ? 
; 
 
_publ_section_comment 
; 
 ? 
; 
 
_publ_section_acknowledgements 
; 
The Materials Chemistry Laboratory at the University of Illinois was 
supported in part by grants NSF CHE 95-03145 and NSF CHE 03-43032 
from the National Science Foundation. 
; 
 
loop_ 
 _publ_author_name 
 _publ_author_address 
'Gray, Danielle L.' 
; 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
; 
'Fuller, Amy L.' 
; 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
; 
'Gao, Yi-Gui' 
; 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
; 
 
loop_ 
 _exptl_crystal_face_index_h 
 _exptl_crystal_face_index_k 
 _exptl_crystal_face_index_l 
 _exptl_crystal_face_perp_dist 
    1.00    0.00    1.00    0.1240 
   -1.00    0.00   -1.00    0.1310 
    0.00   -1.00   -2.00    0.1280 
   -1.00    2.00    1.00    0.0880 
    0.00    1.00   -2.00    0.0750 
   -1.00   -2.00    2.00    0.0900 
    1.00    0.00   -2.00    0.1110 
   -1.00    0.00    2.00    0.1350 
    0.00    1.00    3.00    0.1030 
    1.00   -1.00    3.00    0.1380 
    1.00    3.00    2.00    0.0930