# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mk101
_database_code_depnum_ccdc_archive 'CCDC 1037224'
_audit_update_record             
;
2014-12-02 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H43 N P2'
_chemical_formula_weight         383.51

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.7199(5)
_cell_length_b                   12.3613(5)
_cell_length_c                   28.1443(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.935(4)
_cell_angle_gamma                90.00
_cell_volume                     4738.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9161
_cell_measurement_theta_min      2.9080
_cell_measurement_theta_max      28.7470

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1696
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98466
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1419
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            115355
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_sigmaI/netI    0.0655
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         30.92
_reflns_number_total             14008
_reflns_number_gt                9480
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44)  
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44)  
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The hydrogens at N and N' were refined freely. Methyls were refined as
 rigid groups allowed to rotate but not tip. Other hydrogens were included
 using a riding model starting from calculated positions. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0462P)²+1.7847P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14008
_refine_ls_number_parameters     483
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_ref         0.1289
_refine_ls_wR_factor_gt          0.1126
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.002
_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
P1 P 0.92093(3) 0.80529(3) 0.531220(14) 0.01352(10) Uani 1 1 d . . .
P2 P 0.86781(3) 0.78818(4) 0.323732(15) 0.01645(10) Uani 1 1 d . . .
N N 0.78751(11) 0.85672(12) 0.42690(5) 0.0161(3) Uani 1 1 d . . .
H01 H 0.8431(15) 0.8798(16) 0.4268(7) 0.018(5) Uiso 1 1 d . . .
C1 C 0.74545(13) 0.82887(13) 0.46727(6) 0.0158(3) Uani 1 1 d . . .
C2 C 0.65543(13) 0.78580(14) 0.45221(6) 0.0189(4) Uani 1 1 d . . .
H2 H 0.6096 0.7595 0.4722 0.023 Uiso 1 1 calc R . .
C3 C 0.64224(13) 0.78732(14) 0.40116(6) 0.0188(4) Uani 1 1 d . . .
H3 H 0.5861 0.7623 0.3811 0.023 Uiso 1 1 calc R . .
C4 C 0.72485(13) 0.83121(13) 0.38625(6) 0.0166(3) Uani 1 1 d . . .
C5 C 0.79377(13) 0.85743(14) 0.51623(6) 0.0195(4) Uani 1 1 d . . .
H5A H 0.7529 0.8291 0.5401 0.023 Uiso 1 1 calc R . .
H5B H 0.7952 0.9372 0.5193 0.023 Uiso 1 1 calc R . .
C6 C 0.89829(13) 0.65973(13) 0.54775(6) 0.0172(3) Uani 1 1 d . . .
C7 C 0.98742(16) 0.61231(15) 0.57814(7) 0.0302(5) Uani 1 1 d . . .
H7A H 0.9933 0.6442 0.6102 0.045 Uiso 1 1 calc R . .
H7B H 1.0467 0.6284 0.5632 0.045 Uiso 1 1 calc R . .
H7C H 0.9797 0.5338 0.5805 0.045 Uiso 1 1 calc R . .
C8 C 0.88626(14) 0.59975(14) 0.49950(6) 0.0233(4) Uani 1 1 d . . .
H8A H 0.8759 0.5225 0.5049 0.035 Uiso 1 1 calc R . .
H8B H 0.9456 0.6094 0.4838 0.035 Uiso 1 1 calc R . .
H8C H 0.8296 0.6292 0.4790 0.035 Uiso 1 1 calc R . .
C9 C 0.80564(16) 0.63868(16) 0.57170(7) 0.0302(5) Uani 1 1 d . . .
H9A H 0.8015 0.5615 0.5792 0.045 Uiso 1 1 calc R . .
H9B H 0.7477 0.6601 0.5499 0.045 Uiso 1 1 calc R . .
H9C H 0.8085 0.6809 0.6013 0.045 Uiso 1 1 calc R . .
C10 C 0.96334(13) 0.88677(14) 0.58682(6) 0.0181(4) Uani 1 1 d . . .
C11 C 0.90923(15) 0.86451(16) 0.63040(6) 0.0260(4) Uani 1 1 d . . .
H11A H 0.9205 0.7894 0.6407 0.039 Uiso 1 1 calc R . .
H11B H 0.8387 0.8766 0.6218 0.039 Uiso 1 1 calc R . .
H11C H 0.9339 0.9133 0.6565 0.039 Uiso 1 1 calc R . .
C12 C 1.07358(14) 0.86630(17) 0.59981(7) 0.0306(5) Uani 1 1 d . . .
H12D H 1.0989 0.9132 0.6266 0.046 Uiso 1 1 calc R . .
H12E H 1.1080 0.8822 0.5721 0.046 Uiso 1 1 calc R . .
H12F H 1.0843 0.7904 0.6091 0.046 Uiso 1 1 calc R . .
C13 C 0.95124(16) 1.00714(15) 0.57364(7) 0.0289(4) Uani 1 1 d . . .
H13D H 0.9866 1.0513 0.5990 0.043 Uiso 1 1 calc R . .
H13E H 0.8814 1.0262 0.5700 0.043 Uiso 1 1 calc R . .
H13F H 0.9780 1.0206 0.5434 0.043 Uiso 1 1 calc R . .
C14 C 0.75106(13) 0.85317(14) 0.33720(6) 0.0188(4) Uani 1 1 d . . .
H14C H 0.7568 0.9324 0.3331 0.023 Uiso 1 1 calc R . .
H14D H 0.6968 0.8275 0.3135 0.023 Uiso 1 1 calc R . .
C15 C 0.83431(13) 0.63976(14) 0.32225(6) 0.0190(4) Uani 1 1 d . . .
C16 C 0.84767(14) 0.60483(15) 0.37499(6) 0.0232(4) Uani 1 1 d . . .
H16A H 0.8379 0.5265 0.3770 0.035 Uiso 1 1 calc R . .
H16B H 0.7995 0.6423 0.3921 0.035 Uiso 1 1 calc R . .
H16C H 0.9141 0.6233 0.3895 0.035 Uiso 1 1 calc R . .
C17 C 0.72989(14) 0.61108(15) 0.30011(7) 0.0239(4) Uani 1 1 d . . .
H17D H 0.7214 0.5324 0.3003 0.036 Uiso 1 1 calc R . .
H17E H 0.7192 0.6377 0.2671 0.036 Uiso 1 1 calc R . .
H17F H 0.6823 0.6448 0.3188 0.036 Uiso 1 1 calc R . .
C18 C 0.90886(15) 0.57583(16) 0.29671(7) 0.0292(4) Uani 1 1 d . . .
H18A H 0.9756 0.5989 0.3089 0.044 Uiso 1 1 calc R . .
H18B H 0.8969 0.5895 0.2622 0.044 Uiso 1 1 calc R . .
H18C H 0.9016 0.4984 0.3028 0.044 Uiso 1 1 calc R . .
C19 C 0.87544(14) 0.83953(15) 0.26094(6) 0.0225(4) Uani 1 1 d . . .
C20 C 0.79095(14) 0.80844(16) 0.22259(6) 0.0255(4) Uani 1 1 d . . .
H20D H 0.7981 0.8473 0.1928 0.038 Uiso 1 1 calc R . .
H20E H 0.7282 0.8279 0.2336 0.038 Uiso 1 1 calc R . .
H20F H 0.7926 0.7303 0.2168 0.038 Uiso 1 1 calc R . .
C21 C 0.88045(16) 0.96335(16) 0.26500(7) 0.0324(5) Uani 1 1 d . . .
H21D H 0.9329 0.9838 0.2902 0.049 Uiso 1 1 calc R . .
H21E H 0.8176 0.9911 0.2730 0.049 Uiso 1 1 calc R . .
H21F H 0.8941 0.9941 0.2344 0.049 Uiso 1 1 calc R . .
C22 C 0.97347(15) 0.80318(18) 0.24502(7) 0.0319(5) Uani 1 1 d . . .
H22D H 0.9723 0.7247 0.2399 0.048 Uiso 1 1 calc R . .
H22E H 1.0272 0.8218 0.2699 0.048 Uiso 1 1 calc R . .
H22F H 0.9834 0.8398 0.2151 0.048 Uiso 1 1 calc R . .
P1' P 0.41578(3) 0.69680(3) 0.535132(14) 0.01325(9) Uani 1 1 d . . .
P2' P 0.37019(3) 0.72855(4) 0.330147(15) 0.01784(10) Uani 1 1 d . . .
N' N 0.28694(11) 0.64763(12) 0.43151(5) 0.0152(3) Uani 1 1 d . . .
H01' H 0.3433(14) 0.6278(15) 0.4337(6) 0.013(5) Uiso 1 1 d . . .
C1' C 0.23969(13) 0.67181(13) 0.47076(6) 0.0155(3) Uani 1 1 d . . .
C2' C 0.14769(13) 0.70695(14) 0.45385(6) 0.0183(4) Uani 1 1 d . . .
H2' H 0.0984 0.7293 0.4727 0.022 Uiso 1 1 calc R . .
C3' C 0.13874(13) 0.70418(14) 0.40300(6) 0.0175(3) Uani 1 1 d . . .
H3' H 0.0822 0.7239 0.3819 0.021 Uiso 1 1 calc R . .
C4' C 0.22593(12) 0.66805(13) 0.38978(6) 0.0159(3) Uani 1 1 d . . .
C5' C 0.28585(12) 0.65138(14) 0.52107(6) 0.0179(3) Uani 1 1 d . . .
H5'1 H 0.2830 0.5728 0.5275 0.021 Uiso 1 1 calc R . .
H5'2 H 0.2459 0.6882 0.5433 0.021 Uiso 1 1 calc R . .
C6' C 0.40242(13) 0.84006(13) 0.55619(6) 0.0171(3) Uani 1 1 d . . .
C7' C 0.35981(15) 0.85702(16) 0.60343(6) 0.0270(4) Uani 1 1 d . . .
H7'1 H 0.4062 0.8299 0.6299 0.040 Uiso 1 1 calc R . .
H7'2 H 0.2976 0.8177 0.6025 0.040 Uiso 1 1 calc R . .
H7'3 H 0.3483 0.9344 0.6080 0.040 Uiso 1 1 calc R . .
C8' C 0.33591(15) 0.89758(15) 0.51646(7) 0.0261(4) Uani 1 1 d . . .
H8'1 H 0.3367 0.9756 0.5227 0.039 Uiso 1 1 calc R . .
H8'2 H 0.2687 0.8703 0.5156 0.039 Uiso 1 1 calc R . .
H8'3 H 0.3598 0.8837 0.4856 0.039 Uiso 1 1 calc R . .
C9' C 0.50337(15) 0.89500(15) 0.55920(7) 0.0288(4) Uani 1 1 d . . .
H9'1 H 0.4965 0.9721 0.5661 0.043 Uiso 1 1 calc R . .
H9'2 H 0.5300 0.8865 0.5286 0.043 Uiso 1 1 calc R . .
H9'3 H 0.5481 0.8614 0.5848 0.043 Uiso 1 1 calc R . .
C10' C 0.45653(13) 0.60695(14) 0.58831(6) 0.0184(4) Uani 1 1 d . . .
C11' C 0.38299(14) 0.58896(16) 0.62413(6) 0.0253(4) Uani 1 1 d . . .
H11D H 0.4108 0.5385 0.6490 0.038 Uiso 1 1 calc R . .
H11E H 0.3222 0.5588 0.6075 0.038 Uiso 1 1 calc R . .
H11F H 0.3688 0.6581 0.6389 0.038 Uiso 1 1 calc R . .
C12' C 0.55297(14) 0.65000(18) 0.61463(7) 0.0300(5) Uani 1 1 d . . .
H12A H 0.5400 0.7162 0.6320 0.045 Uiso 1 1 calc R . .
H12B H 0.5988 0.6659 0.5914 0.045 Uiso 1 1 calc R . .
H12C H 0.5818 0.5954 0.6374 0.045 Uiso 1 1 calc R . .
C13' C 0.47841(18) 0.49709(16) 0.56630(7) 0.0352(5) Uani 1 1 d . . .
H13A H 0.5006 0.4458 0.5919 0.053 Uiso 1 1 calc R . .
H13B H 0.5299 0.5060 0.5453 0.053 Uiso 1 1 calc R . .
H13C H 0.4187 0.4694 0.5476 0.053 Uiso 1 1 calc R . .
C14' C 0.25781(13) 0.65196(15) 0.34142(6) 0.0199(4) Uani 1 1 d . . .
H14A H 0.2032 0.6735 0.3170 0.024 Uiso 1 1 calc R . .
H14B H 0.2700 0.5739 0.3370 0.024 Uiso 1 1 calc R . .
C15' C 0.32872(14) 0.87398(14) 0.33279(6) 0.0209(4) Uani 1 1 d . . .
C16' C 0.33604(15) 0.89955(15) 0.38653(6) 0.0248(4) Uani 1 1 d . . .
H16D H 0.3219 0.9764 0.3909 0.037 Uiso 1 1 calc R . .
H16E H 0.4025 0.8832 0.4017 0.037 Uiso 1 1 calc R . .
H16F H 0.2884 0.8554 0.4012 0.037 Uiso 1 1 calc R . .
C17' C 0.22451(14) 0.89920(16) 0.31013(7) 0.0257(4) Uani 1 1 d . . .
H17A H 0.2113 0.9765 0.3136 0.039 Uiso 1 1 calc R . .
H17B H 0.1776 0.8570 0.3262 0.039 Uiso 1 1 calc R . .
H17C H 0.2177 0.8803 0.2761 0.039 Uiso 1 1 calc R . .
C18' C 0.40177(16) 0.94823(17) 0.31116(7) 0.0315(5) Uani 1 1 d . . .
H18D H 0.3927 0.9411 0.2762 0.047 Uiso 1 1 calc R . .
H18E H 0.4690 0.9275 0.3235 0.047 Uiso 1 1 calc R . .
H18F H 0.3902 1.0235 0.3199 0.047 Uiso 1 1 calc R . .
C19' C 0.38042(14) 0.68839(16) 0.26605(6) 0.0230(4) Uani 1 1 d . . .
C20' C 0.29242(14) 0.71592(16) 0.22901(6) 0.0251(4) Uani 1 1 d . . .
H20A H 0.2895 0.7943 0.2239 0.038 Uiso 1 1 calc R . .
H20B H 0.2317 0.6915 0.2408 0.038 Uiso 1 1 calc R . .
H20C H 0.2998 0.6795 0.1987 0.038 Uiso 1 1 calc R . .
C21' C 0.39654(16) 0.56542(17) 0.26712(7) 0.0327(5) Uani 1 1 d . . .
H21A H 0.4103 0.5408 0.2355 0.049 Uiso 1 1 calc R . .
H21B H 0.3373 0.5294 0.2755 0.049 Uiso 1 1 calc R . .
H21C H 0.4522 0.5477 0.2910 0.049 Uiso 1 1 calc R . .
C22' C 0.47414(15) 0.7388(2) 0.25027(7) 0.0345(5) Uani 1 1 d . . .
H22A H 0.4886 0.7046 0.2205 0.052 Uiso 1 1 calc R . .
H22B H 0.5293 0.7273 0.2753 0.052 Uiso 1 1 calc R . .
H22C H 0.4641 0.8166 0.2450 0.052 Uiso 1 1 calc R . .


_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
P1 C5 1.8599(18) . ?
P1 C10 1.8925(17) . ?
P1 C6 1.8935(17) . ?
P2 C14 1.8711(18) . ?
P2 C15 1.8906(18) . ?
P2 C19 1.8925(18) . ?
N C1 1.379(2) . ?
N C4 1.382(2) . ?
C1 C2 1.365(2) . ?
C1 C5 1.497(2) . ?
C2 C3 1.426(2) . ?
C3 C4 1.367(2) . ?
C4 C14 1.493(2) . ?
C6 C7 1.522(3) . ?
C6 C9 1.531(2) . ?
C6 C8 1.538(2) . ?
C10 C11 1.533(2) . ?
C10 C12 1.534(3) . ?
C10 C13 1.538(2) . ?
C15 C17 1.533(2) . ?
C15 C16 1.535(2) . ?
C15 C18 1.538(2) . ?
C19 C20 1.534(2) . ?
C19 C22 1.535(3) . ?
C19 C21 1.536(3) . ?
P1' C5' 1.8653(17) . ?
P1' C6' 1.8834(17) . ?
P1' C10' 1.8932(17) . ?
P2' C14' 1.8689(18) . ?
P2' C15' 1.8898(19) . ?
P2' C19' 1.8924(18) . ?
N' C1' 1.379(2) . ?
N' C4' 1.381(2) . ?
C1' C2' 1.365(2) . ?
C1' C5' 1.501(2) . ?
C2' C3' 1.422(2) . ?
C3' C4' 1.370(2) . ?
C4' C14' 1.492(2) . ?
C6' C7' 1.530(2) . ?
C6' C8' 1.531(2) . ?
C6' C9' 1.536(3) . ?
C10' C11' 1.526(2) . ?
C10' C12' 1.532(3) . ?
C10' C13' 1.537(3) . ?
C15' C17' 1.526(3) . ?
C15' C16' 1.537(2) . ?
C15' C18' 1.538(3) . ?
C19' C20' 1.535(2) . ?
C19' C21' 1.536(3) . ?
C19' C22' 1.542(3) . ?

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
C5 P1 C10 100.92(8) . . ?
C5 P1 C6 101.99(8) . . ?
C10 P1 C6 110.23(8) . . ?
C14 P2 C15 102.08(8) . . ?
C14 P2 C19 100.98(8) . . ?
C15 P2 C19 110.22(8) . . ?
C1 N C4 110.17(15) . . ?
C2 C1 N 107.13(15) . . ?
C2 C1 C5 131.41(16) . . ?
N C1 C5 121.11(16) . . ?
C1 C2 C3 107.93(15) . . ?
C4 C3 C2 107.77(15) . . ?
C3 C4 N 107.00(15) . . ?
C3 C4 C14 131.08(16) . . ?
N C4 C14 121.92(15) . . ?
C1 C5 P1 115.21(11) . . ?
C7 C6 C9 109.90(15) . . ?
C7 C6 C8 107.68(15) . . ?
C9 C6 C8 107.48(15) . . ?
C7 C6 P1 111.06(13) . . ?
C9 C6 P1 116.05(12) . . ?
C8 C6 P1 104.15(11) . . ?
C11 C10 C12 109.78(15) . . ?
C11 C10 C13 108.55(15) . . ?
C12 C10 C13 106.97(16) . . ?
C11 C10 P1 115.83(12) . . ?
C12 C10 P1 107.78(12) . . ?
C13 C10 P1 107.58(12) . . ?
C4 C14 P2 114.64(12) . . ?
C17 C15 C16 108.94(15) . . ?
C17 C15 C18 109.44(15) . . ?
C16 C15 C18 107.38(15) . . ?
C17 C15 P2 116.49(13) . . ?
C16 C15 P2 104.56(12) . . ?
C18 C15 P2 109.59(13) . . ?
C20 C19 C22 109.60(15) . . ?
C20 C19 C21 108.97(16) . . ?
C22 C19 C21 106.29(16) . . ?
C20 C19 P2 116.78(12) . . ?
C22 C19 P2 108.88(13) . . ?
C21 C19 P2 105.77(12) . . ?
C5' P1' C6' 102.88(8) . . ?
C5' P1' C10' 100.06(8) . . ?
C6' P1' C10' 109.48(8) . . ?
C14' P2' C15' 102.52(8) . . ?
C14' P2' C19' 100.75(8) . . ?
C15' P2' C19' 110.15(8) . . ?
C1' N' C4' 110.26(15) . . ?
C2' C1' N' 107.10(15) . . ?
C2' C1' C5' 130.50(15) . . ?
N' C1' C5' 122.23(15) . . ?
C1' C2' C3' 107.88(15) . . ?
C4' C3' C2' 108.01(15) . . ?
C3' C4' N' 106.75(14) . . ?
C3' C4' C14' 130.76(16) . . ?
N' C4' C14' 122.49(15) . . ?
C1' C5' P1' 115.67(11) . . ?
C7' C6' C8' 108.33(15) . . ?
C7' C6' C9' 109.16(15) . . ?
C8' C6' C9' 106.80(15) . . ?
C7' C6' P1' 117.66(12) . . ?
C8' C6' P1' 106.20(11) . . ?
C9' C6' P1' 108.17(12) . . ?
C11' C10' C12' 109.43(15) . . ?
C11' C10' C13' 108.32(16) . . ?
C12' C10' C13' 107.61(16) . . ?
C11' C10' P1' 116.87(12) . . ?
C12' C10' P1' 109.50(12) . . ?
C13' C10' P1' 104.66(12) . . ?
C4' C14' P2' 115.21(12) . . ?
C17' C15' C16' 108.42(15) . . ?
C17' C15' C18' 109.58(15) . . ?
C16' C15' C18' 107.38(15) . . ?
C17' C15' P2' 116.70(13) . . ?
C16' C15' P2' 104.49(12) . . ?
C18' C15' P2' 109.78(13) . . ?
C20' C19' C21' 109.41(16) . . ?
C20' C19' C22' 109.24(15) . . ?
C21' C19' C22' 106.42(16) . . ?
C20' C19' P2' 116.52(12) . . ?
C21' C19' P2' 105.55(12) . . ?
C22' C19' P2' 109.20(13) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N C1 C2 -0.22(19) . . . . ?
C4 N C1 C5 -174.13(14) . . . . ?
N C1 C2 C3 0.06(19) . . . . ?
C5 C1 C2 C3 173.10(17) . . . . ?
C1 C2 C3 C4 0.1(2) . . . . ?
C2 C3 C4 N -0.25(19) . . . . ?
C2 C3 C4 C14 -179.45(17) . . . . ?
C1 N C4 C3 0.30(19) . . . . ?
C1 N C4 C14 179.59(15) . . . . ?
C2 C1 C5 P1 130.70(17) . . . . ?
N C1 C5 P1 -57.1(2) . . . . ?
C10 P1 C5 C1 166.38(13) . . . . ?
C6 P1 C5 C1 -79.98(14) . . . . ?
C5 P1 C6 C7 -159.31(12) . . . . ?
C10 P1 C6 C7 -52.77(14) . . . . ?
C5 P1 C6 C9 -32.86(15) . . . . ?
C10 P1 C6 C9 73.69(15) . . . . ?
C5 P1 C6 C8 85.05(12) . . . . ?
C10 P1 C6 C8 -168.41(11) . . . . ?
C5 P1 C10 C11 65.22(15) . . . . ?
C6 P1 C10 C11 -42.04(16) . . . . ?
C5 P1 C10 C12 -171.41(13) . . . . ?
C6 P1 C10 C12 81.34(14) . . . . ?
C5 P1 C10 C13 -56.38(14) . . . . ?
C6 P1 C10 C13 -163.64(12) . . . . ?
C3 C4 C14 P2 -123.62(18) . . . . ?
N C4 C14 P2 57.3(2) . . . . ?
C15 P2 C14 C4 68.31(14) . . . . ?
C19 P2 C14 C4 -178.01(13) . . . . ?
C14 P2 C15 C17 37.70(14) . . . . ?
C19 P2 C15 C17 -68.94(15) . . . . ?
C14 P2 C15 C16 -82.56(13) . . . . ?
C19 P2 C15 C16 170.79(12) . . . . ?
C14 P2 C15 C18 162.59(13) . . . . ?
C19 P2 C15 C18 55.95(15) . . . . ?
C14 P2 C19 C20 -60.75(16) . . . . ?
C15 P2 C19 C20 46.63(17) . . . . ?
C14 P2 C19 C22 174.52(13) . . . . ?
C15 P2 C19 C22 -78.10(14) . . . . ?
C14 P2 C19 C21 60.65(14) . . . . ?
C15 P2 C19 C21 168.03(13) . . . . ?
C4' N' C1' C2' 0.52(19) . . . . ?
C4' N' C1' C5' 176.25(15) . . . . ?
N' C1' C2' C3' -0.05(19) . . . . ?
C5' C1' C2' C3' -175.29(16) . . . . ?
C1' C2' C3' C4' -0.4(2) . . . . ?
C2' C3' C4' N' 0.74(19) . . . . ?
C2' C3' C4' C14' -178.51(17) . . . . ?
C1' N' C4' C3' -0.79(19) . . . . ?
C1' N' C4' C14' 178.53(15) . . . . ?
C2' C1' C5' P1' -138.93(17) . . . . ?
N' C1' C5' P1' 46.4(2) . . . . ?
C6' P1' C5' C1' 89.75(14) . . . . ?
C10' P1' C5' C1' -157.43(13) . . . . ?
C5' P1' C6' C7' 67.27(15) . . . . ?
C10' P1' C6' C7' -38.44(16) . . . . ?
C5' P1' C6' C8' -54.20(13) . . . . ?
C10' P1' C6' C8' -159.92(12) . . . . ?
C5' P1' C6' C9' -168.53(12) . . . . ?
C10' P1' C6' C9' 85.75(13) . . . . ?
C5' P1' C10' C11' -39.91(15) . . . . ?
C6' P1' C10' C11' 67.72(16) . . . . ?
C5' P1' C10' C12' -165.01(13) . . . . ?
C6' P1' C10' C12' -57.38(14) . . . . ?
C5' P1' C10' C13' 79.87(14) . . . . ?
C6' P1' C10' C13' -172.50(13) . . . . ?
C3' C4' C14' P2' 122.51(18) . . . . ?
N' C4' C14' P2' -56.6(2) . . . . ?
C15' P2' C14' C4' -64.67(14) . . . . ?
C19' P2' C14' C4' -178.33(13) . . . . ?
C14' P2' C15' C17' -39.43(15) . . . . ?
C19' P2' C15' C17' 67.13(15) . . . . ?
C14' P2' C15' C16' 80.26(13) . . . . ?
C19' P2' C15' C16' -173.18(12) . . . . ?
C14' P2' C15' C18' -164.86(13) . . . . ?
C19' P2' C15' C18' -58.30(15) . . . . ?
C14' P2' C19' C20' 58.98(16) . . . . ?
C15' P2' C19' C20' -48.76(16) . . . . ?
C14' P2' C19' C21' -62.65(14) . . . . ?
C15' P2' C19' C21' -170.38(13) . . . . ?
C14' P2' C19' C22' -176.70(14) . . . . ?
C15' P2' C19' C22' 75.56(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.934
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.063
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mk90
_database_code_depnum_ccdc_archive 'CCDC 1037225'
_audit_update_record             
;
2014-12-02 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H68 Li2 N2 P4'
_chemical_formula_weight         666.68

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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   24.1538(5)
_cell_length_b                   13.7672(3)
_cell_length_c                   12.0771(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4016.00(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25760
_cell_measurement_theta_min      2.7920
_cell_measurement_theta_max      30.5140

_exptl_crystal_description       trapezoid
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1456
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96407
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44)  
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1419
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            103142
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         30.89
_reflns_number_total             11890
_reflns_number_gt                10639
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44)  
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44)  
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44)  
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 One i-propyl group is disordered and was refined on two positions.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0371P)²+1.0398P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(5)
_chemical_absolute_configuration .
_refine_ls_number_reflns         11890
_refine_ls_number_parameters     426
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0821
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.003
_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
Li1 Li 0.67838(11) 0.25547(19) 0.5415(2) 0.0188(5) Uani 1 1 d . A .
Li2 Li 0.57768(10) 0.26165(19) 0.5826(2) 0.0195(5) Uani 1 1 d . . .
N1 N 0.62946(5) 0.13783(9) 0.58178(10) 0.0143(2) Uani 1 1 d . . .
N2 N 0.62641(5) 0.37367(9) 0.52611(10) 0.0151(2) Uani 1 1 d . . .
P1 P 0.715987(15) 0.15439(3) 0.38247(3) 0.01417(7) Uani 1 1 d . . .
P2 P 0.540135(16) 0.20873(3) 0.76991(3) 0.01882(8) Uani 1 1 d . . .
P4 P 0.514563(15) 0.28680(3) 0.42099(3) 0.01643(8) Uani 1 1 d . . .
C1 C 0.63675(6) 0.06250(10) 0.50660(13) 0.0158(3) Uani 1 1 d . . .
C2 C 0.63401(6) -0.02659(11) 0.55855(14) 0.0197(3) Uani 1 1 d . . .
H2 H 0.6378 -0.0885 0.5247 0.024 Uiso 1 1 calc R . .
C3 C 0.62454(6) -0.00774(11) 0.67197(14) 0.0204(3) Uani 1 1 d . . .
H3 H 0.6205 -0.0545 0.7292 0.025 Uiso 1 1 calc R . .
C4 C 0.62234(6) 0.09192(11) 0.68336(13) 0.0164(3) Uani 1 1 d . . .
C5 C 0.65159(6) 0.08150(11) 0.38779(13) 0.0164(3) Uani 1 1 d . . .
H5A H 0.6211 0.1171 0.3509 0.020 Uiso 1 1 calc R . .
H5B H 0.6571 0.0192 0.3485 0.020 Uiso 1 1 calc R . .
C6 C 0.73471(6) 0.16003(11) 0.23356(12) 0.0189(3) Uani 1 1 d . . .
H6 H 0.7464 0.0937 0.2092 0.023 Uiso 1 1 calc R . .
C7 C 0.78354(7) 0.22930(12) 0.21762(14) 0.0258(3) Uani 1 1 d . . .
H7A H 0.7954 0.2279 0.1400 0.039 Uiso 1 1 calc R . .
H7B H 0.8143 0.2090 0.2651 0.039 Uiso 1 1 calc R . .
H7C H 0.7722 0.2954 0.2375 0.039 Uiso 1 1 calc R . .
C8 C 0.68534(7) 0.19173(13) 0.16251(14) 0.0250(3) Uani 1 1 d . . .
H8A H 0.6721 0.2553 0.1877 0.037 Uiso 1 1 calc R . .
H8B H 0.6555 0.1439 0.1695 0.037 Uiso 1 1 calc R . .
H8C H 0.6968 0.1962 0.0848 0.037 Uiso 1 1 calc R . .
C9 C 0.76976(6) 0.07096(11) 0.43763(13) 0.0183(3) Uani 1 1 d . . .
H9 H 0.8060 0.0951 0.4087 0.022 Uiso 1 1 calc R . .
C10 C 0.77286(6) 0.07910(12) 0.56419(13) 0.0214(3) Uani 1 1 d . . .
H10A H 0.7379 0.0569 0.5966 0.032 Uiso 1 1 calc R . .
H10B H 0.7794 0.1469 0.5850 0.032 Uiso 1 1 calc R . .
H10C H 0.8033 0.0387 0.5917 0.032 Uiso 1 1 calc R . .
C11 C 0.76504(7) -0.03504(11) 0.40114(14) 0.0233(3) Uani 1 1 d . . .
H11A H 0.7975 -0.0712 0.4272 0.035 Uiso 1 1 calc R . .
H11B H 0.7632 -0.0382 0.3202 0.035 Uiso 1 1 calc R . .
H11C H 0.7314 -0.0637 0.4327 0.035 Uiso 1 1 calc R . .
C12 C 0.60826(6) 0.14817(12) 0.78554(12) 0.0190(3) Uani 1 1 d . . .
H12A H 0.6372 0.1976 0.7994 0.023 Uiso 1 1 calc R . .
H12B H 0.6072 0.1038 0.8500 0.023 Uiso 1 1 calc R . .
C13 C 0.52677(7) 0.25168(13) 0.91302(14) 0.0260(3) Uani 1 1 d . . .
H13 H 0.5314 0.1955 0.9647 0.031 Uiso 1 1 calc R . .
C14 C 0.56905(10) 0.32928(18) 0.94381(18) 0.0465(5) Uani 1 1 d . . .
H14A H 0.5657 0.3844 0.8928 0.070 Uiso 1 1 calc R . .
H14B H 0.6064 0.3020 0.9387 0.070 Uiso 1 1 calc R . .
H14C H 0.5622 0.3514 1.0197 0.070 Uiso 1 1 calc R . .
C15 C 0.46817(8) 0.2907(2) 0.92551(18) 0.0473(6) Uani 1 1 d . . .
H15A H 0.4632 0.3162 1.0006 0.071 Uiso 1 1 calc R . .
H15B H 0.4416 0.2383 0.9123 0.071 Uiso 1 1 calc R . .
H15C H 0.4621 0.3429 0.8717 0.071 Uiso 1 1 calc R . .
C16 C 0.49448(7) 0.10213(13) 0.74597(15) 0.0246(3) Uani 1 1 d . . .
H16 H 0.5115 0.0664 0.6824 0.030 Uiso 1 1 calc R . .
C17 C 0.43664(7) 0.13048(15) 0.70672(17) 0.0341(4) Uani 1 1 d . . .
H17A H 0.4177 0.0731 0.6773 0.051 Uiso 1 1 calc R . .
H17B H 0.4396 0.1799 0.6486 0.051 Uiso 1 1 calc R . .
H17C H 0.4155 0.1567 0.7691 0.051 Uiso 1 1 calc R . .
C18 C 0.49197(7) 0.02855(14) 0.84032(18) 0.0344(4) Uani 1 1 d . . .
H18A H 0.4731 0.0576 0.9040 0.052 Uiso 1 1 calc R . .
H18B H 0.5297 0.0099 0.8616 0.052 Uiso 1 1 calc R . .
H18C H 0.4716 -0.0291 0.8159 0.052 Uiso 1 1 calc R . .
C19 C 0.64814(6) 0.45481(10) 0.57829(13) 0.0159(3) Uani 1 1 d . . .
C20 C 0.63982(6) 0.53742(11) 0.51628(13) 0.0185(3) Uani 1 1 d . . .
H20 H 0.6514 0.6015 0.5343 0.022 Uiso 1 1 calc R . .
C21 C 0.61061(6) 0.50796(11) 0.42015(14) 0.0187(3) Uani 1 1 d . . .
H21 H 0.5983 0.5486 0.3616 0.022 Uiso 1 1 calc R . .
C22 C 0.60361(6) 0.40874(11) 0.42816(13) 0.0157(3) Uani 1 1 d . . .
C23 C 0.67933(6) 0.44511(11) 0.68541(13) 0.0186(3) Uani 1 1 d . A .
H23A H 0.6548 0.4181 0.7434 0.022 Uiso 1 1 calc R . .
H23B H 0.6925 0.5096 0.7102 0.022 Uiso 1 1 calc R . .
C27 C 0.77423(6) 0.35514(12) 0.79913(13) 0.0197(3) Uani 1 1 d . A .
H27 H 0.7874 0.4215 0.8204 0.024 Uiso 1 1 calc R . .
C28 C 0.82439(7) 0.28791(15) 0.79022(17) 0.0338(4) Uani 1 1 d . . .
H28A H 0.8430 0.2841 0.8622 0.051 Uiso 1 1 calc R . .
H28B H 0.8502 0.3136 0.7349 0.051 Uiso 1 1 calc R . .
H28C H 0.8122 0.2229 0.7678 0.051 Uiso 1 1 calc R . .
C29 C 0.73513(7) 0.31831(14) 0.88843(14) 0.0292(4) Uani 1 1 d . . .
H29A H 0.7212 0.2539 0.8678 0.044 Uiso 1 1 calc R . .
H29B H 0.7039 0.3634 0.8961 0.044 Uiso 1 1 calc R . .
H29C H 0.7550 0.3139 0.9590 0.044 Uiso 1 1 calc R . .
C30 C 0.57475(6) 0.34160(11) 0.34894(12) 0.0180(3) Uani 1 1 d . . .
H30A H 0.6005 0.2900 0.3242 0.022 Uiso 1 1 calc R . .
H30B H 0.5621 0.3782 0.2830 0.022 Uiso 1 1 calc R . .
C31 C 0.48326(7) 0.19325(12) 0.32836(14) 0.0231(3) Uani 1 1 d . . .
H31 H 0.4433 0.2107 0.3191 0.028 Uiso 1 1 calc R . .
C32 C 0.50828(8) 0.18753(14) 0.21280(15) 0.0333(4) Uani 1 1 d . . .
H32A H 0.5476 0.1708 0.2184 0.050 Uiso 1 1 calc R . .
H32B H 0.5044 0.2505 0.1758 0.050 Uiso 1 1 calc R . .
H32C H 0.4890 0.1376 0.1698 0.050 Uiso 1 1 calc R . .
C33 C 0.48503(8) 0.09414(12) 0.38634(17) 0.0319(4) Uani 1 1 d . . .
H33A H 0.4663 0.0457 0.3403 0.048 Uiso 1 1 calc R . .
H33B H 0.4663 0.0988 0.4581 0.048 Uiso 1 1 calc R . .
H33C H 0.5236 0.0747 0.3977 0.048 Uiso 1 1 calc R . .
C34 C 0.46454(6) 0.38822(11) 0.41820(15) 0.0221(3) Uani 1 1 d . . .
H34 H 0.4846 0.4468 0.4461 0.027 Uiso 1 1 calc R . .
C35 C 0.44171(8) 0.41480(14) 0.30433(17) 0.0332(4) Uani 1 1 d . . .
H35A H 0.4183 0.3619 0.2770 0.050 Uiso 1 1 calc R . .
H35B H 0.4725 0.4252 0.2528 0.050 Uiso 1 1 calc R . .
H35C H 0.4197 0.4744 0.3100 0.050 Uiso 1 1 calc R . .
C36 C 0.41726(7) 0.36907(14) 0.49924(17) 0.0313(4) Uani 1 1 d . . .
H36A H 0.3938 0.4270 0.5046 0.047 Uiso 1 1 calc R . .
H36B H 0.4325 0.3537 0.5724 0.047 Uiso 1 1 calc R . .
H36C H 0.3951 0.3142 0.4728 0.047 Uiso 1 1 calc R . .
P3 P 0.739119(15) 0.36297(3) 0.66293(3) 0.01646(8) Uani 1 1 d D . .
C24 C 0.78213(11) 0.4458(2) 0.5741(2) 0.0191(5) Uani 0.744(5) 1 d PDU A 1
H24 H 0.7557 0.4794 0.5231 0.023 Uiso 0.744(5) 1 calc PR A 1
C25 C 0.82170(10) 0.3885(2) 0.5004(2) 0.0327(7) Uani 0.744(5) 1 d PD A 1
H25A H 0.8380 0.4321 0.4452 0.049 Uiso 0.744(5) 1 calc PR A 1
H25B H 0.8014 0.3365 0.4629 0.049 Uiso 0.744(5) 1 calc PR A 1
H25C H 0.8512 0.3603 0.5460 0.049 Uiso 0.744(5) 1 calc PR A 1
C26 C 0.8127(3) 0.5258(3) 0.6367(4) 0.0238(9) Uani 0.744(5) 1 d PDU A 1
H26A H 0.8425 0.4970 0.6811 0.036 Uiso 0.744(5) 1 calc PR A 1
H26B H 0.7868 0.5598 0.6856 0.036 Uiso 0.744(5) 1 calc PR A 1
H26C H 0.8286 0.5720 0.5837 0.036 Uiso 0.744(5) 1 calc PR A 1
C24' C 0.7956(3) 0.4233(6) 0.5867(6) 0.0177(19) Uiso 0.256(5) 1 d PDU A 2
H24' H 0.8307 0.3868 0.6001 0.021 Uiso 0.256(5) 1 calc PR A 2
C25' C 0.7826(3) 0.4197(5) 0.4657(5) 0.0229(16) Uiso 0.256(5) 1 d PD A 2
H25D H 0.7793 0.3518 0.4421 0.034 Uiso 0.256(5) 1 calc PR A 2
H25E H 0.8124 0.4513 0.4240 0.034 Uiso 0.256(5) 1 calc PR A 2
H25F H 0.7476 0.4536 0.4517 0.034 Uiso 0.256(5) 1 calc PR A 2
C26' C 0.8036(8) 0.5297(11) 0.6262(17) 0.033(5) Uiso 0.256(5) 1 d PDU A 2
H26D H 0.8124 0.5302 0.7054 0.049 Uiso 0.256(5) 1 calc PR A 2
H26E H 0.7694 0.5664 0.6134 0.049 Uiso 0.256(5) 1 calc PR A 2
H26F H 0.8340 0.5597 0.5848 0.049 Uiso 0.256(5) 1 calc PR A 2


_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
Li1 N1 2.063(3) . ?
Li1 N2 2.064(3) . ?
Li1 Li2 2.484(4) . ?
Li1 P1 2.540(3) . ?
Li1 P3 2.548(3) . ?
Li2 N2 2.056(3) . ?
Li2 N1 2.114(3) . ?
Li2 P4 2.501(3) . ?
Li2 P2 2.544(3) . ?
N1 C1 1.3896(19) . ?
N1 C4 1.3906(19) . ?
N2 C19 1.3859(18) . ?
N2 C22 1.3914(19) . ?
P1 C5 1.8523(14) . ?
P1 C6 1.8561(15) . ?
P1 C9 1.8574(15) . ?
P2 C12 1.8542(15) . ?
P2 C13 1.8551(17) . ?
P2 C16 1.8583(18) . ?
P4 C34 1.8467(16) . ?
P4 C30 1.8546(15) . ?
P4 C31 1.8660(16) . ?
C1 C2 1.379(2) . ?
C1 C5 1.502(2) . ?
C2 C3 1.413(2) . ?
C3 C4 1.380(2) . ?
C4 C12 1.496(2) . ?
C6 C7 1.529(2) . ?
C6 C8 1.533(2) . ?
C9 C11 1.529(2) . ?
C9 C10 1.534(2) . ?
C13 C15 1.522(2) . ?
C13 C14 1.524(3) . ?
C16 C18 1.526(2) . ?
C16 C17 1.526(2) . ?
C19 C20 1.376(2) . ?
C19 C23 1.503(2) . ?
C20 C21 1.418(2) . ?
C21 C22 1.380(2) . ?
C22 C30 1.502(2) . ?
C23 P3 1.8541(15) . ?
C27 C29 1.521(2) . ?
C27 C28 1.528(2) . ?
C27 P3 1.8538(15) . ?
C31 C32 1.523(3) . ?
C31 C33 1.534(2) . ?
C34 C35 1.526(2) . ?
C34 C36 1.527(2) . ?
P3 C24' 1.844(7) . ?
P3 C24 1.879(2) . ?
C24 C25 1.525(3) . ?
C24 C26 1.528(4) . ?
C24' C25' 1.495(9) . ?
C24' C26' 1.552(13) . ?

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
N1 Li1 N2 106.98(12) . . ?
N1 Li1 Li2 54.48(9) . . ?
N2 Li1 Li2 52.79(9) . . ?
N1 Li1 P1 87.30(10) . . ?
N2 Li1 P1 125.55(13) . . ?
Li2 Li1 P1 121.34(12) . . ?
N1 Li1 P3 130.56(13) . . ?
N2 Li1 P3 86.80(10) . . ?
Li2 Li1 P3 115.40(12) . . ?
P1 Li1 P3 123.19(10) . . ?
N2 Li2 N1 105.34(12) . . ?
N2 Li2 Li1 53.06(9) . . ?
N1 Li2 Li1 52.57(9) . . ?
N2 Li2 P4 89.21(10) . . ?
N1 Li2 P4 117.94(12) . . ?
Li1 Li2 P4 116.47(12) . . ?
N2 Li2 P2 135.55(13) . . ?
N1 Li2 P2 89.09(10) . . ?
Li1 Li2 P2 121.13(12) . . ?
P4 Li2 P2 121.09(10) . . ?
C1 N1 C4 104.65(12) . . ?
C1 N1 Li1 111.07(12) . . ?
C4 N1 Li1 129.46(12) . . ?
C1 N1 Li2 132.82(12) . . ?
C4 N1 Li2 106.80(11) . . ?
Li1 N1 Li2 72.96(11) . . ?
C19 N2 C22 104.88(12) . . ?
C19 N2 Li2 132.10(13) . . ?
C22 N2 Li2 108.41(12) . . ?
C19 N2 Li1 111.36(12) . . ?
C22 N2 Li1 126.24(12) . . ?
Li2 N2 Li1 74.15(11) . . ?
C5 P1 C6 105.12(7) . . ?
C5 P1 C9 103.87(7) . . ?
C6 P1 C9 101.71(7) . . ?
C5 P1 Li1 88.30(8) . . ?
C6 P1 Li1 142.85(8) . . ?
C9 P1 Li1 108.52(8) . . ?
C12 P2 C13 101.70(7) . . ?
C12 P2 C16 100.80(8) . . ?
C13 P2 C16 107.06(8) . . ?
C12 P2 Li2 84.43(8) . . ?
C13 P2 Li2 143.06(9) . . ?
C16 P2 Li2 107.42(8) . . ?
C34 P4 C30 101.35(7) . . ?
C34 P4 C31 104.23(7) . . ?
C30 P4 C31 108.49(7) . . ?
C34 P4 Li2 121.18(8) . . ?
C30 P4 Li2 86.83(8) . . ?
C31 P4 Li2 128.27(8) . . ?
C2 C1 N1 111.12(14) . . ?
C2 C1 C5 126.94(14) . . ?
N1 C1 C5 121.63(13) . . ?
C1 C2 C3 106.59(14) . . ?
C4 C3 C2 106.59(14) . . ?
C3 C4 N1 111.04(14) . . ?
C3 C4 C12 127.27(14) . . ?
N1 C4 C12 121.37(13) . . ?
C1 C5 P1 109.14(10) . . ?
C7 C6 C8 110.62(13) . . ?
C7 C6 P1 109.64(11) . . ?
C8 C6 P1 111.40(11) . . ?
C11 C9 C10 111.13(13) . . ?
C11 C9 P1 115.78(11) . . ?
C10 C9 P1 110.26(11) . . ?
C4 C12 P2 110.51(10) . . ?
C15 C13 C14 110.58(18) . . ?
C15 C13 P2 111.52(13) . . ?
C14 C13 P2 109.52(13) . . ?
C18 C16 C17 111.43(14) . . ?
C18 C16 P2 115.57(13) . . ?
C17 C16 P2 112.93(13) . . ?
C20 C19 N2 111.30(14) . . ?
C20 C19 C23 127.95(14) . . ?
N2 C19 C23 120.63(13) . . ?
C19 C20 C21 106.37(13) . . ?
C22 C21 C20 106.66(14) . . ?
C21 C22 N2 110.77(13) . . ?
C21 C22 C30 128.42(14) . . ?
N2 C22 C30 120.78(13) . . ?
C19 C23 P3 108.58(10) . . ?
C29 C27 C28 109.90(15) . . ?
C29 C27 P3 111.38(10) . . ?
C28 C27 P3 109.60(11) . . ?
C22 C30 P4 108.38(10) . . ?
C32 C31 C33 111.17(15) . . ?
C32 C31 P4 115.11(12) . . ?
C33 C31 P4 109.20(12) . . ?
C35 C34 C36 110.41(14) . . ?
C35 C34 P4 115.73(13) . . ?
C36 C34 P4 110.31(12) . . ?
C24' P3 C27 97.5(2) . . ?
C24' P3 C23 112.0(3) . . ?
C27 P3 C23 105.18(7) . . ?
C24' P3 C24 14.6(2) . . ?
C27 P3 C24 106.80(10) . . ?
C23 P3 C24 98.30(11) . . ?
C24' P3 Li1 113.6(2) . . ?
C27 P3 Li1 137.75(8) . . ?
C23 P3 Li1 89.43(8) . . ?
C24 P3 Li1 110.01(10) . . ?
C25 C24 C26 111.0(3) . . ?
C25 C24 P3 111.49(19) . . ?
C26 C24 P3 115.0(2) . . ?
C25' C24' C26' 111.0(10) . . ?
C25' C24' P3 108.5(5) . . ?
C26' C24' P3 111.3(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Li1 Li2 N2 -172.94(15) . . . . ?
P1 Li1 Li2 N2 -113.10(15) . . . . ?
P3 Li1 Li2 N2 64.01(12) . . . . ?
N2 Li1 Li2 N1 172.94(15) . . . . ?
P1 Li1 Li2 N1 59.84(13) . . . . ?
P3 Li1 Li2 N1 -123.05(14) . . . . ?
N1 Li1 Li2 P4 -106.14(14) . . . . ?
N2 Li1 Li2 P4 66.80(12) . . . . ?
P1 Li1 Li2 P4 -46.30(18) . . . . ?
P3 Li1 Li2 P4 130.81(12) . . . . ?
N1 Li1 Li2 P2 60.95(12) . . . . ?
N2 Li1 Li2 P2 -126.11(16) . . . . ?
P1 Li1 Li2 P2 120.79(14) . . . . ?
P3 Li1 Li2 P2 -62.10(17) . . . . ?
N2 Li1 N1 C1 124.20(13) . . . . ?
Li2 Li1 N1 C1 130.07(13) . . . . ?
P1 Li1 N1 C1 -2.25(13) . . . . ?
P3 Li1 N1 C1 -135.18(15) . . . . ?
N2 Li1 N1 C4 -103.87(16) . . . . ?
Li2 Li1 N1 C4 -98.00(16) . . . . ?
P1 Li1 N1 C4 129.68(13) . . . . ?
P3 Li1 N1 C4 -3.3(2) . . . . ?
N2 Li1 N1 Li2 -5.87(12) . . . . ?
P1 Li1 N1 Li2 -132.32(11) . . . . ?
P3 Li1 N1 Li2 94.75(17) . . . . ?
N2 Li2 N1 C1 -97.37(17) . . . . ?
Li1 Li2 N1 C1 -103.21(16) . . . . ?
P4 Li2 N1 C1 0.1(2) . . . . ?
P2 Li2 N1 C1 125.24(14) . . . . ?
N2 Li2 N1 C4 132.85(13) . . . . ?
Li1 Li2 N1 C4 127.01(13) . . . . ?
P4 Li2 N1 C4 -129.73(12) . . . . ?
P2 Li2 N1 C4 -4.54(12) . . . . ?
N2 Li2 N1 Li1 5.84(12) . . . . ?
P4 Li2 N1 Li1 103.27(14) . . . . ?
P2 Li2 N1 Li1 -131.55(11) . . . . ?
N1 Li2 N2 C19 -110.51(16) . . . . ?
Li1 Li2 N2 C19 -104.70(17) . . . . ?
P4 Li2 N2 C19 130.67(14) . . . . ?
P2 Li2 N2 C19 -5.7(3) . . . . ?
N1 Li2 N2 C22 117.78(13) . . . . ?
Li1 Li2 N2 C22 123.58(13) . . . . ?
P4 Li2 N2 C22 -1.05(12) . . . . ?
P2 Li2 N2 C22 -137.39(16) . . . . ?
N1 Li2 N2 Li1 -5.81(12) . . . . ?
P4 Li2 N2 Li1 -124.63(11) . . . . ?
P2 Li2 N2 Li1 99.03(18) . . . . ?
N1 Li1 N2 C19 135.59(13) . . . . ?
Li2 Li1 N2 C19 129.59(14) . . . . ?
P1 Li1 N2 C19 -125.34(14) . . . . ?
P3 Li1 N2 C19 4.00(13) . . . . ?
N1 Li1 N2 C22 -95.47(16) . . . . ?
Li2 Li1 N2 C22 -101.47(15) . . . . ?
P1 Li1 N2 C22 3.6(2) . . . . ?
P3 Li1 N2 C22 132.94(12) . . . . ?
N1 Li1 N2 Li2 6.00(12) . . . . ?
P1 Li1 N2 Li2 105.07(15) . . . . ?
P3 Li1 N2 Li2 -125.59(11) . . . . ?
N1 Li1 P1 C5 23.46(9) . . . . ?
N2 Li1 P1 C5 -85.54(14) . . . . ?
Li2 Li1 P1 C5 -21.33(14) . . . . ?
P3 Li1 P1 C5 161.79(12) . . . . ?
N1 Li1 P1 C6 136.59(11) . . . . ?
N2 Li1 P1 C6 27.6(2) . . . . ?
Li2 Li1 P1 C6 91.80(17) . . . . ?
P3 Li1 P1 C6 -85.07(17) . . . . ?
N1 Li1 P1 C9 -80.60(10) . . . . ?
N2 Li1 P1 C9 170.39(13) . . . . ?
Li2 Li1 P1 C9 -125.39(13) . . . . ?
P3 Li1 P1 C9 57.73(14) . . . . ?
N2 Li2 P2 C12 -84.43(18) . . . . ?
N1 Li2 P2 C12 26.77(9) . . . . ?
Li1 Li2 P2 C12 -17.20(14) . . . . ?
P4 Li2 P2 C12 149.30(12) . . . . ?
N2 Li2 P2 C13 17.7(3) . . . . ?
N1 Li2 P2 C13 128.86(12) . . . . ?
Li1 Li2 P2 C13 84.90(18) . . . . ?
P4 Li2 P2 C13 -108.61(15) . . . . ?
N2 Li2 P2 C16 175.97(16) . . . . ?
N1 Li2 P2 C16 -72.83(10) . . . . ?
Li1 Li2 P2 C16 -116.79(14) . . . . ?
P4 Li2 P2 C16 49.70(13) . . . . ?
N2 Li2 P4 C34 -77.07(11) . . . . ?
N1 Li2 P4 C34 175.95(10) . . . . ?
Li1 Li2 P4 C34 -124.35(12) . . . . ?
P2 Li2 P4 C34 68.55(14) . . . . ?
N2 Li2 P4 C30 24.28(9) . . . . ?
N1 Li2 P4 C30 -82.70(12) . . . . ?
Li1 Li2 P4 C30 -23.00(13) . . . . ?
P2 Li2 P4 C30 169.90(12) . . . . ?
N2 Li2 P4 C31 135.43(9) . . . . ?
N1 Li2 P4 C31 28.45(17) . . . . ?
Li1 Li2 P4 C31 88.15(15) . . . . ?
P2 Li2 P4 C31 -78.95(14) . . . . ?
C4 N1 C1 C2 0.31(16) . . . . ?
Li1 N1 C1 C2 143.90(13) . . . . ?
Li2 N1 C1 C2 -130.19(15) . . . . ?
C4 N1 C1 C5 -173.72(12) . . . . ?
Li1 N1 C1 C5 -30.13(18) . . . . ?
Li2 N1 C1 C5 55.8(2) . . . . ?
N1 C1 C2 C3 0.03(17) . . . . ?
C5 C1 C2 C3 173.67(14) . . . . ?
C1 C2 C3 C4 -0.37(18) . . . . ?
C2 C3 C4 N1 0.58(17) . . . . ?
C2 C3 C4 C12 174.21(14) . . . . ?
C1 N1 C4 C3 -0.55(16) . . . . ?
Li1 N1 C4 C3 -134.70(15) . . . . ?
Li2 N1 C4 C3 143.81(13) . . . . ?
C1 N1 C4 C12 -174.61(13) . . . . ?
Li1 N1 C4 C12 51.2(2) . . . . ?
Li2 N1 C4 C12 -30.25(17) . . . . ?
C2 C1 C5 P1 -116.82(15) . . . . ?
N1 C1 C5 P1 56.21(16) . . . . ?
C6 P1 C5 C1 173.20(10) . . . . ?
C9 P1 C5 C1 66.75(11) . . . . ?
Li1 P1 C5 C1 -41.92(11) . . . . ?
C5 P1 C6 C7 173.01(11) . . . . ?
C9 P1 C6 C7 -78.95(12) . . . . ?
Li1 P1 C6 C7 65.21(17) . . . . ?
C5 P1 C6 C8 50.23(12) . . . . ?
C9 P1 C6 C8 158.27(11) . . . . ?
Li1 P1 C6 C8 -57.56(18) . . . . ?
C5 P1 C9 C11 39.56(13) . . . . ?
C6 P1 C9 C11 -69.45(12) . . . . ?
Li1 P1 C9 C11 132.45(12) . . . . ?
C5 P1 C9 C10 -87.67(11) . . . . ?
C6 P1 C9 C10 163.32(11) . . . . ?
Li1 P1 C9 C10 5.22(13) . . . . ?
C3 C4 C12 P2 -110.32(16) . . . . ?
N1 C4 C12 P2 62.71(16) . . . . ?
C13 P2 C12 C4 169.59(11) . . . . ?
C16 P2 C12 C4 59.43(12) . . . . ?
Li2 P2 C12 C4 -47.29(12) . . . . ?
C12 P2 C13 C15 -171.05(15) . . . . ?
C16 P2 C13 C15 -65.76(17) . . . . ?
Li2 P2 C13 C15 92.59(19) . . . . ?
C12 P2 C13 C14 66.22(15) . . . . ?
C16 P2 C13 C14 171.51(14) . . . . ?
Li2 P2 C13 C14 -30.1(2) . . . . ?
C12 P2 C16 C18 61.68(14) . . . . ?
C13 P2 C16 C18 -44.25(15) . . . . ?
Li2 P2 C16 C18 149.18(13) . . . . ?
C12 P2 C16 C17 -168.35(13) . . . . ?
C13 P2 C16 C17 85.72(14) . . . . ?
Li2 P2 C16 C17 -80.85(15) . . . . ?
C22 N2 C19 C20 -0.30(16) . . . . ?
Li2 N2 C19 C20 -133.18(16) . . . . ?
Li1 N2 C19 C20 139.22(13) . . . . ?
C22 N2 C19 C23 -176.73(13) . . . . ?
Li2 N2 C19 C23 50.4(2) . . . . ?
Li1 N2 C19 C23 -37.20(18) . . . . ?
N2 C19 C20 C21 0.82(17) . . . . ?
C23 C19 C20 C21 176.92(14) . . . . ?
C19 C20 C21 C22 -1.00(17) . . . . ?
C20 C21 C22 N2 0.86(17) . . . . ?
C20 C21 C22 C30 179.18(14) . . . . ?
C19 N2 C22 C21 -0.36(16) . . . . ?
Li2 N2 C22 C21 144.67(13) . . . . ?
Li1 N2 C22 C21 -131.81(14) . . . . ?
C19 N2 C22 C30 -178.83(13) . . . . ?
Li2 N2 C22 C30 -33.80(17) . . . . ?
Li1 N2 C22 C30 49.7(2) . . . . ?
C20 C19 C23 P3 -117.22(15) . . . . ?
N2 C19 C23 P3 58.55(16) . . . . ?
C21 C22 C30 P4 -116.84(15) . . . . ?
N2 C22 C30 P4 61.33(15) . . . . ?
C34 P4 C30 C22 76.82(11) . . . . ?
C31 P4 C30 C22 -173.82(10) . . . . ?
Li2 P4 C30 C22 -44.36(11) . . . . ?
C34 P4 C31 C32 101.69(14) . . . . ?
C30 P4 C31 C32 -5.70(15) . . . . ?
Li2 P4 C31 C32 -106.62(15) . . . . ?
C34 P4 C31 C33 -132.47(12) . . . . ?
C30 P4 C31 C33 120.14(12) . . . . ?
Li2 P4 C31 C33 19.22(16) . . . . ?
C30 P4 C34 C35 68.58(13) . . . . ?
C31 P4 C34 C35 -44.03(14) . . . . ?
Li2 P4 C34 C35 161.76(12) . . . . ?
C30 P4 C34 C36 -165.18(12) . . . . ?
C31 P4 C34 C36 82.21(13) . . . . ?
Li2 P4 C34 C36 -72.00(14) . . . . ?
C29 C27 P3 C24' 173.0(3) . . . . ?
C28 C27 P3 C24' -65.1(3) . . . . ?
C29 C27 P3 C23 57.73(13) . . . . ?
C28 C27 P3 C23 179.56(12) . . . . ?
C29 C27 P3 C24 161.51(14) . . . . ?
C28 C27 P3 C24 -76.66(15) . . . . ?
C29 C27 P3 Li1 -48.73(17) . . . . ?
C28 C27 P3 Li1 73.10(16) . . . . ?
C19 C23 P3 C24' 75.6(3) . . . . ?
C19 C23 P3 C27 -179.56(10) . . . . ?
C19 C23 P3 C24 70.43(12) . . . . ?
C19 C23 P3 Li1 -39.72(11) . . . . ?
N1 Li1 P3 C24' 155.8(3) . . . . ?
N2 Li1 P3 C24' -94.5(3) . . . . ?
Li2 Li1 P3 C24' -140.3(3) . . . . ?
P1 Li1 P3 C24' 36.7(3) . . . . ?
N1 Li1 P3 C27 21.9(2) . . . . ?
N2 Li1 P3 C27 131.58(10) . . . . ?
Li2 Li1 P3 C27 85.77(16) . . . . ?
P1 Li1 P3 C27 -97.18(14) . . . . ?
N1 Li1 P3 C23 -90.35(16) . . . . ?
N2 Li1 P3 C23 19.34(9) . . . . ?
Li2 Li1 P3 C23 -26.47(13) . . . . ?
P1 Li1 P3 C23 150.58(12) . . . . ?
N1 Li1 P3 C24 171.02(17) . . . . ?
N2 Li1 P3 C24 -79.29(13) . . . . ?
Li2 Li1 P3 C24 -125.10(15) . . . . ?
P1 Li1 P3 C24 51.95(16) . . . . ?
C24' P3 C24 C25 44.3(10) . . . . ?
C27 P3 C24 C25 96.12(19) . . . . ?
C23 P3 C24 C25 -155.19(19) . . . . ?
Li1 P3 C24 C25 -62.8(2) . . . . ?
C24' P3 C24 C26 -83.2(11) . . . . ?
C27 P3 C24 C26 -31.4(4) . . . . ?
C23 P3 C24 C26 77.3(4) . . . . ?
Li1 P3 C24 C26 169.8(3) . . . . ?
C27 P3 C24' C25' 168.0(5) . . . . ?
C23 P3 C24' C25' -82.2(5) . . . . ?
C24 P3 C24' C25' -61.4(10) . . . . ?
Li1 P3 C24' C25' 17.2(6) . . . . ?
C27 P3 C24' C26' -69.6(9) . . . . ?
C23 P3 C24' C26' 40.2(10) . . . . ?
C24 P3 C24' C26' 61.0(12) . . . . ?
Li1 P3 C24' C26' 139.7(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.051
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mk97
_database_code_depnum_ccdc_archive 'CCDC 1037226'
_audit_update_record             
;
2014-12-02 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H42 Br N Ni P2'
_chemical_formula_weight         521.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
N N 0.0311 0.0180 '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           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.4257(2)
_cell_length_b                   14.4710(3)
_cell_length_c                   15.0601(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2490.06(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    33151
_cell_measurement_theta_min      4.2190
_cell_measurement_theta_max      75.5700

_exptl_crystal_description       irregular
_exptl_crystal_colour            'intense red'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_absorpt_coefficient_mu    4.257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72361
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52074
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.24
_diffrn_reflns_theta_max         75.69
_reflns_number_total             5154
_reflns_number_gt                4997
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0311P)²+1.4708P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(14)
_chemical_absolute_configuration .
_refine_ls_number_reflns         5154
_refine_ls_number_parameters     256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0241
_refine_ls_wR_factor_ref         0.0599
_refine_ls_wR_factor_gt          0.0593
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
Ni Ni 0.75211(3) 0.30066(2) 0.26864(2) 0.01412(8) Uani 1 1 d . . .
Br Br 0.71795(2) 0.439409(16) 0.196294(17) 0.02837(7) Uani 1 1 d . . .
P1 P 0.60040(5) 0.22344(3) 0.21048(3) 0.01392(10) Uani 1 1 d . . .
P2 P 0.90017(5) 0.35534(4) 0.34919(3) 0.01397(10) Uani 1 1 d . . .
N N 0.78178(16) 0.19117(12) 0.32820(11) 0.0157(3) Uani 1 1 d . . .
C1 C 0.70713(19) 0.11618(14) 0.33359(14) 0.0156(4) Uani 1 1 d . . .
C2 C 0.7476(2) 0.05661(15) 0.39784(13) 0.0190(4) Uani 1 1 d . . .
H2 H 0.7125 0.0000 0.4153 0.023 Uiso 1 1 calc R . .
C3 C 0.8519(2) 0.09555(15) 0.43331(16) 0.0212(5) Uani 1 1 d . . .
H3 H 0.8994 0.0700 0.4789 0.025 Uiso 1 1 calc R . .
C4 C 0.87085(19) 0.17725(15) 0.38889(14) 0.0170(4) Uani 1 1 d . . .
C5 C 0.6035(2) 0.11383(15) 0.27372(16) 0.0212(4) Uani 1 1 d . . .
H5A H 0.5309 0.1071 0.3090 0.025 Uiso 1 1 calc R . .
H5B H 0.6093 0.0607 0.2325 0.025 Uiso 1 1 calc R . .
C6 C 0.6193(2) 0.18812(16) 0.09154(15) 0.0212(5) Uani 1 1 d . . .
C7 C 0.7389(3) 0.1392(2) 0.08888(19) 0.0390(6) Uani 1 1 d . . .
H7A H 0.7548 0.1180 0.0283 0.059 Uiso 1 1 calc R . .
H7B H 0.7377 0.0860 0.1292 0.059 Uiso 1 1 calc R . .
H7C H 0.8002 0.1824 0.1075 0.059 Uiso 1 1 calc R . .
C8 C 0.6259(3) 0.27132(19) 0.02941(17) 0.0354(7) Uani 1 1 d . . .
H8A H 0.6849 0.3148 0.0514 0.053 Uiso 1 1 calc R . .
H8B H 0.5495 0.3020 0.0272 0.053 Uiso 1 1 calc R . .
H8C H 0.6476 0.2506 -0.0303 0.053 Uiso 1 1 calc R . .
C9 C 0.5240(3) 0.12172(18) 0.05920(17) 0.0307(6) Uani 1 1 d . . .
H9A H 0.4493 0.1547 0.0550 0.046 Uiso 1 1 calc R . .
H9B H 0.5163 0.0704 0.1013 0.046 Uiso 1 1 calc R . .
H9C H 0.5454 0.0975 0.0006 0.046 Uiso 1 1 calc R . .
C10 C 0.45135(19) 0.27181(15) 0.23550(15) 0.0182(4) Uani 1 1 d . . .
C11 C 0.4184(2) 0.35026(18) 0.17137(18) 0.0291(6) Uani 1 1 d . . .
H11A H 0.4052 0.3247 0.1119 0.044 Uiso 1 1 calc R . .
H11B H 0.4822 0.3955 0.1691 0.044 Uiso 1 1 calc R . .
H11C H 0.3468 0.3806 0.1922 0.044 Uiso 1 1 calc R . .
C12 C 0.3530(2) 0.19997(17) 0.23371(19) 0.0270(5) Uani 1 1 d . . .
H12A H 0.2785 0.2299 0.2482 0.041 Uiso 1 1 calc R . .
H12B H 0.3694 0.1515 0.2774 0.041 Uiso 1 1 calc R . .
H12C H 0.3481 0.1725 0.1744 0.041 Uiso 1 1 calc R . .
C13 C 0.4633(2) 0.3109(2) 0.32996(17) 0.0300(6) Uani 1 1 d . . .
H13A H 0.5182 0.3629 0.3295 0.045 Uiso 1 1 calc R . .
H13B H 0.4927 0.2626 0.3697 0.045 Uiso 1 1 calc R . .
H13C H 0.3867 0.3321 0.3509 0.045 Uiso 1 1 calc R . .
C14 C 0.9652(2) 0.24745(15) 0.39192(16) 0.0203(5) Uani 1 1 d . . .
H14A H 1.0321 0.2282 0.3544 0.024 Uiso 1 1 calc R . .
H14B H 0.9933 0.2561 0.4536 0.024 Uiso 1 1 calc R . .
C15 C 1.0249(2) 0.41619(16) 0.29302(16) 0.0215(5) Uani 1 1 d . . .
C16 C 1.0367(2) 0.36956(19) 0.20154(18) 0.0312(6) Uani 1 1 d . . .
H16A H 0.9642 0.3783 0.1678 0.047 Uiso 1 1 calc R . .
H16B H 1.0513 0.3033 0.2095 0.047 Uiso 1 1 calc R . .
H16C H 1.1022 0.3974 0.1691 0.047 Uiso 1 1 calc R . .
C17 C 1.0024(2) 0.51965(17) 0.27947(17) 0.0270(5) Uani 1 1 d . . .
H17A H 1.0011 0.5508 0.3373 0.040 Uiso 1 1 calc R . .
H17B H 0.9269 0.5283 0.2498 0.040 Uiso 1 1 calc R . .
H17C H 1.0648 0.5460 0.2427 0.040 Uiso 1 1 calc R . .
C18 C 1.1408(2) 0.40393(18) 0.34351(18) 0.0267(5) Uani 1 1 d . . .
H18A H 1.2043 0.4334 0.3101 0.040 Uiso 1 1 calc R . .
H18B H 1.1576 0.3379 0.3504 0.040 Uiso 1 1 calc R . .
H18C H 1.1344 0.4327 0.4022 0.040 Uiso 1 1 calc R . .
C19 C 0.84782(19) 0.41794(15) 0.45050(14) 0.0171(4) Uani 1 1 d . . .
C20 C 0.7709(2) 0.50081(16) 0.42572(15) 0.0235(5) Uani 1 1 d . . .
H20A H 0.7409 0.5298 0.4799 0.035 Uiso 1 1 calc R . .
H20B H 0.7052 0.4798 0.3891 0.035 Uiso 1 1 calc R . .
H20C H 0.8175 0.5458 0.3923 0.035 Uiso 1 1 calc R . .
C21 C 0.7703(2) 0.35000(16) 0.50338(15) 0.0224(5) Uani 1 1 d . . .
H21A H 0.8177 0.2973 0.5229 0.034 Uiso 1 1 calc R . .
H21B H 0.7064 0.3280 0.4655 0.034 Uiso 1 1 calc R . .
H21C H 0.7377 0.3816 0.5553 0.034 Uiso 1 1 calc R . .
C22 C 0.9493(2) 0.44978(18) 0.50929(15) 0.0219(5) Uani 1 1 d . . .
H22A H 0.9949 0.4969 0.4779 0.033 Uiso 1 1 calc R . .
H22B H 0.9997 0.3969 0.5231 0.033 Uiso 1 1 calc R . .
H22C H 0.9183 0.4759 0.5645 0.033 Uiso 1 1 calc R . .


_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
Ni N 1.8520(18) . ?
Ni P2 2.2270(6) . ?
Ni P1 2.2407(6) . ?
Ni Br 2.3175(4) . ?
P1 C5 1.851(2) . ?
P1 C6 1.875(2) . ?
P1 C10 1.879(2) . ?
P2 C14 1.845(2) . ?
P2 C19 1.872(2) . ?
P2 C15 1.876(2) . ?
N C1 1.383(3) . ?
N C4 1.383(3) . ?
C1 C2 1.376(3) . ?
C1 C5 1.489(3) . ?
C2 C3 1.422(3) . ?
C3 C4 1.375(3) . ?
C4 C14 1.482(3) . ?
C6 C8 1.527(3) . ?
C6 C9 1.531(3) . ?
C6 C7 1.540(4) . ?
C10 C12 1.531(3) . ?
C10 C13 1.537(3) . ?
C10 C11 1.537(3) . ?
C15 C17 1.533(3) . ?
C15 C18 1.538(3) . ?
C15 C16 1.540(3) . ?
C19 C22 1.530(3) . ?
C19 C20 1.533(3) . ?
C19 C21 1.544(3) . ?

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
N Ni P2 84.32(6) . . ?
N Ni P1 84.51(6) . . ?
P2 Ni P1 167.90(2) . . ?
N Ni Br 178.67(6) . . ?
P2 Ni Br 94.371(19) . . ?
P1 Ni Br 96.778(19) . . ?
C5 P1 C6 104.82(10) . . ?
C5 P1 C10 103.50(11) . . ?
C6 P1 C10 113.41(10) . . ?
C5 P1 Ni 102.21(7) . . ?
C6 P1 Ni 114.86(8) . . ?
C10 P1 Ni 115.90(7) . . ?
C14 P2 C19 104.71(10) . . ?
C14 P2 C15 104.38(11) . . ?
C19 P2 C15 112.51(10) . . ?
C14 P2 Ni 101.27(7) . . ?
C19 P2 Ni 111.91(7) . . ?
C15 P2 Ni 119.86(8) . . ?
C1 N C4 107.51(17) . . ?
C1 N Ni 125.94(15) . . ?
C4 N Ni 125.42(15) . . ?
C2 C1 N 108.99(19) . . ?
C2 C1 C5 132.8(2) . . ?
N C1 C5 118.23(18) . . ?
C1 C2 C3 107.32(19) . . ?
C4 C3 C2 106.8(2) . . ?
C3 C4 N 109.3(2) . . ?
C3 C4 C14 133.5(2) . . ?
N C4 C14 117.13(19) . . ?
C1 C5 P1 107.90(15) . . ?
C8 C6 C9 109.6(2) . . ?
C8 C6 C7 107.6(2) . . ?
C9 C6 C7 109.5(2) . . ?
C8 C6 P1 112.10(16) . . ?
C9 C6 P1 113.15(17) . . ?
C7 C6 P1 104.61(17) . . ?
C12 C10 C13 109.4(2) . . ?
C12 C10 C11 108.1(2) . . ?
C13 C10 C11 109.4(2) . . ?
C12 C10 P1 114.13(15) . . ?
C13 C10 P1 104.00(16) . . ?
C11 C10 P1 111.77(16) . . ?
C4 C14 P2 106.03(15) . . ?
C17 C15 C18 108.83(19) . . ?
C17 C15 C16 108.9(2) . . ?
C18 C15 C16 108.4(2) . . ?
C17 C15 P2 113.03(16) . . ?
C18 C15 P2 112.15(16) . . ?
C16 C15 P2 105.34(15) . . ?
C22 C19 C20 109.86(18) . . ?
C22 C19 C21 109.13(19) . . ?
C20 C19 C21 107.17(18) . . ?
C22 C19 P2 112.03(15) . . ?
C20 C19 P2 111.30(15) . . ?
C21 C19 P2 107.18(15) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N Ni P1 C5 6.89(10) . . . . ?
P2 Ni P1 C5 -15.79(16) . . . . ?
Br Ni P1 C5 -172.79(8) . . . . ?
N Ni P1 C6 -105.99(10) . . . . ?
P2 Ni P1 C6 -128.67(14) . . . . ?
Br Ni P1 C6 74.34(8) . . . . ?
N Ni P1 C10 118.64(10) . . . . ?
P2 Ni P1 C10 95.96(15) . . . . ?
Br Ni P1 C10 -61.04(8) . . . . ?
N Ni P2 C14 13.92(9) . . . . ?
P1 Ni P2 C14 36.61(15) . . . . ?
Br Ni P2 C14 -166.30(8) . . . . ?
N Ni P2 C19 -97.13(9) . . . . ?
P1 Ni P2 C19 -74.44(15) . . . . ?
Br Ni P2 C19 82.65(8) . . . . ?
N Ni P2 C15 127.90(10) . . . . ?
P1 Ni P2 C15 150.59(14) . . . . ?
Br Ni P2 C15 -52.32(9) . . . . ?
P2 Ni N C1 163.78(17) . . . . ?
P1 Ni N C1 -11.57(16) . . . . ?
Br Ni N C1 154(3) . . . . ?
P2 Ni N C4 -2.57(16) . . . . ?
P1 Ni N C4 -177.91(17) . . . . ?
Br Ni N C4 -12(3) . . . . ?
C4 N C1 C2 1.0(2) . . . . ?
Ni N C1 C2 -167.39(14) . . . . ?
C4 N C1 C5 -179.39(19) . . . . ?
Ni N C1 C5 12.3(3) . . . . ?
N C1 C2 C3 -0.5(2) . . . . ?
C5 C1 C2 C3 180.0(2) . . . . ?
C1 C2 C3 C4 -0.2(3) . . . . ?
C2 C3 C4 N 0.8(3) . . . . ?
C2 C3 C4 C14 -177.1(2) . . . . ?
C1 N C4 C3 -1.1(2) . . . . ?
Ni N C4 C3 167.33(15) . . . . ?
C1 N C4 C14 177.19(18) . . . . ?
Ni N C4 C14 -14.4(3) . . . . ?
C2 C1 C5 P1 175.7(2) . . . . ?
N C1 C5 P1 -3.8(2) . . . . ?
C6 P1 C5 C1 116.80(17) . . . . ?
C10 P1 C5 C1 -124.11(16) . . . . ?
Ni P1 C5 C1 -3.34(17) . . . . ?
C5 P1 C6 C8 -176.7(2) . . . . ?
C10 P1 C6 C8 71.1(2) . . . . ?
Ni P1 C6 C8 -65.4(2) . . . . ?
C5 P1 C6 C9 58.8(2) . . . . ?
C10 P1 C6 C9 -53.4(2) . . . . ?
Ni P1 C6 C9 170.08(15) . . . . ?
C5 P1 C6 C7 -60.36(19) . . . . ?
C10 P1 C6 C7 -172.55(17) . . . . ?
Ni P1 C6 C7 50.96(18) . . . . ?
C5 P1 C10 C12 -42.5(2) . . . . ?
C6 P1 C10 C12 70.5(2) . . . . ?
Ni P1 C10 C12 -153.51(15) . . . . ?
C5 P1 C10 C13 76.57(17) . . . . ?
C6 P1 C10 C13 -170.44(15) . . . . ?
Ni P1 C10 C13 -34.43(17) . . . . ?
C5 P1 C10 C11 -165.55(17) . . . . ?
C6 P1 C10 C11 -52.6(2) . . . . ?
Ni P1 C10 C11 83.45(17) . . . . ?
C3 C4 C14 P2 -157.4(2) . . . . ?
N C4 C14 P2 24.8(2) . . . . ?
C19 P2 C14 C4 93.34(16) . . . . ?
C15 P2 C14 C4 -148.24(15) . . . . ?
Ni P2 C14 C4 -23.13(16) . . . . ?
C14 P2 C15 C17 -161.09(17) . . . . ?
C19 P2 C15 C17 -48.1(2) . . . . ?
Ni P2 C15 C17 86.59(17) . . . . ?
C14 P2 C15 C18 -37.60(19) . . . . ?
C19 P2 C15 C18 75.36(19) . . . . ?
Ni P2 C15 C18 -149.92(14) . . . . ?
C14 P2 C15 C16 80.14(18) . . . . ?
C19 P2 C15 C16 -166.90(16) . . . . ?
Ni P2 C15 C16 -32.18(19) . . . . ?
C14 P2 C19 C22 67.19(18) . . . . ?
C15 P2 C19 C22 -45.57(19) . . . . ?
Ni P2 C19 C22 176.05(14) . . . . ?
C14 P2 C19 C20 -169.37(16) . . . . ?
C15 P2 C19 C20 77.87(18) . . . . ?
Ni P2 C19 C20 -60.51(17) . . . . ?
C14 P2 C19 C21 -52.49(17) . . . . ?
C15 P2 C19 C21 -165.25(15) . . . . ?
Ni P2 C19 C21 56.37(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        75.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.055
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mk109
_database_code_depnum_ccdc_archive 'CCDC 1037227'
_audit_update_record             
;
2014-12-02 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H90 Hg N2 Ni2 P4'
_chemical_formula_weight         1161.13

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.9339(5)
_cell_length_b                   16.4179(5)
_cell_length_c                   24.9947(8)
_cell_angle_alpha                108.376(3)
_cell_angle_beta                 96.539(3)
_cell_angle_gamma                97.870(3)
_cell_volume                     5299.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    28539
_cell_measurement_theta_min      2.5910
_cell_measurement_theta_max      29.8110

_exptl_crystal_description       'cut tablet'
_exptl_crystal_colour            'red-olive dichroic'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2400
_exptl_absorpt_coefficient_mu    3.747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76320
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1419
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            294221
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         30.94
_reflns_number_total             31636
_reflns_number_gt                23002
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0236P)²+0.9753P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         31636
_refine_ls_number_parameters     1111
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0760
_refine_ls_wR_factor_gt          0.0672
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.004
_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
Hg Hg 0.973348(8) 0.267762(7) 0.197391(5) 0.01274(3) Uani 1 1 d . . .
Ni1 Ni 1.13318(3) 0.23210(3) 0.246829(17) 0.01312(9) Uani 1 1 d . . .
Ni2 Ni 0.81395(3) 0.30676(2) 0.149933(17) 0.01210(8) Uani 1 1 d . . .
P1 P 1.11967(6) 0.29807(5) 0.33724(4) 0.01534(18) Uani 1 1 d . . .
P2 P 1.17867(6) 0.14751(5) 0.16889(4) 0.01512(18) Uani 1 1 d . . .
P3 P 0.88725(6) 0.42742(5) 0.13790(4) 0.01395(17) Uani 1 1 d . . .
P4 P 0.70428(6) 0.19582(5) 0.15063(4) 0.01447(17) Uani 1 1 d . . .
N1 N 1.25206(19) 0.21198(17) 0.28361(11) 0.0166(6) Uani 1 1 d . . .
N2 N 0.69917(19) 0.33724(17) 0.11636(12) 0.0162(6) Uani 1 1 d . . .
C1 C 1.2993(2) 0.2582(2) 0.33792(14) 0.0200(7) Uani 1 1 d . . .
C2 C 1.3839(2) 0.2263(2) 0.34882(15) 0.0237(8) Uani 1 1 d . . .
H2 H 1.4302 0.2466 0.3832 0.028 Uiso 1 1 calc R . .
C3 C 1.3872(2) 0.1572(2) 0.29813(16) 0.0241(8) Uani 1 1 d . . .
H3 H 1.4369 0.1227 0.2920 0.029 Uiso 1 1 calc R . .
C4 C 1.3050(2) 0.1497(2) 0.25961(15) 0.0224(8) Uani 1 1 d . . .
C5 C 1.2495(2) 0.3255(2) 0.37302(14) 0.0219(8) Uani 1 1 d . . .
H5A H 1.2800 0.3845 0.3746 0.026 Uiso 1 1 calc R . .
H5B H 1.2540 0.3240 0.4125 0.026 Uiso 1 1 calc R . .
C6 C 1.0785(3) 0.4057(2) 0.36518(14) 0.0238(8) Uani 1 1 d . . .
C7 C 0.9667(3) 0.3945(2) 0.35157(15) 0.0244(8) Uani 1 1 d . . .
H7A H 0.9477 0.4520 0.3602 0.037 Uiso 1 1 calc R . .
H7B H 0.9364 0.3633 0.3748 0.037 Uiso 1 1 calc R . .
H7C H 0.9442 0.3609 0.3109 0.037 Uiso 1 1 calc R . .
C8 C 1.1256(3) 0.4611(2) 0.33232(17) 0.0322(9) Uani 1 1 d . . .
H8A H 1.1078 0.4295 0.2911 0.048 Uiso 1 1 calc R . .
H8B H 1.1972 0.4726 0.3433 0.048 Uiso 1 1 calc R . .
H8C H 1.1018 0.5166 0.3415 0.048 Uiso 1 1 calc R . .
C9 C 1.1143(3) 0.4547(3) 0.42938(16) 0.0436(12) Uani 1 1 d . . .
H9A H 1.1004 0.5141 0.4392 0.065 Uiso 1 1 calc R . .
H9B H 1.1853 0.4574 0.4383 0.065 Uiso 1 1 calc R . .
H9C H 1.0802 0.4239 0.4516 0.065 Uiso 1 1 calc R . .
C10 C 1.0613(2) 0.2155(2) 0.36749(14) 0.0202(7) Uani 1 1 d . . .
C11 C 0.9593(3) 0.1756(2) 0.33346(16) 0.0283(9) Uani 1 1 d . . .
H11D H 0.9297 0.1295 0.3468 0.042 Uiso 1 1 calc R . .
H11E H 0.9636 0.1506 0.2928 0.042 Uiso 1 1 calc R . .
H11F H 0.9186 0.2208 0.3387 0.042 Uiso 1 1 calc R . .
C12 C 1.0529(3) 0.2537(3) 0.43092(16) 0.0374(10) Uani 1 1 d . . .
H12A H 1.0079 0.2954 0.4355 0.056 Uiso 1 1 calc R . .
H12B H 1.1179 0.2837 0.4531 0.056 Uiso 1 1 calc R . .
H12C H 1.0277 0.2065 0.4446 0.056 Uiso 1 1 calc R . .
C13 C 1.1205(3) 0.1422(2) 0.36085(18) 0.0340(10) Uani 1 1 d . . .
H13D H 1.1869 0.1663 0.3828 0.051 Uiso 1 1 calc R . .
H13E H 1.1245 0.1150 0.3204 0.051 Uiso 1 1 calc R . .
H13F H 1.0882 0.0983 0.3751 0.051 Uiso 1 1 calc R . .
C14 C 1.2624(2) 0.0897(2) 0.20032(14) 0.0208(7) Uani 1 1 d . . .
H14C H 1.2257 0.0343 0.2013 0.025 Uiso 1 1 calc R . .
H14D H 1.3152 0.0763 0.1774 0.025 Uiso 1 1 calc R . .
C15 C 1.2623(2) 0.2073(2) 0.13365(14) 0.0170(7) Uani 1 1 d . . .
C16 C 1.3070(2) 0.1474(2) 0.08621(14) 0.0222(8) Uani 1 1 d . . .
H16D H 1.3578 0.1828 0.0747 0.033 Uiso 1 1 calc R . .
H16E H 1.2554 0.1156 0.0532 0.033 Uiso 1 1 calc R . .
H16F H 1.3363 0.1057 0.1005 0.033 Uiso 1 1 calc R . .
C17 C 1.3450(2) 0.2673(2) 0.18126(15) 0.0245(8) Uani 1 1 d . . .
H17A H 1.3831 0.2318 0.1971 0.037 Uiso 1 1 calc R . .
H17B H 1.3165 0.3055 0.2116 0.037 Uiso 1 1 calc R . .
H17C H 1.3881 0.3030 0.1655 0.037 Uiso 1 1 calc R . .
C18 C 1.2074(3) 0.2655(2) 0.10919(16) 0.0259(8) Uani 1 1 d . . .
H18A H 1.2543 0.3055 0.0986 0.039 Uiso 1 1 calc R . .
H18B H 1.1727 0.2993 0.1380 0.039 Uiso 1 1 calc R . .
H18C H 1.1598 0.2291 0.0752 0.039 Uiso 1 1 calc R . .
C19 C 1.0884(2) 0.0548(2) 0.11491(15) 0.0209(7) Uani 1 1 d . . .
C20 C 1.0348(3) 0.0861(2) 0.07014(14) 0.0250(8) Uani 1 1 d . . .
H20A H 1.0789 0.0945 0.0437 0.038 Uiso 1 1 calc R . .
H20B H 1.0148 0.1416 0.0893 0.038 Uiso 1 1 calc R . .
H20C H 0.9765 0.0424 0.0488 0.038 Uiso 1 1 calc R . .
C21 C 1.0138(2) 0.0275(2) 0.14985(16) 0.0268(9) Uani 1 1 d . . .
H21A H 0.9794 0.0756 0.1656 0.040 Uiso 1 1 calc R . .
H21B H 1.0485 0.0133 0.1812 0.040 Uiso 1 1 calc R . .
H21C H 0.9662 -0.0239 0.1250 0.040 Uiso 1 1 calc R . .
C22 C 1.1324(3) -0.0249(2) 0.08462(16) 0.0283(9) Uani 1 1 d . . .
H22A H 1.0807 -0.0696 0.0568 0.042 Uiso 1 1 calc R . .
H22B H 1.1606 -0.0487 0.1129 0.042 Uiso 1 1 calc R . .
H22C H 1.1840 -0.0072 0.0648 0.042 Uiso 1 1 calc R . .
C23 C 0.6983(2) 0.3968(2) 0.08839(14) 0.0171(7) Uani 1 1 d . . .
C24 C 0.6026(2) 0.4039(2) 0.07288(14) 0.0178(7) Uani 1 1 d . . .
H24 H 0.5811 0.4407 0.0531 0.021 Uiso 1 1 calc R . .
C25 C 0.5421(2) 0.3457(2) 0.09210(14) 0.0197(7) Uani 1 1 d . . .
H25 H 0.4724 0.3359 0.0874 0.024 Uiso 1 1 calc R . .
C26 C 0.6034(2) 0.3064(2) 0.11865(14) 0.0183(7) Uani 1 1 d . . .
C27 C 0.7953(2) 0.4395(2) 0.08198(14) 0.0186(7) Uani 1 1 d . . .
H27A H 0.7957 0.5019 0.0875 0.022 Uiso 1 1 calc R . .
H27B H 0.8102 0.4108 0.0434 0.022 Uiso 1 1 calc R . .
C28 C 0.8906(2) 0.5285(2) 0.20101(14) 0.0186(7) Uani 1 1 d . . .
C29 C 0.7846(3) 0.5339(2) 0.21072(15) 0.0271(9) Uani 1 1 d . . .
H29A H 0.7532 0.4789 0.2140 0.041 Uiso 1 1 calc R . .
H29B H 0.7480 0.5443 0.1784 0.041 Uiso 1 1 calc R . .
H29C H 0.7849 0.5820 0.2460 0.041 Uiso 1 1 calc R . .
C30 C 0.9365(3) 0.6138(2) 0.19361(15) 0.0245(8) Uani 1 1 d . . .
H30A H 0.9353 0.6630 0.2279 0.037 Uiso 1 1 calc R . .
H30B H 0.8990 0.6211 0.1603 0.037 Uiso 1 1 calc R . .
H30C H 1.0047 0.6117 0.1878 0.037 Uiso 1 1 calc R . .
C31 C 0.9471(3) 0.5191(2) 0.25354(15) 0.0289(9) Uani 1 1 d . . .
H31A H 1.0168 0.5224 0.2501 0.043 Uiso 1 1 calc R . .
H31B H 0.9212 0.4627 0.2569 0.043 Uiso 1 1 calc R . .
H31C H 0.9399 0.5663 0.2876 0.043 Uiso 1 1 calc R . .
C32 C 1.0037(2) 0.4332(2) 0.10653(15) 0.0205(7) Uani 1 1 d . . .
C33 C 0.9959(3) 0.3412(2) 0.06294(15) 0.0261(8) Uani 1 1 d . . .
H33A H 1.0556 0.3381 0.0457 0.039 Uiso 1 1 calc R . .
H33B H 0.9388 0.3291 0.0330 0.039 Uiso 1 1 calc R . .
H33C H 0.9882 0.2979 0.0824 0.039 Uiso 1 1 calc R . .
C34 C 1.0935(2) 0.4535(2) 0.15235(15) 0.0227(8) Uani 1 1 d . . .
H34A H 1.1519 0.4452 0.1342 0.034 Uiso 1 1 calc R . .
H34B H 1.0847 0.4143 0.1746 0.034 Uiso 1 1 calc R . .
H34C H 1.1019 0.5141 0.1777 0.034 Uiso 1 1 calc R . .
C35 C 1.0151(3) 0.4994(2) 0.07474(16) 0.0288(9) Uani 1 1 d . . .
H35A H 1.0229 0.5587 0.1021 0.043 Uiso 1 1 calc R . .
H35B H 0.9566 0.4878 0.0458 0.043 Uiso 1 1 calc R . .
H35C H 1.0732 0.4939 0.0561 0.043 Uiso 1 1 calc R . .
C36 C 0.5891(2) 0.2390(2) 0.14715(15) 0.0195(7) Uani 1 1 d . . .
H36A H 0.5335 0.1915 0.1249 0.023 Uiso 1 1 calc R . .
H36B H 0.5745 0.2655 0.1861 0.023 Uiso 1 1 calc R . .
C37 C 0.6999(2) 0.1569(2) 0.21369(14) 0.0188(7) Uani 1 1 d . . .
C38 C 0.5982(2) 0.1111(2) 0.21722(16) 0.0274(8) Uani 1 1 d . . .
H38A H 0.5760 0.0587 0.1833 0.041 Uiso 1 1 calc R . .
H38B H 0.5513 0.1509 0.2189 0.041 Uiso 1 1 calc R . .
H38C H 0.6024 0.0944 0.2517 0.041 Uiso 1 1 calc R . .
C39 C 0.7736(2) 0.0967(2) 0.21495(15) 0.0227(8) Uani 1 1 d . . .
H39A H 0.8376 0.1239 0.2101 0.034 Uiso 1 1 calc R . .
H39B H 0.7506 0.0409 0.1839 0.034 Uiso 1 1 calc R . .
H39C H 0.7799 0.0867 0.2517 0.034 Uiso 1 1 calc R . .
C40 C 0.7307(3) 0.2400(2) 0.26605(14) 0.0239(8) Uani 1 1 d . . .
H40A H 0.7312 0.2246 0.3009 0.036 Uiso 1 1 calc R . .
H40B H 0.6839 0.2793 0.2653 0.036 Uiso 1 1 calc R . .
H40C H 0.7966 0.2692 0.2654 0.036 Uiso 1 1 calc R . .
C41 C 0.6843(2) 0.1015(2) 0.08126(14) 0.0188(7) Uani 1 1 d . . .
C42 C 0.6513(3) 0.1341(2) 0.03258(14) 0.0273(8) Uani 1 1 d . . .
H42A H 0.6989 0.1852 0.0345 0.041 Uiso 1 1 calc R . .
H42B H 0.5866 0.1503 0.0361 0.041 Uiso 1 1 calc R . .
H42C H 0.6473 0.0877 -0.0041 0.041 Uiso 1 1 calc R . .
C43 C 0.7835(3) 0.0738(2) 0.07214(15) 0.0242(8) Uani 1 1 d . . .
H43A H 0.7755 0.0267 0.0354 0.036 Uiso 1 1 calc R . .
H43B H 0.8077 0.0533 0.1031 0.036 Uiso 1 1 calc R . .
H43C H 0.8309 0.1238 0.0721 0.036 Uiso 1 1 calc R . .
C44 C 0.6086(3) 0.0220(2) 0.07776(16) 0.0305(9) Uani 1 1 d . . .
H44A H 0.5461 0.0403 0.0856 0.046 Uiso 1 1 calc R . .
H44B H 0.6325 -0.0036 0.1061 0.046 Uiso 1 1 calc R . .
H44C H 0.5988 -0.0215 0.0394 0.046 Uiso 1 1 calc R . .
Hg' Hg 0.521469(8) 0.749499(7) 0.303201(5) 0.01230(3) Uani 1 1 d . . .
Ni1' Ni 0.68200(3) 0.71069(2) 0.348473(17) 0.01093(8) Uani 1 1 d . . .
Ni2' Ni 0.36141(3) 0.77700(3) 0.249934(17) 0.01306(9) Uani 1 1 d . . .
P1' P 0.78968(6) 0.82608(5) 0.35103(3) 0.01221(16) Uani 1 1 d . . .
P2' P 0.60459(6) 0.60288(5) 0.37269(4) 0.01595(18) Uani 1 1 d . . .
P3' P 0.38140(6) 0.71050(5) 0.16095(4) 0.01469(17) Uani 1 1 d . . .
P4' P 0.30992(6) 0.86070(5) 0.32541(4) 0.01423(17) Uani 1 1 d . . .
N1' N 0.79853(19) 0.67095(16) 0.37118(11) 0.0151(6) Uani 1 1 d . . .
N2' N 0.24268(19) 0.79192(18) 0.21037(12) 0.0195(6) Uani 1 1 d . . .
C1' C 0.8937(2) 0.7144(2) 0.37930(13) 0.0152(7) Uani 1 1 d . . .
C2' C 0.9554(2) 0.6786(2) 0.40857(13) 0.0164(7) Uani 1 1 d . . .
H2' H 1.0246 0.6965 0.4197 0.020 Uiso 1 1 calc R . .
C3' C 0.8960(2) 0.6095(2) 0.41910(14) 0.0181(7) Uani 1 1 d . . .
H3' H 0.9174 0.5726 0.4388 0.022 Uiso 1 1 calc R . .
C4' C 0.8014(2) 0.6069(2) 0.39514(14) 0.0157(7) Uani 1 1 d . . .
C5' C 0.9072(2) 0.7864(2) 0.35461(14) 0.0157(7) Uani 1 1 d . . .
H5'1 H 0.9245 0.7644 0.3159 0.019 Uiso 1 1 calc R . .
H5'2 H 0.9607 0.8342 0.3791 0.019 Uiso 1 1 calc R . .
C6' C 0.7930(2) 0.8697(2) 0.28996(13) 0.0134(6) Uani 1 1 d . . .
C7' C 0.8944(2) 0.9173(2) 0.28706(15) 0.0215(8) Uani 1 1 d . . .
H7'1 H 0.9417 0.8776 0.2842 0.032 Uiso 1 1 calc R . .
H7'2 H 0.9166 0.9685 0.3217 0.032 Uiso 1 1 calc R . .
H7'3 H 0.8897 0.9360 0.2534 0.032 Uiso 1 1 calc R . .
C8' C 0.7177(2) 0.9290(2) 0.29057(14) 0.0197(7) Uani 1 1 d . . .
H8'1 H 0.7107 0.9414 0.2546 0.030 Uiso 1 1 calc R . .
H8'2 H 0.7399 0.9839 0.3226 0.030 Uiso 1 1 calc R . .
H8'3 H 0.6542 0.9000 0.2949 0.030 Uiso 1 1 calc R . .
C9' C 0.7623(2) 0.7888(2) 0.23586(14) 0.0202(7) Uani 1 1 d . . .
H9'1 H 0.7600 0.8068 0.2020 0.030 Uiso 1 1 calc R . .
H9'2 H 0.6972 0.7579 0.2363 0.030 Uiso 1 1 calc R . .
H9'3 H 0.8101 0.7499 0.2347 0.030 Uiso 1 1 calc R . .
C10' C 0.8075(2) 0.9182(2) 0.42186(14) 0.0160(7) Uani 1 1 d . . .
C11' C 0.7060(2) 0.9387(2) 0.43246(14) 0.0196(7) Uani 1 1 d . . .
H11A H 0.7126 0.9849 0.4695 0.029 Uiso 1 1 calc R . .
H11B H 0.6634 0.8861 0.4325 0.029 Uiso 1 1 calc R . .
H11C H 0.6772 0.9583 0.4021 0.029 Uiso 1 1 calc R . .
C12' C 0.8769(2) 1.0016(2) 0.42594(15) 0.0227(8) Uani 1 1 d . . .
H12D H 0.8478 1.0279 0.3993 0.034 Uiso 1 1 calc R . .
H12E H 0.9400 0.9872 0.4160 0.034 Uiso 1 1 calc R . .
H12F H 0.8873 1.0430 0.4650 0.034 Uiso 1 1 calc R . .
C13' C 0.8501(2) 0.8861(2) 0.46923(14) 0.0212(7) Uani 1 1 d . . .
H13A H 0.8460 0.9275 0.5066 0.032 Uiso 1 1 calc R . .
H13B H 0.9190 0.8817 0.4667 0.032 Uiso 1 1 calc R . .
H13C H 0.8126 0.8286 0.4646 0.032 Uiso 1 1 calc R . .
C14' C 0.7064(2) 0.5469(2) 0.38769(15) 0.0220(8) Uani 1 1 d . . .
H14A H 0.7012 0.5322 0.4229 0.026 Uiso 1 1 calc R . .
H14B H 0.7029 0.4921 0.3556 0.026 Uiso 1 1 calc R . .
C15' C 0.5114(2) 0.5099(2) 0.32113(15) 0.0203(7) Uani 1 1 d . . .
C16' C 0.5492(3) 0.4917(2) 0.26403(15) 0.0247(8) Uani 1 1 d . . .
H16A H 0.6140 0.4753 0.2680 0.037 Uiso 1 1 calc R . .
H16B H 0.5544 0.5443 0.2531 0.037 Uiso 1 1 calc R . .
H16C H 0.5033 0.4438 0.2345 0.037 Uiso 1 1 calc R . .
C17' C 0.5002(3) 0.4247(2) 0.33543(16) 0.0271(8) Uani 1 1 d . . .
H17D H 0.4809 0.4356 0.3732 0.041 Uiso 1 1 calc R . .
H17E H 0.5630 0.4040 0.3356 0.041 Uiso 1 1 calc R . .
H17F H 0.4497 0.3802 0.3066 0.041 Uiso 1 1 calc R . .
C18' C 0.4101(2) 0.5344(2) 0.31519(15) 0.0243(8) Uani 1 1 d . . .
H18D H 0.3667 0.4897 0.2824 0.036 Uiso 1 1 calc R . .
H18E H 0.4158 0.5909 0.3092 0.036 Uiso 1 1 calc R . .
H18F H 0.3826 0.5383 0.3501 0.036 Uiso 1 1 calc R . .
C19' C 0.5662(2) 0.6453(2) 0.44503(14) 0.0198(7) Uani 1 1 d . . .
C20' C 0.5301(3) 0.5752(2) 0.47022(16) 0.0327(9) Uani 1 1 d . . .
H20D H 0.5183 0.6033 0.5091 0.049 Uiso 1 1 calc R . .
H20E H 0.5801 0.5389 0.4712 0.049 Uiso 1 1 calc R . .
H20F H 0.4689 0.5387 0.4465 0.049 Uiso 1 1 calc R . .
C21' C 0.4869(3) 0.6999(2) 0.44304(15) 0.0267(8) Uani 1 1 d . . .
H21D H 0.4247 0.6616 0.4222 0.040 Uiso 1 1 calc R . .
H21E H 0.5061 0.7413 0.4235 0.040 Uiso 1 1 calc R . .
H21F H 0.4788 0.7321 0.4821 0.040 Uiso 1 1 calc R . .
C22' C 0.6578(3) 0.7071(2) 0.48463(15) 0.0305(9) Uani 1 1 d . . .
H22D H 0.6427 0.7314 0.5232 0.046 Uiso 1 1 calc R . .
H22E H 0.6775 0.7546 0.4701 0.046 Uiso 1 1 calc R . .
H22F H 0.7115 0.6746 0.4858 0.046 Uiso 1 1 calc R . .
C23' C 0.1979(2) 0.7434(2) 0.15566(15) 0.0207(7) Uani 1 1 d . . .
C24' C 0.1136(2) 0.7727(2) 0.14273(15) 0.0251(8) Uani 1 1 d . . .
H24' H 0.0690 0.7503 0.1076 0.030 Uiso 1 1 calc R . .
C25' C 0.1057(3) 0.8430(2) 0.19182(16) 0.0255(8) Uani 1 1 d . . .
H25' H 0.0548 0.8763 0.1959 0.031 Uiso 1 1 calc R . .
C26' C 0.1864(2) 0.8533(2) 0.23234(14) 0.0201(7) Uani 1 1 d . . .
C27' C 0.2528(2) 0.6782(2) 0.12258(15) 0.0226(8) Uani 1 1 d . . .
H27C H 0.2500 0.6790 0.0830 0.027 Uiso 1 1 calc R . .
H27D H 0.2244 0.6187 0.1210 0.027 Uiso 1 1 calc R . .
C28' C 0.4375(2) 0.7940(2) 0.13072(14) 0.0174(7) Uani 1 1 d . . .
C29' C 0.3754(3) 0.8660(2) 0.13716(17) 0.0317(9) Uani 1 1 d . . .
H29D H 0.3714 0.8932 0.1776 0.048 Uiso 1 1 calc R . .
H29E H 0.3092 0.8404 0.1154 0.048 Uiso 1 1 calc R . .
H29F H 0.4062 0.9102 0.1226 0.048 Uiso 1 1 calc R . .
C30' C 0.4451(3) 0.7563(3) 0.06748(15) 0.0330(9) Uani 1 1 d . . .
H30D H 0.4672 0.8040 0.0535 0.050 Uiso 1 1 calc R . .
H30E H 0.3806 0.7242 0.0457 0.050 Uiso 1 1 calc R . .
H30F H 0.4925 0.7167 0.0627 0.050 Uiso 1 1 calc R . .
C31' C 0.5394(3) 0.8363(2) 0.16525(16) 0.0283(9) Uani 1 1 d . . .
H31D H 0.5823 0.7927 0.1591 0.042 Uiso 1 1 calc R . .
H31E H 0.5348 0.8590 0.2060 0.042 Uiso 1 1 calc R . .
H31F H 0.5667 0.8843 0.1529 0.042 Uiso 1 1 calc R . .
C32' C 0.4283(2) 0.6051(2) 0.13583(14) 0.0183(7) Uani 1 1 d . . .
C33' C 0.3816(3) 0.5494(2) 0.16815(16) 0.0270(8) Uani 1 1 d . . .
H33D H 0.4053 0.4939 0.1586 0.040 Uiso 1 1 calc R . .
H33E H 0.3099 0.5380 0.1572 0.040 Uiso 1 1 calc R . .
H33F H 0.3995 0.5805 0.2094 0.040 Uiso 1 1 calc R . .
C34' C 0.5396(2) 0.6186(2) 0.15115(15) 0.0227(8) Uani 1 1 d . . .
H34D H 0.5602 0.6543 0.1916 0.034 Uiso 1 1 calc R . .
H34E H 0.5704 0.6483 0.1273 0.034 Uiso 1 1 calc R . .
H34F H 0.5598 0.5618 0.1444 0.034 Uiso 1 1 calc R . .
C35' C 0.3976(3) 0.5549(2) 0.07147(15) 0.0367(10) Uani 1 1 d . . .
H35D H 0.4301 0.5878 0.0499 0.055 Uiso 1 1 calc R . .
H35E H 0.3262 0.5473 0.0611 0.055 Uiso 1 1 calc R . .
H35F H 0.4170 0.4975 0.0624 0.055 Uiso 1 1 calc R . .
C36' C 0.2260(2) 0.9153(2) 0.29136(14) 0.0213(8) Uani 1 1 d . . .
H36C H 0.1719 0.9285 0.3133 0.026 Uiso 1 1 calc R . .
H36D H 0.2621 0.9707 0.2898 0.026 Uiso 1 1 calc R . .
C37' C 0.3967(2) 0.9550(2) 0.38046(14) 0.0190(7) Uani 1 1 d . . .
C38' C 0.4727(2) 0.9838(2) 0.34714(16) 0.0246(8) Uani 1 1 d . . .
H38D H 0.5208 1.0339 0.3731 0.037 Uiso 1 1 calc R . .
H38E H 0.4395 1.0005 0.3165 0.037 Uiso 1 1 calc R . .
H38F H 0.5064 0.9355 0.3305 0.037 Uiso 1 1 calc R . .
C39' C 0.4489(2) 0.9257(2) 0.42621(14) 0.0231(8) Uani 1 1 d . . .
H39D H 0.4746 0.8730 0.4079 0.035 Uiso 1 1 calc R . .
H39E H 0.4024 0.9132 0.4504 0.035 Uiso 1 1 calc R . .
H39F H 0.5033 0.9722 0.4497 0.035 Uiso 1 1 calc R . .
C40' C 0.3495(3) 1.0341(2) 0.40875(15) 0.0249(8) Uani 1 1 d . . .
H40D H 0.2954 1.0156 0.4267 0.037 Uiso 1 1 calc R . .
H40E H 0.3240 1.0576 0.3796 0.037 Uiso 1 1 calc R . .
H40F H 0.3989 1.0793 0.4379 0.037 Uiso 1 1 calc R . .
C41' C 0.2249(2) 0.7993(2) 0.35902(14) 0.0175(7) Uani 1 1 d . . .
C42' C 0.2790(2) 0.7398(2) 0.38244(15) 0.0226(8) Uani 1 1 d . . .
H42D H 0.2319 0.7004 0.3934 0.034 Uiso 1 1 calc R . .
H42E H 0.3279 0.7753 0.4160 0.034 Uiso 1 1 calc R . .
H42F H 0.3121 0.7053 0.3530 0.034 Uiso 1 1 calc R . .
C43' C 0.1818(2) 0.8596(2) 0.40683(14) 0.0208(7) Uani 1 1 d . . .
H43D H 0.1325 0.8246 0.4195 0.031 Uiso 1 1 calc R . .
H43E H 0.1510 0.9005 0.3925 0.031 Uiso 1 1 calc R . .
H43F H 0.2345 0.8924 0.4391 0.031 Uiso 1 1 calc R . .
C44' C 0.1414(2) 0.7419(2) 0.31153(14) 0.0214(8) Uani 1 1 d . . .
H44D H 0.1686 0.7031 0.2809 0.032 Uiso 1 1 calc R . .
H44E H 0.1050 0.7789 0.2962 0.032 Uiso 1 1 calc R . .
H44F H 0.0969 0.7069 0.3270 0.032 Uiso 1 1 calc R . .
C81 C 0.6816(3) 0.6895(2) 0.02402(16) 0.0298(9) Uani 1 1 d . . .
H81 H 0.6186 0.6567 0.0048 0.036 Uiso 1 1 calc R . .
C82 C 0.6982(3) 0.7789(3) 0.04117(17) 0.0313(9) Uani 1 1 d . . .
H82 H 0.6469 0.8082 0.0333 0.038 Uiso 1 1 calc R . .
C83 C 0.7885(3) 0.8259(3) 0.0696(2) 0.0420(11) Uani 1 1 d . . .
H83 H 0.7995 0.8878 0.0817 0.050 Uiso 1 1 calc R . .
C84 C 0.8638(3) 0.7838(3) 0.0808(2) 0.0422(11) Uani 1 1 d . . .
H84 H 0.9265 0.8168 0.1005 0.051 Uiso 1 1 calc R . .
C85 C 0.8479(3) 0.6944(2) 0.06346(17) 0.0317(9) Uani 1 1 d . . .
H85 H 0.8993 0.6651 0.0711 0.038 Uiso 1 1 calc R . .
C86 C 0.7570(3) 0.6476(2) 0.03496(17) 0.0347(10) Uani 1 1 d . . .
H86 H 0.7459 0.5856 0.0226 0.042 Uiso 1 1 calc R . .
C91 C 0.6608(3) 0.3082(3) 0.42024(17) 0.0348(10) Uani 1 1 d . . .
H91 H 0.6145 0.3371 0.4061 0.042 Uiso 1 1 calc R . .
C92 C 0.7495(3) 0.3552(3) 0.45229(19) 0.0454(12) Uani 1 1 d . . .
H92 H 0.7651 0.4162 0.4596 0.054 Uiso 1 1 calc R . .
C93 C 0.8158(3) 0.3137(3) 0.47395(19) 0.0424(11) Uani 1 1 d . . .
H93 H 0.8769 0.3462 0.4964 0.051 Uiso 1 1 calc R . .
C94 C 0.7936(3) 0.2259(2) 0.46312(17) 0.0321(9) Uani 1 1 d . . .
H94 H 0.8390 0.1971 0.4780 0.039 Uiso 1 1 calc R . .
C95 C 0.7053(3) 0.1794(3) 0.43062(19) 0.0393(11) Uani 1 1 d . . .
H95 H 0.6896 0.1183 0.4231 0.047 Uiso 1 1 calc R . .
C96 C 0.6392(3) 0.2204(3) 0.40877(18) 0.0362(10) Uani 1 1 d . . .
H96 H 0.5787 0.1875 0.3857 0.043 Uiso 1 1 calc R . .


_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
Hg Ni1 2.6488(4) . ?
Hg Ni2 2.6491(4) . ?
Ni1 N1 1.922(3) . ?
Ni1 P1 2.2191(9) . ?
Ni1 P2 2.2230(9) . ?
Ni2 N2 1.921(3) . ?
Ni2 P4 2.2174(9) . ?
Ni2 P3 2.2248(9) . ?
P1 C5 1.852(3) . ?
P1 C6 1.880(3) . ?
P1 C10 1.885(4) . ?
P2 C14 1.855(3) . ?
P2 C19 1.875(3) . ?
P2 C15 1.888(3) . ?
P3 C27 1.863(3) . ?
P3 C32 1.884(3) . ?
P3 C28 1.885(3) . ?
P4 C36 1.846(3) . ?
P4 C37 1.882(3) . ?
P4 C41 1.887(3) . ?
N1 C1 1.365(4) . ?
N1 C4 1.367(4) . ?
N2 C23 1.370(4) . ?
N2 C26 1.375(4) . ?
C1 C2 1.386(4) . ?
C1 C5 1.487(4) . ?
C2 C3 1.420(5) . ?
C3 C4 1.374(5) . ?
C4 C14 1.496(5) . ?
C6 C7 1.529(5) . ?
C6 C8 1.537(5) . ?
C6 C9 1.538(5) . ?
C10 C11 1.514(5) . ?
C10 C13 1.528(4) . ?
C10 C12 1.535(5) . ?
C15 C18 1.528(4) . ?
C15 C17 1.533(5) . ?
C15 C16 1.537(4) . ?
C19 C20 1.534(5) . ?
C19 C22 1.537(4) . ?
C19 C21 1.539(5) . ?
C23 C24 1.378(4) . ?
C23 C27 1.484(4) . ?
C24 C25 1.419(5) . ?
C25 C26 1.371(4) . ?
C26 C36 1.497(4) . ?
C28 C31 1.514(5) . ?
C28 C30 1.533(5) . ?
C28 C29 1.533(4) . ?
C32 C34 1.519(5) . ?
C32 C35 1.537(5) . ?
C32 C33 1.540(5) . ?
C37 C39 1.524(4) . ?
C37 C40 1.531(5) . ?
C37 C38 1.536(4) . ?
C41 C42 1.526(5) . ?
C41 C43 1.533(4) . ?
C41 C44 1.535(5) . ?
Hg' Ni2' 2.6322(4) . ?
Hg' Ni1' 2.6379(4) . ?
Ni1' N1' 1.923(3) . ?
Ni1' P2' 2.2280(9) . ?
Ni1' P1' 2.2288(9) . ?
Ni2' N2' 1.915(3) . ?
Ni2' P4' 2.2149(9) . ?
Ni2' P3' 2.2157(9) . ?
P1' C5' 1.847(3) . ?
P1' C6' 1.882(3) . ?
P1' C10' 1.895(3) . ?
P2' C14' 1.858(3) . ?
P2' C15' 1.875(3) . ?
P2' C19' 1.889(3) . ?
P3' C27' 1.855(3) . ?
P3' C32' 1.880(3) . ?
P3' C28' 1.886(3) . ?
P4' C36' 1.854(3) . ?
P4' C37' 1.875(3) . ?
P4' C41' 1.886(3) . ?
N1' C4' 1.368(4) . ?
N1' C1' 1.378(4) . ?
N2' C23' 1.370(4) . ?
N2' C26' 1.377(4) . ?
C1' C2' 1.373(4) . ?
C1' C5' 1.496(4) . ?
C2' C3' 1.421(5) . ?
C3' C4' 1.372(4) . ?
C4' C14' 1.493(4) . ?
C6' C8' 1.524(4) . ?
C6' C9' 1.535(4) . ?
C6' C7' 1.539(4) . ?
C10' C11' 1.530(4) . ?
C10' C12' 1.532(4) . ?
C10' C13' 1.534(4) . ?
C15' C18' 1.524(4) . ?
C15' C16' 1.532(5) . ?
C15' C17' 1.542(4) . ?
C19' C21' 1.522(4) . ?
C19' C20' 1.530(5) . ?
C19' C22' 1.537(5) . ?
C23' C24' 1.371(4) . ?
C23' C27' 1.493(4) . ?
C24' C25' 1.422(5) . ?
C25' C26' 1.377(5) . ?
C26' C36' 1.494(5) . ?
C28' C31' 1.522(5) . ?
C28' C30' 1.527(5) . ?
C28' C29' 1.537(4) . ?
C32' C34' 1.522(4) . ?
C32' C33' 1.529(5) . ?
C32' C35' 1.537(5) . ?
C37' C39' 1.523(5) . ?
C37' C38' 1.533(5) . ?
C37' C40' 1.543(4) . ?
C41' C42' 1.527(4) . ?
C41' C44' 1.527(4) . ?
C41' C43' 1.532(4) . ?
C81 C82 1.370(5) . ?
C81 C86 1.380(5) . ?
C82 C83 1.367(5) . ?
C83 C84 1.382(5) . ?
C84 C85 1.371(5) . ?
C85 C86 1.373(5) . ?
C91 C96 1.362(5) . ?
C91 C92 1.374(6) . ?
C92 C93 1.379(5) . ?
C93 C94 1.364(5) . ?
C94 C95 1.371(5) . ?
C95 C96 1.372(5) . ?

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
Ni1 Hg Ni2 178.699(13) . . ?
N1 Ni1 P1 80.98(8) . . ?
N1 Ni1 P2 82.44(8) . . ?
P1 Ni1 P2 162.53(4) . . ?
N1 Ni1 Hg 177.26(8) . . ?
P1 Ni1 Hg 98.24(3) . . ?
P2 Ni1 Hg 98.58(3) . . ?
N2 Ni2 P4 81.95(8) . . ?
N2 Ni2 P3 82.08(8) . . ?
P4 Ni2 P3 164.03(4) . . ?
N2 Ni2 Hg 178.95(8) . . ?
P4 Ni2 Hg 98.82(3) . . ?
P3 Ni2 Hg 97.15(3) . . ?
C5 P1 C6 101.64(16) . . ?
C5 P1 C10 103.54(16) . . ?
C6 P1 C10 111.88(16) . . ?
C5 P1 Ni1 101.79(11) . . ?
C6 P1 Ni1 125.07(12) . . ?
C10 P1 Ni1 109.72(11) . . ?
C14 P2 C19 102.26(15) . . ?
C14 P2 C15 102.56(15) . . ?
C19 P2 C15 111.77(15) . . ?
C14 P2 Ni1 101.11(11) . . ?
C19 P2 Ni1 120.75(11) . . ?
C15 P2 Ni1 114.91(10) . . ?
C27 P3 C32 102.45(15) . . ?
C27 P3 C28 102.77(15) . . ?
C32 P3 C28 111.43(15) . . ?
C27 P3 Ni2 101.59(11) . . ?
C32 P3 Ni2 122.84(11) . . ?
C28 P3 Ni2 112.49(11) . . ?
C36 P4 C37 101.77(15) . . ?
C36 P4 C41 103.08(15) . . ?
C37 P4 C41 111.57(15) . . ?
C36 P4 Ni2 101.87(11) . . ?
C37 P4 Ni2 123.76(11) . . ?
C41 P4 Ni2 111.50(11) . . ?
C1 N1 C4 108.0(3) . . ?
C1 N1 Ni1 126.0(2) . . ?
C4 N1 Ni1 126.0(2) . . ?
C23 N2 C26 107.8(3) . . ?
C23 N2 Ni2 126.1(2) . . ?
C26 N2 Ni2 126.0(2) . . ?
N1 C1 C2 109.4(3) . . ?
N1 C1 C5 116.4(3) . . ?
C2 C1 C5 134.0(3) . . ?
C1 C2 C3 106.1(3) . . ?
C4 C3 C2 107.2(3) . . ?
N1 C4 C3 109.3(3) . . ?
N1 C4 C14 116.0(3) . . ?
C3 C4 C14 134.8(3) . . ?
C1 C5 P1 105.8(2) . . ?
C7 C6 C8 109.2(3) . . ?
C7 C6 C9 110.0(3) . . ?
C8 C6 C9 107.7(3) . . ?
C7 C6 P1 110.9(2) . . ?
C8 C6 P1 104.5(2) . . ?
C9 C6 P1 114.4(2) . . ?
C11 C10 C13 107.8(3) . . ?
C11 C10 C12 108.6(3) . . ?
C13 C10 C12 107.9(3) . . ?
C11 C10 P1 108.4(2) . . ?
C13 C10 P1 110.0(2) . . ?
C12 C10 P1 114.0(3) . . ?
C4 C14 P2 106.6(2) . . ?
C18 C15 C17 107.4(3) . . ?
C18 C15 C16 109.1(3) . . ?
C17 C15 C16 109.4(3) . . ?
C18 C15 P2 110.1(2) . . ?
C17 C15 P2 106.3(2) . . ?
C16 C15 P2 114.3(2) . . ?
C20 C19 C22 109.5(3) . . ?
C20 C19 C21 108.9(3) . . ?
C22 C19 C21 108.7(3) . . ?
C20 C19 P2 110.5(2) . . ?
C22 C19 P2 114.8(2) . . ?
C21 C19 P2 104.3(2) . . ?
N2 C23 C24 109.1(3) . . ?
N2 C23 C27 116.7(3) . . ?
C24 C23 C27 134.2(3) . . ?
C23 C24 C25 106.9(3) . . ?
C26 C25 C24 106.9(3) . . ?
C25 C26 N2 109.3(3) . . ?
C25 C26 C36 135.0(3) . . ?
N2 C26 C36 115.8(3) . . ?
C23 C27 P3 106.2(2) . . ?
C31 C28 C30 109.1(3) . . ?
C31 C28 C29 108.2(3) . . ?
C30 C28 C29 108.4(3) . . ?
C31 C28 P3 108.7(2) . . ?
C30 C28 P3 114.4(2) . . ?
C29 C28 P3 107.9(2) . . ?
C34 C32 C35 108.9(3) . . ?
C34 C32 C33 109.8(3) . . ?
C35 C32 C33 108.2(3) . . ?
C34 C32 P3 110.9(2) . . ?
C35 C32 P3 114.4(2) . . ?
C33 C32 P3 104.4(2) . . ?
C26 C36 P4 107.1(2) . . ?
C39 C37 C40 109.0(3) . . ?
C39 C37 C38 109.1(3) . . ?
C40 C37 C38 108.1(3) . . ?
C39 C37 P4 110.7(2) . . ?
C40 C37 P4 104.7(2) . . ?
C38 C37 P4 115.0(2) . . ?
C42 C41 C43 107.1(3) . . ?
C42 C41 C44 108.6(3) . . ?
C43 C41 C44 109.5(3) . . ?
C42 C41 P4 108.2(2) . . ?
C43 C41 P4 108.0(2) . . ?
C44 C41 P4 115.0(2) . . ?
Ni2' Hg' Ni1' 175.056(13) . . ?
N1' Ni1' P2' 84.06(8) . . ?
N1' Ni1' P1' 83.10(8) . . ?
P2' Ni1' P1' 161.56(4) . . ?
N1' Ni1' Hg' 172.09(8) . . ?
P2' Ni1' Hg' 95.72(3) . . ?
P1' Ni1' Hg' 98.80(2) . . ?
N2' Ni2' P4' 82.54(8) . . ?
N2' Ni2' P3' 81.07(8) . . ?
P4' Ni2' P3' 162.65(4) . . ?
N2' Ni2' Hg' 177.60(9) . . ?
P4' Ni2' Hg' 98.40(3) . . ?
P3' Ni2' Hg' 98.20(3) . . ?
C5' P1' C6' 102.19(14) . . ?
C5' P1' C10' 102.38(14) . . ?
C6' P1' C10' 111.02(14) . . ?
C5' P1' Ni1' 102.19(10) . . ?
C6' P1' Ni1' 123.70(10) . . ?
C10' P1' Ni1' 112.01(11) . . ?
C14' P2' C15' 101.91(15) . . ?
C14' P2' C19' 102.37(16) . . ?
C15' P2' C19' 112.31(16) . . ?
C14' P2' Ni1' 102.05(11) . . ?
C15' P2' Ni1' 123.19(11) . . ?
C19' P2' Ni1' 111.57(11) . . ?
C27' P3' C32' 101.79(15) . . ?
C27' P3' C28' 103.07(15) . . ?
C32' P3' C28' 112.44(15) . . ?
C27' P3' Ni2' 101.80(11) . . ?
C32' P3' Ni2' 124.98(11) . . ?
C28' P3' Ni2' 109.43(10) . . ?
C36' P4' C37' 102.81(15) . . ?
C36' P4' C41' 102.56(15) . . ?
C37' P4' C41' 111.94(15) . . ?
C36' P4' Ni2' 101.11(11) . . ?
C37' P4' Ni2' 120.61(11) . . ?
C41' P4' Ni2' 114.49(10) . . ?
C4' N1' C1' 106.9(3) . . ?
C4' N1' Ni1' 125.5(2) . . ?
C1' N1' Ni1' 125.9(2) . . ?
C23' N2' C26' 107.7(3) . . ?
C23' N2' Ni2' 126.5(2) . . ?
C26' N2' Ni2' 125.8(2) . . ?
C2' C1' N1' 109.6(3) . . ?
C2' C1' C5' 134.9(3) . . ?
N1' C1' C5' 115.5(3) . . ?
C1' C2' C3' 106.9(3) . . ?
C4' C3' C2' 106.3(3) . . ?
N1' C4' C3' 110.4(3) . . ?
N1' C4' C14' 116.2(3) . . ?
C3' C4' C14' 133.3(3) . . ?
C1' C5' P1' 107.1(2) . . ?
C8' C6' C9' 108.4(3) . . ?
C8' C6' C7' 109.7(3) . . ?
C9' C6' C7' 107.9(3) . . ?
C8' C6' P1' 110.5(2) . . ?
C9' C6' P1' 104.9(2) . . ?
C7' C6' P1' 115.1(2) . . ?
C11' C10' C12' 109.9(3) . . ?
C11' C10' C13' 108.4(3) . . ?
C12' C10' C13' 107.3(3) . . ?
C11' C10' P1' 107.5(2) . . ?
C12' C10' P1' 115.1(2) . . ?
C13' C10' P1' 108.4(2) . . ?
C4' C14' P2' 108.3(2) . . ?
C18' C15' C16' 109.8(3) . . ?
C18' C15' C17' 107.7(3) . . ?
C16' C15' C17' 107.8(3) . . ?
C18' C15' P2' 111.6(2) . . ?
C16' C15' P2' 104.7(2) . . ?
C17' C15' P2' 115.2(2) . . ?
C21' C19' C20' 108.5(3) . . ?
C21' C19' C22' 107.0(3) . . ?
C20' C19' C22' 109.6(3) . . ?
C21' C19' P2' 110.8(2) . . ?
C20' C19' P2' 115.2(2) . . ?
C22' C19' P2' 105.3(2) . . ?
N2' C23' C24' 109.5(3) . . ?
N2' C23' C27' 115.8(3) . . ?
C24' C23' C27' 134.5(3) . . ?
C23' C24' C25' 107.0(3) . . ?
C26' C25' C24' 106.7(3) . . ?
N2' C26' C25' 109.1(3) . . ?
N2' C26' C36' 115.6(3) . . ?
C25' C26' C36' 135.2(3) . . ?
C23' C27' P3' 106.0(2) . . ?
C31' C28' C30' 109.4(3) . . ?
C31' C28' C29' 107.8(3) . . ?
C30' C28' C29' 107.5(3) . . ?
C31' C28' P3' 108.4(2) . . ?
C30' C28' P3' 113.8(2) . . ?
C29' C28' P3' 109.8(2) . . ?
C34' C32' C33' 108.8(3) . . ?
C34' C32' C35' 108.9(3) . . ?
C33' C32' C35' 108.0(3) . . ?
C34' C32' P3' 112.0(2) . . ?
C33' C32' P3' 104.7(2) . . ?
C35' C32' P3' 114.1(2) . . ?
C26' C36' P4' 106.5(2) . . ?
C39' C37' C38' 108.8(3) . . ?
C39' C37' C40' 109.9(3) . . ?
C38' C37' C40' 107.9(3) . . ?
C39' C37' P4' 110.8(2) . . ?
C38' C37' P4' 104.4(2) . . ?
C40' C37' P4' 114.7(2) . . ?
C42' C41' C44' 108.1(3) . . ?
C42' C41' C43' 109.5(3) . . ?
C44' C41' C43' 109.2(3) . . ?
C42' C41' P4' 109.9(2) . . ?
C44' C41' P4' 107.0(2) . . ?
C43' C41' P4' 113.0(2) . . ?
C82 C81 C86 119.5(4) . . ?
C83 C82 C81 120.1(4) . . ?
C82 C83 C84 120.4(4) . . ?
C85 C84 C83 119.8(4) . . ?
C84 C85 C86 119.5(4) . . ?
C85 C86 C81 120.7(4) . . ?
C96 C91 C92 120.0(4) . . ?
C91 C92 C93 120.1(4) . . ?
C94 C93 C92 119.9(4) . . ?
C93 C94 C95 119.6(4) . . ?
C94 C95 C96 120.7(4) . . ?
C91 C96 C95 119.8(4) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni2 Hg Ni1 N1 -42.9(19) . . . . ?
Ni2 Hg Ni1 P1 30.3(6) . . . . ?
Ni2 Hg Ni1 P2 -154.4(6) . . . . ?
Ni1 Hg Ni2 N2 21(5) . . . . ?
Ni1 Hg Ni2 P4 -116.5(6) . . . . ?
Ni1 Hg Ni2 P3 63.6(6) . . . . ?
N1 Ni1 P1 C5 24.14(14) . . . . ?
P2 Ni1 P1 C5 42.62(18) . . . . ?
Hg Ni1 P1 C5 -153.21(11) . . . . ?
N1 Ni1 P1 C6 137.60(17) . . . . ?
P2 Ni1 P1 C6 156.08(17) . . . . ?
Hg Ni1 P1 C6 -39.74(15) . . . . ?
N1 Ni1 P1 C10 -85.06(14) . . . . ?
P2 Ni1 P1 C10 -66.58(17) . . . . ?
Hg Ni1 P1 C10 97.60(11) . . . . ?
N1 Ni1 P2 C14 21.24(14) . . . . ?
P1 Ni1 P2 C14 2.84(18) . . . . ?
Hg Ni1 P2 C14 -161.33(12) . . . . ?
N1 Ni1 P2 C19 132.88(16) . . . . ?
P1 Ni1 P2 C19 114.47(17) . . . . ?
Hg Ni1 P2 C19 -49.69(13) . . . . ?
N1 Ni1 P2 C15 -88.36(14) . . . . ?
P1 Ni1 P2 C15 -106.77(16) . . . . ?
Hg Ni1 P2 C15 89.07(12) . . . . ?
N2 Ni2 P3 C27 -20.66(13) . . . . ?
P4 Ni2 P3 C27 -19.38(18) . . . . ?
Hg Ni2 P3 C27 160.06(11) . . . . ?
N2 Ni2 P3 C32 -133.89(16) . . . . ?
P4 Ni2 P3 C32 -132.62(17) . . . . ?
Hg Ni2 P3 C32 46.82(14) . . . . ?
N2 Ni2 P3 C28 88.56(14) . . . . ?
P4 Ni2 P3 C28 89.83(17) . . . . ?
Hg Ni2 P3 C28 -90.73(12) . . . . ?
N2 Ni2 P4 C36 -21.77(14) . . . . ?
P3 Ni2 P4 C36 -23.04(18) . . . . ?
Hg Ni2 P4 C36 157.52(11) . . . . ?
N2 Ni2 P4 C37 -134.81(15) . . . . ?
P3 Ni2 P4 C37 -136.08(16) . . . . ?
Hg Ni2 P4 C37 44.48(13) . . . . ?
N2 Ni2 P4 C41 87.58(14) . . . . ?
P3 Ni2 P4 C41 86.31(17) . . . . ?
Hg Ni2 P4 C41 -93.13(11) . . . . ?
P1 Ni1 N1 C1 -20.6(3) . . . . ?
P2 Ni1 N1 C1 164.9(3) . . . . ?
Hg Ni1 N1 C1 52.9(18) . . . . ?
P1 Ni1 N1 C4 160.5(3) . . . . ?
P2 Ni1 N1 C4 -14.0(3) . . . . ?
Hg Ni1 N1 C4 -125.9(16) . . . . ?
P4 Ni2 N2 C23 -165.4(3) . . . . ?
P3 Ni2 N2 C23 14.3(2) . . . . ?
Hg Ni2 N2 C23 57(5) . . . . ?
P4 Ni2 N2 C26 18.1(2) . . . . ?
P3 Ni2 N2 C26 -162.2(3) . . . . ?
Hg Ni2 N2 C26 -119(5) . . . . ?
C4 N1 C1 C2 0.7(4) . . . . ?
Ni1 N1 C1 C2 -178.3(2) . . . . ?
C4 N1 C1 C5 -175.8(3) . . . . ?
Ni1 N1 C1 C5 5.1(4) . . . . ?
N1 C1 C2 C3 0.0(4) . . . . ?
C5 C1 C2 C3 175.7(4) . . . . ?
C1 C2 C3 C4 -0.8(4) . . . . ?
C1 N1 C4 C3 -1.2(4) . . . . ?
Ni1 N1 C4 C3 177.8(2) . . . . ?
C1 N1 C4 C14 177.8(3) . . . . ?
Ni1 N1 C4 C14 -3.2(4) . . . . ?
C2 C3 C4 N1 1.2(4) . . . . ?
C2 C3 C4 C14 -177.5(4) . . . . ?
N1 C1 C5 P1 17.9(4) . . . . ?
C2 C1 C5 P1 -157.6(4) . . . . ?
C6 P1 C5 C1 -158.3(2) . . . . ?
C10 P1 C5 C1 85.6(2) . . . . ?
Ni1 P1 C5 C1 -28.3(2) . . . . ?
C5 P1 C6 C7 -167.6(2) . . . . ?
C10 P1 C6 C7 -57.7(3) . . . . ?
Ni1 P1 C6 C7 78.8(3) . . . . ?
C5 P1 C6 C8 74.9(3) . . . . ?
C10 P1 C6 C8 -175.2(2) . . . . ?
Ni1 P1 C6 C8 -38.6(3) . . . . ?
C5 P1 C6 C9 -42.5(3) . . . . ?
C10 P1 C6 C9 67.3(3) . . . . ?
Ni1 P1 C6 C9 -156.1(3) . . . . ?
C5 P1 C10 C11 -169.7(2) . . . . ?
C6 P1 C10 C11 81.6(3) . . . . ?
Ni1 P1 C10 C11 -61.7(2) . . . . ?
C5 P1 C10 C13 -52.1(3) . . . . ?
C6 P1 C10 C13 -160.8(2) . . . . ?
Ni1 P1 C10 C13 55.9(3) . . . . ?
C5 P1 C10 C12 69.3(3) . . . . ?
C6 P1 C10 C12 -39.4(3) . . . . ?
Ni1 P1 C10 C12 177.3(2) . . . . ?
N1 C4 C14 P2 22.4(4) . . . . ?
C3 C4 C14 P2 -159.0(4) . . . . ?
C19 P2 C14 C4 -153.4(2) . . . . ?
C15 P2 C14 C4 90.7(2) . . . . ?
Ni1 P2 C14 C4 -28.2(2) . . . . ?
C14 P2 C15 C18 -175.3(2) . . . . ?
C19 P2 C15 C18 75.8(3) . . . . ?
Ni1 P2 C15 C18 -66.6(2) . . . . ?
C14 P2 C15 C17 -59.3(2) . . . . ?
C19 P2 C15 C17 -168.2(2) . . . . ?
Ni1 P2 C15 C17 49.4(2) . . . . ?
C14 P2 C15 C16 61.5(3) . . . . ?
C19 P2 C15 C16 -47.4(3) . . . . ?
Ni1 P2 C15 C16 170.2(2) . . . . ?
C14 P2 C19 C20 -160.3(2) . . . . ?
C15 P2 C19 C20 -51.2(3) . . . . ?
Ni1 P2 C19 C20 88.7(2) . . . . ?
C14 P2 C19 C22 -35.9(3) . . . . ?
C15 P2 C19 C22 73.1(3) . . . . ?
Ni1 P2 C19 C22 -146.9(2) . . . . ?
C14 P2 C19 C21 82.9(2) . . . . ?
C15 P2 C19 C21 -168.0(2) . . . . ?
Ni1 P2 C19 C21 -28.1(3) . . . . ?
C26 N2 C23 C24 0.0(4) . . . . ?
Ni2 N2 C23 C24 -177.0(2) . . . . ?
C26 N2 C23 C27 179.1(3) . . . . ?
Ni2 N2 C23 C27 2.0(4) . . . . ?
N2 C23 C24 C25 -0.2(4) . . . . ?
C27 C23 C24 C25 -179.1(3) . . . . ?
C23 C24 C25 C26 0.4(4) . . . . ?
C24 C25 C26 N2 -0.4(4) . . . . ?
C24 C25 C26 C36 -178.9(3) . . . . ?
C23 N2 C26 C25 0.3(4) . . . . ?
Ni2 N2 C26 C25 177.3(2) . . . . ?
C23 N2 C26 C36 179.1(3) . . . . ?
Ni2 N2 C26 C36 -3.9(4) . . . . ?
N2 C23 C27 P3 -20.8(3) . . . . ?
C24 C23 C27 P3 158.0(3) . . . . ?
C32 P3 C27 C23 154.7(2) . . . . ?
C28 P3 C27 C23 -89.6(2) . . . . ?
Ni2 P3 C27 C23 26.9(2) . . . . ?
C27 P3 C28 C31 168.8(2) . . . . ?
C32 P3 C28 C31 -82.2(3) . . . . ?
Ni2 P3 C28 C31 60.3(3) . . . . ?
C27 P3 C28 C30 -69.1(3) . . . . ?
C32 P3 C28 C30 40.0(3) . . . . ?
Ni2 P3 C28 C30 -177.5(2) . . . . ?
C27 P3 C28 C29 51.6(3) . . . . ?
C32 P3 C28 C29 160.7(2) . . . . ?
Ni2 P3 C28 C29 -56.8(2) . . . . ?
C27 P3 C32 C34 162.0(2) . . . . ?
C28 P3 C32 C34 52.7(3) . . . . ?
Ni2 P3 C32 C34 -85.2(2) . . . . ?
C27 P3 C32 C35 38.3(3) . . . . ?
C28 P3 C32 C35 -71.0(3) . . . . ?
Ni2 P3 C32 C35 151.1(2) . . . . ?
C27 P3 C32 C33 -79.8(2) . . . . ?
C28 P3 C32 C33 171.0(2) . . . . ?
Ni2 P3 C32 C33 33.0(3) . . . . ?
C25 C26 C36 P4 161.6(3) . . . . ?
N2 C26 C36 P4 -16.8(4) . . . . ?
C37 P4 C36 C26 154.5(2) . . . . ?
C41 P4 C36 C26 -89.7(2) . . . . ?
Ni2 P4 C36 C26 25.9(2) . . . . ?
C36 P4 C37 C39 164.7(2) . . . . ?
C41 P4 C37 C39 55.4(3) . . . . ?
Ni2 P4 C37 C39 -82.2(2) . . . . ?
C36 P4 C37 C40 -78.0(2) . . . . ?
C41 P4 C37 C40 172.7(2) . . . . ?
Ni2 P4 C37 C40 35.1(2) . . . . ?
C36 P4 C37 C38 40.5(3) . . . . ?
C41 P4 C37 C38 -68.8(3) . . . . ?
Ni2 P4 C37 C38 153.6(2) . . . . ?
C36 P4 C41 C42 50.9(3) . . . . ?
C37 P4 C41 C42 159.3(2) . . . . ?
Ni2 P4 C41 C42 -57.7(2) . . . . ?
C36 P4 C41 C43 166.5(2) . . . . ?
C37 P4 C41 C43 -85.0(3) . . . . ?
Ni2 P4 C41 C43 57.9(2) . . . . ?
C36 P4 C41 C44 -70.8(3) . . . . ?
C37 P4 C41 C44 37.6(3) . . . . ?
Ni2 P4 C41 C44 -179.4(2) . . . . ?
Ni2' Hg' Ni1' N1' 6.0(6) . . . . ?
Ni2' Hg' Ni1' P2' -81.98(16) . . . . ?
Ni2' Hg' Ni1' P1' 109.43(16) . . . . ?
Ni1' Hg' Ni2' N2' 51(2) . . . . ?
Ni1' Hg' Ni2' P4' 163.87(15) . . . . ?
Ni1' Hg' Ni2' P3' -21.20(17) . . . . ?
N1' Ni1' P1' C5' 13.63(13) . . . . ?
P2' Ni1' P1' C5' 59.84(16) . . . . ?
Hg' Ni1' P1' C5' -158.62(11) . . . . ?
N1' Ni1' P1' C6' 127.45(14) . . . . ?
P2' Ni1' P1' C6' 173.66(14) . . . . ?
Hg' Ni1' P1' C6' -44.80(12) . . . . ?
N1' Ni1' P1' C10' -95.27(13) . . . . ?
P2' Ni1' P1' C10' -49.06(16) . . . . ?
Hg' Ni1' P1' C10' 92.48(11) . . . . ?
N1' Ni1' P2' C14' -6.80(14) . . . . ?
P1' Ni1' P2' C14' -52.90(17) . . . . ?
Hg' Ni1' P2' C14' 165.25(12) . . . . ?
N1' Ni1' P2' C15' -119.87(15) . . . . ?
P1' Ni1' P2' C15' -165.96(15) . . . . ?
Hg' Ni1' P2' C15' 52.18(13) . . . . ?
N1' Ni1' P2' C19' 101.85(14) . . . . ?
P1' Ni1' P2' C19' 55.76(16) . . . . ?
Hg' Ni1' P2' C19' -86.10(12) . . . . ?
N2' Ni2' P3' C27' -24.03(14) . . . . ?
P4' Ni2' P3' C27' -43.40(18) . . . . ?
Hg' Ni2' P3' C27' 153.65(12) . . . . ?
N2' Ni2' P3' C32' -137.67(16) . . . . ?
P4' Ni2' P3' C32' -157.04(17) . . . . ?
Hg' Ni2' P3' C32' 40.01(14) . . . . ?
N2' Ni2' P3' C28' 84.55(14) . . . . ?
P4' Ni2' P3' C28' 65.18(17) . . . . ?
Hg' Ni2' P3' C28' -97.77(11) . . . . ?
N2' Ni2' P4' C36' -22.00(15) . . . . ?
P3' Ni2' P4' C36' -2.71(18) . . . . ?
Hg' Ni2' P4' C36' 160.23(12) . . . . ?
N2' Ni2' P4' C37' -134.25(15) . . . . ?
P3' Ni2' P4' C37' -114.95(17) . . . . ?
Hg' Ni2' P4' C37' 47.99(13) . . . . ?
N2' Ni2' P4' C41' 87.45(15) . . . . ?
P3' Ni2' P4' C41' 106.74(17) . . . . ?
Hg' Ni2' P4' C41' -90.32(12) . . . . ?
P2' Ni1' N1' C4' -4.9(2) . . . . ?
P1' Ni1' N1' C4' 161.8(3) . . . . ?
Hg' Ni1' N1' C4' -93.8(6) . . . . ?
P2' Ni1' N1' C1' -168.1(3) . . . . ?
P1' Ni1' N1' C1' -1.4(2) . . . . ?
Hg' Ni1' N1' C1' 103.0(6) . . . . ?
P4' Ni2' N2' C23' -164.7(3) . . . . ?
P3' Ni2' N2' C23' 21.0(3) . . . . ?
Hg' Ni2' N2' C23' -52(2) . . . . ?
P4' Ni2' N2' C26' 14.6(3) . . . . ?
P3' Ni2' N2' C26' -159.7(3) . . . . ?
Hg' Ni2' N2' C26' 127.7(19) . . . . ?
C4' N1' C1' C2' -0.7(4) . . . . ?
Ni1' N1' C1' C2' 165.1(2) . . . . ?
C4' N1' C1' C5' 178.5(3) . . . . ?
Ni1' N1' C1' C5' -15.8(4) . . . . ?
N1' C1' C2' C3' 0.1(4) . . . . ?
C5' C1' C2' C3' -178.8(3) . . . . ?
C1' C2' C3' C4' 0.5(4) . . . . ?
C1' N1' C4' C3' 1.0(4) . . . . ?
Ni1' N1' C4' C3' -164.8(2) . . . . ?
C1' N1' C4' C14' -175.8(3) . . . . ?
Ni1' N1' C4' C14' 18.4(4) . . . . ?
C2' C3' C4' N1' -0.9(4) . . . . ?
C2' C3' C4' C14' 175.1(3) . . . . ?
C2' C1' C5' P1' -155.3(3) . . . . ?
N1' C1' C5' P1' 25.8(3) . . . . ?
C6' P1' C5' C1' -152.8(2) . . . . ?
C10' P1' C5' C1' 92.1(2) . . . . ?
Ni1' P1' C5' C1' -24.0(2) . . . . ?
C5' P1' C6' C8' -163.6(2) . . . . ?
C10' P1' C6' C8' -55.0(3) . . . . ?
Ni1' P1' C6' C8' 82.6(2) . . . . ?
C5' P1' C6' C9' 79.8(2) . . . . ?
C10' P1' C6' C9' -171.6(2) . . . . ?
Ni1' P1' C6' C9' -34.0(2) . . . . ?
C5' P1' C6' C7' -38.6(3) . . . . ?
C10' P1' C6' C7' 70.0(2) . . . . ?
Ni1' P1' C6' C7' -152.37(18) . . . . ?
C5' P1' C10' C11' -163.2(2) . . . . ?
C6' P1' C10' C11' 88.4(2) . . . . ?
Ni1' P1' C10' C11' -54.4(2) . . . . ?
C5' P1' C10' C12' 73.9(3) . . . . ?
C6' P1' C10' C12' -34.5(3) . . . . ?
Ni1' P1' C10' C12' -177.3(2) . . . . ?
C5' P1' C10' C13' -46.2(2) . . . . ?
C6' P1' C10' C13' -154.6(2) . . . . ?
Ni1' P1' C10' C13' 62.6(2) . . . . ?
N1' C4' C14' P2' -21.9(4) . . . . ?
C3' C4' C14' P2' 162.3(3) . . . . ?
C15' P2' C14' C4' 144.6(2) . . . . ?
C19' P2' C14' C4' -99.1(3) . . . . ?
Ni1' P2' C14' C4' 16.5(2) . . . . ?
C14' P2' C15' C18' 163.9(2) . . . . ?
C19' P2' C15' C18' 55.1(3) . . . . ?
Ni1' P2' C15' C18' -82.9(2) . . . . ?
C14' P2' C15' C16' -77.4(2) . . . . ?
C19' P2' C15' C16' 173.8(2) . . . . ?
Ni1' P2' C15' C16' 35.8(3) . . . . ?
C14' P2' C15' C17' 40.8(3) . . . . ?
C19' P2' C15' C17' -68.1(3) . . . . ?
Ni1' P2' C15' C17' 153.9(2) . . . . ?
C14' P2' C19' C21' 175.9(2) . . . . ?
C15' P2' C19' C21' -75.6(3) . . . . ?
Ni1' P2' C19' C21' 67.4(3) . . . . ?
C14' P2' C19' C20' -60.5(3) . . . . ?
C15' P2' C19' C20' 48.0(3) . . . . ?
Ni1' P2' C19' C20' -169.0(2) . . . . ?
C14' P2' C19' C22' 60.4(2) . . . . ?
C15' P2' C19' C22' 169.0(2) . . . . ?
Ni1' P2' C19' C22' -48.0(2) . . . . ?
C26' N2' C23' C24' -0.4(4) . . . . ?
Ni2' N2' C23' C24' 179.0(2) . . . . ?
C26' N2' C23' C27' 174.7(3) . . . . ?
Ni2' N2' C23' C27' -5.9(4) . . . . ?
N2' C23' C24' C25' 0.1(4) . . . . ?
C27' C23' C24' C25' -173.8(4) . . . . ?
C23' C24' C25' C26' 0.3(4) . . . . ?
C23' N2' C26' C25' 0.6(4) . . . . ?
Ni2' N2' C26' C25' -178.8(2) . . . . ?
C23' N2' C26' C36' -177.5(3) . . . . ?
Ni2' N2' C26' C36' 3.1(4) . . . . ?
C24' C25' C26' N2' -0.5(4) . . . . ?
C24' C25' C26' C36' 177.0(4) . . . . ?
N2' C23' C27' P3' -17.2(4) . . . . ?
C24' C23' C27' P3' 156.3(4) . . . . ?
C32' P3' C27' C23' 157.9(2) . . . . ?
C28' P3' C27' C23' -85.5(3) . . . . ?
Ni2' P3' C27' C23' 28.0(2) . . . . ?
C27' P3' C28' C31' 171.5(2) . . . . ?
C32' P3' C28' C31' -79.7(3) . . . . ?
Ni2' P3' C28' C31' 63.8(2) . . . . ?
C27' P3' C28' C30' -66.5(3) . . . . ?
C32' P3' C28' C30' 42.3(3) . . . . ?
Ni2' P3' C28' C30' -174.3(2) . . . . ?
C27' P3' C28' C29' 54.0(3) . . . . ?
C32' P3' C28' C29' 162.8(2) . . . . ?
Ni2' P3' C28' C29' -53.7(3) . . . . ?
C27' P3' C32' C34' 167.5(2) . . . . ?
C28' P3' C32' C34' 57.9(3) . . . . ?
Ni2' P3' C32' C34' -78.8(3) . . . . ?
C27' P3' C32' C33' -74.8(2) . . . . ?
C28' P3' C32' C33' 175.6(2) . . . . ?
Ni2' P3' C32' C33' 38.9(3) . . . . ?
C27' P3' C32' C35' 43.2(3) . . . . ?
C28' P3' C32' C35' -66.5(3) . . . . ?
Ni2' P3' C32' C35' 156.8(2) . . . . ?
N2' C26' C36' P4' -22.8(4) . . . . ?
C25' C26' C36' P4' 159.7(4) . . . . ?
C37' P4' C36' C26' 154.3(2) . . . . ?
C41' P4' C36' C26' -89.4(2) . . . . ?
Ni2' P4' C36' C26' 29.1(2) . . . . ?
C36' P4' C37' C39' 160.6(2) . . . . ?
C41' P4' C37' C39' 51.2(3) . . . . ?
Ni2' P4' C37' C39' -88.1(2) . . . . ?
C36' P4' C37' C38' -82.5(2) . . . . ?
C41' P4' C37' C38' 168.2(2) . . . . ?
Ni2' P4' C37' C38' 28.9(2) . . . . ?
C36' P4' C37' C40' 35.4(3) . . . . ?
C41' P4' C37' C40' -73.9(3) . . . . ?
Ni2' P4' C37' C40' 146.8(2) . . . . ?
C36' P4' C41' C42' 172.3(2) . . . . ?
C37' P4' C41' C42' -78.2(3) . . . . ?
Ni2' P4' C41' C42' 63.7(2) . . . . ?
C36' P4' C41' C44' 55.2(2) . . . . ?
C37' P4' C41' C44' 164.7(2) . . . . ?
Ni2' P4' C41' C44' -53.4(2) . . . . ?
C36' P4' C41' C43' -65.1(3) . . . . ?
C37' P4' C41' C43' 44.5(3) . . . . ?
Ni2' P4' C41' C43' -173.6(2) . . . . ?
C86 C81 C82 C83 -0.9(6) . . . . ?
C81 C82 C83 C84 0.6(7) . . . . ?
C82 C83 C84 C85 -0.2(7) . . . . ?
C83 C84 C85 C86 0.1(7) . . . . ?
C84 C85 C86 C81 -0.5(7) . . . . ?
C82 C81 C86 C85 0.9(6) . . . . ?
C96 C91 C92 C93 -1.5(7) . . . . ?
C91 C92 C93 C94 0.5(7) . . . . ?
C92 C93 C94 C95 0.1(7) . . . . ?
C93 C94 C95 C96 0.2(7) . . . . ?
C92 C91 C96 C95 1.7(7) . . . . ?
C94 C95 C96 C91 -1.1(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.941
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.358
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.148
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mk93
_database_code_depnum_ccdc_archive 'CCDC 1037228'
_audit_update_record             
;
2014-12-02 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H35 N Ni P2'
_chemical_formula_weight         386.12

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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   13.2113(6)
_cell_length_b                   14.5597(8)
_cell_length_c                   21.1415(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4066.6(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6169
_cell_measurement_theta_min      2.8020
_cell_measurement_theta_max      27.5330

_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    1.109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98294
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1419
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            60953
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         30.85
_reflns_number_total             6061
_reflns_number_gt                4315
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44)  
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44)  
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The hydrogen at Ni was refined freely. Methyls were refined as rigid
 groups allowed to rotate but not tip. Other hydrogens were included using
 a riding model starting from calculated positions.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0307P)²+0.9041P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6061
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.0887
_refine_ls_wR_factor_gt          0.0783
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
Ni Ni 0.579087(17) 0.248307(17) 0.348706(12) 0.01485(7) Uani 1 1 d . . .
H01 H 0.6534(18) 0.1763(17) 0.3450(12) 0.045(8) Uiso 1 1 d . . .
P1 P 0.65406(4) 0.31944(3) 0.42430(3) 0.01523(11) Uani 1 1 d . . .
P2 P 0.48348(4) 0.19290(3) 0.27556(3) 0.01531(11) Uani 1 1 d . . .
N N 0.48164(11) 0.34094(11) 0.35496(8) 0.0150(3) Uani 1 1 d . . .
C1 C 0.47671(14) 0.40712(13) 0.40103(9) 0.0147(4) Uani 1 1 d . . .
C2 C 0.39098(14) 0.45972(13) 0.39169(10) 0.0165(4) Uani 1 1 d . . .
H2 H 0.3691 0.5100 0.4169 0.020 Uiso 1 1 calc R . .
C3 C 0.34196(14) 0.42410(13) 0.33715(10) 0.0174(4) Uani 1 1 d . . .
H3 H 0.2810 0.4462 0.3188 0.021 Uiso 1 1 calc R . .
C4 C 0.39946(13) 0.35143(13) 0.31583(10) 0.0152(4) Uani 1 1 d . . .
C5 C 0.55904(14) 0.40606(14) 0.45012(10) 0.0192(4) Uani 1 1 d . . .
H5A H 0.5309 0.3892 0.4919 0.023 Uiso 1 1 calc R . .
H5B H 0.5908 0.4675 0.4535 0.023 Uiso 1 1 calc R . .
C6 C 0.68928(14) 0.25733(14) 0.49669(10) 0.0190(4) Uani 1 1 d . . .
H6 H 0.6985 0.3028 0.5317 0.023 Uiso 1 1 calc R . .
C7 C 0.60284(16) 0.19186(16) 0.51439(11) 0.0280(5) Uani 1 1 d . . .
H7A H 0.5929 0.1471 0.4803 0.042 Uiso 1 1 calc R . .
H7B H 0.5404 0.2271 0.5206 0.042 Uiso 1 1 calc R . .
H7C H 0.6200 0.1595 0.5536 0.042 Uiso 1 1 calc R . .
C8 C 0.78774(16) 0.20405(16) 0.48796(11) 0.0281(5) Uani 1 1 d . . .
H8A H 0.8023 0.1688 0.5264 0.042 Uiso 1 1 calc R . .
H8B H 0.8432 0.2471 0.4799 0.042 Uiso 1 1 calc R . .
H8C H 0.7809 0.1620 0.4520 0.042 Uiso 1 1 calc R . .
C9 C 0.76595(14) 0.38610(14) 0.40005(10) 0.0201(4) Uani 1 1 d . . .
H9 H 0.8189 0.3409 0.3869 0.024 Uiso 1 1 calc R . .
C10 C 0.81231(17) 0.44539(16) 0.45225(12) 0.0315(5) Uani 1 1 d . . .
H10A H 0.8716 0.4778 0.4356 0.047 Uiso 1 1 calc R . .
H10B H 0.8329 0.4062 0.4877 0.047 Uiso 1 1 calc R . .
H10C H 0.7622 0.4902 0.4669 0.047 Uiso 1 1 calc R . .
C11 C 0.73884(17) 0.44243(16) 0.34152(11) 0.0289(5) Uani 1 1 d . . .
H11A H 0.6876 0.4883 0.3527 0.043 Uiso 1 1 calc R . .
H11B H 0.7120 0.4016 0.3087 0.043 Uiso 1 1 calc R . .
H11C H 0.7996 0.4735 0.3256 0.043 Uiso 1 1 calc R . .
C12 C 0.39471(14) 0.28908(14) 0.25978(10) 0.0177(4) Uani 1 1 d . . .
H12A H 0.4150 0.3224 0.2210 0.021 Uiso 1 1 calc R . .
H12B H 0.3250 0.2655 0.2540 0.021 Uiso 1 1 calc R . .
C13 C 0.40151(15) 0.09753(14) 0.30093(11) 0.0219(5) Uani 1 1 d . . .
H13 H 0.3424 0.0940 0.2715 0.026 Uiso 1 1 calc R . .
C14 C 0.36229(17) 0.11829(16) 0.36742(11) 0.0305(5) Uani 1 1 d . . .
H14A H 0.3117 0.0722 0.3794 0.046 Uiso 1 1 calc R . .
H14B H 0.3313 0.1794 0.3680 0.046 Uiso 1 1 calc R . .
H14C H 0.4187 0.1165 0.3975 0.046 Uiso 1 1 calc R . .
C15 C 0.45722(17) 0.00555(15) 0.29940(13) 0.0344(6) Uani 1 1 d . . .
H15A H 0.5188 0.0097 0.3251 0.052 Uiso 1 1 calc R . .
H15B H 0.4754 -0.0095 0.2557 0.052 Uiso 1 1 calc R . .
H15C H 0.4132 -0.0426 0.3165 0.052 Uiso 1 1 calc R . .
C16 C 0.53417(15) 0.16088(15) 0.19805(10) 0.0226(5) Uani 1 1 d . . .
H16 H 0.5670 0.0993 0.2024 0.027 Uiso 1 1 calc R . .
C17 C 0.45350(16) 0.15314(15) 0.14709(10) 0.0255(5) Uani 1 1 d . . .
H17A H 0.4274 0.2144 0.1370 0.038 Uiso 1 1 calc R . .
H17B H 0.3980 0.1144 0.1624 0.038 Uiso 1 1 calc R . .
H17C H 0.4830 0.1256 0.1090 0.038 Uiso 1 1 calc R . .
C18 C 0.61531(18) 0.2290(2) 0.17930(12) 0.0467(8) Uani 1 1 d . . .
H18A H 0.6494 0.2075 0.1409 0.070 Uiso 1 1 calc R . .
H18B H 0.6648 0.2346 0.2136 0.070 Uiso 1 1 calc R . .
H18C H 0.5843 0.2890 0.1712 0.070 Uiso 1 1 calc R . .


_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
Ni N 1.8691(15) . ?
Ni P1 2.1466(6) . ?
Ni P2 2.1535(6) . ?
P1 C6 1.837(2) . ?
P1 C9 1.841(2) . ?
P1 C5 1.861(2) . ?
P2 C16 1.831(2) . ?
P2 C13 1.841(2) . ?
P2 C12 1.8568(19) . ?
N C1 1.372(2) . ?
N C4 1.374(2) . ?
C1 C2 1.381(3) . ?
C1 C5 1.504(3) . ?
C2 C3 1.421(3) . ?
C3 C4 1.378(3) . ?
C4 C12 1.494(3) . ?
C6 C8 1.526(3) . ?
C6 C7 1.534(3) . ?
C9 C11 1.527(3) . ?
C9 C10 1.529(3) . ?
C13 C14 1.528(3) . ?
C13 C15 1.529(3) . ?
C16 C18 1.513(3) . ?
C16 C17 1.520(3) . ?

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
N Ni P1 85.24(5) . . ?
N Ni P2 85.24(5) . . ?
P1 Ni P2 170.40(2) . . ?
C6 P1 C9 106.74(9) . . ?
C6 P1 C5 105.07(9) . . ?
C9 P1 C5 105.42(9) . . ?
C6 P1 Ni 119.97(7) . . ?
C9 P1 Ni 114.67(7) . . ?
C5 P1 Ni 103.53(6) . . ?
C16 P2 C13 106.49(10) . . ?
C16 P2 C12 105.21(10) . . ?
C13 P2 C12 104.45(9) . . ?
C16 P2 Ni 121.58(7) . . ?
C13 P2 Ni 114.73(7) . . ?
C12 P2 Ni 102.53(6) . . ?
C1 N C4 108.18(15) . . ?
C1 N Ni 126.15(13) . . ?
C4 N Ni 125.60(13) . . ?
N C1 C2 109.09(17) . . ?
N C1 C5 116.65(16) . . ?
C2 C1 C5 134.22(18) . . ?
C1 C2 C3 106.70(17) . . ?
C4 C3 C2 107.12(17) . . ?
N C4 C3 108.91(17) . . ?
N C4 C12 116.31(16) . . ?
C3 C4 C12 134.64(18) . . ?
C1 C5 P1 107.00(13) . . ?
C8 C6 C7 110.38(18) . . ?
C8 C6 P1 111.43(14) . . ?
C7 C6 P1 108.69(14) . . ?
C11 C9 C10 112.06(19) . . ?
C11 C9 P1 108.70(14) . . ?
C10 C9 P1 114.72(15) . . ?
C4 C12 P2 106.82(13) . . ?
C14 C13 C15 110.85(19) . . ?
C14 C13 P2 108.56(14) . . ?
C15 C13 P2 111.81(15) . . ?
C18 C16 C17 111.08(19) . . ?
C18 C16 P2 109.07(16) . . ?
C17 C16 P2 113.38(14) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N Ni P1 C6 126.38(9) . . . . ?
P2 Ni P1 C6 118.88(15) . . . . ?
N Ni P1 C9 -104.51(9) . . . . ?
P2 Ni P1 C9 -112.01(16) . . . . ?
N Ni P1 C5 9.79(9) . . . . ?
P2 Ni P1 C5 2.30(17) . . . . ?
N Ni P2 C16 129.71(10) . . . . ?
P1 Ni P2 C16 137.21(15) . . . . ?
N Ni P2 C13 -99.74(9) . . . . ?
P1 Ni P2 C13 -92.24(16) . . . . ?
N Ni P2 C12 12.83(8) . . . . ?
P1 Ni P2 C12 20.33(17) . . . . ?
P1 Ni N C1 -8.08(15) . . . . ?
P2 Ni N C1 170.67(16) . . . . ?
P1 Ni N C4 175.49(16) . . . . ?
P2 Ni N C4 -5.76(15) . . . . ?
C4 N C1 C2 0.4(2) . . . . ?
Ni N C1 C2 -176.56(13) . . . . ?
C4 N C1 C5 178.48(16) . . . . ?
Ni N C1 C5 1.5(2) . . . . ?
N C1 C2 C3 -0.4(2) . . . . ?
C5 C1 C2 C3 -178.0(2) . . . . ?
C1 C2 C3 C4 0.2(2) . . . . ?
C1 N C4 C3 -0.2(2) . . . . ?
Ni N C4 C3 176.72(13) . . . . ?
C1 N C4 C12 176.18(16) . . . . ?
Ni N C4 C12 -6.8(2) . . . . ?
C2 C3 C4 N 0.0(2) . . . . ?
C2 C3 C4 C12 -175.5(2) . . . . ?
N C1 C5 P1 7.4(2) . . . . ?
C2 C1 C5 P1 -175.07(19) . . . . ?
C6 P1 C5 C1 -138.08(14) . . . . ?
C9 P1 C5 C1 109.35(14) . . . . ?
Ni P1 C5 C1 -11.44(14) . . . . ?
C9 P1 C6 C8 -51.46(17) . . . . ?
C5 P1 C6 C8 -163.09(15) . . . . ?
Ni P1 C6 C8 81.12(15) . . . . ?
C9 P1 C6 C7 -173.31(14) . . . . ?
C5 P1 C6 C7 75.05(16) . . . . ?
Ni P1 C6 C7 -40.73(16) . . . . ?
C6 P1 C9 C11 -177.51(14) . . . . ?
C5 P1 C9 C11 -66.11(16) . . . . ?
Ni P1 C9 C11 47.08(16) . . . . ?
C6 P1 C9 C10 -51.19(18) . . . . ?
C5 P1 C9 C10 60.20(18) . . . . ?
Ni P1 C9 C10 173.40(14) . . . . ?
N C4 C12 P2 17.2(2) . . . . ?
C3 C4 C12 P2 -167.5(2) . . . . ?
C16 P2 C12 C4 -146.86(14) . . . . ?
C13 P2 C12 C4 101.18(14) . . . . ?
Ni P2 C12 C4 -18.81(14) . . . . ?
C16 P2 C13 C14 176.56(14) . . . . ?
C12 P2 C13 C14 -72.40(16) . . . . ?
Ni P2 C13 C14 39.03(16) . . . . ?
C16 P2 C13 C15 53.96(18) . . . . ?
C12 P2 C13 C15 165.00(16) . . . . ?
Ni P2 C13 C15 -83.57(17) . . . . ?
C13 P2 C16 C18 -170.85(16) . . . . ?
C12 P2 C16 C18 78.64(17) . . . . ?
Ni P2 C16 C18 -36.89(19) . . . . ?
C13 P2 C16 C17 64.81(18) . . . . ?
C12 P2 C16 C17 -45.70(18) . . . . ?
Ni P2 C16 C17 -161.23(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.947
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.087
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mk96b
_database_code_depnum_ccdc_archive 'CCDC 1037229'
_audit_update_record             
;
2014-12-02 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H43 N Ni P2'
_chemical_formula_weight         442.22

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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.0422(2)
_cell_length_b                   14.7303(2)
_cell_length_c                   14.7768(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2403.53(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    59607
_cell_measurement_theta_min      2.2860
_cell_measurement_theta_max      30.5860

_exptl_crystal_description       irregular
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93247
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1419
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            209772
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         31.05
_reflns_number_total             7458
_reflns_number_gt                7082
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The hydridic hydrogen at Ni was refined freely. Methyls were refined as
 rigid groups allowed to rotate but not tip. Other hydrogens were included
 using a riding model starting from calculated positions.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0245P)²+0.3993P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(6)
_chemical_absolute_configuration .
_refine_ls_number_reflns         7458
_refine_ls_number_parameters     251
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0204
_refine_ls_wR_factor_ref         0.0474
_refine_ls_wR_factor_gt          0.0463
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_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
Ni Ni 0.499101(13) 0.520653(8) 0.445181(8) 0.01152(3) Uani 1 1 d . . .
H01 H 0.4687(15) 0.4766(12) 0.3676(12) 0.041(5) Uiso 1 1 d . . .
P1 P 0.35456(2) 0.457179(17) 0.520483(17) 0.01107(5) Uani 1 1 d . . .
P2 P 0.63776(2) 0.605480(17) 0.385997(17) 0.01155(5) Uani 1 1 d . . .
N N 0.53564(8) 0.58089(6) 0.55317(6) 0.01295(16) Uani 1 1 d . . .
C1 C 0.46382(9) 0.58231(7) 0.62884(7) 0.01309(19) Uani 1 1 d . . .
C2 C 0.50625(12) 0.64811(7) 0.68771(7) 0.01613(19) Uani 1 1 d . . .
H2 H 0.4729 0.6636 0.7449 0.019 Uiso 1 1 calc R . .
C3 C 0.60961(11) 0.68805(7) 0.64586(7) 0.0169(2) Uani 1 1 d . . .
H3 H 0.6588 0.7352 0.6699 0.020 Uiso 1 1 calc R . .
C4 C 0.62448(10) 0.64496(7) 0.56346(7) 0.01394(19) Uani 1 1 d . . .
C5 C 0.35986(10) 0.51661(7) 0.63215(7) 0.01519(18) Uani 1 1 d . . .
H5A H 0.2830 0.5494 0.6431 0.018 Uiso 1 1 calc R . .
H5B H 0.3720 0.4722 0.6816 0.018 Uiso 1 1 calc R . .
C6 C 0.19983(10) 0.48274(8) 0.47569(7) 0.01488(19) Uani 1 1 d . . .
C7 C 0.17712(12) 0.43241(9) 0.38676(9) 0.0254(3) Uani 1 1 d . . .
H7A H 0.1037 0.4563 0.3581 0.038 Uiso 1 1 calc R . .
H7B H 0.1667 0.3675 0.3990 0.038 Uiso 1 1 calc R . .
H7C H 0.2464 0.4412 0.3462 0.038 Uiso 1 1 calc R . .
C8 C 0.09587(11) 0.46360(10) 0.54150(9) 0.0287(3) Uani 1 1 d . . .
H8A H 0.0907 0.3982 0.5528 0.043 Uiso 1 1 calc R . .
H8B H 0.0196 0.4850 0.5152 0.043 Uiso 1 1 calc R . .
H8C H 0.1108 0.4954 0.5987 0.043 Uiso 1 1 calc R . .
C9 C 0.20434(11) 0.58485(8) 0.45467(10) 0.0234(2) Uani 1 1 d . . .
H9A H 0.2274 0.6183 0.5094 0.035 Uiso 1 1 calc R . .
H9B H 0.1244 0.6053 0.4343 0.035 Uiso 1 1 calc R . .
H9C H 0.2641 0.5961 0.4069 0.035 Uiso 1 1 calc R . .
C10 C 0.37936(11) 0.33479(7) 0.54898(8) 0.0167(2) Uani 1 1 d . . .
C11 C 0.50961(15) 0.33160(9) 0.58489(9) 0.0315(3) Uani 1 1 d . . .
H11A H 0.5301 0.2691 0.6017 0.047 Uiso 1 1 calc R . .
H11B H 0.5166 0.3709 0.6381 0.047 Uiso 1 1 calc R . .
H11C H 0.5653 0.3527 0.5378 0.047 Uiso 1 1 calc R . .
C12 C 0.29236(15) 0.29714(9) 0.62011(10) 0.0322(3) Uani 1 1 d . . .
H12A H 0.3208 0.2374 0.6402 0.048 Uiso 1 1 calc R . .
H12B H 0.2113 0.2912 0.5938 0.048 Uiso 1 1 calc R . .
H12C H 0.2892 0.3386 0.6719 0.048 Uiso 1 1 calc R . .
C13 C 0.37400(14) 0.27565(8) 0.46382(8) 0.0272(3) Uani 1 1 d . . .
H13A H 0.2898 0.2706 0.4434 0.041 Uiso 1 1 calc R . .
H13B H 0.4056 0.2151 0.4776 0.041 Uiso 1 1 calc R . .
H13C H 0.4231 0.3034 0.4160 0.041 Uiso 1 1 calc R . .
C14 C 0.71419(10) 0.65256(7) 0.48772(7) 0.0154(2) Uani 1 1 d . . .
H14A H 0.7883 0.6175 0.5018 0.018 Uiso 1 1 calc R . .
H14B H 0.7369 0.7168 0.4777 0.018 Uiso 1 1 calc R . .
C15 C 0.57254(10) 0.70711(7) 0.32762(7) 0.0145(2) Uani 1 1 d . . .
C16 C 0.49617(12) 0.75785(7) 0.39849(7) 0.0189(2) Uani 1 1 d . . .
H16A H 0.4367 0.7161 0.4248 0.028 Uiso 1 1 calc R . .
H16B H 0.4540 0.8086 0.3694 0.028 Uiso 1 1 calc R . .
H16C H 0.5492 0.7811 0.4463 0.028 Uiso 1 1 calc R . .
C17 C 0.48681(12) 0.67679(8) 0.25157(8) 0.0213(2) Uani 1 1 d . . .
H17A H 0.4426 0.7295 0.2283 0.032 Uiso 1 1 calc R . .
H17B H 0.4291 0.6322 0.2753 0.032 Uiso 1 1 calc R . .
H17C H 0.5340 0.6493 0.2026 0.032 Uiso 1 1 calc R . .
C18 C 0.66857(11) 0.77173(8) 0.28924(8) 0.0190(2) Uani 1 1 d . . .
H18A H 0.7266 0.7874 0.3369 0.028 Uiso 1 1 calc R . .
H18B H 0.6292 0.8271 0.2671 0.028 Uiso 1 1 calc R . .
H18C H 0.7112 0.7419 0.2392 0.028 Uiso 1 1 calc R . .
C19 C 0.76150(10) 0.54978(8) 0.32014(8) 0.0177(2) Uani 1 1 d . . .
C20 C 0.72173(12) 0.52903(9) 0.22279(8) 0.0253(3) Uani 1 1 d . . .
H20A H 0.7816 0.4893 0.1940 0.038 Uiso 1 1 calc R . .
H20B H 0.7154 0.5858 0.1886 0.038 Uiso 1 1 calc R . .
H20C H 0.6428 0.4987 0.2236 0.038 Uiso 1 1 calc R . .
C21 C 0.78295(12) 0.45887(8) 0.36939(10) 0.0265(3) Uani 1 1 d . . .
H21A H 0.8027 0.4706 0.4330 0.040 Uiso 1 1 calc R . .
H21B H 0.8502 0.4265 0.3406 0.040 Uiso 1 1 calc R . .
H21C H 0.7095 0.4217 0.3659 0.040 Uiso 1 1 calc R . .
C22 C 0.88041(11) 0.60363(9) 0.31950(9) 0.0237(2) Uani 1 1 d . . .
H22A H 0.9434 0.5680 0.2891 0.036 Uiso 1 1 calc R . .
H22B H 0.9054 0.6162 0.3819 0.036 Uiso 1 1 calc R . .
H22C H 0.8684 0.6610 0.2872 0.036 Uiso 1 1 calc R . .


_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
Ni N 1.8699(9) . ?
Ni P1 2.1587(3) . ?
Ni P2 2.1611(3) . ?
P1 C5 1.8688(10) . ?
P1 C6 1.8705(11) . ?
P1 C10 1.8715(10) . ?
P2 C14 1.8582(11) . ?
P2 C19 1.8674(11) . ?
P2 C15 1.8719(11) . ?
N C4 1.3698(13) . ?
N C1 1.3711(14) . ?
C1 C2 1.3841(14) . ?
C1 C5 1.5023(14) . ?
C2 C3 1.4252(17) . ?
C3 C4 1.3828(15) . ?
C4 C14 1.4988(15) . ?
C6 C7 1.5295(16) . ?
C6 C8 1.5307(16) . ?
C6 C9 1.5366(16) . ?
C10 C12 1.5282(17) . ?
C10 C13 1.5316(16) . ?
C10 C11 1.5338(19) . ?
C15 C18 1.5337(15) . ?
C15 C17 1.5357(16) . ?
C15 C16 1.5383(15) . ?
C19 C22 1.5340(16) . ?
C19 C20 1.5347(17) . ?
C19 C21 1.5424(17) . ?

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
N Ni P1 85.71(3) . . ?
N Ni P2 85.30(3) . . ?
P1 Ni P2 169.378(11) . . ?
C5 P1 C6 104.29(5) . . ?
C5 P1 C10 104.36(5) . . ?
C6 P1 C10 114.03(5) . . ?
C5 P1 Ni 103.24(4) . . ?
C6 P1 Ni 113.94(4) . . ?
C10 P1 Ni 115.15(4) . . ?
C14 P2 C19 104.67(5) . . ?
C14 P2 C15 104.42(5) . . ?
C19 P2 C15 113.13(5) . . ?
C14 P2 Ni 102.14(4) . . ?
C19 P2 Ni 118.38(4) . . ?
C15 P2 Ni 112.11(4) . . ?
C4 N C1 108.25(9) . . ?
C4 N Ni 125.19(8) . . ?
C1 N Ni 125.34(7) . . ?
N C1 C2 109.11(9) . . ?
N C1 C5 117.30(9) . . ?
C2 C1 C5 133.58(10) . . ?
C1 C2 C3 106.71(9) . . ?
C4 C3 C2 106.72(9) . . ?
N C4 C3 109.21(10) . . ?
N C4 C14 116.22(9) . . ?
C3 C4 C14 134.56(10) . . ?
C1 C5 P1 107.28(7) . . ?
C7 C6 C8 109.49(10) . . ?
C7 C6 C9 107.82(10) . . ?
C8 C6 C9 109.45(10) . . ?
C7 C6 P1 110.87(8) . . ?
C8 C6 P1 115.03(8) . . ?
C9 C6 P1 103.82(8) . . ?
C12 C10 C13 109.54(10) . . ?
C12 C10 C11 109.90(11) . . ?
C13 C10 C11 107.65(10) . . ?
C12 C10 P1 114.35(8) . . ?
C13 C10 P1 110.94(8) . . ?
C11 C10 P1 104.15(8) . . ?
C4 C14 P2 106.02(7) . . ?
C18 C15 C17 109.64(9) . . ?
C18 C15 C16 109.22(9) . . ?
C17 C15 C16 107.55(9) . . ?
C18 C15 P2 113.62(8) . . ?
C17 C15 P2 109.99(7) . . ?
C16 C15 P2 106.61(7) . . ?
C22 C19 C20 110.01(10) . . ?
C22 C19 C21 108.69(10) . . ?
C20 C19 C21 108.26(10) . . ?
C22 C19 P2 113.72(8) . . ?
C20 C19 P2 111.51(8) . . ?
C21 C19 P2 104.35(8) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N Ni P1 C5 5.98(5) . . . . ?
P2 Ni P1 C5 -26.28(8) . . . . ?
N Ni P1 C6 118.43(5) . . . . ?
P2 Ni P1 C6 86.17(8) . . . . ?
N Ni P1 C10 -107.10(5) . . . . ?
P2 Ni P1 C10 -139.36(7) . . . . ?
N Ni P2 C14 13.30(5) . . . . ?
P1 Ni P2 C14 45.58(8) . . . . ?
N Ni P2 C19 127.54(5) . . . . ?
P1 Ni P2 C19 159.82(7) . . . . ?
N Ni P2 C15 -97.94(5) . . . . ?
P1 Ni P2 C15 -65.66(8) . . . . ?
P1 Ni N C4 -176.98(9) . . . . ?
P2 Ni N C4 -2.65(8) . . . . ?
P1 Ni N C1 -11.11(8) . . . . ?
P2 Ni N C1 163.23(8) . . . . ?
C4 N C1 C2 0.45(12) . . . . ?
Ni N C1 C2 -167.43(7) . . . . ?
C4 N C1 C5 -179.80(9) . . . . ?
Ni N C1 C5 12.32(13) . . . . ?
N C1 C2 C3 -0.49(12) . . . . ?
C5 C1 C2 C3 179.82(11) . . . . ?
C1 C2 C3 C4 0.34(12) . . . . ?
C1 N C4 C3 -0.23(12) . . . . ?
Ni N C4 C3 167.67(7) . . . . ?
C1 N C4 C14 178.92(9) . . . . ?
Ni N C4 C14 -13.18(13) . . . . ?
C2 C3 C4 N -0.07(12) . . . . ?
C2 C3 C4 C14 -179.00(12) . . . . ?
N C1 C5 P1 -4.91(12) . . . . ?
C2 C1 C5 P1 174.76(11) . . . . ?
C6 P1 C5 C1 -121.50(8) . . . . ?
C10 P1 C5 C1 118.57(8) . . . . ?
Ni P1 C5 C1 -2.15(8) . . . . ?
C5 P1 C6 C7 -175.64(8) . . . . ?
C10 P1 C6 C7 -62.46(9) . . . . ?
Ni P1 C6 C7 72.54(9) . . . . ?
C5 P1 C6 C8 -50.75(10) . . . . ?
C10 P1 C6 C8 62.44(10) . . . . ?
Ni P1 C6 C8 -162.56(8) . . . . ?
C5 P1 C6 C9 68.81(8) . . . . ?
C10 P1 C6 C9 -178.00(8) . . . . ?
Ni P1 C6 C9 -43.01(8) . . . . ?
C5 P1 C10 C12 53.91(11) . . . . ?
C6 P1 C10 C12 -59.24(11) . . . . ?
Ni P1 C10 C12 166.33(9) . . . . ?
C5 P1 C10 C13 178.40(9) . . . . ?
C6 P1 C10 C13 65.25(10) . . . . ?
Ni P1 C10 C13 -69.18(9) . . . . ?
C5 P1 C10 C11 -66.06(9) . . . . ?
C6 P1 C10 C11 -179.20(8) . . . . ?
Ni P1 C10 C11 46.37(9) . . . . ?
N C4 C14 P2 22.90(11) . . . . ?
C3 C4 C14 P2 -158.23(11) . . . . ?
C19 P2 C14 C4 -145.91(7) . . . . ?
C15 P2 C14 C4 94.98(8) . . . . ?
Ni P2 C14 C4 -21.94(7) . . . . ?
C14 P2 C15 C18 67.03(9) . . . . ?
C19 P2 C15 C18 -46.18(9) . . . . ?
Ni P2 C15 C18 176.83(7) . . . . ?
C14 P2 C15 C17 -169.65(8) . . . . ?
C19 P2 C15 C17 77.14(9) . . . . ?
Ni P2 C15 C17 -59.85(8) . . . . ?
C14 P2 C15 C16 -53.34(9) . . . . ?
C19 P2 C15 C16 -166.55(7) . . . . ?
Ni P2 C15 C16 56.46(8) . . . . ?
C14 P2 C19 C22 -39.98(10) . . . . ?
C15 P2 C19 C22 73.08(10) . . . . ?
Ni P2 C19 C22 -152.83(7) . . . . ?
C14 P2 C19 C20 -165.07(8) . . . . ?
C15 P2 C19 C20 -52.01(10) . . . . ?
Ni P2 C19 C20 82.08(9) . . . . ?
C14 P2 C19 C21 78.29(9) . . . . ?
C15 P2 C19 C21 -168.65(8) . . . . ?
Ni P2 C19 C21 -34.56(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        30.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.047
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mk91
_database_code_depnum_ccdc_archive 'CCDC 1037230'
_audit_update_record             
;
2014-12-02 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H35 N Ni O2 P2'
_chemical_formula_weight         430.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.7937(4)
_cell_length_b                   13.5622(3)
_cell_length_c                   20.6530(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4423.79(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    18641
_cell_measurement_theta_min      4.2600
_cell_measurement_theta_max      76.6600

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1840
_exptl_absorpt_coefficient_mu    2.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.38359
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42437
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         4.28
_diffrn_reflns_theta_max         76.87
_reflns_number_total             4648
_reflns_number_gt                4158
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The hydrogen at C19 was found and refined freely. Methyls were refined as
 rigid groups allowed to rotate but not tip. Other hydrogens were included
 using a riding model starting from calculated positions.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0315P)²+1.2219P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4648
_refine_ls_number_parameters     238
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0667
_refine_ls_wR_factor_gt          0.0644
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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
Ni Ni 0.541643(14) 0.198582(16) 0.345333(11) 0.02362(7) Uani 1 1 d . . .
P1 P 0.60730(2) 0.24920(2) 0.433927(16) 0.02473(8) Uani 1 1 d . . .
P2 P 0.45237(2) 0.16461(2) 0.266963(16) 0.02417(8) Uani 1 1 d . . .
N N 0.47628(7) 0.31043(8) 0.35612(6) 0.0262(2) Uani 1 1 d . . .
O1 O 0.60004(7) 0.07802(7) 0.33417(5) 0.0329(2) Uani 1 1 d . . .
O2 O 0.70986(8) 0.15824(9) 0.29082(7) 0.0492(3) Uani 1 1 d . . .
C1 C 0.47596(9) 0.37075(10) 0.41015(7) 0.0280(3) Uani 1 1 d . . .
C2 C 0.40694(10) 0.43244(11) 0.40713(8) 0.0354(3) Uani 1 1 d . . .
H2 H 0.3913 0.4807 0.4382 0.042 Uiso 1 1 calc R . .
C3 C 0.36342(10) 0.41022(11) 0.34869(8) 0.0364(3) Uani 1 1 d . . .
H3 H 0.3133 0.4412 0.3333 0.044 Uiso 1 1 calc R . .
C4 C 0.40707(9) 0.33592(10) 0.31862(7) 0.0287(3) Uani 1 1 d . . .
C5 C 0.54806(9) 0.36118(10) 0.45682(7) 0.0306(3) Uani 1 1 d . . .
H5A H 0.5265 0.3552 0.5017 0.037 Uiso 1 1 calc R . .
H5B H 0.5852 0.4198 0.4543 0.037 Uiso 1 1 calc R . .
C6 C 0.59858(10) 0.16665(11) 0.50432(7) 0.0316(3) Uani 1 1 d . . .
H6 H 0.6185 0.2032 0.5435 0.038 Uiso 1 1 calc R . .
C7 C 0.50553(11) 0.13881(13) 0.51443(8) 0.0430(4) Uani 1 1 d . . .
H7A H 0.4852 0.1016 0.4768 0.064 Uiso 1 1 calc R . .
H7B H 0.4717 0.1989 0.5195 0.064 Uiso 1 1 calc R . .
H7C H 0.5002 0.0982 0.5535 0.064 Uiso 1 1 calc R . .
C8 C 0.65442(12) 0.07565(12) 0.49564(8) 0.0423(4) Uani 1 1 d . . .
H8A H 0.6468 0.0313 0.5326 0.064 Uiso 1 1 calc R . .
H8B H 0.7139 0.0959 0.4930 0.064 Uiso 1 1 calc R . .
H8C H 0.6384 0.0414 0.4557 0.064 Uiso 1 1 calc R . .
C9 C 0.71958(9) 0.28402(11) 0.43025(7) 0.0334(3) Uani 1 1 d . . .
H9 H 0.7519 0.2239 0.4171 0.040 Uiso 1 1 calc R . .
C10 C 0.75534(11) 0.31768(14) 0.49552(9) 0.0449(4) Uani 1 1 d . . .
H10A H 0.8143 0.3386 0.4900 0.067 Uiso 1 1 calc R . .
H10B H 0.7529 0.2630 0.5264 0.067 Uiso 1 1 calc R . .
H10C H 0.7217 0.3730 0.5119 0.067 Uiso 1 1 calc R . .
C11 C 0.73346(11) 0.36157(13) 0.37761(9) 0.0452(4) Uani 1 1 d . . .
H11A H 0.7070 0.4238 0.3908 0.068 Uiso 1 1 calc R . .
H11B H 0.7080 0.3388 0.3370 0.068 Uiso 1 1 calc R . .
H11C H 0.7943 0.3718 0.3713 0.068 Uiso 1 1 calc R . .
C12 C 0.39415(9) 0.28076(10) 0.25655(7) 0.0305(3) Uani 1 1 d . . .
H12A H 0.4169 0.3186 0.2194 0.037 Uiso 1 1 calc R . .
H12B H 0.3332 0.2679 0.2491 0.037 Uiso 1 1 calc R . .
C13 C 0.37230(9) 0.07310(10) 0.29118(7) 0.0291(3) Uani 1 1 d . . .
H13 H 0.3284 0.0700 0.2564 0.035 Uiso 1 1 calc R . .
C14 C 0.32928(10) 0.10770(12) 0.35341(7) 0.0373(3) Uani 1 1 d . . .
H14A H 0.2857 0.0600 0.3660 0.056 Uiso 1 1 calc R . .
H14B H 0.3030 0.1722 0.3461 0.056 Uiso 1 1 calc R . .
H14C H 0.3715 0.1131 0.3880 0.056 Uiso 1 1 calc R . .
C15 C 0.41096(11) -0.02961(12) 0.29840(9) 0.0424(4) Uani 1 1 d . . .
H15A H 0.4572 -0.0273 0.3300 0.064 Uiso 1 1 calc R . .
H15B H 0.4330 -0.0516 0.2565 0.064 Uiso 1 1 calc R . .
H15C H 0.3674 -0.0758 0.3134 0.064 Uiso 1 1 calc R . .
C16 C 0.49199(9) 0.12510(11) 0.18764(6) 0.0297(3) Uani 1 1 d . . .
H16 H 0.5165 0.0576 0.1930 0.036 Uiso 1 1 calc R . .
C17 C 0.42156(11) 0.11804(13) 0.13677(7) 0.0411(4) Uani 1 1 d . . .
H17A H 0.3982 0.1838 0.1287 0.062 Uiso 1 1 calc R . .
H17B H 0.3766 0.0745 0.1527 0.062 Uiso 1 1 calc R . .
H17C H 0.4448 0.0913 0.0964 0.062 Uiso 1 1 calc R . .
C18 C 0.56330(10) 0.19306(12) 0.16472(7) 0.0371(3) Uani 1 1 d . . .
H18A H 0.5889 0.1659 0.1253 0.056 Uiso 1 1 calc R . .
H18B H 0.6065 0.1982 0.1986 0.056 Uiso 1 1 calc R . .
H18C H 0.5402 0.2587 0.1555 0.056 Uiso 1 1 calc R . .
C19 C 0.67238(10) 0.08390(12) 0.30700(7) 0.0356(3) Uani 1 1 d . . .
H19 H 0.6984(13) 0.0178(16) 0.3010(10) 0.053(6) Uiso 1 1 d . . .


_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
Ni N 1.8484(11) . ?
Ni O1 1.8914(10) . ?
Ni P2 2.1954(4) . ?
Ni P1 2.2123(4) . ?
P1 C9 1.8366(15) . ?
P1 C6 1.8401(14) . ?
P1 C5 1.8454(14) . ?
P2 C16 1.8337(14) . ?
P2 C12 1.8366(14) . ?
P2 C13 1.8411(14) . ?
N C1 1.3835(17) . ?
N C4 1.3836(18) . ?
O1 C19 1.2754(19) . ?
O2 C19 1.216(2) . ?
C1 C2 1.376(2) . ?
C1 C5 1.4975(19) . ?
C2 C3 1.421(2) . ?
C3 C4 1.370(2) . ?
C4 C12 1.4982(19) . ?
C6 C8 1.527(2) . ?
C6 C7 1.532(2) . ?
C9 C11 1.528(2) . ?
C9 C10 1.531(2) . ?
C13 C14 1.528(2) . ?
C13 C15 1.528(2) . ?
C16 C18 1.530(2) . ?
C16 C17 1.533(2) . ?

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
N Ni O1 175.22(5) . . ?
N Ni P2 84.40(4) . . ?
O1 Ni P2 92.40(3) . . ?
N Ni P1 84.69(4) . . ?
O1 Ni P1 98.07(3) . . ?
P2 Ni P1 167.392(17) . . ?
C9 P1 C6 105.16(7) . . ?
C9 P1 C5 106.77(7) . . ?
C6 P1 C5 105.09(7) . . ?
C9 P1 Ni 119.88(5) . . ?
C6 P1 Ni 115.44(5) . . ?
C5 P1 Ni 103.27(5) . . ?
C16 P2 C12 108.47(7) . . ?
C16 P2 C13 106.27(6) . . ?
C12 P2 C13 105.43(7) . . ?
C16 P2 Ni 120.06(5) . . ?
C12 P2 Ni 103.17(5) . . ?
C13 P2 Ni 112.47(5) . . ?
C1 N C4 107.51(11) . . ?
C1 N Ni 125.77(10) . . ?
C4 N Ni 125.36(9) . . ?
C19 O1 Ni 115.87(10) . . ?
C2 C1 N 109.02(12) . . ?
C2 C1 C5 133.20(13) . . ?
N C1 C5 117.71(12) . . ?
C1 C2 C3 107.02(13) . . ?
C4 C3 C2 107.32(13) . . ?
C3 C4 N 109.12(13) . . ?
C3 C4 C12 133.37(13) . . ?
N C4 C12 117.51(12) . . ?
C1 C5 P1 106.98(9) . . ?
C8 C6 C7 111.77(13) . . ?
C8 C6 P1 110.82(10) . . ?
C7 C6 P1 109.24(11) . . ?
C11 C9 C10 111.60(13) . . ?
C11 C9 P1 110.17(11) . . ?
C10 C9 P1 113.35(11) . . ?
C4 C12 P2 105.07(9) . . ?
C14 C13 C15 112.07(13) . . ?
C14 C13 P2 109.09(10) . . ?
C15 C13 P2 111.50(10) . . ?
C18 C16 C17 111.08(12) . . ?
C18 C16 P2 110.57(10) . . ?
C17 C16 P2 112.52(10) . . ?
O2 C19 O1 127.51(14) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N Ni P1 C9 -116.06(7) . . . . ?
O1 Ni P1 C9 67.86(7) . . . . ?
P2 Ni P1 C9 -146.25(9) . . . . ?
N Ni P1 C6 116.55(7) . . . . ?
O1 Ni P1 C6 -59.52(6) . . . . ?
P2 Ni P1 C6 86.36(9) . . . . ?
N Ni P1 C5 2.45(6) . . . . ?
O1 Ni P1 C5 -173.62(6) . . . . ?
P2 Ni P1 C5 -27.74(10) . . . . ?
N Ni P2 C16 132.95(7) . . . . ?
O1 Ni P2 C16 -50.60(6) . . . . ?
P1 Ni P2 C16 163.16(9) . . . . ?
N Ni P2 C12 12.20(6) . . . . ?
O1 Ni P2 C12 -171.36(6) . . . . ?
P1 Ni P2 C12 42.41(10) . . . . ?
N Ni P2 C13 -100.91(6) . . . . ?
O1 Ni P2 C13 75.53(6) . . . . ?
P1 Ni P2 C13 -70.70(9) . . . . ?
O1 Ni N C1 115.2(6) . . . . ?
P2 Ni N C1 163.27(12) . . . . ?
P1 Ni N C1 -10.39(11) . . . . ?
O1 Ni N C4 -49.9(6) . . . . ?
P2 Ni N C4 -1.76(11) . . . . ?
P1 Ni N C4 -175.42(12) . . . . ?
N Ni O1 C19 153.7(6) . . . . ?
P2 Ni O1 C19 105.87(10) . . . . ?
P1 Ni O1 C19 -81.17(10) . . . . ?
C4 N C1 C2 0.77(16) . . . . ?
Ni N C1 C2 -166.46(10) . . . . ?
C4 N C1 C5 -176.65(12) . . . . ?
Ni N C1 C5 16.11(18) . . . . ?
N C1 C2 C3 -0.66(17) . . . . ?
C5 C1 C2 C3 176.21(15) . . . . ?
C1 C2 C3 C4 0.30(18) . . . . ?
C2 C3 C4 N 0.18(18) . . . . ?
C2 C3 C4 C12 -179.94(16) . . . . ?
C1 N C4 C3 -0.58(16) . . . . ?
Ni N C4 C3 166.72(11) . . . . ?
C1 N C4 C12 179.51(12) . . . . ?
Ni N C4 C12 -13.19(18) . . . . ?
C2 C1 C5 P1 172.24(15) . . . . ?
N C1 C5 P1 -11.10(16) . . . . ?
C9 P1 C5 C1 131.01(10) . . . . ?
C6 P1 C5 C1 -117.64(10) . . . . ?
Ni P1 C5 C1 3.74(10) . . . . ?
C9 P1 C6 C8 -60.26(12) . . . . ?
C5 P1 C6 C8 -172.76(11) . . . . ?
Ni P1 C6 C8 74.19(11) . . . . ?
C9 P1 C6 C7 176.17(11) . . . . ?
C5 P1 C6 C7 63.67(12) . . . . ?
Ni P1 C6 C7 -49.38(12) . . . . ?
C6 P1 C9 C11 -174.09(11) . . . . ?
C5 P1 C9 C11 -62.79(12) . . . . ?
Ni P1 C9 C11 53.92(12) . . . . ?
C6 P1 C9 C10 -48.24(13) . . . . ?
C5 P1 C9 C10 63.06(13) . . . . ?
Ni P1 C9 C10 179.78(10) . . . . ?
C3 C4 C12 P2 -158.12(16) . . . . ?
N C4 C12 P2 21.77(16) . . . . ?
C16 P2 C12 C4 -148.58(10) . . . . ?
C13 P2 C12 C4 97.93(10) . . . . ?
Ni P2 C12 C4 -20.22(10) . . . . ?
C16 P2 C13 C14 -173.61(10) . . . . ?
C12 P2 C13 C14 -58.60(11) . . . . ?
Ni P2 C13 C14 53.12(11) . . . . ?
C16 P2 C13 C15 62.08(12) . . . . ?
C12 P2 C13 C15 177.10(11) . . . . ?
Ni P2 C13 C15 -71.19(11) . . . . ?
C12 P2 C16 C18 70.55(12) . . . . ?
C13 P2 C16 C18 -176.51(10) . . . . ?
Ni P2 C16 C18 -47.54(12) . . . . ?
C12 P2 C16 C17 -54.30(13) . . . . ?
C13 P2 C16 C17 58.64(12) . . . . ?
Ni P2 C16 C17 -172.39(9) . . . . ?
Ni O1 C19 O2 4.4(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        75.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.039
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_wb30may
_database_code_depnum_ccdc_archive 'CCDC 1037231'
_audit_update_record             
;
2014-12-02 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            wb30may14
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H45 N Ni P2'
_chemical_formula_weight         456.25

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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.4225(4)
_cell_length_b                   14.6398(5)
_cell_length_c                   14.9390(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2498.15(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9911
_cell_measurement_theta_min      3.0618
_cell_measurement_theta_max      23.8077

_exptl_crystal_description       chunk
_exptl_crystal_colour            'clear light gold-yellow'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8529
_exptl_absorpt_correction_T_max  0.8677
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           ?
_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.4167
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23103
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         23.85
_reflns_number_total             3827
_reflns_number_gt                3627
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0235P)²+0.5524P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.012(10)
_chemical_absolute_configuration .
_refine_ls_number_reflns         3827
_refine_ls_number_parameters     257
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0210
_refine_ls_wR_factor_ref         0.0499
_refine_ls_wR_factor_gt          0.0488
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001

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
Ni Ni 0.74910(2) 0.303657(15) 0.266486(15) 0.02026(8) Uani 1 1 d . . .
P1 P 0.60044(5) 0.22621(3) 0.20915(3) 0.01942(12) Uani 1 1 d . . .
P2 P 0.89386(5) 0.35759(3) 0.34832(3) 0.01939(12) Uani 1 1 d . . .
N N 0.78155(13) 0.19297(11) 0.32740(10) 0.0204(4) Uani 1 1 d . . .
C1 C 0.70872(17) 0.11894(14) 0.33264(13) 0.0213(5) Uani 1 1 d . . .
C2 C 0.7490(2) 0.05963(13) 0.39693(12) 0.0278(5) Uani 1 1 d . . .
H2 H 0.7142 0.0035 0.4145 0.033 Uiso 1 1 calc R . .
C3 C 0.8531(2) 0.09885(14) 0.43183(15) 0.0290(6) Uani 1 1 d . . .
H3 H 0.9017 0.0737 0.4772 0.035 Uiso 1 1 calc R . .
C4 C 0.87041(18) 0.17992(14) 0.38774(13) 0.0233(5) Uani 1 1 d . . .
C5 C 0.60372(19) 0.11722(14) 0.27316(15) 0.0287(5) Uani 1 1 d . . .
H5A H 0.5316 0.1110 0.3094 0.034 Uiso 1 1 calc R . .
H5B H 0.6084 0.0647 0.2315 0.034 Uiso 1 1 calc R . .
C6 C 0.6187(2) 0.18955(15) 0.08974(14) 0.0286(5) Uani 1 1 d . . .
C7 C 0.7387(3) 0.1419(2) 0.08728(19) 0.0616(8) Uani 1 1 d . . .
H7A H 0.7561 0.1228 0.0258 0.092 Uiso 1 1 calc R . .
H7B H 0.7371 0.0882 0.1264 0.092 Uiso 1 1 calc R . .
H7C H 0.7992 0.1844 0.1080 0.092 Uiso 1 1 calc R . .
C8 C 0.6248(3) 0.27133(18) 0.02651(16) 0.0582(9) Uani 1 1 d . . .
H8A H 0.6836 0.3147 0.0483 0.087 Uiso 1 1 calc R . .
H8B H 0.5482 0.3014 0.0242 0.087 Uiso 1 1 calc R . .
H8C H 0.6465 0.2504 -0.0336 0.087 Uiso 1 1 calc R . .
C9 C 0.5248(3) 0.12329(18) 0.05701(17) 0.0482(7) Uani 1 1 d . . .
H9A H 0.4511 0.1563 0.0481 0.072 Uiso 1 1 calc R . .
H9B H 0.5133 0.0751 0.1017 0.072 Uiso 1 1 calc R . .
H9C H 0.5497 0.0959 0.0003 0.072 Uiso 1 1 calc R . .
C10 C 0.44918(18) 0.27101(15) 0.23354(15) 0.0273(5) Uani 1 1 d . . .
C11 C 0.4150(2) 0.34910(19) 0.1706(2) 0.0511(7) Uani 1 1 d . . .
H11A H 0.4075 0.3256 0.1094 0.077 Uiso 1 1 calc R . .
H11B H 0.4756 0.3965 0.1722 0.077 Uiso 1 1 calc R . .
H11C H 0.3401 0.3752 0.1898 0.077 Uiso 1 1 calc R . .
C12 C 0.3513(2) 0.19938(17) 0.22943(19) 0.0444(6) Uani 1 1 d . . .
H12A H 0.2768 0.2276 0.2466 0.067 Uiso 1 1 calc R . .
H12B H 0.3693 0.1493 0.2707 0.067 Uiso 1 1 calc R . .
H12C H 0.3452 0.1755 0.1683 0.067 Uiso 1 1 calc R . .
C13 C 0.4573(2) 0.3078(2) 0.32916(16) 0.0474(7) Uani 1 1 d . . .
H13A H 0.5086 0.3615 0.3302 0.071 Uiso 1 1 calc R . .
H13B H 0.4896 0.2605 0.3685 0.071 Uiso 1 1 calc R . .
H13C H 0.3791 0.3250 0.3501 0.071 Uiso 1 1 calc R . .
C14 C 0.96200(19) 0.25191(14) 0.39146(15) 0.0271(5) Uani 1 1 d . . .
H14A H 1.0300 0.2345 0.3541 0.033 Uiso 1 1 calc R . .
H14B H 0.9891 0.2609 0.4538 0.033 Uiso 1 1 calc R . .
C15 C 1.0198(2) 0.42072(16) 0.29556(15) 0.0318(6) Uani 1 1 d . . .
C16 C 1.0355(2) 0.3755(2) 0.20354(17) 0.0521(8) Uani 1 1 d . . .
H16A H 0.9651 0.3856 0.1673 0.078 Uiso 1 1 calc R . .
H16B H 1.0481 0.3098 0.2114 0.078 Uiso 1 1 calc R . .
H16C H 1.1033 0.4024 0.1732 0.078 Uiso 1 1 calc R . .
C17 C 0.9943(2) 0.52322(16) 0.28191(18) 0.0432(7) Uani 1 1 d . . .
H17A H 0.9900 0.5536 0.3403 0.065 Uiso 1 1 calc R . .
H17B H 0.9196 0.5305 0.2504 0.065 Uiso 1 1 calc R . .
H17C H 1.0572 0.5507 0.2463 0.065 Uiso 1 1 calc R . .
C18 C 1.1344(2) 0.41061(19) 0.34816(18) 0.0425(7) Uani 1 1 d . . .
H18A H 1.1976 0.4419 0.3161 0.064 Uiso 1 1 calc R . .
H18B H 1.1536 0.3457 0.3543 0.064 Uiso 1 1 calc R . .
H18C H 1.1251 0.4378 0.4077 0.064 Uiso 1 1 calc R . .
C19 C 0.83860(19) 0.41627(14) 0.45200(14) 0.0244(5) Uani 1 1 d . . .
C20 C 0.7603(3) 0.49765(15) 0.42677(15) 0.0370(6) Uani 1 1 d . . .
H20A H 0.7266 0.5243 0.4812 0.055 Uiso 1 1 calc R . .
H20B H 0.6972 0.4767 0.3874 0.055 Uiso 1 1 calc R . .
H20C H 0.8072 0.5439 0.3957 0.055 Uiso 1 1 calc R . .
C21 C 0.7622(2) 0.34716(16) 0.50199(14) 0.0359(5) Uani 1 1 d . . .
H21A H 0.8109 0.2963 0.5228 0.054 Uiso 1 1 calc R . .
H21B H 0.7014 0.3239 0.4617 0.054 Uiso 1 1 calc R . .
H21C H 0.7253 0.3770 0.5535 0.054 Uiso 1 1 calc R . .
C22 C 0.9373(2) 0.44899(16) 0.51328(15) 0.0339(6) Uani 1 1 d . . .
H22A H 0.9794 0.4993 0.4844 0.051 Uiso 1 1 calc R . .
H22B H 0.9916 0.3985 0.5246 0.051 Uiso 1 1 calc R . .
H22C H 0.9042 0.4702 0.5701 0.051 Uiso 1 1 calc R . .
C23 C 0.7176(2) 0.41836(15) 0.20370(18) 0.0428(7) Uani 1 1 d . . .
H23A H 0.7669 0.4669 0.2288 0.064 Uiso 1 1 calc R . .
H23B H 0.6350 0.4347 0.2110 0.064 Uiso 1 1 calc R . .
H23C H 0.7353 0.4110 0.1399 0.064 Uiso 1 1 calc R . .


_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
Ni N 1.8951(16) . ?
Ni C23 1.957(2) . ?
Ni P2 2.2027(6) . ?
Ni P1 2.2142(6) . ?
P1 C5 1.860(2) . ?
P1 C6 1.875(2) . ?
P1 C10 1.884(2) . ?
P2 C14 1.848(2) . ?
P2 C19 1.880(2) . ?
P2 C15 1.882(2) . ?
N C1 1.368(3) . ?
N C4 1.371(3) . ?
C1 C2 1.374(3) . ?
C1 C5 1.493(3) . ?
C2 C3 1.420(3) . ?
C3 C4 1.372(3) . ?
C4 C14 1.486(3) . ?
C6 C9 1.526(3) . ?
C6 C8 1.527(3) . ?
C6 C7 1.538(4) . ?
C10 C13 1.530(3) . ?
C10 C11 1.531(3) . ?
C10 C12 1.534(3) . ?
C15 C18 1.534(3) . ?
C15 C16 1.536(3) . ?
C15 C17 1.542(3) . ?
C19 C22 1.530(3) . ?
C19 C21 1.531(3) . ?
C19 C20 1.536(3) . ?

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
N Ni C23 179.29(9) . . ?
N Ni P2 83.87(5) . . ?
C23 Ni P2 95.53(7) . . ?
N Ni P1 84.14(5) . . ?
C23 Ni P1 96.50(7) . . ?
P2 Ni P1 166.89(2) . . ?
C5 P1 C6 103.96(10) . . ?
C5 P1 C10 102.58(10) . . ?
C6 P1 C10 112.70(10) . . ?
C5 P1 Ni 102.99(7) . . ?
C6 P1 Ni 115.43(8) . . ?
C10 P1 Ni 116.76(7) . . ?
C14 P2 C19 103.69(10) . . ?
C14 P2 C15 103.61(11) . . ?
C19 P2 C15 112.15(10) . . ?
C14 P2 Ni 102.10(7) . . ?
C19 P2 Ni 111.65(7) . . ?
C15 P2 Ni 121.14(7) . . ?
C1 N C4 107.59(17) . . ?
C1 N Ni 125.85(13) . . ?
C4 N Ni 125.43(14) . . ?
N C1 C2 109.67(19) . . ?
N C1 C5 117.88(17) . . ?
C2 C1 C5 132.4(2) . . ?
C1 C2 C3 106.37(18) . . ?
C4 C3 C2 107.11(19) . . ?
N C4 C3 109.3(2) . . ?
N C4 C14 116.55(18) . . ?
C3 C4 C14 134.2(2) . . ?
C1 C5 P1 107.92(14) . . ?
C9 C6 C8 109.4(2) . . ?
C9 C6 C7 109.3(2) . . ?
C8 C6 C7 107.5(2) . . ?
C9 C6 P1 114.12(16) . . ?
C8 C6 P1 111.67(15) . . ?
C7 C6 P1 104.58(16) . . ?
C13 C10 C11 109.0(2) . . ?
C13 C10 C12 108.8(2) . . ?
C11 C10 C12 107.5(2) . . ?
C13 C10 P1 104.32(16) . . ?
C11 C10 P1 112.02(16) . . ?
C12 C10 P1 115.01(15) . . ?
C4 C14 P2 106.51(14) . . ?
C18 C15 C16 108.5(2) . . ?
C18 C15 C17 108.8(2) . . ?
C16 C15 C17 108.8(2) . . ?
C18 C15 P2 112.96(17) . . ?
C16 C15 P2 104.63(16) . . ?
C17 C15 P2 112.91(17) . . ?
C22 C19 C21 109.60(19) . . ?
C22 C19 C20 109.45(19) . . ?
C21 C19 C20 107.48(19) . . ?
C22 C19 P2 112.87(15) . . ?
C21 C19 P2 106.94(14) . . ?
C20 C19 P2 110.34(15) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N Ni P1 C5 7.46(9) . . . . ?
C23 Ni P1 C5 -172.84(12) . . . . ?
P2 Ni P1 C5 -16.48(14) . . . . ?
N Ni P1 C6 -105.11(9) . . . . ?
C23 Ni P1 C6 74.58(12) . . . . ?
P2 Ni P1 C6 -129.05(12) . . . . ?
N Ni P1 C10 118.97(9) . . . . ?
C23 Ni P1 C10 -61.33(12) . . . . ?
P2 Ni P1 C10 95.04(13) . . . . ?
N Ni P2 C14 13.99(9) . . . . ?
C23 Ni P2 C14 -165.65(11) . . . . ?
P1 Ni P2 C14 37.94(14) . . . . ?
N Ni P2 C19 -96.23(9) . . . . ?
C23 Ni P2 C19 84.14(11) . . . . ?
P1 Ni P2 C19 -72.27(13) . . . . ?
N Ni P2 C15 128.24(10) . . . . ?
C23 Ni P2 C15 -51.40(12) . . . . ?
P1 Ni P2 C15 152.19(13) . . . . ?
C23 Ni N C1 -166(23) . . . . ?
P2 Ni N C1 163.10(16) . . . . ?
P1 Ni N C1 -11.59(15) . . . . ?
C23 Ni N C4 28(8) . . . . ?
P2 Ni N C4 -3.24(15) . . . . ?
P1 Ni N C4 -177.93(16) . . . . ?
C4 N C1 C2 1.1(2) . . . . ?
Ni N C1 C2 -167.21(14) . . . . ?
C4 N C1 C5 179.65(18) . . . . ?
Ni N C1 C5 11.3(3) . . . . ?
N C1 C2 C3 -1.0(2) . . . . ?
C5 C1 C2 C3 -179.2(2) . . . . ?
C1 C2 C3 C4 0.4(2) . . . . ?
C1 N C4 C3 -0.9(2) . . . . ?
Ni N C4 C3 167.55(14) . . . . ?
C1 N C4 C14 178.49(17) . . . . ?
Ni N C4 C14 -13.1(2) . . . . ?
C2 C3 C4 N 0.3(2) . . . . ?
C2 C3 C4 C14 -178.9(2) . . . . ?
N C1 C5 P1 -2.6(2) . . . . ?
C2 C1 C5 P1 175.5(2) . . . . ?
C6 P1 C5 C1 116.20(16) . . . . ?
C10 P1 C5 C1 -126.23(15) . . . . ?
Ni P1 C5 C1 -4.57(16) . . . . ?
C5 P1 C6 C9 58.34(19) . . . . ?
C10 P1 C6 C9 -52.0(2) . . . . ?
Ni P1 C6 C9 170.35(15) . . . . ?
C5 P1 C6 C8 -176.92(19) . . . . ?
C10 P1 C6 C8 72.8(2) . . . . ?
Ni P1 C6 C8 -64.9(2) . . . . ?
C5 P1 C6 C7 -61.00(18) . . . . ?
C10 P1 C6 C7 -171.32(17) . . . . ?
Ni P1 C6 C7 51.01(18) . . . . ?
C5 P1 C10 C13 75.73(17) . . . . ?
C6 P1 C10 C13 -173.09(16) . . . . ?
Ni P1 C10 C13 -36.02(17) . . . . ?
C5 P1 C10 C11 -166.45(17) . . . . ?
C6 P1 C10 C11 -55.3(2) . . . . ?
Ni P1 C10 C11 81.80(18) . . . . ?
C5 P1 C10 C12 -43.37(19) . . . . ?
C6 P1 C10 C12 67.8(2) . . . . ?
Ni P1 C10 C12 -155.12(15) . . . . ?
N C4 C14 P2 23.8(2) . . . . ?
C3 C4 C14 P2 -157.1(2) . . . . ?
C19 P2 C14 C4 93.15(16) . . . . ?
C15 P2 C14 C4 -149.57(15) . . . . ?
Ni P2 C14 C4 -22.99(15) . . . . ?
C14 P2 C15 C18 -37.43(19) . . . . ?
C19 P2 C15 C18 73.76(19) . . . . ?
Ni P2 C15 C18 -150.89(14) . . . . ?
C14 P2 C15 C16 80.37(19) . . . . ?
C19 P2 C15 C16 -168.44(17) . . . . ?
Ni P2 C15 C16 -33.1(2) . . . . ?
C14 P2 C15 C17 -161.42(17) . . . . ?
C19 P2 C15 C17 -50.2(2) . . . . ?
Ni P2 C15 C17 85.11(18) . . . . ?
C14 P2 C19 C22 67.05(17) . . . . ?
C15 P2 C19 C22 -44.09(19) . . . . ?
Ni P2 C19 C22 176.25(13) . . . . ?
C14 P2 C19 C21 -53.55(17) . . . . ?
C15 P2 C19 C21 -164.69(15) . . . . ?
Ni P2 C19 C21 55.65(16) . . . . ?
C14 P2 C19 C20 -170.14(17) . . . . ?
C15 P2 C19 C20 78.72(19) . . . . ?
Ni P2 C19 C20 -60.95(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        23.85
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.037

#=============================================================================
#  end of cif data for "MB30may" (compound 6b)
#=============================================================================


#=============================================================================
#  end of combined cif data
#=============================================================================
