# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_COMPOUND_4
_database_code_depnum_ccdc_archive 'CCDC 1017478'
_audit_update_record             
;
2015-02-20 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H31 Cl Ni O3 P2'
_chemical_formula_sum            'C18 H31 Cl Ni O3 P2'
_chemical_formula_weight         451.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.2454(14)
_cell_length_b                   14.3018(16)
_cell_length_c                   14.9082(17)
_cell_angle_alpha                71.876(2)
_cell_angle_beta                 69.050(3)
_cell_angle_gamma                71.933(3)
_cell_volume                     2258.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4262
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      25.21

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.106
_exptl_absorpt_coefficient_mu    1.132
_shelx_estimated_absorpt_T_min   0.655
_shelx_estimated_absorpt_T_max   0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.605466
_exptl_absorpt_correction_T_max  0.745214
_exptl_absorpt_process_details   '(Sheldrick, 2007)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            8230
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.827
_diffrn_reflns_theta_max         25.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8230
_reflns_number_gt                6165
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 7.34A (Bruker, 2006)'
_computing_structure_solution    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.12 (Sheldrick, 2000)'
_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0572P)²+0.3290P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8230
_refine_ls_number_parameters     474
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.1007
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.35083(4) 0.63872(3) 0.23918(3) 0.04358(14) Uani 1 1 d . . . . .
Cl1 Cl 0.50761(9) 0.59005(8) 0.11894(7) 0.0576(3) Uani 1 1 d . . . . .
P1 P 0.38332(10) 0.78217(8) 0.23024(8) 0.0515(3) Uani 1 1 d . . . . .
P2 P 0.27348(9) 0.50944(7) 0.28113(7) 0.0460(2) Uani 1 1 d . . . . .
O1 O 0.2802(3) 0.8266(2) 0.3230(2) 0.0617(8) Uani 1 1 d . . . . .
O2 O -0.0277(3) 0.7264(2) 0.6153(2) 0.0601(8) Uani 1 1 d D . . . .
H2 H -0.020(4) 0.774(3) 0.625(4) 0.090 Uiso 1 1 d D U . . .
O3 O 0.1677(2) 0.51658(19) 0.38627(19) 0.0539(7) Uani 1 1 d . . . . .
C1 C 0.2273(3) 0.6707(3) 0.3515(3) 0.0472(9) Uani 1 1 d . . . . .
C2 C 0.2078(3) 0.7585(3) 0.3818(3) 0.0505(10) Uani 1 1 d . . . . .
C3 C 0.1233(3) 0.7813(3) 0.4678(3) 0.0516(10) Uani 1 1 d . . . . .
H3 H 0.1126 0.8415 0.4849 0.062 Uiso 1 1 calc R U . . .
C4 C 0.0557(3) 0.7115(3) 0.5272(3) 0.0490(9) Uani 1 1 d . . . . .
C5 C 0.0679(3) 0.6232(3) 0.5009(3) 0.0488(9) Uani 1 1 d . . . . .
H5 H 0.0203 0.5775 0.5404 0.059 Uiso 1 1 calc R U . . .
C6 C 0.1530(3) 0.6057(3) 0.4142(3) 0.0449(9) Uani 1 1 d . . . . .
C7 C 0.3636(4) 0.8862(3) 0.1239(3) 0.0664(13) Uani 1 1 d . . . . .
H7 H 0.4297 0.8696 0.0663 0.080 Uiso 1 1 calc R U . . .
C8 C 0.3684(6) 0.9877(4) 0.1351(4) 0.105(2) Uani 1 1 d . . . . .
H8A H 0.3535 1.0396 0.0791 0.158 Uiso 1 1 calc R U . . .
H8B H 0.4463 0.9835 0.1393 0.158 Uiso 1 1 calc R U . . .
H8C H 0.3085 1.0036 0.1940 0.158 Uiso 1 1 calc R U . . .
C9 C 0.2487(5) 0.8919(4) 0.1050(4) 0.1036(19) Uani 1 1 d . . . . .
H9A H 0.2412 0.9425 0.0463 0.155 Uiso 1 1 calc R U . . .
H9B H 0.1819 0.9092 0.1599 0.155 Uiso 1 1 calc R U . . .
H9C H 0.2497 0.8277 0.0968 0.155 Uiso 1 1 calc R U . . .
C10 C 0.5190(4) 0.7821(4) 0.2542(3) 0.0699(13) Uani 1 1 d . . . . .
H10 H 0.5068 0.8459 0.2719 0.084 Uiso 1 1 calc R U . . .
C11 C 0.6296(4) 0.7740(5) 0.1636(4) 0.1005(19) Uani 1 1 d . . . . .
H11A H 0.6994 0.7716 0.1803 0.151 Uiso 1 1 calc R U . . .
H11B H 0.6179 0.8317 0.1110 0.151 Uiso 1 1 calc R U . . .
H11C H 0.6407 0.7136 0.1429 0.151 Uiso 1 1 calc R U . . .
C12 C 0.5377(5) 0.6954(4) 0.3432(4) 0.0984(18) Uani 1 1 d . . . . .
H12A H 0.6037 0.6993 0.3613 0.148 Uiso 1 1 calc R U . . .
H12B H 0.5549 0.6319 0.3261 0.148 Uiso 1 1 calc R U . . .
H12C H 0.4662 0.7010 0.3977 0.148 Uiso 1 1 calc R U . . .
C13 C 0.1889(4) 0.5019(3) 0.2054(3) 0.0610(11) Uani 1 1 d . . . . .
H13 H 0.1445 0.4485 0.2417 0.073 Uiso 1 1 calc R U . . .
C14 C 0.2742(5) 0.4748(4) 0.1084(3) 0.0855(16) Uani 1 1 d . . . . .
H14A H 0.2284 0.4748 0.0679 0.128 Uiso 1 1 calc R U . . .
H14B H 0.3249 0.4090 0.1222 0.128 Uiso 1 1 calc R U . . .
H14C H 0.3229 0.5236 0.0743 0.128 Uiso 1 1 calc R U . . .
C15 C 0.0985(5) 0.6020(4) 0.1881(5) 0.104(2) Uani 1 1 d . . . . .
H15A H 0.0533 0.5984 0.1487 0.156 Uiso 1 1 calc R U . . .
H15B H 0.1404 0.6555 0.1544 0.156 Uiso 1 1 calc R U . . .
H15C H 0.0450 0.6149 0.2504 0.156 Uiso 1 1 calc R U . . .
C16 C 0.3706(4) 0.3856(3) 0.3105(3) 0.0629(12) Uani 1 1 d . . . . .
H16 H 0.4396 0.3780 0.2520 0.076 Uiso 1 1 calc R U . . .
C17 C 0.3115(4) 0.2971(3) 0.3369(4) 0.0799(15) Uani 1 1 d . . . . .
H17A H 0.3670 0.2350 0.3533 0.120 Uiso 1 1 calc R U . . .
H17B H 0.2889 0.2968 0.2816 0.120 Uiso 1 1 calc R U . . .
H17C H 0.2413 0.3041 0.3923 0.120 Uiso 1 1 calc R U . . .
C18 C 0.4178(5) 0.3845(4) 0.3931(4) 0.0956(18) Uani 1 1 d . . . . .
H18A H 0.4774 0.3234 0.4038 0.143 Uiso 1 1 calc R U . . .
H18B H 0.3527 0.3877 0.4526 0.143 Uiso 1 1 calc R U . . .
H18C H 0.4529 0.4416 0.3747 0.143 Uiso 1 1 calc R U . . .
Ni2 Ni 0.84539(4) 0.13804(3) 0.26909(3) 0.04399(14) Uani 1 1 d . . . . .
Cl2 Cl 1.00058(9) 0.08759(8) 0.32796(8) 0.0600(3) Uani 1 1 d . . . . .
P3 P 0.76827(10) 0.00856(7) 0.34959(8) 0.0482(3) Uani 1 1 d . . . . .
P4 P 0.88038(9) 0.28020(8) 0.17123(8) 0.0494(3) Uani 1 1 d . . . . .
O21 O 0.6561(2) 0.0199(2) 0.3078(2) 0.0584(8) Uani 1 1 d . . . . .
O22 O 0.4560(3) 0.2322(2) 0.0726(2) 0.0625(8) Uani 1 1 d D . . . .
H22 H 0.469(5) 0.279(3) 0.030(3) 0.094 Uiso 1 1 d D U . . .
O23 O 0.7794(2) 0.3227(2) 0.1105(2) 0.0605(8) Uani 1 1 d . . . . .
C21 C 0.7211(3) 0.1705(3) 0.2116(3) 0.0457(9) Uani 1 1 d . . . . .
C22 C 0.6417(3) 0.1083(3) 0.2350(3) 0.0487(10) Uani 1 1 d . . . . .
C23 C 0.5543(3) 0.1276(3) 0.1901(3) 0.0521(10) Uani 1 1 d . . . . .
H23 H 0.5039 0.0836 0.2083 0.063 Uiso 1 1 calc R U . . .
C24 C 0.5435(3) 0.2150(3) 0.1169(3) 0.0487(9) Uani 1 1 d . . . . .
C25 C 0.6159(4) 0.2820(3) 0.0909(3) 0.0534(10) Uani 1 1 d . . . . .
H25 H 0.6064 0.3414 0.0432 0.064 Uiso 1 1 calc R U . . .
C26 C 0.7028(3) 0.2578(3) 0.1381(3) 0.0485(9) Uani 1 1 d . . . . .
C27 C 0.6921(4) -0.0072(3) 0.4818(3) 0.0597(11) Uani 1 1 d . . . . .
H27 H 0.6442 -0.0576 0.5009 0.072 Uiso 1 1 calc R U . . .
C28 C 0.7809(5) -0.0454(4) 0.5426(3) 0.0808(15) Uani 1 1 d . . . . .
H28A H 0.7377 -0.0493 0.6110 0.121 Uiso 1 1 calc R U . . .
H28B H 0.8331 0.0003 0.5215 0.121 Uiso 1 1 calc R U . . .
H28C H 0.8277 -0.1112 0.5333 0.121 Uiso 1 1 calc R U . . .
C29 C 0.6064(4) 0.0925(4) 0.5009(4) 0.0838(15) Uani 1 1 d . . . . .
H29A H 0.5572 0.0825 0.5682 0.126 Uiso 1 1 calc R U . . .
H29B H 0.5563 0.1164 0.4578 0.126 Uiso 1 1 calc R U . . .
H29C H 0.6518 0.1415 0.4888 0.126 Uiso 1 1 calc R U . . .
C30 C 0.8621(4) -0.1140(3) 0.3272(4) 0.0708(13) Uani 1 1 d . . . . .
H30 H 0.9293 -0.1298 0.3545 0.085 Uiso 1 1 calc R U . . .
C31 C 0.7976(5) -0.1999(3) 0.3745(4) 0.1001(19) Uani 1 1 d . . . . .
H31A H 0.8523 -0.2617 0.3605 0.150 Uiso 1 1 calc R U . . .
H31B H 0.7317 -0.1865 0.3484 0.150 Uiso 1 1 calc R U . . .
H31C H 0.7679 -0.2060 0.4445 0.150 Uiso 1 1 calc R U . . .
C32 C 0.9136(5) -0.1038(4) 0.2156(4) 0.111(2) Uani 1 1 d . . . . .
H32A H 0.9698 -0.1652 0.2022 0.167 Uiso 1 1 calc R U . . .
H32B H 0.9535 -0.0488 0.1872 0.167 Uiso 1 1 calc R U . . .
H32C H 0.8496 -0.0911 0.1874 0.167 Uiso 1 1 calc R U . . .
C33 C 1.0190(4) 0.2786(4) 0.0700(3) 0.0671(12) Uani 1 1 d . . . . .
H33 H 1.0087 0.3424 0.0210 0.081 Uiso 1 1 calc R U . . .
C34 C 1.1266(4) 0.2702(4) 0.1036(4) 0.0913(17) Uani 1 1 d . . . . .
H34A H 1.1969 0.2719 0.0478 0.137 Uiso 1 1 calc R U . . .
H34B H 1.1390 0.2078 0.1511 0.137 Uiso 1 1 calc R U . . .
H34C H 1.1113 0.3257 0.1330 0.137 Uiso 1 1 calc R U . . .
C35 C 1.0380(5) 0.1928(4) 0.0215(4) 0.0996(19) Uani 1 1 d . . . . .
H35A H 1.1050 0.1963 -0.0370 0.149 Uiso 1 1 calc R U . . .
H35B H 0.9672 0.1992 0.0043 0.149 Uiso 1 1 calc R U . . .
H35C H 1.0538 0.1292 0.0666 0.149 Uiso 1 1 calc R U . . .
C36 C 0.8584(4) 0.3863(3) 0.2231(3) 0.0612(12) Uani 1 1 d . . . . .
H36 H 0.9250 0.3725 0.2506 0.073 Uiso 1 1 calc R U . . .
C37 C 0.7429(5) 0.3935(4) 0.3080(4) 0.0938(17) Uani 1 1 d . . . . .
H37A H 0.7368 0.4445 0.3399 0.141 Uiso 1 1 calc R U . . .
H37B H 0.7437 0.3296 0.3547 0.141 Uiso 1 1 calc R U . . .
H37C H 0.6753 0.4108 0.2830 0.141 Uiso 1 1 calc R U . . .
C38 C 0.8597(5) 0.4867(3) 0.1474(4) 0.0917(17) Uani 1 1 d . . . . .
H38A H 0.8524 0.5386 0.1786 0.138 Uiso 1 1 calc R U . . .
H38B H 0.7938 0.5035 0.1204 0.138 Uiso 1 1 calc R U . . .
H38C H 0.9339 0.4810 0.0954 0.138 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.881(4) . ?
Ni1 P2 2.1565(11) . ?
Ni1 P1 2.1641(11) . ?
Ni1 Cl1 2.2068(11) . ?
P1 O1 1.646(3) . ?
P1 C10 1.820(4) . ?
P1 C7 1.835(4) . ?
P2 O3 1.646(3) . ?
P2 C16 1.824(4) . ?
P2 C13 1.828(4) . ?
O1 C2 1.396(4) . ?
O2 C4 1.376(4) . ?
O2 H2 0.78(3) . ?
O3 C6 1.402(4) . ?
C1 C2 1.389(5) . ?
C1 C6 1.392(5) . ?
C2 C3 1.386(5) . ?
C3 C4 1.380(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(5) . ?
C5 C6 1.378(5) . ?
C5 H5 0.9300 . ?
C7 C9 1.505(7) . ?
C7 C8 1.533(6) . ?
C7 H7 0.9800 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.538(6) . ?
C10 C12 1.538(7) . ?
C10 H10 0.9800 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C15 1.526(6) . ?
C13 C14 1.533(6) . ?
C13 H13 0.9800 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.527(6) . ?
C16 C18 1.531(7) . ?
C16 H16 0.9800 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
Ni2 C21 1.874(4) . ?
Ni2 P3 2.1570(11) . ?
Ni2 P4 2.1665(11) . ?
Ni2 Cl2 2.2024(11) . ?
P3 O21 1.648(3) . ?
P3 C30 1.828(4) . ?
P3 C27 1.829(4) . ?
P4 O23 1.646(3) . ?
P4 C36 1.818(4) . ?
P4 C33 1.824(4) . ?
O21 C22 1.397(4) . ?
O22 C24 1.373(5) . ?
O22 H22 0.78(3) . ?
O23 C26 1.391(4) . ?
C21 C26 1.399(5) . ?
C21 C22 1.401(5) . ?
C22 C23 1.372(5) . ?
C23 C24 1.387(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.380(5) . ?
C25 C26 1.380(5) . ?
C25 H25 0.9300 . ?
C27 C29 1.526(6) . ?
C27 C28 1.527(6) . ?
C27 H27 0.9800 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.515(6) . ?
C30 C32 1.531(7) . ?
C30 H30 0.9800 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.529(6) . ?
C33 C35 1.529(6) . ?
C33 H33 0.9800 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.525(6) . ?
C36 C38 1.526(6) . ?
C36 H36 0.9800 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?

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
C1 Ni1 P2 81.65(11) . . ?
C1 Ni1 P1 82.00(11) . . ?
P2 Ni1 P1 163.49(4) . . ?
C1 Ni1 Cl1 173.51(12) . . ?
P2 Ni1 Cl1 97.45(4) . . ?
P1 Ni1 Cl1 99.06(4) . . ?
O1 P1 C10 100.52(18) . . ?
O1 P1 C7 102.40(19) . . ?
C10 P1 C7 107.6(2) . . ?
O1 P1 Ni1 106.36(10) . . ?
C10 P1 Ni1 118.31(17) . . ?
C7 P1 Ni1 118.76(16) . . ?
O3 P2 C16 102.94(17) . . ?
O3 P2 C13 101.00(17) . . ?
C16 P2 C13 108.2(2) . . ?
O3 P2 Ni1 106.85(10) . . ?
C16 P2 Ni1 116.95(15) . . ?
C13 P2 Ni1 118.46(14) . . ?
C2 O1 P1 111.5(2) . . ?
C4 O2 H2 107(4) . . ?
C6 O3 P2 111.3(2) . . ?
C2 C1 C6 114.6(3) . . ?
C2 C1 Ni1 122.4(3) . . ?
C6 C1 Ni1 122.9(3) . . ?
C3 C2 C1 124.1(3) . . ?
C3 C2 O1 118.3(3) . . ?
C1 C2 O1 117.6(3) . . ?
C4 C3 C2 117.6(3) . . ?
C4 C3 H3 121.2 . . ?
C2 C3 H3 121.2 . . ?
O2 C4 C3 121.6(3) . . ?
O2 C4 C5 116.6(3) . . ?
C3 C4 C5 121.7(3) . . ?
C6 C5 C4 117.5(3) . . ?
C6 C5 H5 121.3 . . ?
C4 C5 H5 121.3 . . ?
C5 C6 C1 124.4(3) . . ?
C5 C6 O3 118.6(3) . . ?
C1 C6 O3 117.0(3) . . ?
C9 C7 C8 111.8(4) . . ?
C9 C7 P1 109.1(3) . . ?
C8 C7 P1 113.3(4) . . ?
C9 C7 H7 107.5 . . ?
C8 C7 H7 107.5 . . ?
P1 C7 H7 107.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C12 111.4(4) . . ?
C11 C10 P1 112.4(3) . . ?
C12 C10 P1 108.7(3) . . ?
C11 C10 H10 108.1 . . ?
C12 C10 H10 108.1 . . ?
P1 C10 H10 108.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C15 C13 C14 112.1(4) . . ?
C15 C13 P2 109.0(3) . . ?
C14 C13 P2 110.5(3) . . ?
C15 C13 H13 108.4 . . ?
C14 C13 H13 108.4 . . ?
P2 C13 H13 108.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C18 111.6(4) . . ?
C17 C16 P2 114.3(3) . . ?
C18 C16 P2 108.0(3) . . ?
C17 C16 H16 107.5 . . ?
C18 C16 H16 107.5 . . ?
P2 C16 H16 107.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 Ni2 P3 81.62(11) . . ?
C21 Ni2 P4 82.14(11) . . ?
P3 Ni2 P4 163.73(5) . . ?
C21 Ni2 Cl2 174.09(12) . . ?
P3 Ni2 Cl2 96.54(4) . . ?
P4 Ni2 Cl2 99.71(4) . . ?
O21 P3 C30 101.86(18) . . ?
O21 P3 C27 100.55(17) . . ?
C30 P3 C27 108.1(2) . . ?
O21 P3 Ni2 106.86(10) . . ?
C30 P3 Ni2 116.46(16) . . ?
C27 P3 Ni2 120.14(14) . . ?
O23 P4 C36 101.84(18) . . ?
O23 P4 C33 101.13(18) . . ?
C36 P4 C33 106.9(2) . . ?
O23 P4 Ni2 106.03(10) . . ?
C36 P4 Ni2 119.40(15) . . ?
C33 P4 Ni2 118.59(16) . . ?
C22 O21 P3 111.6(2) . . ?
C24 O22 H22 102(4) . . ?
C26 O23 P4 112.1(2) . . ?
C26 C21 C22 114.0(3) . . ?
C26 C21 Ni2 122.6(3) . . ?
C22 C21 Ni2 123.4(3) . . ?
C23 C22 O21 119.0(3) . . ?
C23 C22 C21 124.5(4) . . ?
O21 C22 C21 116.5(3) . . ?
C22 C23 C24 117.8(3) . . ?
C22 C23 H23 121.1 . . ?
C24 C23 H23 121.1 . . ?
O22 C24 C25 121.7(3) . . ?
O22 C24 C23 116.6(3) . . ?
C25 C24 C23 121.6(4) . . ?
C24 C25 C26 117.8(4) . . ?
C24 C25 H25 121.1 . . ?
C26 C25 H25 121.1 . . ?
C25 C26 O23 118.6(3) . . ?
C25 C26 C21 124.3(3) . . ?
O23 C26 C21 117.1(3) . . ?
C29 C27 C28 112.1(4) . . ?
C29 C27 P3 108.8(3) . . ?
C28 C27 P3 111.9(3) . . ?
C29 C27 H27 107.9 . . ?
C28 C27 H27 107.9 . . ?
P3 C27 H27 107.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C32 110.9(4) . . ?
C31 C30 P3 114.1(4) . . ?
C32 C30 P3 108.0(3) . . ?
C31 C30 H30 107.9 . . ?
C32 C30 H30 107.9 . . ?
P3 C30 H30 107.9 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C35 112.2(4) . . ?
C34 C33 P4 112.2(3) . . ?
C35 C33 P4 108.5(3) . . ?
C34 C33 H33 107.9 . . ?
C35 C33 H33 107.9 . . ?
P4 C33 H33 107.9 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 C38 110.8(4) . . ?
C37 C36 P4 110.1(3) . . ?
C38 C36 P4 113.7(3) . . ?
C37 C36 H36 107.3 . . ?
C38 C36 H36 107.3 . . ?
P4 C36 H36 107.3 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?

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
C10 P1 O1 C2 -120.8(3) . . . . ?
C7 P1 O1 C2 128.4(3) . . . . ?
Ni1 P1 O1 C2 3.1(3) . . . . ?
C16 P2 O3 C6 127.7(3) . . . . ?
C13 P2 O3 C6 -120.5(3) . . . . ?
Ni1 P2 O3 C6 4.0(3) . . . . ?
P2 Ni1 C1 C2 -178.4(3) . . . . ?
P1 Ni1 C1 C2 -0.7(3) . . . . ?
P2 Ni1 C1 C6 5.7(3) . . . . ?
P1 Ni1 C1 C6 -176.6(3) . . . . ?
C6 C1 C2 C3 0.9(6) . . . . ?
Ni1 C1 C2 C3 -175.3(3) . . . . ?
C6 C1 C2 O1 179.2(3) . . . . ?
Ni1 C1 C2 O1 3.0(5) . . . . ?
P1 O1 C2 C3 174.5(3) . . . . ?
P1 O1 C2 C1 -3.9(5) . . . . ?
C1 C2 C3 C4 0.8(6) . . . . ?
O1 C2 C3 C4 -177.5(4) . . . . ?
C2 C3 C4 O2 178.1(4) . . . . ?
C2 C3 C4 C5 -2.3(6) . . . . ?
O2 C4 C5 C6 -178.4(3) . . . . ?
C3 C4 C5 C6 2.0(6) . . . . ?
C4 C5 C6 C1 0.0(6) . . . . ?
C4 C5 C6 O3 179.6(3) . . . . ?
C2 C1 C6 C5 -1.3(6) . . . . ?
Ni1 C1 C6 C5 174.8(3) . . . . ?
C2 C1 C6 O3 179.0(3) . . . . ?
Ni1 C1 C6 O3 -4.8(5) . . . . ?
P2 O3 C6 C5 -179.9(3) . . . . ?
P2 O3 C6 C1 -0.2(4) . . . . ?
O1 P1 C7 C9 -71.8(4) . . . . ?
C10 P1 C7 C9 -177.2(4) . . . . ?
Ni1 P1 C7 C9 45.0(4) . . . . ?
O1 P1 C7 C8 53.5(4) . . . . ?
C10 P1 C7 C8 -51.9(4) . . . . ?
Ni1 P1 C7 C8 170.2(3) . . . . ?
O1 P1 C10 C11 -163.0(4) . . . . ?
C7 P1 C10 C11 -56.3(4) . . . . ?
Ni1 P1 C10 C11 81.8(4) . . . . ?
O1 P1 C10 C12 73.3(4) . . . . ?
C7 P1 C10 C12 180.0(3) . . . . ?
Ni1 P1 C10 C12 -41.9(4) . . . . ?
O3 P2 C13 C15 67.0(4) . . . . ?
C16 P2 C13 C15 174.7(4) . . . . ?
Ni1 P2 C13 C15 -49.2(4) . . . . ?
O3 P2 C13 C14 -169.4(3) . . . . ?
C16 P2 C13 C14 -61.7(3) . . . . ?
Ni1 P2 C13 C14 74.4(3) . . . . ?
O3 P2 C16 C17 64.8(4) . . . . ?
C13 P2 C16 C17 -41.6(4) . . . . ?
Ni1 P2 C16 C17 -178.4(3) . . . . ?
O3 P2 C16 C18 -60.1(3) . . . . ?
C13 P2 C16 C18 -166.5(3) . . . . ?
Ni1 P2 C16 C18 56.7(3) . . . . ?
C30 P3 O21 C22 -123.4(3) . . . . ?
C27 P3 O21 C22 125.4(3) . . . . ?
Ni2 P3 O21 C22 -0.8(3) . . . . ?
C36 P4 O23 C26 -125.6(3) . . . . ?
C33 P4 O23 C26 124.3(3) . . . . ?
Ni2 P4 O23 C26 0.0(3) . . . . ?
P3 Ni2 C21 C26 -179.5(3) . . . . ?
P4 Ni2 C21 C26 1.5(3) . . . . ?
P3 Ni2 C21 C22 -2.2(3) . . . . ?
P4 Ni2 C21 C22 178.7(3) . . . . ?
P3 O21 C22 C23 178.0(3) . . . . ?
P3 O21 C22 C21 -0.7(4) . . . . ?
C26 C21 C22 C23 1.2(6) . . . . ?
Ni2 C21 C22 C23 -176.3(3) . . . . ?
C26 C21 C22 O21 179.8(3) . . . . ?
Ni2 C21 C22 O21 2.4(5) . . . . ?
O21 C22 C23 C24 -178.8(3) . . . . ?
C21 C22 C23 C24 -0.2(6) . . . . ?
C22 C23 C24 O22 179.5(3) . . . . ?
C22 C23 C24 C25 -1.5(6) . . . . ?
O22 C24 C25 C26 -178.9(4) . . . . ?
C23 C24 C25 C26 2.1(6) . . . . ?
C24 C25 C26 O23 177.8(4) . . . . ?
C24 C25 C26 C21 -1.0(6) . . . . ?
P4 O23 C26 C25 -177.8(3) . . . . ?
P4 O23 C26 C21 1.1(4) . . . . ?
C22 C21 C26 C25 -0.6(6) . . . . ?
Ni2 C21 C26 C25 176.9(3) . . . . ?
C22 C21 C26 O23 -179.4(3) . . . . ?
Ni2 C21 C26 O23 -1.9(5) . . . . ?
O21 P3 C27 C29 -69.6(3) . . . . ?
C30 P3 C27 C29 -175.9(3) . . . . ?
Ni2 P3 C27 C29 47.1(4) . . . . ?
O21 P3 C27 C28 165.9(3) . . . . ?
C30 P3 C27 C28 59.6(4) . . . . ?
Ni2 P3 C27 C28 -77.4(3) . . . . ?
O21 P3 C30 C31 -56.1(4) . . . . ?
C27 P3 C30 C31 49.3(4) . . . . ?
Ni2 P3 C30 C31 -171.9(3) . . . . ?
O21 P3 C30 C32 67.7(4) . . . . ?
C27 P3 C30 C32 173.1(3) . . . . ?
Ni2 P3 C30 C32 -48.1(4) . . . . ?
O23 P4 C33 C34 164.0(3) . . . . ?
C36 P4 C33 C34 57.8(4) . . . . ?
Ni2 P4 C33 C34 -80.7(4) . . . . ?
O23 P4 C33 C35 -71.5(4) . . . . ?
C36 P4 C33 C35 -177.7(3) . . . . ?
Ni2 P4 C33 C35 43.8(4) . . . . ?
O23 P4 C36 C37 73.7(3) . . . . ?
C33 P4 C36 C37 179.4(3) . . . . ?
Ni2 P4 C36 C37 -42.5(4) . . . . ?
O23 P4 C36 C38 -51.2(4) . . . . ?
C33 P4 C36 C38 54.4(4) . . . . ?
Ni2 P4 C36 C38 -167.5(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 Cl2 0.78(3) 2.39(3) 3.171(3) 175(5) 2_666
O22 H22 Cl1 0.78(3) 2.41(3) 3.177(3) 168(5) 2_665

_refine_diff_density_max         0.606
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.074

####################################################################### 
# 
# 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_COMPOUND_5
_database_code_depnum_ccdc_archive 'CCDC 1017479'
_audit_update_record             
;
2015-02-20 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H39 Cl Ni O3 P2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C22.50 H40 Cl2 Ni O3 P2'
_chemical_formula_weight         550.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.1590(11)
_cell_length_b                   20.230(2)
_cell_length_c                   13.9587(15)
_cell_angle_alpha                90
_cell_angle_beta                 102.917(2)
_cell_angle_gamma                90
_cell_volume                     2796.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6248
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      25.01

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             1164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.162
_exptl_absorpt_coefficient_mu    1.020
_shelx_estimated_absorpt_T_min   0.759
_shelx_estimated_absorpt_T_max   0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7769
_exptl_absorpt_correction_T_max  0.8734
_exptl_absorpt_process_details   '(Sheldrick, 2007)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker Smart Apex CCD diffractometer 01-670-01'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            22474
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.804
_diffrn_reflns_theta_max         25.377
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5123
_reflns_number_gt                3903
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 7.34A (Bruker, 2006)'
_computing_structure_solution    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.12 (Sheldrick, 2000)'
_refine_special_details          
;
The compound display disorder affecting the CH2Cl2 solvent, 
which was modeled with SIMU and DELU restraints on anisotropic 
displacement parameters and SADI geometrical restraints.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0628P)²+0.5704P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5123
_refine_ls_number_parameters     331
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1233
_refine_ls_wR_factor_gt          0.1141
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.64453(4) 0.25883(2) 0.52023(3) 0.04569(16) Uani 1 1 d . . . . .
Cl1 Cl 0.56250(13) 0.31983(5) 0.62506(9) 0.0856(4) Uani 1 1 d . . . . .
P1 P 0.53109(9) 0.16800(4) 0.52774(6) 0.0465(2) Uani 1 1 d . . . . .
P2 P 0.77936(9) 0.33313(4) 0.48149(6) 0.0460(2) Uani 1 1 d . . . . .
O1 O 0.5761(2) 0.11653(10) 0.44893(16) 0.0532(6) Uani 1 1 d . . . . .
O2 O 0.8740(3) 0.09239(12) 0.2352(2) 0.0709(8) Uani 1 1 d . . . . .
H2 H 0.927(5) 0.113(2) 0.217(4) 0.106 Uiso 1 1 d . U . . .
O3 O 0.8583(2) 0.29639(10) 0.40497(16) 0.0498(6) Uani 1 1 d . . . . .
C1 C 0.7160(3) 0.20776(14) 0.4309(2) 0.0404(7) Uani 1 1 d . . . . .
C2 C 0.6751(3) 0.14284(15) 0.4058(2) 0.0450(8) Uani 1 1 d . . . . .
C3 C 0.7273(3) 0.10405(16) 0.3421(2) 0.0504(8) Uani 1 1 d . . . . .
H3 H 0.6980 0.0608 0.3284 0.060 Uiso 1 1 calc R U . . .
C4 C 0.8247(3) 0.13149(16) 0.2990(2) 0.0492(8) Uani 1 1 d . . . . .
C5 C 0.8704(3) 0.19558(15) 0.3201(2) 0.0463(8) Uani 1 1 d . . . . .
H5 H 0.9368 0.2136 0.2917 0.056 Uiso 1 1 calc R U . . .
C6 C 0.8142(3) 0.23164(14) 0.3845(2) 0.0415(7) Uani 1 1 d . . . . .
C7 C 0.3469(4) 0.1739(2) 0.4759(3) 0.0639(10) Uani 1 1 d . . . . .
C8 C 0.3314(5) 0.2253(3) 0.3941(4) 0.1052(17) Uani 1 1 d . . . . .
H8A H 0.3571 0.2680 0.4222 0.158 Uiso 1 1 calc R U . . .
H8B H 0.2390 0.2266 0.3582 0.158 Uiso 1 1 calc R U . . .
H8C H 0.3884 0.2137 0.3503 0.158 Uiso 1 1 calc R U . . .
C9 C 0.2717(4) 0.1981(3) 0.5532(4) 0.0953(15) Uani 1 1 d . . . . .
H9A H 0.1779 0.2042 0.5230 0.143 Uiso 1 1 calc R U . . .
H9B H 0.3097 0.2393 0.5803 0.143 Uiso 1 1 calc R U . . .
H9C H 0.2805 0.1658 0.6047 0.143 Uiso 1 1 calc R U . . .
C10 C 0.2840(4) 0.1095(2) 0.4297(3) 0.0894(14) Uani 1 1 d . . . . .
H10A H 0.1890 0.1159 0.4039 0.134 Uiso 1 1 calc R U . . .
H10B H 0.2971 0.0754 0.4788 0.134 Uiso 1 1 calc R U . . .
H10C H 0.3262 0.0967 0.3776 0.134 Uiso 1 1 calc R U . . .
C11 C 0.5761(4) 0.11856(17) 0.6423(2) 0.0570(9) Uani 1 1 d . . . . .
C12 C 0.5553(5) 0.1587(2) 0.7305(3) 0.0823(13) Uani 1 1 d . . . . .
H12A H 0.5927 0.1351 0.7900 0.123 Uiso 1 1 calc R U . . .
H12B H 0.4604 0.1655 0.7253 0.123 Uiso 1 1 calc R U . . .
H12C H 0.5996 0.2007 0.7316 0.123 Uiso 1 1 calc R U . . .
C13 C 0.7274(5) 0.1048(3) 0.6565(4) 0.1015(16) Uani 1 1 d . . . . .
H13A H 0.7434 0.0811 0.6007 0.152 Uiso 1 1 calc R U . . .
H13B H 0.7578 0.0788 0.7149 0.152 Uiso 1 1 calc R U . . .
H13C H 0.7758 0.1459 0.6630 0.152 Uiso 1 1 calc R U . . .
C14 C 0.5012(5) 0.05288(18) 0.6380(3) 0.0810(13) Uani 1 1 d . . . . .
H14A H 0.4069 0.0611 0.6336 0.122 Uiso 1 1 calc R U . . .
H14B H 0.5374 0.0278 0.6963 0.122 Uiso 1 1 calc R U . . .
H14C H 0.5120 0.0284 0.5814 0.122 Uiso 1 1 calc R U . . .
C15 C 0.9267(4) 0.35637(18) 0.5808(3) 0.0608(10) Uani 1 1 d . . . . .
C16 C 1.0484(4) 0.3814(2) 0.5417(3) 0.0905(14) Uani 1 1 d . . . . .
H16A H 1.1247 0.3873 0.5957 0.136 Uiso 1 1 calc R U . . .
H16B H 1.0258 0.4228 0.5085 0.136 Uiso 1 1 calc R U . . .
H16C H 1.0703 0.3496 0.4966 0.136 Uiso 1 1 calc R U . . .
C17 C 0.9691(4) 0.2919(2) 0.6374(3) 0.0827(13) Uani 1 1 d . . . . .
H17A H 1.0496 0.2995 0.6873 0.124 Uiso 1 1 calc R U . . .
H17B H 0.9863 0.2586 0.5928 0.124 Uiso 1 1 calc R U . . .
H17C H 0.8980 0.2774 0.6676 0.124 Uiso 1 1 calc R U . . .
C18 C 0.8876(5) 0.4079(3) 0.6499(4) 0.1064(17) Uani 1 1 d . . . . .
H18A H 0.8089 0.3931 0.6711 0.160 Uiso 1 1 calc R U . . .
H18B H 0.8685 0.4492 0.6158 0.160 Uiso 1 1 calc R U . . .
H18C H 0.9609 0.4136 0.7060 0.160 Uiso 1 1 calc R U . . .
C19 C 0.6986(4) 0.40322(18) 0.4039(3) 0.0654(11) Uani 1 1 d . . . . .
C20 C 0.7945(5) 0.4422(2) 0.3580(4) 0.0896(14) Uani 1 1 d . . . . .
H20A H 0.8563 0.4661 0.4082 0.134 Uiso 1 1 calc R U . . .
H20B H 0.7445 0.4728 0.3112 0.134 Uiso 1 1 calc R U . . .
H20C H 0.8441 0.4126 0.3254 0.134 Uiso 1 1 calc R U . . .
C21 C 0.5971(6) 0.3698(3) 0.3190(4) 0.131(2) Uani 1 1 d . . . . .
H21A H 0.5493 0.4030 0.2757 0.196 Uiso 1 1 calc R U . . .
H21B H 0.5341 0.3440 0.3452 0.196 Uiso 1 1 calc R U . . .
H21C H 0.6449 0.3415 0.2831 0.196 Uiso 1 1 calc R U . . .
C22 C 0.6272(7) 0.4493(3) 0.4602(5) 0.143(3) Uani 1 1 d . . . . .
H22A H 0.5685 0.4780 0.4150 0.215 Uiso 1 1 calc R U . . .
H22B H 0.6926 0.4753 0.5048 0.215 Uiso 1 1 calc R U . . .
H22C H 0.5749 0.4240 0.4965 0.215 Uiso 1 1 calc R U . . .
C23 C 0.439(4) 0.5019(16) 0.033(3) 0.162(4) Uani 0.25 1 d D U P A -1
H23A H 0.3411 0.5016 0.0213 0.195 Uiso 0.25 1 calc R U P A -1
H23B H 0.4761 0.5329 0.0850 0.195 Uiso 0.25 1 calc R U P A -1
Cl2 Cl 0.5001(19) 0.5172(10) -0.0808(14) 0.175(4) Uani 0.25 1 d D U P A -1
Cl3 Cl 0.5129(16) 0.4178(6) 0.0571(10) 0.139(3) Uani 0.25 1 d D U P A -1
C23A C 0.537(4) 0.5314(17) 0.023(3) 0.164(5) Uani 0.25 1 d . U P B -2
H23C H 0.5030 0.5593 0.0684 0.197 Uiso 0.25 1 calc R U P B -2
H23D H 0.6277 0.5466 0.0249 0.197 Uiso 0.25 1 calc R U P B -2
Cl2A Cl 0.557(3) 0.4621(15) 0.075(2) 0.162(6) Uani 0.25 1 d D U P B -2
Cl3A Cl 0.461(3) 0.5526(14) -0.073(2) 0.152(5) Uani 0.25 1 d D U P B -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
Ni1 C1 1.885(3) . ?
Ni1 P2 2.1815(9) . ?
Ni1 P1 2.1839(9) . ?
Ni1 Cl1 2.2145(10) . ?
P1 O1 1.652(2) . ?
P1 C7 1.853(4) . ?
P1 C11 1.855(3) . ?
P2 O3 1.649(2) . ?
P2 C15 1.859(4) . ?
P2 C19 1.860(4) . ?
O1 C2 1.388(3) . ?
O2 C4 1.367(4) . ?
O2 H2 0.76(5) . ?
O3 C6 1.393(3) . ?
C1 C6 1.392(4) . ?
C1 C2 1.398(4) . ?
C2 C3 1.378(4) . ?
C3 C4 1.384(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(4) . ?
C5 C6 1.377(4) . ?
C5 H5 0.9300 . ?
C7 C8 1.527(6) . ?
C7 C10 1.529(6) . ?
C7 C9 1.534(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C14 1.526(5) . ?
C11 C12 1.528(5) . ?
C11 C13 1.530(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C18 1.531(5) . ?
C15 C17 1.535(5) . ?
C15 C16 1.544(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.504(5) . ?
C19 C22 1.505(6) . ?
C19 C21 1.543(6) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 Cl2 1.86(3) . ?
C23 Cl3 1.86(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23A Cl3A 1.45(5) . ?
C23A Cl2A 1.57(4) . ?
C23A H23C 0.9700 . ?
C23A H23D 0.9700 . ?

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
C1 Ni1 P2 81.82(9) . . ?
C1 Ni1 P1 81.72(9) . . ?
P2 Ni1 P1 163.52(4) . . ?
C1 Ni1 Cl1 179.26(10) . . ?
P2 Ni1 Cl1 97.45(4) . . ?
P1 Ni1 Cl1 99.01(4) . . ?
O1 P1 C7 100.76(15) . . ?
O1 P1 C11 100.53(14) . . ?
C7 P1 C11 113.85(17) . . ?
O1 P1 Ni1 105.70(8) . . ?
C7 P1 Ni1 115.12(13) . . ?
C11 P1 Ni1 117.64(12) . . ?
O3 P2 C15 99.78(15) . . ?
O3 P2 C19 100.48(15) . . ?
C15 P2 C19 114.73(18) . . ?
O3 P2 Ni1 105.87(8) . . ?
C15 P2 Ni1 115.78(12) . . ?
C19 P2 Ni1 116.72(13) . . ?
C2 O1 P1 112.48(18) . . ?
C4 O2 H2 107(4) . . ?
C6 O3 P2 112.05(18) . . ?
C6 C1 C2 114.4(3) . . ?
C6 C1 Ni1 122.7(2) . . ?
C2 C1 Ni1 123.0(2) . . ?
C3 C2 O1 118.8(3) . . ?
C3 C2 C1 124.1(3) . . ?
O1 C2 C1 117.0(2) . . ?
C2 C3 C4 117.9(3) . . ?
C2 C3 H3 121.1 . . ?
C4 C3 H3 121.1 . . ?
O2 C4 C3 116.9(3) . . ?
O2 C4 C5 121.7(3) . . ?
C3 C4 C5 121.4(3) . . ?
C6 C5 C4 117.8(3) . . ?
C6 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?
C5 C6 C1 124.4(3) . . ?
C5 C6 O3 118.0(3) . . ?
C1 C6 O3 117.5(2) . . ?
C8 C7 C10 107.6(4) . . ?
C8 C7 C9 109.0(4) . . ?
C10 C7 C9 109.9(3) . . ?
C8 C7 P1 105.2(3) . . ?
C10 C7 P1 113.6(3) . . ?
C9 C7 P1 111.3(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C11 C12 109.7(3) . . ?
C14 C11 C13 108.9(3) . . ?
C12 C11 C13 107.9(4) . . ?
C14 C11 P1 114.2(3) . . ?
C12 C11 P1 110.9(3) . . ?
C13 C11 P1 104.9(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18 C15 C17 109.7(4) . . ?
C18 C15 C16 109.9(3) . . ?
C17 C15 C16 107.8(3) . . ?
C18 C15 P2 111.3(3) . . ?
C17 C15 P2 104.8(3) . . ?
C16 C15 P2 113.2(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C22 109.3(4) . . ?
C20 C19 C21 106.7(4) . . ?
C22 C19 C21 110.8(4) . . ?
C20 C19 P2 113.8(3) . . ?
C22 C19 P2 111.7(3) . . ?
C21 C19 P2 104.2(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Cl2 C23 Cl3 96.2(18) . . ?
Cl2 C23 H23A 112.5 . . ?
Cl3 C23 H23A 112.5 . . ?
Cl2 C23 H23B 112.5 . . ?
Cl3 C23 H23B 112.5 . . ?
H23A C23 H23B 110.0 . . ?
Cl3A C23A Cl2A 133(3) . . ?
Cl3A C23A H23C 104.0 . . ?
Cl2A C23A H23C 104.0 . . ?
Cl3A C23A H23D 104.0 . . ?
Cl2A C23A H23D 104.0 . . ?
H23C C23A H23D 105.5 . . ?

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
C7 P1 O1 C2 123.5(2) . . . . ?
C11 P1 O1 C2 -119.5(2) . . . . ?
Ni1 P1 O1 C2 3.3(2) . . . . ?
C15 P2 O3 C6 122.8(2) . . . . ?
C19 P2 O3 C6 -119.5(2) . . . . ?
Ni1 P2 O3 C6 2.3(2) . . . . ?
P2 Ni1 C1 C6 2.0(3) . . . . ?
P1 Ni1 C1 C6 -178.8(3) . . . . ?
P2 Ni1 C1 C2 -178.1(3) . . . . ?
P1 Ni1 C1 C2 1.1(3) . . . . ?
P1 O1 C2 C3 176.8(3) . . . . ?
P1 O1 C2 C1 -2.8(4) . . . . ?
C6 C1 C2 C3 1.1(5) . . . . ?
Ni1 C1 C2 C3 -178.8(3) . . . . ?
C6 C1 C2 O1 -179.3(3) . . . . ?
Ni1 C1 C2 O1 0.8(4) . . . . ?
O1 C2 C3 C4 179.3(3) . . . . ?
C1 C2 C3 C4 -1.1(5) . . . . ?
C2 C3 C4 O2 -179.3(3) . . . . ?
C2 C3 C4 C5 1.0(5) . . . . ?
O2 C4 C5 C6 179.4(3) . . . . ?
C3 C4 C5 C6 -0.9(5) . . . . ?
C4 C5 C6 C1 0.9(5) . . . . ?
C4 C5 C6 O3 -179.1(3) . . . . ?
C2 C1 C6 C5 -1.0(5) . . . . ?
Ni1 C1 C6 C5 178.9(3) . . . . ?
C2 C1 C6 O3 179.1(3) . . . . ?
Ni1 C1 C6 O3 -1.0(4) . . . . ?
P2 O3 C6 C5 178.9(2) . . . . ?
P2 O3 C6 C1 -1.1(4) . . . . ?
O1 P1 C7 C8 -82.7(3) . . . . ?
C11 P1 C7 C8 170.6(3) . . . . ?
Ni1 P1 C7 C8 30.5(3) . . . . ?
O1 P1 C7 C10 34.7(3) . . . . ?
C11 P1 C7 C10 -72.0(3) . . . . ?
Ni1 P1 C7 C10 147.8(3) . . . . ?
O1 P1 C7 C9 159.4(3) . . . . ?
C11 P1 C7 C9 52.7(4) . . . . ?
Ni1 P1 C7 C9 -87.4(3) . . . . ?
O1 P1 C11 C14 -60.6(3) . . . . ?
C7 P1 C11 C14 46.3(3) . . . . ?
Ni1 P1 C11 C14 -174.7(2) . . . . ?
O1 P1 C11 C12 174.9(3) . . . . ?
C7 P1 C11 C12 -78.3(3) . . . . ?
Ni1 P1 C11 C12 60.8(3) . . . . ?
O1 P1 C11 C13 58.6(3) . . . . ?
C7 P1 C11 C13 165.5(3) . . . . ?
Ni1 P1 C11 C13 -55.5(3) . . . . ?
O3 P2 C15 C18 164.5(3) . . . . ?
C19 P2 C15 C18 58.1(4) . . . . ?
Ni1 P2 C15 C18 -82.4(3) . . . . ?
O3 P2 C15 C17 -77.0(3) . . . . ?
C19 P2 C15 C17 176.6(3) . . . . ?
Ni1 P2 C15 C17 36.0(3) . . . . ?
O3 P2 C15 C16 40.2(3) . . . . ?
C19 P2 C15 C16 -66.2(3) . . . . ?
Ni1 P2 C15 C16 153.2(3) . . . . ?
O3 P2 C19 C20 -50.8(3) . . . . ?
C15 P2 C19 C20 55.2(4) . . . . ?
Ni1 P2 C19 C20 -164.7(3) . . . . ?
O3 P2 C19 C22 -175.2(4) . . . . ?
C15 P2 C19 C22 -69.3(4) . . . . ?
Ni1 P2 C19 C22 70.9(4) . . . . ?
O3 P2 C19 C21 65.1(3) . . . . ?
C15 P2 C19 C21 171.0(3) . . . . ?
Ni1 P2 C19 C21 -48.8(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 Cl1 0.76(5) 2.50(5) 3.240(3) 168(5) 4_665

_refine_diff_density_max         0.440
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.066

####################################################################### 
# 
# 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_COMPOUND_6
_database_code_depnum_ccdc_archive 'CCDC 1017480'
_audit_update_record             
;
2015-02-20 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H23 Cl Ni O3 P2'
_chemical_formula_sum            'C30 H23 Cl Ni O3 P2'
_chemical_formula_weight         587.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.125(2)
_cell_length_b                   10.0580(10)
_cell_length_c                   17.403(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.493(2)
_cell_angle_gamma                90
_cell_volume                     2647.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6506
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      25.19

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_F_000             1208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.986
_shelx_estimated_absorpt_T_min   0.694
_shelx_estimated_absorpt_T_max   0.943
__exptl_absorpt_correction_type  empirical
_exptl_absorpt_correction_T_min  0.7816
_exptl_absorpt_correction_T_max  0.9444
_exptl_absorpt_process_details   'SHELXTL V 6.12 (Sheldrick, 2000)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker Smart Apex CCD diffractometer 01-670-01'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            21292
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.339
_diffrn_reflns_theta_max         25.359
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4842
_reflns_number_gt                3372
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 7.34A (Bruker, 2006)'
_computing_structure_solution    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.12 (Sheldrick, 2000)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0337P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4842
_refine_ls_number_parameters     337
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.0861
_refine_ls_wR_factor_gt          0.0808
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_restrained_S_all      0.886
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.72568(2) 0.88741(4) 0.13838(2) 0.03351(13) Uani 1 1 d . . . . .
Cl Cl 0.69126(6) 0.67807(8) 0.16058(5) 0.0531(2) Uani 1 1 d . . . . .
P1 P 0.85024(5) 0.86274(8) 0.07834(5) 0.0400(2) Uani 1 1 d . . . . .
P2 P 0.61274(5) 0.97140(8) 0.19589(5) 0.0348(2) Uani 1 1 d . . . . .
O1 O 0.87674(14) 1.0120(2) 0.04769(14) 0.0533(6) Uani 1 1 d . . . . .
O2 O 0.62156(13) 1.13438(18) 0.18856(12) 0.0420(5) Uani 1 1 d . . . . .
O3 O 0.80555(19) 1.4654(2) 0.07590(17) 0.0767(8) Uani 1 1 d D . . . .
H3A H 0.806(3) 1.541(2) 0.099(2) 0.092 Uiso 1 1 d D U . . .
C1 C 0.74951(19) 1.0679(3) 0.11939(16) 0.0324(7) Uani 1 1 d . . . . .
C2 C 0.8215(2) 1.1095(3) 0.07735(18) 0.0398(8) Uani 1 1 d . . . . .
C3 C 0.8402(2) 1.2417(3) 0.06179(19) 0.0498(9) Uani 1 1 d . . . . .
H3 H 0.8887 1.2657 0.0323 0.060 Uiso 1 1 calc R U . . .
C4 C 0.7844(2) 1.3362(3) 0.09160(19) 0.0482(9) Uani 1 1 d . . . . .
C5 C 0.7102(2) 1.3028(3) 0.13346(17) 0.0385(8) Uani 1 1 d . . . . .
H5 H 0.6718 1.3675 0.1518 0.046 Uiso 1 1 calc R U . . .
C6 C 0.69579(19) 1.1702(3) 0.14657(16) 0.0329(7) Uani 1 1 d . . . . .
C7 C 0.8572(2) 0.7687(3) -0.00904(18) 0.0403(8) Uani 1 1 d . . . . .
C8 C 0.9192(2) 0.6711(4) -0.0220(2) 0.0610(10) Uani 1 1 d . . . . .
H8 H 0.9601 0.6500 0.0163 0.073 Uiso 1 1 calc R U . . .
C9 C 0.9211(3) 0.6042(4) -0.0914(2) 0.0788(13) Uani 1 1 d . . . . .
H9 H 0.9631 0.5383 -0.0995 0.095 Uiso 1 1 calc R U . . .
C10 C 0.8621(3) 0.6345(4) -0.1472(2) 0.0713(12) Uani 1 1 d . . . . .
H10 H 0.8642 0.5905 -0.1942 0.086 Uiso 1 1 calc R U . . .
C11 C 0.8003(3) 0.7280(5) -0.1352(2) 0.0824(13) Uani 1 1 d . . . . .
H11 H 0.7597 0.7482 -0.1739 0.099 Uiso 1 1 calc R U . . .
C12 C 0.7967(3) 0.7937(4) -0.0665(2) 0.0717(12) Uani 1 1 d . . . . .
H12 H 0.7525 0.8564 -0.0586 0.086 Uiso 1 1 calc R U . . .
C13 C 0.9457(2) 0.8150(3) 0.13470(19) 0.0466(8) Uani 1 1 d . . . . .
C14 C 0.9405(3) 0.7120(4) 0.1859(2) 0.0682(11) Uani 1 1 d . . . . .
H14 H 0.8875 0.6663 0.1911 0.082 Uiso 1 1 calc R U . . .
C15 C 1.0131(3) 0.6746(5) 0.2303(2) 0.0894(15) Uani 1 1 d . . . . .
H15 H 1.0088 0.6032 0.2640 0.107 Uiso 1 1 calc R U . . .
C16 C 1.0896(4) 0.7416(7) 0.2244(3) 0.1049(19) Uani 1 1 d . . . . .
H16 H 1.1380 0.7184 0.2549 0.126 Uiso 1 1 calc R U . . .
C17 C 1.0957(3) 0.8435(7) 0.1736(3) 0.126(2) Uani 1 1 d . . . . .
H17 H 1.1490 0.8889 0.1692 0.151 Uiso 1 1 calc R U . . .
C18 C 1.0246(3) 0.8816(5) 0.1282(3) 0.0897(14) Uani 1 1 d . . . . .
H18 H 1.0301 0.9515 0.0936 0.108 Uiso 1 1 calc R U . . .
C19 C 0.5044(2) 0.9382(3) 0.15707(17) 0.0358(7) Uani 1 1 d . . . . .
C20 C 0.4959(2) 0.8851(3) 0.08452(19) 0.0518(9) Uani 1 1 d . . . . .
H20 H 0.5462 0.8621 0.0572 0.062 Uiso 1 1 calc R U . . .
C21 C 0.4128(3) 0.8655(4) 0.0518(2) 0.0632(11) Uani 1 1 d . . . . .
H21 H 0.4075 0.8307 0.0025 0.076 Uiso 1 1 calc R U . . .
C22 C 0.3400(2) 0.8971(4) 0.0919(2) 0.0617(10) Uani 1 1 d . . . . .
H22 H 0.2844 0.8832 0.0701 0.074 Uiso 1 1 calc R U . . .
C23 C 0.3470(2) 0.9495(4) 0.1641(2) 0.0617(10) Uani 1 1 d . . . . .
H23 H 0.2963 0.9709 0.1913 0.074 Uiso 1 1 calc R U . . .
C24 C 0.4286(2) 0.9707(3) 0.19669(19) 0.0475(9) Uani 1 1 d . . . . .
H24 H 0.4330 1.0070 0.2457 0.057 Uiso 1 1 calc R U . . .
C25 C 0.6022(2) 0.9487(3) 0.29767(17) 0.0398(8) Uani 1 1 d . . . . .
C26 C 0.5644(2) 0.8333(4) 0.3263(2) 0.0576(10) Uani 1 1 d . . . . .
H26 H 0.5416 0.7705 0.2922 0.069 Uiso 1 1 calc R U . . .
C27 C 0.5600(3) 0.8107(4) 0.4029(2) 0.0735(12) Uani 1 1 d . . . . .
H27 H 0.5337 0.7332 0.4209 0.088 Uiso 1 1 calc R U . . .
C28 C 0.5939(3) 0.9002(5) 0.4536(2) 0.0877(15) Uani 1 1 d . . . . .
H28 H 0.5910 0.8838 0.5061 0.105 Uiso 1 1 calc R U . . .
C29 C 0.6321(4) 1.0145(5) 0.4274(2) 0.0955(16) Uani 1 1 d . . . . .
H29 H 0.6554 1.0755 0.4623 0.115 Uiso 1 1 calc R U . . .
C30 C 0.6365(3) 1.0399(4) 0.3493(2) 0.0713(12) Uani 1 1 d . . . . .
H30 H 0.6623 1.1180 0.3317 0.086 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.880(3) . ?
Ni1 P2 2.1593(9) . ?
Ni1 P1 2.1764(9) . ?
Ni1 Cl 2.2038(9) . ?
P1 O1 1.644(2) . ?
P1 C7 1.795(3) . ?
P1 C13 1.804(3) . ?
P2 O2 1.650(2) . ?
P2 C25 1.794(3) . ?
P2 C19 1.799(3) . ?
O1 C2 1.390(3) . ?
O2 C6 1.392(3) . ?
O3 C4 1.367(4) . ?
O3 H3A 0.863(10) . ?
C1 C2 1.383(4) . ?
C1 C6 1.396(4) . ?
C2 C3 1.387(4) . ?
C3 C4 1.375(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(4) . ?
C5 C6 1.371(4) . ?
C5 H5 0.9300 . ?
C7 C12 1.373(4) . ?
C7 C8 1.377(4) . ?
C8 C9 1.382(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.349(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.344(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.367(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.370(5) . ?
C13 C18 1.373(5) . ?
C14 C15 1.389(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.344(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.358(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.383(6) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.376(4) . ?
C19 C24 1.382(4) . ?
C20 C21 1.390(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.346(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.367(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.370(4) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C30 1.381(4) . ?
C25 C26 1.388(4) . ?
C26 C27 1.356(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.357(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.367(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.386(5) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?

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
C1 Ni1 P2 81.80(9) . . ?
C1 Ni1 P1 81.82(9) . . ?
P2 Ni1 P1 163.46(3) . . ?
C1 Ni1 Cl 177.38(9) . . ?
P2 Ni1 Cl 95.94(3) . . ?
P1 Ni1 Cl 100.49(3) . . ?
O1 P1 C7 100.98(13) . . ?
O1 P1 C13 102.90(15) . . ?
C7 P1 C13 105.54(15) . . ?
O1 P1 Ni1 105.43(8) . . ?
C7 P1 Ni1 121.61(10) . . ?
C13 P1 Ni1 117.48(11) . . ?
O2 P2 C25 102.16(13) . . ?
O2 P2 C19 103.25(12) . . ?
C25 P2 C19 105.01(14) . . ?
O2 P2 Ni1 106.74(8) . . ?
C25 P2 Ni1 119.00(11) . . ?
C19 P2 Ni1 118.38(11) . . ?
C2 O1 P1 112.02(18) . . ?
C6 O2 P2 111.33(17) . . ?
C4 O3 H3A 139(3) . . ?
C2 C1 C6 114.8(3) . . ?
C2 C1 Ni1 122.6(2) . . ?
C6 C1 Ni1 122.6(2) . . ?
C1 C2 C3 123.8(3) . . ?
C1 C2 O1 117.5(3) . . ?
C3 C2 O1 118.7(3) . . ?
C4 C3 C2 117.5(3) . . ?
C4 C3 H3 121.2 . . ?
C2 C3 H3 121.2 . . ?
O3 C4 C3 115.8(3) . . ?
O3 C4 C5 121.9(3) . . ?
C3 C4 C5 122.3(3) . . ?
C6 C5 C4 117.0(3) . . ?
C6 C5 H5 121.5 . . ?
C4 C5 H5 121.5 . . ?
C5 C6 O2 118.0(3) . . ?
C5 C6 C1 124.6(3) . . ?
O2 C6 C1 117.5(3) . . ?
C12 C7 C8 117.5(3) . . ?
C12 C7 P1 118.5(3) . . ?
C8 C7 P1 124.0(3) . . ?
C7 C8 C9 120.6(4) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C10 C9 C8 120.1(4) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 C9 120.1(4) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.6(4) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C7 121.1(4) . . ?
C11 C12 H12 119.5 . . ?
C7 C12 H12 119.5 . . ?
C14 C13 C18 118.5(4) . . ?
C14 C13 P1 120.4(3) . . ?
C18 C13 P1 121.1(3) . . ?
C13 C14 C15 121.2(4) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C16 C15 C14 119.9(5) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 119.5(5) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C16 C17 C18 121.6(5) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
C13 C18 C17 119.3(5) . . ?
C13 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 C24 118.6(3) . . ?
C20 C19 P2 119.6(2) . . ?
C24 C19 P2 121.7(2) . . ?
C19 C20 C21 120.5(3) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C22 C21 C20 119.7(3) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 120.7(3) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C24 120.2(3) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C19 120.3(3) . . ?
C23 C24 H24 119.8 . . ?
C19 C24 H24 119.8 . . ?
C30 C25 C26 118.4(3) . . ?
C30 C25 P2 121.4(3) . . ?
C26 C25 P2 120.0(3) . . ?
C27 C26 C25 121.1(4) . . ?
C27 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C26 C27 C28 120.4(4) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C27 C28 C29 120.0(4) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C30 120.4(4) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C25 C30 C29 119.7(4) . . ?
C25 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?

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
C7 P1 O1 C2 136.0(2) . . . . ?
C13 P1 O1 C2 -115.1(2) . . . . ?
Ni1 P1 O1 C2 8.6(2) . . . . ?
C25 P2 O2 C6 127.4(2) . . . . ?
C19 P2 O2 C6 -123.8(2) . . . . ?
Ni1 P2 O2 C6 1.8(2) . . . . ?
P2 Ni1 C1 C2 -178.5(3) . . . . ?
P1 Ni1 C1 C2 3.8(2) . . . . ?
P2 Ni1 C1 C6 1.4(2) . . . . ?
P1 Ni1 C1 C6 -176.3(3) . . . . ?
C6 C1 C2 C3 -0.6(5) . . . . ?
Ni1 C1 C2 C3 179.3(3) . . . . ?
C6 C1 C2 O1 -179.0(3) . . . . ?
Ni1 C1 C2 O1 0.9(4) . . . . ?
P1 O1 C2 C1 -6.8(4) . . . . ?
P1 O1 C2 C3 174.7(2) . . . . ?
C1 C2 C3 C4 1.4(5) . . . . ?
O1 C2 C3 C4 179.8(3) . . . . ?
C2 C3 C4 O3 179.2(3) . . . . ?
C2 C3 C4 C5 -2.2(5) . . . . ?
O3 C4 C5 C6 -179.3(3) . . . . ?
C3 C4 C5 C6 2.2(5) . . . . ?
C4 C5 C6 O2 180.0(3) . . . . ?
C4 C5 C6 C1 -1.4(5) . . . . ?
P2 O2 C6 C5 177.8(2) . . . . ?
P2 O2 C6 C1 -0.9(3) . . . . ?
C2 C1 C6 C5 0.6(4) . . . . ?
Ni1 C1 C6 C5 -179.3(2) . . . . ?
C2 C1 C6 O2 179.3(3) . . . . ?
Ni1 C1 C6 O2 -0.7(4) . . . . ?
O1 P1 C7 C12 -67.4(3) . . . . ?
C13 P1 C7 C12 -174.2(3) . . . . ?
Ni1 P1 C7 C12 48.6(3) . . . . ?
O1 P1 C7 C8 113.4(3) . . . . ?
C13 P1 C7 C8 6.5(3) . . . . ?
Ni1 P1 C7 C8 -130.7(3) . . . . ?
C12 C7 C8 C9 1.7(5) . . . . ?
P1 C7 C8 C9 -179.0(3) . . . . ?
C7 C8 C9 C10 0.2(6) . . . . ?
C8 C9 C10 C11 -1.2(7) . . . . ?
C9 C10 C11 C12 0.2(7) . . . . ?
C10 C11 C12 C7 1.8(7) . . . . ?
C8 C7 C12 C11 -2.7(6) . . . . ?
P1 C7 C12 C11 178.0(3) . . . . ?
O1 P1 C13 C14 163.1(3) . . . . ?
C7 P1 C13 C14 -91.5(3) . . . . ?
Ni1 P1 C13 C14 47.8(3) . . . . ?
O1 P1 C13 C18 -16.1(3) . . . . ?
C7 P1 C13 C18 89.4(3) . . . . ?
Ni1 P1 C13 C18 -131.3(3) . . . . ?
C18 C13 C14 C15 -0.3(6) . . . . ?
P1 C13 C14 C15 -179.5(3) . . . . ?
C13 C14 C15 C16 1.3(7) . . . . ?
C14 C15 C16 C17 -1.6(8) . . . . ?
C15 C16 C17 C18 0.9(9) . . . . ?
C14 C13 C18 C17 -0.4(6) . . . . ?
P1 C13 C18 C17 178.7(4) . . . . ?
C16 C17 C18 C13 0.2(8) . . . . ?
O2 P2 C19 C20 104.3(3) . . . . ?
C25 P2 C19 C20 -149.0(3) . . . . ?
Ni1 P2 C19 C20 -13.3(3) . . . . ?
O2 P2 C19 C24 -72.5(3) . . . . ?
C25 P2 C19 C24 34.2(3) . . . . ?
Ni1 P2 C19 C24 169.8(2) . . . . ?
C24 C19 C20 C21 0.5(5) . . . . ?
P2 C19 C20 C21 -176.5(3) . . . . ?
C19 C20 C21 C22 -0.9(6) . . . . ?
C20 C21 C22 C23 0.6(6) . . . . ?
C21 C22 C23 C24 0.1(6) . . . . ?
C22 C23 C24 C19 -0.5(5) . . . . ?
C20 C19 C24 C23 0.3(5) . . . . ?
P2 C19 C24 C23 177.1(3) . . . . ?
O2 P2 C25 C30 -26.0(3) . . . . ?
C19 P2 C25 C30 -133.5(3) . . . . ?
Ni1 P2 C25 C30 91.1(3) . . . . ?
O2 P2 C25 C26 158.4(3) . . . . ?
C19 P2 C25 C26 50.9(3) . . . . ?
Ni1 P2 C25 C26 -84.5(3) . . . . ?
C30 C25 C26 C27 0.7(6) . . . . ?
P2 C25 C26 C27 176.4(3) . . . . ?
C25 C26 C27 C28 -0.8(6) . . . . ?
C26 C27 C28 C29 0.4(7) . . . . ?
C27 C28 C29 C30 0.2(8) . . . . ?
C26 C25 C30 C29 -0.1(6) . . . . ?
P2 C25 C30 C29 -175.7(3) . . . . ?
C28 C29 C30 C25 -0.3(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3A Cl 0.863(10) 2.47(3) 3.127(3) 134(3) 1_565

_refine_diff_density_max         0.470
_refine_diff_density_min         -0.223
_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_COMPOUND_7
_database_code_depnum_ccdc_archive 'CCDC 1017481'
_audit_update_record             
;
2015-02-20 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H43 Cl Ni O4 P2'
_chemical_formula_sum            'C29 H43 Cl Ni O4 P2'
_chemical_formula_weight         611.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.0299(15)
_cell_length_b                   27.236(5)
_cell_length_c                   15.128(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.306(4)
_cell_angle_gamma                90
_cell_volume                     3244.2(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4374
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      24.05
_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_F_000             1296
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.809
_shelx_estimated_absorpt_T_min   0.782
_shelx_estimated_absorpt_T_max   0.961
_exptl_absorpt_correction_type   Analytical
_exptl_absorpt_correction_T_min  0.8091
_exptl_absorpt_correction_T_max  0.9554
_exptl_absorpt_process_details   'SHELXTL V 6.12 (Sheldrick, 2008)'
_exptl_absorpt_special_details   
;
The compound display disorder affecting the phenyl ring of the 
benzoate moiety included, which was modeled with SIMU and DELU 
restraints on anisotropic displacement parameters and SAME 
geometrical restraints
;
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            26672
_diffrn_reflns_av_unetI/netI     0.1110
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.030
_diffrn_reflns_theta_max         25.328
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5920
_reflns_number_gt                3125
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 7.34A (Bruker, 2006)'
_computing_structure_solution    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.12 (Sheldrick, 2000)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0177P)²] 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         5920
_refine_ls_number_parameters     392
_refine_ls_number_restraints     212
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.0817
_refine_ls_wR_factor_gt          0.0691
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_restrained_S_all      0.819
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.48328(6) 0.13042(2) 0.67957(3) 0.04660(16) Uani 1 1 d . . . . .
Cl Cl 0.60526(14) 0.19750(4) 0.64183(8) 0.0807(4) Uani 1 1 d . . . . .
P1 P 0.32960(13) 0.11380(4) 0.54714(7) 0.0461(3) Uani 1 1 d . . . . .
P2 P 0.60631(13) 0.12722(4) 0.82182(7) 0.0537(3) Uani 1 1 d . . . . .
O1 O 0.2351(3) 0.06082(8) 0.56011(16) 0.0550(7) Uani 1 1 d . . . . .
O2 O 0.5053(3) 0.08340(10) 0.86534(17) 0.0627(8) Uani 1 1 d . . . . .
O3 O 0.1080(3) -0.04699(10) 0.78521(19) 0.0709(9) Uani 1 1 d . . . . .
O4 O 0.3136(4) -0.10121(11) 0.7809(2) 0.0987(12) Uani 1 1 d . . . . .
C1 C 0.2634(5) 0.04619(14) 0.6494(3) 0.0470(10) Uani 1 1 d . . . . .
C2 C 0.3741(5) 0.07422(13) 0.7117(3) 0.0448(10) Uani 1 1 d . . . . .
C3 C 0.3960(5) 0.05717(15) 0.8006(3) 0.0509(11) Uani 1 1 d . . . . .
C4 C 0.3147(5) 0.01676(15) 0.8261(3) 0.0597(12) Uani 1 1 d . . . . .
H4 H 0.3326 0.0067 0.8860 0.072 Uiso 1 1 calc R U . . .
C5 C 0.2062(5) -0.00829(14) 0.7602(3) 0.0556(11) Uani 1 1 d . . . . .
C6 C 0.1772(5) 0.00533(13) 0.6711(3) 0.0552(11) Uani 1 1 d . . . . .
H6 H 0.1030 -0.0121 0.6273 0.066 Uiso 1 1 calc R U . . .
C7 C 0.4447(5) 0.09711(15) 0.4563(3) 0.0544(11) Uani 1 1 d . . . . .
C8 C 0.5013(6) 0.14314(15) 0.4111(3) 0.0899(15) Uani 1 1 d . . . . .
H8A H 0.5771 0.1338 0.3723 0.135 Uiso 1 1 calc R U . . .
H8B H 0.5584 0.1652 0.4566 0.135 Uiso 1 1 calc R U . . .
H8C H 0.4035 0.1592 0.3763 0.135 Uiso 1 1 calc R U . . .
C9 C 0.3431(5) 0.06306(15) 0.3850(3) 0.0775(14) Uani 1 1 d . . . . .
H9A H 0.2501 0.0809 0.3498 0.116 Uiso 1 1 calc R U . . .
H9B H 0.2999 0.0359 0.4142 0.116 Uiso 1 1 calc R U . . .
H9C H 0.4155 0.0510 0.3464 0.116 Uiso 1 1 calc R U . . .
C10 C 0.6033(5) 0.06977(15) 0.5062(3) 0.0816(14) Uani 1 1 d . . . . .
H10A H 0.6682 0.0582 0.4634 0.122 Uiso 1 1 calc R U . . .
H10B H 0.5691 0.0424 0.5384 0.122 Uiso 1 1 calc R U . . .
H10C H 0.6716 0.0917 0.5481 0.122 Uiso 1 1 calc R U . . .
C11 C 0.1419(5) 0.15317(14) 0.5098(3) 0.0538(11) Uani 1 1 d . . . . .
C12 C 0.0545(5) 0.15625(14) 0.5913(3) 0.0734(13) Uani 1 1 d . . . . .
H12A H -0.0419 0.1777 0.5774 0.110 Uiso 1 1 calc R U . . .
H12B H 0.1331 0.1689 0.6423 0.110 Uiso 1 1 calc R U . . .
H12C H 0.0177 0.1241 0.6051 0.110 Uiso 1 1 calc R U . . .
C13 C 0.1931(5) 0.20519(15) 0.4865(3) 0.0885(15) Uani 1 1 d . . . . .
H13A H 0.2330 0.2045 0.4307 0.133 Uiso 1 1 calc R U . . .
H13B H 0.2818 0.2171 0.5337 0.133 Uiso 1 1 calc R U . . .
H13C H 0.0965 0.2266 0.4806 0.133 Uiso 1 1 calc R U . . .
C14 C 0.0151(5) 0.13181(16) 0.4302(3) 0.0881(15) Uani 1 1 d . . . . .
H14A H -0.0865 0.1513 0.4196 0.132 Uiso 1 1 calc R U . . .
H14B H -0.0122 0.0987 0.4437 0.132 Uiso 1 1 calc R U . . .
H14C H 0.0645 0.1321 0.3773 0.132 Uiso 1 1 calc R U . . .
C15 C 0.8239(5) 0.10184(19) 0.8437(3) 0.0789(14) Uani 1 1 d . . . . .
C16 C 0.8125(6) 0.0548(2) 0.7872(4) 0.158(3) Uani 1 1 d . . . . .
H16A H 0.7813 0.0630 0.7244 0.237 Uiso 1 1 calc R U . . .
H16B H 0.7284 0.0334 0.8034 0.237 Uiso 1 1 calc R U . . .
H16C H 0.9208 0.0386 0.7984 0.237 Uiso 1 1 calc R U . . .
C17 C 0.8927(6) 0.0887(2) 0.9420(3) 0.128(2) Uani 1 1 d . . . . .
H17A H 1.0011 0.0729 0.9471 0.192 Uiso 1 1 calc R U . . .
H17B H 0.8150 0.0668 0.9629 0.192 Uiso 1 1 calc R U . . .
H17C H 0.9053 0.1180 0.9778 0.192 Uiso 1 1 calc R U . . .
C18 C 0.9450(6) 0.1367(2) 0.8112(4) 0.146(3) Uani 1 1 d . . . . .
H18A H 0.9780 0.1620 0.8552 0.219 Uiso 1 1 calc R U . . .
H18B H 0.8902 0.1512 0.7551 0.219 Uiso 1 1 calc R U . . .
H18C H 1.0439 0.1190 0.8024 0.219 Uiso 1 1 calc R U . . .
C19 C 0.5739(6) 0.17933(17) 0.8945(3) 0.0736(14) Uani 1 1 d . . . . .
C20 C 0.5881(7) 0.16537(19) 0.9933(3) 0.133(2) Uani 1 1 d . . . . .
H20A H 0.6988 0.1520 1.0162 0.200 Uiso 1 1 calc R U . . .
H20B H 0.5033 0.1413 0.9986 0.200 Uiso 1 1 calc R U . . .
H20C H 0.5712 0.1940 1.0275 0.200 Uiso 1 1 calc R U . . .
C21 C 0.6978(7) 0.22067(18) 0.8883(4) 0.154(3) Uani 1 1 d . . . . .
H21A H 0.6939 0.2287 0.8261 0.230 Uiso 1 1 calc R U . . .
H21B H 0.8106 0.2105 0.9155 0.230 Uiso 1 1 calc R U . . .
H21C H 0.6672 0.2490 0.9193 0.230 Uiso 1 1 calc R U . . .
C22 C 0.3958(6) 0.19635(19) 0.8580(4) 0.140(2) Uani 1 1 d . . . . .
H22A H 0.3722 0.2250 0.8904 0.210 Uiso 1 1 calc R U . . .
H22B H 0.3174 0.1707 0.8652 0.210 Uiso 1 1 calc R U . . .
H22C H 0.3841 0.2042 0.7952 0.210 Uiso 1 1 calc R U . . .
C23 C 0.1734(7) -0.09245(17) 0.7917(3) 0.0621(13) Uani 1 1 d . . . . .
C24 C 0.0486(6) -0.12936(15) 0.8092(3) 0.0664(11) Uani 1 1 d D U . . .
C25 C 0.1061(16) -0.1773(2) 0.8045(15) 0.0826(19) Uani 0.59(2) 1 d D U P A 1
H25 H 0.2149 -0.1834 0.7947 0.099 Uiso 0.59(2) 1 calc R U P A 1
C26 C -0.002(2) -0.2161(2) 0.8147(10) 0.092(2) Uani 0.59(2) 1 d D U P A 1
H26 H 0.0349 -0.2484 0.8119 0.111 Uiso 0.59(2) 1 calc R U P A 1
C27 C -0.1628(17) -0.2063(5) 0.8291(10) 0.091(2) Uani 0.59(2) 1 d D U P A 1
H27 H -0.2357 -0.2323 0.8338 0.109 Uiso 0.59(2) 1 calc R U P A 1
C28 C -0.2189(11) -0.1587(5) 0.8367(9) 0.081(2) Uani 0.59(2) 1 d D U P A 1
H28 H -0.3267 -0.1526 0.8480 0.097 Uiso 0.59(2) 1 calc R U P A 1
C29 C -0.1092(14) -0.1201(3) 0.8269(17) 0.0698(18) Uani 0.59(2) 1 d D U P A 1
H29 H -0.1437 -0.0879 0.8325 0.084 Uiso 0.59(2) 1 calc R U P A 1
C25A C 0.064(2) -0.1800(3) 0.803(2) 0.082(2) Uani 0.41(2) 1 d D U P A 2
H25A H 0.1635 -0.1936 0.7916 0.099 Uiso 0.41(2) 1 calc R U P A 2
C26A C -0.070(3) -0.2103(4) 0.8142(16) 0.089(2) Uani 0.41(2) 1 d D U P A 2
H26A H -0.0629 -0.2441 0.8073 0.106 Uiso 0.41(2) 1 calc R U P A 2
C27A C -0.215(2) -0.1896(7) 0.8355(14) 0.089(2) Uani 0.41(2) 1 d D U P A 2
H27A H -0.3010 -0.2100 0.8469 0.106 Uiso 0.41(2) 1 calc R U P A 2
C28A C -0.2333(13) -0.1394(7) 0.8402(13) 0.080(2) Uani 0.41(2) 1 d D U P A 2
H28A H -0.3326 -0.1258 0.8525 0.096 Uiso 0.41(2) 1 calc R U P A 2
C29A C -0.100(2) -0.1093(4) 0.826(3) 0.072(2) Uani 0.41(2) 1 d D U P A 2
H29A H -0.1113 -0.0753 0.8282 0.087 Uiso 0.41(2) 1 calc R U P 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
Ni C2 1.875(4) . ?
Ni P1 2.1845(12) . ?
Ni P2 2.1865(12) . ?
Ni Cl 2.2005(12) . ?
P1 O1 1.660(2) . ?
P1 C11 1.846(4) . ?
P1 C7 1.857(4) . ?
P2 O2 1.650(3) . ?
P2 C19 1.844(4) . ?
P2 C15 1.847(4) . ?
O1 C1 1.384(4) . ?
O2 C3 1.380(4) . ?
O3 C23 1.341(5) . ?
O3 C5 1.412(4) . ?
O4 C23 1.192(5) . ?
C1 C6 1.383(5) . ?
C1 C2 1.390(5) . ?
C2 C3 1.401(5) . ?
C3 C4 1.373(5) . ?
C4 C5 1.371(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.372(5) . ?
C6 H6 0.9300 . ?
C7 C9 1.531(5) . ?
C7 C8 1.538(5) . ?
C7 C10 1.540(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C14 1.532(5) . ?
C11 C12 1.535(5) . ?
C11 C13 1.536(5) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C18 1.509(6) . ?
C15 C17 1.523(5) . ?
C15 C16 1.533(6) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C22 1.502(5) . ?
C19 C21 1.517(6) . ?
C19 C20 1.525(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.480(5) . ?
C24 C29 1.369(6) . ?
C24 C29A 1.381(7) . ?
C24 C25 1.392(6) . ?
C24 C25A 1.388(6) . ?
C25 C26 1.393(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.381(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.384(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.397(6) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C25A C26A 1.394(7) . ?
C25A H25A 0.9300 . ?
C26A C27A 1.382(7) . ?
C26A H26A 0.9300 . ?
C27A C28A 1.381(7) . ?
C27A H27A 0.9300 . ?
C28A C29A 1.398(7) . ?
C28A H28A 0.9300 . ?
C29A H29A 0.9300 . ?

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
C2 Ni P1 81.92(13) . . ?
C2 Ni P2 81.75(13) . . ?
P1 Ni P2 163.61(5) . . ?
C2 Ni Cl 178.49(11) . . ?
P1 Ni Cl 97.71(4) . . ?
P2 Ni Cl 98.64(5) . . ?
O1 P1 C11 100.16(16) . . ?
O1 P1 C7 100.37(16) . . ?
C11 P1 C7 114.27(18) . . ?
O1 P1 Ni 105.12(10) . . ?
C11 P1 Ni 116.14(13) . . ?
C7 P1 Ni 117.13(14) . . ?
O2 P2 C19 100.43(19) . . ?
O2 P2 C15 100.3(2) . . ?
C19 P2 C15 114.8(2) . . ?
O2 P2 Ni 105.00(10) . . ?
C19 P2 Ni 117.81(16) . . ?
C15 P2 Ni 114.86(15) . . ?
C1 O1 P1 112.0(2) . . ?
C3 O2 P2 112.7(2) . . ?
C23 O3 C5 118.5(3) . . ?
C6 C1 O1 118.0(4) . . ?
C6 C1 C2 124.4(4) . . ?
O1 C1 C2 117.6(3) . . ?
C1 C2 C3 114.3(4) . . ?
C1 C2 Ni 122.9(3) . . ?
C3 C2 Ni 122.8(3) . . ?
C4 C3 O2 119.1(4) . . ?
C4 C3 C2 123.9(4) . . ?
O2 C3 C2 116.9(4) . . ?
C5 C4 C3 117.6(4) . . ?
C5 C4 H4 121.2 . . ?
C3 C4 H4 121.2 . . ?
C4 C5 C6 122.8(4) . . ?
C4 C5 O3 119.0(4) . . ?
C6 C5 O3 118.0(4) . . ?
C5 C6 C1 117.0(4) . . ?
C5 C6 H6 121.5 . . ?
C1 C6 H6 121.5 . . ?
C9 C7 C8 110.1(3) . . ?
C9 C7 C10 109.2(3) . . ?
C8 C7 C10 108.9(3) . . ?
C9 C7 P1 113.3(3) . . ?
C8 C7 P1 111.2(3) . . ?
C10 C7 P1 103.8(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C11 C12 108.3(3) . . ?
C14 C11 C13 109.7(3) . . ?
C12 C11 C13 108.6(3) . . ?
C14 C11 P1 113.4(3) . . ?
C12 C11 P1 105.1(3) . . ?
C13 C11 P1 111.5(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18 C15 C17 109.4(4) . . ?
C18 C15 C16 108.3(4) . . ?
C17 C15 C16 108.5(4) . . ?
C18 C15 P2 110.7(3) . . ?
C17 C15 P2 114.4(3) . . ?
C16 C15 P2 105.2(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C19 C21 109.7(5) . . ?
C22 C19 C20 108.6(4) . . ?
C21 C19 C20 108.8(4) . . ?
C22 C19 P2 104.7(3) . . ?
C21 C19 P2 111.3(3) . . ?
C20 C19 P2 113.6(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O4 C23 O3 122.8(4) . . ?
O4 C23 C24 125.4(5) . . ?
O3 C23 C24 111.8(4) . . ?
C29 C24 C25 120.7(5) . . ?
C29A C24 C25A 119.7(6) . . ?
C29 C24 C23 126.6(6) . . ?
C29A C24 C23 113.8(7) . . ?
C25 C24 C23 112.7(6) . . ?
C25A C24 C23 126.3(7) . . ?
C26 C25 C24 119.2(5) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C27 C26 C25 119.4(6) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
C26 C27 C28 121.7(7) . . ?
C26 C27 H27 119.1 . . ?
C28 C27 H27 119.1 . . ?
C27 C28 C29 118.2(6) . . ?
C27 C28 H28 120.9 . . ?
C29 C28 H28 120.9 . . ?
C24 C29 C28 120.6(5) . . ?
C24 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C26A C25A C24 120.0(6) . . ?
C26A C25A H25A 120.0 . . ?
C24 C25A H25A 120.0 . . ?
C27A C26A C25A 119.4(7) . . ?
C27A C26A H26A 120.3 . . ?
C25A C26A H26A 120.3 . . ?
C26A C27A C28A 121.3(8) . . ?
C26A C27A H27A 119.3 . . ?
C28A C27A H27A 119.3 . . ?
C27A C28A C29A 118.7(7) . . ?
C27A C28A H28A 120.7 . . ?
C29A C28A H28A 120.7 . . ?
C24 C29A C28A 120.7(6) . . ?
C24 C29A H29A 119.6 . . ?
C28A C29A H29A 119.6 . . ?

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
C11 P1 O1 C1 -113.7(3) . . . . ?
C7 P1 O1 C1 129.1(3) . . . . ?
Ni P1 O1 C1 7.1(2) . . . . ?
C19 P2 O2 C3 132.0(3) . . . . ?
C15 P2 O2 C3 -110.1(3) . . . . ?
Ni P2 O2 C3 9.3(3) . . . . ?
P1 O1 C1 C6 173.3(3) . . . . ?
P1 O1 C1 C2 -5.5(4) . . . . ?
C6 C1 C2 C3 1.3(5) . . . . ?
O1 C1 C2 C3 179.9(3) . . . . ?
C6 C1 C2 Ni -178.2(3) . . . . ?
O1 C1 C2 Ni 0.5(5) . . . . ?
P1 Ni C2 C1 3.3(3) . . . . ?
P2 Ni C2 C1 -175.1(3) . . . . ?
P1 Ni C2 C3 -176.1(3) . . . . ?
P2 Ni C2 C3 5.5(3) . . . . ?
P2 O2 C3 C4 174.2(3) . . . . ?
P2 O2 C3 C2 -6.4(4) . . . . ?
C1 C2 C3 C4 -0.9(5) . . . . ?
Ni C2 C3 C4 178.5(3) . . . . ?
C1 C2 C3 O2 179.7(3) . . . . ?
Ni C2 C3 O2 -0.9(5) . . . . ?
O2 C3 C4 C5 179.6(3) . . . . ?
C2 C3 C4 C5 0.2(6) . . . . ?
C3 C4 C5 C6 0.2(6) . . . . ?
C3 C4 C5 O3 -173.8(3) . . . . ?
C23 O3 C5 C4 -89.3(5) . . . . ?
C23 O3 C5 C6 96.4(4) . . . . ?
C4 C5 C6 C1 0.1(6) . . . . ?
O3 C5 C6 C1 174.2(3) . . . . ?
O1 C1 C6 C5 -179.5(3) . . . . ?
C2 C1 C6 C5 -0.9(6) . . . . ?
O1 P1 C7 C9 38.4(3) . . . . ?
C11 P1 C7 C9 -67.8(3) . . . . ?
Ni P1 C7 C9 151.5(2) . . . . ?
O1 P1 C7 C8 163.2(3) . . . . ?
C11 P1 C7 C8 56.9(3) . . . . ?
Ni P1 C7 C8 -83.8(3) . . . . ?
O1 P1 C7 C10 -79.9(3) . . . . ?
C11 P1 C7 C10 173.9(3) . . . . ?
Ni P1 C7 C10 33.2(3) . . . . ?
O1 P1 C11 C14 -52.0(3) . . . . ?
C7 P1 C11 C14 54.3(3) . . . . ?
Ni P1 C11 C14 -164.6(2) . . . . ?
O1 P1 C11 C12 66.1(3) . . . . ?
C7 P1 C11 C12 172.5(2) . . . . ?
Ni P1 C11 C12 -46.4(3) . . . . ?
O1 P1 C11 C13 -176.4(3) . . . . ?
C7 P1 C11 C13 -70.0(3) . . . . ?
Ni P1 C11 C13 71.1(3) . . . . ?
O2 P2 C15 C18 -178.7(3) . . . . ?
C19 P2 C15 C18 -72.0(4) . . . . ?
Ni P2 C15 C18 69.3(4) . . . . ?
O2 P2 C15 C17 -54.5(4) . . . . ?
C19 P2 C15 C17 52.2(5) . . . . ?
Ni P2 C15 C17 -166.5(3) . . . . ?
O2 P2 C15 C16 64.5(4) . . . . ?
C19 P2 C15 C16 171.2(4) . . . . ?
Ni P2 C15 C16 -47.5(4) . . . . ?
O2 P2 C19 C22 -78.9(4) . . . . ?
C15 P2 C19 C22 174.5(4) . . . . ?
Ni P2 C19 C22 34.4(4) . . . . ?
O2 P2 C19 C21 162.7(4) . . . . ?
C15 P2 C19 C21 56.1(4) . . . . ?
Ni P2 C19 C21 -84.1(4) . . . . ?
O2 P2 C19 C20 39.5(4) . . . . ?
C15 P2 C19 C20 -67.1(4) . . . . ?
Ni P2 C19 C20 152.7(3) . . . . ?
C5 O3 C23 O4 3.2(7) . . . . ?
C5 O3 C23 C24 -174.1(4) . . . . ?
O4 C23 C24 C29 176.0(14) . . . . ?
O3 C23 C24 C29 -6.7(14) . . . . ?
O4 C23 C24 C29A 175.2(18) . . . . ?
O3 C23 C24 C29A -7.5(19) . . . . ?
O4 C23 C24 C25 -5.1(12) . . . . ?
O3 C23 C24 C25 172.1(11) . . . . ?
O4 C23 C24 C25A -10.0(19) . . . . ?
O3 C23 C24 C25A 167.3(18) . . . . ?
C29 C24 C25 C26 2(2) . . . . ?
C23 C24 C25 C26 -176.6(12) . . . . ?
C24 C25 C26 C27 0(2) . . . . ?
C25 C26 C27 C28 -2.2(17) . . . . ?
C26 C27 C28 C29 1.8(19) . . . . ?
C25 C24 C29 C28 -3(3) . . . . ?
C23 C24 C29 C28 175.9(11) . . . . ?
C27 C28 C29 C24 1(2) . . . . ?
C29A C24 C25A C26A 0(4) . . . . ?
C23 C24 C25A C26A -174.6(16) . . . . ?
C24 C25A C26A C27A -3(4) . . . . ?
C25A C26A C27A C28A 4(3) . . . . ?
C26A C27A C28A C29A -2(3) . . . . ?
C25A C24 C29A C28A 2(4) . . . . ?
C23 C24 C29A C28A 177(2) . . . . ?
C27A C28A C29A C24 -1(4) . . . . ?

_refine_diff_density_max         0.547
_refine_diff_density_min         -0.304
_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_COMPOUND_8
_database_code_depnum_ccdc_archive 'CCDC 1017482'
_audit_update_record             
;
2015-02-20 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C30 H45 Cl Ni O5 P2),0.25(C4 H8 Cl8)'
_chemical_formula_sum            'C61 H92 Cl4 Ni2 O10 P4'
_chemical_formula_weight         1368.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.190(2)
_cell_length_b                   26.541(8)
_cell_length_c                   16.598(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.458(6)
_cell_angle_gamma                90
_cell_volume                     3523.1(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2911
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      24.15
_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_F_000             1444
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.827
_shelx_estimated_absorpt_T_min   0.766
_shelx_estimated_absorpt_T_max   0.968
_exptl_absorpt_correction_type   Analytical
_exptl_absorpt_correction_T_min  0.8423
_exptl_absorpt_correction_T_max  0.9546
_exptl_absorpt_process_details   'SHELXTL V 6.12 (Sheldrick, 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker Smart Apex CCD diffractometer 01-670-01'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            28948
_diffrn_reflns_av_unetI/netI     0.1495
_diffrn_reflns_av_R_equivalents  0.1243
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.983
_diffrn_reflns_theta_max         25.457
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6489
_reflns_number_gt                3250
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 7.34A (Bruker, 2006)'
_computing_structure_solution    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.12 (Sheldrick, 2000)'
_refine_special_details          
;
The compound display disorder affecting the CH2Cl2 solvent, 
which was modeled with SIMU and DELU restraints on anisotropic 
displacement parameters and DFIX geometrical constraints
;
