# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1424394'
_audit_update_record             
;
2015-09-15 deposited with the CCDC.
2016-07-19 downloaded from the CCDC.
;
_audit_creation_date             2014-09-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C50 H42 Li2 P4 S6'
_chemical_formula_sum            'C50 H42 Li2 P4 S6'
_chemical_formula_weight         972.95
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C50 H42 S6 P4 Li1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   10.69567(12)
_cell_length_b                   18.19940(19)
_cell_length_c                   11.90927(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.0727(9)
_cell_angle_gamma                90
_cell_volume                     2312.34(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7266
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.1950
_cell_measurement_theta_min      4.4150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.314
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.0862
_exptl_crystal_size_mid          0.0582
_exptl_crystal_size_min          0.0311
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12842
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.989
_diffrn_reflns_theta_min         4.144
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -49.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000  -90.0000 82

#__ type_ start__ end____ width___ exp.time_
  2 omega  -82.00   39.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   19.0000 -150.0000 121

#__ type_ start__ end____ width___ exp.time_
  3 omega   23.00   97.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3676 -125.0000 -120.0000 74

#__ type_ start__ end____ width___ exp.time_
  4 omega   36.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 55

#__ type_ start__ end____ width___ exp.time_
  5 omega   57.00  151.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
  6 omega   84.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000   30.0000 94

#__ type_ start__ end____ width___ exp.time_
  7 omega   36.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -90.0000 55

#__ type_ start__ end____ width___ exp.time_
  8 omega   36.00  116.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -60.0000 80

#__ type_ start__ end____ width___ exp.time_
  9 omega   39.00   99.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  120.0000 60

#__ type_ start__ end____ width___ exp.time_
 10 omega -115.00  -13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  -57.0000  150.0000 102

#__ type_ start__ end____ width___ exp.time_
 11 omega -118.00   -9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  -77.0000  -90.0000 109

#__ type_ start__ end____ width___ exp.time_
 12 omega    9.00  118.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3676   77.0000   90.0000 109

#__ type_ start__ end____ width___ exp.time_
 13 omega   86.00  132.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   90.0000 46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0250334000
_diffrn_orient_matrix_UB_12      0.0817532000
_diffrn_orient_matrix_UB_13      0.0234100000
_diffrn_orient_matrix_UB_21      0.0055251000
_diffrn_orient_matrix_UB_22      -0.0159184000
_diffrn_orient_matrix_UB_23      0.1272960000
_diffrn_orient_matrix_UB_31      0.1421148000
_diffrn_orient_matrix_UB_32      0.0149932000
_diffrn_orient_matrix_UB_33      0.0084729000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3645
_reflns_number_total             4108
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.548
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4108
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0369
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0511P)²+1.5445P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0986
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C22(H22), C21(H21), C16(H16), C8(H8), C20(H20), C11(H11), C24(H24),
 C9(H9), C12(H12), C10(H10), C3(H3), C15(H15), C17(H17), C6(H6), C2(H2),
 C18(H18), C4(H4), C5(H5), C14(H14)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
S2 S 0.80742(6) 0.39678(3) 0.09049(5) 0.02301(15) Uani 1 1 d . . . . .
P2 P 0.82425(5) 0.33797(3) -0.04593(4) 0.01473(14) Uani 1 1 d . . . . .
S1 S 0.76207(6) 0.56235(3) -0.15386(5) 0.02153(15) Uani 1 1 d . . . . .
S3 S 1.01265(5) 0.43334(3) -0.13990(5) 0.01950(15) Uani 1 1 d . . . . .
P1 P 0.74467(5) 0.46414(3) -0.22403(4) 0.01503(14) Uani 1 1 d . . . . .
C13 C 0.9584(2) 0.27610(13) -0.03111(19) 0.0174(5) Uani 1 1 d . . . . .
C23 C 0.4803(2) 0.24116(16) -0.0420(2) 0.0298(6) Uani 1 1 d . . . . .
H23 H 0.4068 0.2475 -0.0027 0.036 Uiso 1 1 calc R . . . .
C22 C 0.4845(2) 0.18628(14) -0.1223(2) 0.0315(6) Uani 1 1 d . . . . .
H22 H 0.4140 0.1553 -0.1380 0.038 Uiso 1 1 calc R . . . .
C21 C 0.5913(2) 0.17666(14) -0.1796(2) 0.0305(6) Uani 1 1 d . . . . .
H21 H 0.5943 0.1388 -0.2342 0.037 Uiso 1 1 calc R . . . .
C16 C 1.1573(2) 0.17802(15) 0.0000(2) 0.0309(6) Uani 1 1 d . . . . .
H16 H 1.2248 0.1442 0.0112 0.037 Uiso 1 1 calc R . . . .
C8 C 0.5448(2) 0.36877(13) -0.27891(18) 0.0170(5) Uani 1 1 d . . . . .
H8 H 0.5985 0.3459 -0.3287 0.020 Uiso 1 1 calc R . . . .
C20 C 0.6942(2) 0.22226(13) -0.1575(2) 0.0248(5) Uani 1 1 d . . . . .
H20 H 0.7673 0.2158 -0.1974 0.030 Uiso 1 1 calc R . . . .
C19 C 0.6905(2) 0.27790(12) -0.07637(19) 0.0178(5) Uani 1 1 d . . . . .
C7 C 0.5862(2) 0.42952(12) -0.21531(18) 0.0160(4) Uani 1 1 d . . . . .
C11 C 0.3864(2) 0.43636(14) -0.13521(19) 0.0217(5) Uani 1 1 d . . . . .
H11 H 0.3319 0.4596 -0.0866 0.026 Uiso 1 1 calc R . . . .
C24 C 0.5826(2) 0.28690(14) -0.01858(19) 0.0234(5) Uani 1 1 d . . . . .
H24 H 0.5791 0.3243 0.0368 0.028 Uiso 1 1 calc R . . . .
C9 C 0.4252(2) 0.34205(13) -0.26903(18) 0.0195(5) Uani 1 1 d . . . . .
H9 H 0.3969 0.3004 -0.3118 0.023 Uiso 1 1 calc R . . . .
C12 C 0.5062(2) 0.46348(13) -0.14391(18) 0.0191(5) Uani 1 1 d . . . . .
H12 H 0.5339 0.5052 -0.1012 0.023 Uiso 1 1 calc R . . . .
C10 C 0.3460(2) 0.37557(14) -0.19709(19) 0.0224(5) Uani 1 1 d . . . . .
H10 H 0.2640 0.3567 -0.1904 0.027 Uiso 1 1 calc R . . . .
C25 C 0.8577(2) 0.39297(12) -0.16974(18) 0.0160(4) Uani 1 1 d . . . . .
H25 H 0.8658 0.3573 -0.2327 0.019 Uiso 1 1 calc R . . . .
C3 C 0.8809(2) 0.44428(15) -0.5376(2) 0.0277(6) Uani 1 1 d . . . . .
H3 H 0.9533 0.4256 -0.5698 0.033 Uiso 1 1 calc R . . . .
C15 C 1.1044(3) 0.20795(19) 0.0906(2) 0.0425(8) Uani 1 1 d . . . . .
H15 H 1.1356 0.1950 0.1646 0.051 Uiso 1 1 calc R . . . .
C17 C 1.1124(2) 0.19711(14) -0.1085(2) 0.0272(6) Uani 1 1 d . . . . .
H17 H 1.1490 0.1768 -0.1719 0.033 Uiso 1 1 calc R . . . .
C1 C 0.7647(2) 0.46592(12) -0.37442(18) 0.0165(5) Uani 1 1 d . . . . .
C6 C 0.6704(2) 0.49754(13) -0.4440(2) 0.0206(5) Uani 1 1 d . . . . .
H6 H 0.5975 0.5159 -0.4126 0.025 Uiso 1 1 calc R . . . .
C2 C 0.8711(2) 0.43921(14) -0.4215(2) 0.0241(5) Uani 1 1 d . . . . .
H2 H 0.9369 0.4176 -0.3749 0.029 Uiso 1 1 calc R . . . .
C18 C 1.0135(2) 0.24620(14) -0.1230(2) 0.0241(5) Uani 1 1 d . . . . .
H18 H 0.9829 0.2596 -0.1970 0.029 Uiso 1 1 calc R . . . .
C4 C 0.7866(2) 0.47612(13) -0.60592(19) 0.0241(5) Uani 1 1 d . . . . .
H4 H 0.7940 0.4798 -0.6847 0.029 Uiso 1 1 calc R . . . .
C5 C 0.6811(2) 0.50270(14) -0.5589(2) 0.0238(5) Uani 1 1 d . . . . .
H5 H 0.6157 0.5246 -0.6056 0.029 Uiso 1 1 calc R . . . .
C14 C 1.0056(3) 0.25708(17) 0.0754(2) 0.0341(7) Uani 1 1 d . . . . .
H14 H 0.9702 0.2778 0.1392 0.041 Uiso 1 1 calc R . . . .
Li1 Li 0.9765(4) 0.5558(3) -0.0735(4) 0.0302(10) Uani 1 1 d . . . A 1


_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
S2 P2 1.9644(8) . ?
S2 Li1 2.489(5) 3_765 ?
P2 C13 1.823(2) . ?
P2 C19 1.817(2) . ?
P2 C25 1.838(2) . ?
S1 P1 1.9762(8) . ?
S1 Li1 2.424(5) . ?
S3 C25 1.825(2) . ?
S3 Li1 2.406(5) . ?
S3 Li1 2.543(5) 3_765 ?
P1 C7 1.818(2) . ?
P1 C25 1.856(2) . ?
P1 C1 1.819(2) . ?
C13 C18 1.390(3) . ?
C13 C14 1.376(3) . ?
C23 C22 1.386(4) . ?
C23 C24 1.387(4) . ?
C22 C21 1.382(4) . ?
C21 C20 1.389(3) . ?
C16 C15 1.366(4) . ?
C16 C17 1.390(4) . ?
C8 C7 1.394(3) . ?
C8 C9 1.382(3) . ?
C20 C19 1.402(3) . ?
C19 C24 1.395(3) . ?
C7 C12 1.393(3) . ?
C11 C12 1.384(3) . ?
C11 C10 1.382(4) . ?
C9 C10 1.388(3) . ?
C3 C2 1.397(3) . ?
C3 C4 1.378(4) . ?
C15 C14 1.386(4) . ?
C17 C18 1.386(3) . ?
C1 C6 1.384(3) . ?
C1 C2 1.392(3) . ?
C6 C5 1.384(3) . ?
C4 C5 1.382(4) . ?
Li1 S2 2.489(5) 3_765 ?
Li1 S3 2.543(5) 3_765 ?
Li1 Li1 2.706(9) 3_765 ?

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
P2 S2 Li1 88.93(11) . 3_765 ?
C13 P2 S2 111.98(8) . . ?
C13 P2 C25 102.57(10) . . ?
C19 P2 S2 112.07(8) . . ?
C19 P2 C13 104.54(10) . . ?
C19 P2 C25 111.28(10) . . ?
C25 P2 S2 113.65(8) . . ?
P1 S1 Li1 100.41(11) . . ?
C25 S3 Li1 105.78(13) . . ?
C25 S3 Li1 101.67(13) . 3_765 ?
Li1 S3 Li1 66.21(18) . 3_765 ?
C7 P1 S1 110.45(8) . . ?
C7 P1 C25 108.96(10) . . ?
C7 P1 C1 103.76(10) . . ?
C25 P1 S1 116.39(7) . . ?
C1 P1 S1 112.71(8) . . ?
C1 P1 C25 103.66(10) . . ?
C18 C13 P2 122.72(17) . . ?
C14 C13 P2 118.64(19) . . ?
C14 C13 C18 118.6(2) . . ?
C22 C23 C24 120.5(2) . . ?
C21 C22 C23 120.0(2) . . ?
C22 C21 C20 120.1(3) . . ?
C15 C16 C17 119.9(2) . . ?
C9 C8 C7 119.5(2) . . ?
C21 C20 C19 120.1(2) . . ?
C20 C19 P2 120.76(18) . . ?
C24 C19 P2 119.90(18) . . ?
C24 C19 C20 119.3(2) . . ?
C8 C7 P1 120.31(17) . . ?
C12 C7 P1 119.76(17) . . ?
C12 C7 C8 119.9(2) . . ?
C10 C11 C12 120.1(2) . . ?
C23 C24 C19 119.9(2) . . ?
C8 C9 C10 120.5(2) . . ?
C11 C12 C7 120.0(2) . . ?
C11 C10 C9 119.9(2) . . ?
P2 C25 P1 120.04(12) . . ?
S3 C25 P2 106.78(11) . . ?
S3 C25 P1 110.29(11) . . ?
C4 C3 C2 120.6(2) . . ?
C16 C15 C14 120.6(3) . . ?
C18 C17 C16 119.2(2) . . ?
C6 C1 P1 117.73(17) . . ?
C6 C1 C2 119.1(2) . . ?
C2 C1 P1 123.18(18) . . ?
C5 C6 C1 120.8(2) . . ?
C1 C2 C3 119.8(2) . . ?
C17 C18 C13 121.1(2) . . ?
C3 C4 C5 119.5(2) . . ?
C4 C5 C6 120.3(2) . . ?
C13 C14 C15 120.5(3) . . ?
S2 Li1 S3 94.45(15) 3_765 3_765 ?
S2 Li1 Li1 100.5(2) 3_765 3_765 ?
S1 Li1 S2 144.0(2) . 3_765 ?
S1 Li1 S3 111.45(18) . 3_765 ?
S1 Li1 Li1 114.8(3) . 3_765 ?
S3 Li1 S2 97.03(16) . 3_765 ?
S3 Li1 S1 94.89(16) . . ?
S3 Li1 S3 113.79(18) . 3_765 ?
S3 Li1 Li1 59.33(17) . 3_765 ?
S3 Li1 Li1 54.46(16) 3_765 3_765 ?

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
S2 P2 C13 C18 -159.52(18) . . . . ?
S2 P2 C13 C14 21.8(2) . . . . ?
S2 P2 C19 C20 -168.36(17) . . . . ?
S2 P2 C19 C24 11.6(2) . . . . ?
S2 P2 C25 S3 65.70(11) . . . . ?
S2 P2 C25 P1 -60.66(14) . . . . ?
P2 C13 C18 C17 -177.48(19) . . . . ?
P2 C13 C14 C15 177.5(2) . . . . ?
P2 C19 C24 C23 179.83(18) . . . . ?
S1 P1 C7 C8 166.72(15) . . . . ?
S1 P1 C7 C12 -13.9(2) . . . . ?
S1 P1 C25 P2 86.21(13) . . . . ?
S1 P1 C25 S3 -38.50(13) . . . . ?
S1 P1 C1 C6 -71.46(19) . . . . ?
S1 P1 C1 C2 106.55(19) . . . . ?
P1 C7 C12 C11 -178.63(17) . . . . ?
P1 C1 C6 C5 178.10(19) . . . . ?
P1 C1 C2 C3 -178.3(2) . . . . ?
C13 P2 C19 C20 -46.9(2) . . . . ?
C13 P2 C19 C24 133.07(19) . . . . ?
C13 P2 C25 S3 -55.38(13) . . . . ?
C13 P2 C25 P1 178.27(13) . . . . ?
C23 C22 C21 C20 -0.5(4) . . . . ?
C22 C23 C24 C19 0.2(4) . . . . ?
C22 C21 C20 C19 0.5(4) . . . . ?
C21 C20 C19 P2 179.84(19) . . . . ?
C21 C20 C19 C24 -0.1(4) . . . . ?
C16 C15 C14 C13 0.6(5) . . . . ?
C16 C17 C18 C13 -0.4(4) . . . . ?
C8 C7 C12 C11 0.8(3) . . . . ?
C8 C9 C10 C11 0.4(3) . . . . ?
C20 C19 C24 C23 -0.2(3) . . . . ?
C19 P2 C13 C18 78.9(2) . . . . ?
C19 P2 C13 C14 -99.8(2) . . . . ?
C19 P2 C25 S3 -166.65(11) . . . . ?
C19 P2 C25 P1 66.99(15) . . . . ?
C7 P1 C25 P2 -39.45(16) . . . . ?
C7 P1 C25 S3 -164.15(11) . . . . ?
C7 P1 C1 C6 48.0(2) . . . . ?
C7 P1 C1 C2 -134.0(2) . . . . ?
C7 C8 C9 C10 0.5(3) . . . . ?
C24 C23 C22 C21 0.2(4) . . . . ?
C9 C8 C7 P1 178.33(17) . . . . ?
C9 C8 C7 C12 -1.0(3) . . . . ?
C12 C11 C10 C9 -0.7(4) . . . . ?
C10 C11 C12 C7 0.1(3) . . . . ?
C25 P2 C13 C18 -37.3(2) . . . . ?
C25 P2 C13 C14 144.0(2) . . . . ?
C25 P2 C19 C20 63.1(2) . . . . ?
C25 P2 C19 C24 -116.92(19) . . . . ?
C25 P1 C7 C8 -64.26(19) . . . . ?
C25 P1 C7 C12 115.12(18) . . . . ?
C25 P1 C1 C6 161.85(18) . . . . ?
C25 P1 C1 C2 -20.1(2) . . . . ?
C3 C4 C5 C6 0.1(4) . . . . ?
C15 C16 C17 C18 -0.4(4) . . . . ?
C17 C16 C15 C14 0.3(5) . . . . ?
C1 P1 C7 C8 45.7(2) . . . . ?
C1 P1 C7 C12 -134.93(18) . . . . ?
C1 P1 C25 P2 -149.46(13) . . . . ?
C1 P1 C25 S3 85.84(13) . . . . ?
C1 C6 C5 C4 0.1(4) . . . . ?
C6 C1 C2 C3 -0.3(4) . . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
C2 C1 C6 C5 0.0(3) . . . . ?
C18 C13 C14 C15 -1.3(4) . . . . ?
C4 C3 C2 C1 0.6(4) . . . . ?
C14 C13 C18 C17 1.2(4) . . . . ?
Li1 S3 C25 P2 -29.01(15) 3_765 . . . ?
Li1 S3 C25 P2 -97.32(15) . . . . ?
Li1 S3 C25 P1 102.98(14) 3_765 . . . ?
Li1 S3 C25 P1 34.67(16) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7 2 -1 0.0197 7.0000 2.0000 -1.0000 -0.0351 -0.1205 1.0163
-7 -3 2 0.0418 -7.0000 -3.0000 2.0000 -0.0232 0.2637 -1.0228
0 2 8 0.0348 0.0000 2.0000 8.0000 0.3508 0.9865 0.0978
-4 7 -4 0.0279 -4.0000 7.0000 -4.0000 0.5788 -0.6427 -0.4974
-1 -11 -2 0.0119 -1.0000 -11.0000 -2.0000 -0.9211 -0.0850 -0.3240
-1 11 2 0.0297 -1.0000 11.0000 2.0000 0.9711 0.0740 0.0398
1 -10 -4 0.0098 1.0000 -10.0000 -4.0000 -0.9362 -0.3445 -0.0417
7 3 -1 0.0148 7.0000 3.0000 -1.0000 0.0466 -0.1364 1.0313
3 3 -7 0.0286 3.0000 3.0000 -7.0000 0.0063 -0.9223 0.4120
-1 10 4 0.0213 -1.0000 10.0000 4.0000 0.9362 0.3445 0.0417

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 1424395'
_audit_update_record             
;
2015-09-15 deposited with the CCDC.
2016-07-19 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H42 Ni1 P4 S6, 2(C7 H8)'
_chemical_formula_sum            'C64 H58 Ni P4 S6'
_chemical_formula_weight         1202.05

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_HALL  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   11.0600(3)
_cell_length_b                   15.7060(4)
_cell_length_c                   16.8660(4)
_cell_angle_alpha                90.000
_cell_angle_beta                 106.2620(10)
_cell_angle_gamma                90.0000
_cell_volume                     2812.55(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    22121
_cell_measurement_theta_min      1.8
_cell_measurement_theta_max      27.6

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1252
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.8342
_exptl_absorpt_correction_T_max  0.9118
_exptl_absorpt_process_details   'SADABS (SHELXTL-NT v5.1, Bruker)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enraf Nonius FR590D,fine-focus sealed tube'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_measurement_device_type  'KappaCCD (Nonius, FR540C)'
_diffrn_measurement_method       'phiω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21124
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         27.00
_reflns_number_total             6131
_reflns_number_gt                5176
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius, 1999)'
_computing_cell_refinement       'DENZO (Otwinowski & Minor 1997)'
_computing_data_reduction        'Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0469P)²+6.3308P] 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         6131
_refine_ls_number_parameters     341
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0596
_refine_ls_wR_factor_ref         0.1440
_refine_ls_wR_factor_gt          0.1361
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.0000 1.0000 0.02436(16) Uani 1 2 d S . .
P1 P 0.12054(8) 0.10554(6) 0.86621(6) 0.0258(2) Uani 1 1 d . . .
P2 P -0.03019(8) 0.21576(6) 0.96205(6) 0.0264(2) Uani 1 1 d . . .
S1 S 0.01699(9) 0.00218(6) 0.85826(6) 0.0308(2) Uani 1 1 d . . .
S2 S -0.15586(9) 0.12647(6) 0.95795(7) 0.0358(2) Uani 1 1 d . . .
S3 S 0.16703(8) 0.09716(5) 1.04292(5) 0.02562(19) Uani 1 1 d . . .
C1 C 0.2855(3) 0.0849(2) 0.8831(2) 0.0256(7) Uani 1 1 d . . .
C2 C 0.3249(4) 0.0029(2) 0.8737(2) 0.0337(8) Uani 1 1 d . . .
H2 H 0.2649 -0.0417 0.8587 0.040 Uiso 1 1 calc R . .
C3 C 0.4505(4) -0.0142(3) 0.8860(3) 0.0384(9) Uani 1 1 d . . .
H3 H 0.4768 -0.0706 0.8791 0.046 Uiso 1 1 calc R . .
C4 C 0.5381(4) 0.0494(3) 0.9082(3) 0.0395(9) Uani 1 1 d . . .
H4 H 0.6249 0.0370 0.9169 0.047 Uiso 1 1 calc R . .
C5 C 0.5003(4) 0.1320(3) 0.9180(2) 0.0376(9) Uani 1 1 d . . .
H5 H 0.5611 0.1761 0.9338 0.045 Uiso 1 1 calc R . .
C6 C 0.3746(4) 0.1497(2) 0.9047(2) 0.0308(8) Uani 1 1 d . . .
H6 H 0.3483 0.2064 0.9102 0.037 Uiso 1 1 calc R . .
C7 C 0.0687(4) 0.1662(2) 0.7707(2) 0.0309(8) Uani 1 1 d . . .
C8 C 0.1525(4) 0.2009(3) 0.7327(2) 0.0402(9) Uani 1 1 d . . .
H8 H 0.2405 0.1927 0.7556 0.048 Uiso 1 1 calc R . .
C9 C 0.1077(5) 0.2481(3) 0.6607(3) 0.0499(11) Uani 1 1 d . . .
H9 H 0.1649 0.2718 0.6340 0.060 Uiso 1 1 calc R . .
C10 C -0.0193(5) 0.2603(3) 0.6282(3) 0.0526(13) Uani 1 1 d . . .
H10 H -0.0498 0.2929 0.5792 0.063 Uiso 1 1 calc R . .
C11 C -0.1023(5) 0.2257(3) 0.6659(3) 0.0470(11) Uani 1 1 d . . .
H11 H -0.1901 0.2351 0.6433 0.056 Uiso 1 1 calc R . .
C12 C -0.0594(4) 0.1775(2) 0.7364(2) 0.0368(9) Uani 1 1 d . . .
H12 H -0.1176 0.1520 0.7613 0.044 Uiso 1 1 calc R . .
C13 C -0.0796(3) 0.2953(2) 0.8822(2) 0.0305(8) Uani 1 1 d . . .
C14 C 0.0084(4) 0.3465(2) 0.8589(2) 0.0342(8) Uani 1 1 d . . .
H14 H 0.0959 0.3407 0.8856 0.041 Uiso 1 1 calc R . .
C15 C -0.0335(4) 0.4055(3) 0.7967(2) 0.0406(9) Uani 1 1 d . . .
H15 H 0.0257 0.4402 0.7803 0.049 Uiso 1 1 calc R . .
C16 C -0.1599(5) 0.4147(3) 0.7581(3) 0.0458(11) Uani 1 1 d . . .
H16 H -0.1875 0.4556 0.7153 0.055 Uiso 1 1 calc R . .
C17 C -0.2469(4) 0.3649(3) 0.7814(3) 0.0454(10) Uani 1 1 d . . .
H17 H -0.3341 0.3713 0.7544 0.054 Uiso 1 1 calc R . .
C18 C -0.2075(4) 0.3059(3) 0.8434(2) 0.0369(9) Uani 1 1 d . . .
H18 H -0.2677 0.2722 0.8598 0.044 Uiso 1 1 calc R . .
C19 C 0.0104(3) 0.2735(2) 1.0586(2) 0.0296(8) Uani 1 1 d . . .
C20 C 0.0767(4) 0.3492(3) 1.0669(2) 0.0398(9) Uani 1 1 d . . .
H20 H 0.0991 0.3727 1.0211 0.048 Uiso 1 1 calc R . .
C21 C 0.1100(4) 0.3904(3) 1.1419(3) 0.0467(11) Uani 1 1 d . . .
H21 H 0.1577 0.4415 1.1479 0.056 Uiso 1 1 calc R . .
C22 C 0.0757(5) 0.3590(3) 1.2077(3) 0.0464(11) Uani 1 1 d . . .
H22 H 0.0989 0.3883 1.2590 0.056 Uiso 1 1 calc R . .
C23 C 0.0078(4) 0.2853(3) 1.1996(3) 0.0459(11) Uani 1 1 d . . .
H23 H -0.0172 0.2637 1.2453 0.055 Uiso 1 1 calc R . .
C24 C -0.0248(4) 0.2418(3) 1.1252(2) 0.0368(9) Uani 1 1 d . . .
H24 H -0.0712 0.1903 1.1200 0.044 Uiso 1 1 calc R . .
C25 C 0.1186(3) 0.1690(2) 0.9569(2) 0.0243(7) Uani 1 1 d . . .
H25 H 0.1828 0.2154 0.9639 0.029 Uiso 1 1 calc R . .
C26 C 0.3642(5) 0.4348(3) 0.8964(3) 0.0582(13) Uani 1 1 d . . .
C27 C 0.2880(5) 0.5024(3) 0.8685(3) 0.0559(13) Uani 1 1 d . . .
H27 H 0.2694 0.5186 0.8121 0.067 Uiso 1 1 calc R . .
C28 C 0.2367(6) 0.5487(4) 0.9223(4) 0.0744(17) Uani 1 1 d . . .
H28 H 0.1833 0.5958 0.9016 0.089 Uiso 1 1 calc R . .
C29 C 0.2609(6) 0.5279(4) 1.0016(4) 0.0711(16) Uani 1 1 d . . .
H29 H 0.2245 0.5590 1.0375 0.085 Uiso 1 1 calc R . .
C30 C 0.3425(6) 0.4583(4) 1.0313(4) 0.0667(15) Uani 1 1 d . . .
H30 H 0.3631 0.4433 1.0881 0.080 Uiso 1 1 calc R . .
C31 C 0.3902(5) 0.4140(3) 0.9801(3) 0.0546(12) Uani 1 1 d . . .
H31 H 0.4435 0.3669 1.0010 0.066 Uiso 1 1 calc R . .
C32 C 0.4203(7) 0.3873(4) 0.8416(4) 0.090(2) Uani 1 1 d . . .
H32A H 0.3569 0.3498 0.8064 0.135 Uiso 1 1 calc R . .
H32B H 0.4906 0.3531 0.8746 0.135 Uiso 1 1 calc R . .
H32C H 0.4514 0.4272 0.8071 0.135 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S3 2.3487(8) . ?
Ni1 S3 2.3487(8) 3_557 ?
Ni1 S1 2.4500(9) 3_557 ?
Ni1 S1 2.4500(9) . ?
Ni1 S2 2.5953(10) . ?
Ni1 S2 2.5953(10) 3_557 ?
P1 C1 1.795(4) . ?
P1 C7 1.820(4) . ?
P1 C25 1.831(3) . ?
P1 S1 1.9695(12) . ?
P2 C13 1.805(4) . ?
P2 C19 1.807(4) . ?
P2 C25 1.826(3) . ?
P2 S2 1.9621(13) . ?
S3 C25 1.797(3) . ?
C1 C2 1.382(5) . ?
C1 C6 1.392(5) . ?
C2 C3 1.372(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.369(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.373(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.378(5) . ?
C7 C12 1.384(5) . ?
C8 C9 1.391(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.370(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.366(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.392(5) . ?
C13 C14 1.402(5) . ?
C14 C15 1.379(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.375(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.380(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.374(6) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.380(5) . ?
C19 C20 1.384(5) . ?
C20 C21 1.376(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.361(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.366(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.385(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 H25 1.0000 . ?
C26 C27 1.356(7) . ?
C26 C31 1.398(7) . ?
C26 C32 1.454(8) . ?
C27 C28 1.401(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.330(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.416(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.328(8) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

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
S3 Ni1 S3 180.00(4) . 3_557 ?
S3 Ni1 S1 88.68(3) . 3_557 ?
S3 Ni1 S1 91.32(3) 3_557 3_557 ?
S3 Ni1 S1 91.32(3) . . ?
S3 Ni1 S1 88.68(3) 3_557 . ?
S1 Ni1 S1 180.0 3_557 . ?
S3 Ni1 S2 89.53(3) . . ?
S3 Ni1 S2 90.47(3) 3_557 . ?
S1 Ni1 S2 92.91(3) 3_557 . ?
S1 Ni1 S2 87.09(3) . . ?
S3 Ni1 S2 90.47(3) . 3_557 ?
S3 Ni1 S2 89.53(3) 3_557 3_557 ?
S1 Ni1 S2 87.09(3) 3_557 3_557 ?
S1 Ni1 S2 92.91(3) . 3_557 ?
S2 Ni1 S2 180.0 . 3_557 ?
C1 P1 C7 106.83(17) . . ?
C1 P1 C25 102.39(16) . . ?
C7 P1 C25 112.30(16) . . ?
C1 P1 S1 114.05(12) . . ?
C7 P1 S1 109.78(13) . . ?
C25 P1 S1 111.29(12) . . ?
C13 P2 C19 105.78(17) . . ?
C13 P2 C25 109.38(16) . . ?
C19 P2 C25 104.17(16) . . ?
C13 P2 S2 113.86(13) . . ?
C19 P2 S2 112.63(13) . . ?
C25 P2 S2 110.49(12) . . ?
P1 S1 Ni1 98.46(4) . . ?
P2 S2 Ni1 97.33(5) . . ?
C25 S3 Ni1 97.38(11) . . ?
C2 C1 C6 119.2(3) . . ?
C2 C1 P1 119.3(3) . . ?
C6 C1 P1 121.5(3) . . ?
C3 C2 C1 120.3(4) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.1(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.7(4) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 120.3(4) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
C8 C7 C12 119.8(4) . . ?
C8 C7 P1 122.2(3) . . ?
C12 C7 P1 118.0(3) . . ?
C7 C8 C9 119.7(4) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 119.9(4) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C11 C10 C9 120.4(4) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 120.4(4) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 119.8(4) . . ?
C11 C12 H12 120.1 . . ?
C7 C12 H12 120.1 . . ?
C18 C13 C14 119.6(4) . . ?
C18 C13 P2 119.3(3) . . ?
C14 C13 P2 121.1(3) . . ?
C15 C14 C13 119.2(4) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C16 C15 C14 120.7(4) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 120.2(4) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C18 C17 C16 120.1(4) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C13 120.2(4) . . ?
C17 C18 H18 119.9 . . ?
C13 C18 H18 119.9 . . ?
C24 C19 C20 119.3(4) . . ?
C24 C19 P2 119.8(3) . . ?
C20 C19 P2 120.9(3) . . ?
C21 C20 C19 119.7(4) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C22 C21 C20 121.0(4) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 C23 119.8(4) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C22 C23 C24 120.3(4) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C19 C24 C23 119.9(4) . . ?
C19 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
S3 C25 P2 106.43(17) . . ?
S3 C25 P1 105.18(17) . . ?
P2 C25 P1 118.68(18) . . ?
S3 C25 H25 108.7 . . ?
P2 C25 H25 108.7 . . ?
P1 C25 H25 108.7 . . ?
C27 C26 C31 117.8(5) . . ?
C27 C26 C32 121.0(6) . . ?
C31 C26 C32 121.2(6) . . ?
C26 C27 C28 120.4(5) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C29 C28 C27 121.4(6) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C28 C29 C30 118.3(6) . . ?
C28 C29 H29 120.9 . . ?
C30 C29 H29 120.9 . . ?
C31 C30 C29 120.3(5) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C30 C31 C26 121.8(5) . . ?
C30 C31 H31 119.1 . . ?
C26 C31 H31 119.1 . . ?
C26 C32 H32A 109.5 . . ?
C26 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C26 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 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
C1 P1 S1 Ni1 98.57(13) . . . . ?
C7 P1 S1 Ni1 -141.61(13) . . . . ?
C25 P1 S1 Ni1 -16.65(12) . . . . ?
S3 Ni1 S1 P1 -15.67(5) . . . . ?
S3 Ni1 S1 P1 164.33(5) 3_557 . . . ?
S1 Ni1 S1 P1 157(100) 3_557 . . . ?
S2 Ni1 S1 P1 73.79(5) . . . . ?
S2 Ni1 S1 P1 -106.21(5) 3_557 . . . ?
C13 P2 S2 Ni1 142.65(13) . . . . ?
C19 P2 S2 Ni1 -96.91(13) . . . . ?
C25 P2 S2 Ni1 19.12(12) . . . . ?
S3 Ni1 S2 P2 13.95(5) . . . . ?
S3 Ni1 S2 P2 -166.05(5) 3_557 . . . ?
S1 Ni1 S2 P2 102.61(5) 3_557 . . . ?
S1 Ni1 S2 P2 -77.39(5) . . . . ?
S2 Ni1 S2 P2 175(100) 3_557 . . . ?
S3 Ni1 S3 C25 -26(100) 3_557 . . . ?
S1 Ni1 S3 C25 -135.93(11) 3_557 . . . ?
S1 Ni1 S3 C25 44.07(11) . . . . ?
S2 Ni1 S3 C25 -43.01(11) . . . . ?
S2 Ni1 S3 C25 136.99(11) 3_557 . . . ?
C7 P1 C1 C2 -109.3(3) . . . . ?
C25 P1 C1 C2 132.5(3) . . . . ?
S1 P1 C1 C2 12.2(3) . . . . ?
C7 P1 C1 C6 70.0(3) . . . . ?
C25 P1 C1 C6 -48.2(3) . . . . ?
S1 P1 C1 C6 -168.5(3) . . . . ?
C6 C1 C2 C3 0.4(6) . . . . ?
P1 C1 C2 C3 179.7(3) . . . . ?
C1 C2 C3 C4 0.4(6) . . . . ?
C2 C3 C4 C5 -0.3(6) . . . . ?
C3 C4 C5 C6 -0.5(6) . . . . ?
C4 C5 C6 C1 1.4(6) . . . . ?
C2 C1 C6 C5 -1.3(5) . . . . ?
P1 C1 C6 C5 179.4(3) . . . . ?
C1 P1 C7 C8 -11.4(4) . . . . ?
C25 P1 C7 C8 100.1(3) . . . . ?
S1 P1 C7 C8 -135.5(3) . . . . ?
C1 P1 C7 C12 168.9(3) . . . . ?
C25 P1 C7 C12 -79.6(3) . . . . ?
S1 P1 C7 C12 44.8(3) . . . . ?
C12 C7 C8 C9 0.9(6) . . . . ?
P1 C7 C8 C9 -178.8(3) . . . . ?
C7 C8 C9 C10 0.4(7) . . . . ?
C8 C9 C10 C11 -0.5(7) . . . . ?
C9 C10 C11 C12 -0.8(7) . . . . ?
C10 C11 C12 C7 2.1(6) . . . . ?
C8 C7 C12 C11 -2.2(6) . . . . ?
P1 C7 C12 C11 177.5(3) . . . . ?
C19 P2 C13 C18 -103.4(3) . . . . ?
C25 P2 C13 C18 145.0(3) . . . . ?
S2 P2 C13 C18 20.8(3) . . . . ?
C19 P2 C13 C14 76.5(3) . . . . ?
C25 P2 C13 C14 -35.1(3) . . . . ?
S2 P2 C13 C14 -159.3(3) . . . . ?
C18 C13 C14 C15 -1.1(6) . . . . ?
P2 C13 C14 C15 179.0(3) . . . . ?
C13 C14 C15 C16 0.4(6) . . . . ?
C14 C15 C16 C17 0.1(7) . . . . ?
C15 C16 C17 C18 0.1(7) . . . . ?
C16 C17 C18 C13 -0.9(6) . . . . ?
C14 C13 C18 C17 1.4(6) . . . . ?
P2 C13 C18 C17 -178.7(3) . . . . ?
C13 P2 C19 C24 138.5(3) . . . . ?
C25 P2 C19 C24 -106.2(3) . . . . ?
S2 P2 C19 C24 13.5(3) . . . . ?
C13 P2 C19 C20 -41.6(4) . . . . ?
C25 P2 C19 C20 73.6(3) . . . . ?
S2 P2 C19 C20 -166.6(3) . . . . ?
C24 C19 C20 C21 2.0(6) . . . . ?
P2 C19 C20 C21 -177.8(3) . . . . ?
C19 C20 C21 C22 -1.8(7) . . . . ?
C20 C21 C22 C23 0.4(7) . . . . ?
C21 C22 C23 C24 0.9(7) . . . . ?
C20 C19 C24 C23 -0.8(6) . . . . ?
P2 C19 C24 C23 179.1(3) . . . . ?
C22 C23 C24 C19 -0.6(7) . . . . ?
Ni1 S3 C25 P2 64.99(15) . . . . ?
Ni1 S3 C25 P1 -61.76(15) . . . . ?
C13 P2 C25 S3 175.56(16) . . . . ?
C19 P2 C25 S3 62.8(2) . . . . ?
S2 P2 C25 S3 -58.35(17) . . . . ?
C13 P2 C25 P1 -66.2(2) . . . . ?
C19 P2 C25 P1 -179.0(2) . . . . ?
S2 P2 C25 P1 59.9(2) . . . . ?
C1 P1 C25 S3 -67.70(19) . . . . ?
C7 P1 C25 S3 178.07(17) . . . . ?
S1 P1 C25 S3 54.54(17) . . . . ?
C1 P1 C25 P2 173.5(2) . . . . ?
C7 P1 C25 P2 59.2(3) . . . . ?
S1 P1 C25 P2 -64.3(2) . . . . ?
C31 C26 C27 C28 -0.8(8) . . . . ?
C32 C26 C27 C28 -178.7(6) . . . . ?
C26 C27 C28 C29 0.1(9) . . . . ?
C27 C28 C29 C30 1.1(9) . . . . ?
C28 C29 C30 C31 -1.8(9) . . . . ?
C29 C30 C31 C26 1.1(8) . . . . ?
C27 C26 C31 C30 0.1(8) . . . . ?
C32 C26 C31 C30 178.0(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.102
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
####################################################################### 
# 
# 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_4b
_database_code_depnum_ccdc_archive 'CCDC 1424396'
_audit_update_record             
;
2015-09-15 deposited with the CCDC.
2016-07-19 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H42 Ni P4 S6'
_chemical_formula_sum            'C50 H42 Ni P4 S6'
_chemical_formula_weight         1017.79

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.297(5)
_cell_length_b                   11.399(5)
_cell_length_c                   12.389(5)
_cell_angle_alpha                75.706(5)
_cell_angle_beta                 83.003(5)
_cell_angle_gamma                66.213(5)
_cell_volume                     1163.9(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    6961
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      25.02

_exptl_crystal_description       Plate
_exptl_crystal_colour            'brown red'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             526
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_type   Integration
_exptl_absorpt_correction_T_min  0.9190
_exptl_absorpt_correction_T_max  0.9830
_exptl_absorpt_process_details   'SADABS (SHELXTL-NT v5.1, Bruker)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enraf Nonius FR590D'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_measurement_device_type  'KappaCCD (Nonius, FR540C)'
_diffrn_measurement_method       'phiω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6961
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4097
_reflns_number_gt                3001
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        DENZO-SMN
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'WinGX v1.70-01 (L. J. Farrugia)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0167P)²+8.3445P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4097
_refine_ls_number_parameters     277
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0705
_refine_ls_wR_factor_ref         0.1545
_refine_ls_wR_factor_gt          0.1357
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.0000 0.5000 0.0259(3) Uani 1 2 d S . .
S1 S 0.24251(18) -0.05717(16) 0.54040(13) 0.0267(4) Uani 1 1 d . . .
S2 S 0.16999(19) 0.10240(16) 0.94500(14) 0.0314(4) Uani 1 1 d . . .
S3 S -0.09756(18) 0.07072(16) 0.65315(14) 0.0304(4) Uani 1 1 d . . .
P1 P 0.22683(17) -0.10538(15) 0.70642(13) 0.0198(3) Uani 1 1 d . . .
P2 P 0.07502(18) 0.15510(15) 0.79957(14) 0.0234(4) Uani 1 1 d . . .
C1 C 0.4150(6) -0.1336(5) 0.7581(5) 0.0197(12) Uani 1 1 d . . .
C2 C 0.5324(7) -0.1168(6) 0.6830(5) 0.0247(13) Uani 1 1 d . . .
H2 H 0.5115 -0.0887 0.6057 0.030 Uiso 1 1 calc R . .
C3 C 0.6784(7) -0.1396(6) 0.7177(6) 0.0305(15) Uani 1 1 d . . .
H3 H 0.7577 -0.1285 0.6649 0.037 Uiso 1 1 calc R . .
C4 C 0.7078(7) -0.1786(7) 0.8298(6) 0.0332(16) Uani 1 1 d . . .
H4 H 0.8077 -0.1934 0.8547 0.040 Uiso 1 1 calc R . .
C5 C 0.5938(8) -0.1964(7) 0.9066(6) 0.0358(16) Uani 1 1 d . . .
H5 H 0.6154 -0.2232 0.9839 0.043 Uiso 1 1 calc R . .
C6 C 0.4474(7) -0.1752(7) 0.8712(5) 0.0312(15) Uani 1 1 d . . .
H6 H 0.3695 -0.1890 0.9241 0.037 Uiso 1 1 calc R . .
C7 C 0.1919(7) -0.2559(6) 0.7590(5) 0.0238(13) Uani 1 1 d . . .
C8 C 0.2008(7) -0.3337(6) 0.6854(6) 0.0277(14) Uani 1 1 d . . .
H8 H 0.2186 -0.3059 0.6079 0.033 Uiso 1 1 calc R . .
C9 C 0.1834(8) -0.4525(6) 0.7268(6) 0.0344(16) Uani 1 1 d . . .
H9 H 0.1894 -0.5063 0.6774 0.041 Uiso 1 1 calc R . .
C10 C 0.1572(7) -0.4921(6) 0.8394(6) 0.0309(15) Uani 1 1 d . . .
H10 H 0.1469 -0.5738 0.8675 0.037 Uiso 1 1 calc R . .
C11 C 0.1462(7) -0.4146(6) 0.9103(6) 0.0318(15) Uani 1 1 d . . .
H11 H 0.1272 -0.4428 0.9876 0.038 Uiso 1 1 calc R . .
C12 C 0.1621(6) -0.2946(6) 0.8722(5) 0.0256(14) Uani 1 1 d . . .
H12 H 0.1528 -0.2406 0.9222 0.031 Uiso 1 1 calc R . .
C13 C 0.1830(7) 0.2224(6) 0.6882(5) 0.0259(14) Uani 1 1 d . . .
C14 C 0.1171(8) 0.2886(6) 0.5835(5) 0.0311(15) Uani 1 1 d . . .
H14 H 0.0132 0.3000 0.5704 0.037 Uiso 1 1 calc R . .
C15 C 0.2032(9) 0.3368(7) 0.5001(6) 0.0422(18) Uani 1 1 d . . .
H15 H 0.1579 0.3836 0.4296 0.051 Uiso 1 1 calc R . .
C16 C 0.3561(9) 0.3174(8) 0.5184(7) 0.046(2) Uani 1 1 d . . .
H16 H 0.4155 0.3497 0.4598 0.055 Uiso 1 1 calc R . .
C17 C 0.4227(8) 0.2519(7) 0.6202(7) 0.0408(18) Uani 1 1 d . . .
H17 H 0.5270 0.2402 0.6323 0.049 Uiso 1 1 calc R . .
C18 C 0.3372(7) 0.2033(6) 0.7049(6) 0.0316(15) Uani 1 1 d . . .
H18 H 0.3837 0.1566 0.7750 0.038 Uiso 1 1 calc R . .
C19 C -0.1240(7) 0.2783(6) 0.8006(5) 0.0260(14) Uani 1 1 d . . .
C20 C -0.2481(7) 0.2404(6) 0.8414(5) 0.0311(15) Uani 1 1 d . . .
H20 H -0.2315 0.1500 0.8624 0.037 Uiso 1 1 calc R . .
C21 C -0.3967(8) 0.3362(7) 0.8510(6) 0.0385(18) Uani 1 1 d . . .
H21 H -0.4831 0.3112 0.8759 0.046 Uiso 1 1 calc R . .
C22 C -0.4203(8) 0.4673(6) 0.8249(6) 0.0364(17) Uani 1 1 d . . .
H22 H -0.5221 0.5320 0.8334 0.044 Uiso 1 1 calc R . .
C23 C -0.2971(8) 0.5043(6) 0.7866(6) 0.0347(16) Uani 1 1 d . . .
H23 H -0.3132 0.5946 0.7690 0.042 Uiso 1 1 calc R . .
C24 C -0.1487(7) 0.4098(6) 0.7734(6) 0.0303(15) Uani 1 1 d . . .
H24 H -0.0637 0.4357 0.7455 0.036 Uiso 1 1 calc R . .
C25 C 0.0536(6) 0.0190(6) 0.7580(5) 0.0235(13) Uani 1 1 d . . .
H25 H 0.0161 -0.0295 0.8266 0.028 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 S1 2.1649(19) 2_556 ?
Ni1 S1 2.1649(19) . ?
Ni1 S3 2.1952(18) 2_556 ?
Ni1 S3 2.1952(18) . ?
S1 P1 1.997(2) . ?
S2 P2 1.952(2) . ?
S3 C25 1.846(6) . ?
P1 C1 1.814(6) . ?
P1 C7 1.822(6) . ?
P1 C25 1.835(6) . ?
P2 C13 1.806(7) . ?
P2 C19 1.817(6) . ?
P2 C25 1.839(6) . ?
C1 C2 1.388(8) . ?
C1 C6 1.393(8) . ?
C2 C3 1.377(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.376(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(9) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.391(9) . ?
C7 C8 1.396(9) . ?
C8 C9 1.392(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.380(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.361(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(9) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.394(9) . ?
C13 C14 1.401(9) . ?
C14 C15 1.373(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(11) . ?
C15 H15 0.9500 . ?
C16 C17 1.372(11) . ?
C16 H16 0.9500 . ?
C17 C18 1.380(10) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.380(9) . ?
C19 C20 1.387(9) . ?
C20 C21 1.387(9) . ?
C20 H20 0.9500 . ?
C21 C22 1.379(10) . ?
C21 H21 0.9500 . ?
C22 C23 1.368(10) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(9) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 H25 1.0000 . ?

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
S1 Ni1 S1 180.00(8) 2_556 . ?
S1 Ni1 S3 94.70(6) 2_556 2_556 ?
S1 Ni1 S3 85.30(6) . 2_556 ?
S1 Ni1 S3 85.30(6) 2_556 . ?
S1 Ni1 S3 94.70(6) . . ?
S3 Ni1 S3 180.0 2_556 . ?
P1 S1 Ni1 100.06(8) . . ?
C25 S3 Ni1 112.50(19) . . ?
C1 P1 C7 107.2(3) . . ?
C1 P1 C25 116.2(3) . . ?
C7 P1 C25 103.1(3) . . ?
C1 P1 S1 106.8(2) . . ?
C7 P1 S1 113.5(2) . . ?
C25 P1 S1 110.1(2) . . ?
C13 P2 C19 107.1(3) . . ?
C13 P2 C25 107.0(3) . . ?
C19 P2 C25 104.5(3) . . ?
C13 P2 S2 113.6(2) . . ?
C19 P2 S2 111.3(2) . . ?
C25 P2 S2 112.8(2) . . ?
C2 C1 C6 118.6(5) . . ?
C2 C1 P1 119.4(4) . . ?
C6 C1 P1 122.0(5) . . ?
C3 C2 C1 121.8(6) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C4 C3 C2 119.0(6) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 120.7(6) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 120.2(6) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 119.8(6) . . ?
C5 C6 H6 120.1 . . ?
C1 C6 H6 120.1 . . ?
C12 C7 C8 120.6(6) . . ?
C12 C7 P1 120.0(5) . . ?
C8 C7 P1 119.3(5) . . ?
C9 C8 C7 119.2(6) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C10 C9 C8 120.1(6) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 C9 120.3(6) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 121.4(6) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C7 C12 C11 118.4(6) . . ?
C7 C12 H12 120.8 . . ?
C11 C12 H12 120.8 . . ?
C18 C13 C14 119.3(6) . . ?
C18 C13 P2 119.5(5) . . ?
C14 C13 P2 121.2(5) . . ?
C15 C14 C13 119.7(6) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 120.2(7) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C17 C16 C15 120.8(7) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C16 C17 C18 119.6(7) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C17 C18 C13 120.4(7) . . ?
C17 C18 H18 119.8 . . ?
C13 C18 H18 119.8 . . ?
C24 C19 C20 119.9(6) . . ?
C24 C19 P2 119.6(5) . . ?
C20 C19 P2 120.0(5) . . ?
C21 C20 C19 119.1(6) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C22 C21 C20 120.7(6) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C23 C22 C21 120.0(6) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.0(6) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C19 C24 C23 120.3(6) . . ?
C19 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
P1 C25 P2 119.3(3) . . ?
P1 C25 S3 104.8(3) . . ?
P2 C25 S3 114.5(3) . . ?
P1 C25 H25 105.7 . . ?
P2 C25 H25 105.7 . . ?
S3 C25 H25 105.7 . . ?

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
S1 Ni1 S1 P1 89(100) 2_556 . . . ?
S3 Ni1 S1 P1 -149.31(9) 2_556 . . . ?
S3 Ni1 S1 P1 30.69(9) . . . . ?
S1 Ni1 S3 C25 166.8(2) 2_556 . . . ?
S1 Ni1 S3 C25 -13.2(2) . . . . ?
S3 Ni1 S3 C25 -55.0(3) 2_556 . . . ?
Ni1 S1 P1 C1 -171.71(19) . . . . ?
Ni1 S1 P1 C7 70.4(2) . . . . ?
Ni1 S1 P1 C25 -44.7(2) . . . . ?
C7 P1 C1 C2 123.3(5) . . . . ?
C25 P1 C1 C2 -122.0(5) . . . . ?
S1 P1 C1 C2 1.3(5) . . . . ?
C7 P1 C1 C6 -55.0(6) . . . . ?
C25 P1 C1 C6 59.7(6) . . . . ?
S1 P1 C1 C6 -177.0(5) . . . . ?
C6 C1 C2 C3 -0.2(9) . . . . ?
P1 C1 C2 C3 -178.6(5) . . . . ?
C1 C2 C3 C4 -0.8(10) . . . . ?
C2 C3 C4 C5 0.8(10) . . . . ?
C3 C4 C5 C6 0.1(11) . . . . ?
C4 C5 C6 C1 -1.1(11) . . . . ?
C2 C1 C6 C5 1.2(9) . . . . ?
P1 C1 C6 C5 179.5(5) . . . . ?
C1 P1 C7 C12 69.0(5) . . . . ?
C25 P1 C7 C12 -54.2(5) . . . . ?
S1 P1 C7 C12 -173.3(4) . . . . ?
C1 P1 C7 C8 -108.8(5) . . . . ?
C25 P1 C7 C8 128.0(5) . . . . ?
S1 P1 C7 C8 8.9(5) . . . . ?
C12 C7 C8 C9 -1.6(9) . . . . ?
P1 C7 C8 C9 176.2(5) . . . . ?
C7 C8 C9 C10 0.1(9) . . . . ?
C8 C9 C10 C11 0.9(10) . . . . ?
C9 C10 C11 C12 -0.6(10) . . . . ?
C8 C7 C12 C11 1.9(8) . . . . ?
P1 C7 C12 C11 -175.9(4) . . . . ?
C10 C11 C12 C7 -0.9(9) . . . . ?
C19 P2 C13 C18 138.9(5) . . . . ?
C25 P2 C13 C18 -109.5(5) . . . . ?
S2 P2 C13 C18 15.6(6) . . . . ?
C19 P2 C13 C14 -44.0(6) . . . . ?
C25 P2 C13 C14 67.6(5) . . . . ?
S2 P2 C13 C14 -167.3(4) . . . . ?
C18 C13 C14 C15 -1.9(9) . . . . ?
P2 C13 C14 C15 -179.0(5) . . . . ?
C13 C14 C15 C16 1.6(10) . . . . ?
C14 C15 C16 C17 -1.1(11) . . . . ?
C15 C16 C17 C18 0.9(11) . . . . ?
C16 C17 C18 C13 -1.2(10) . . . . ?
C14 C13 C18 C17 1.7(9) . . . . ?
P2 C13 C18 C17 178.8(5) . . . . ?
C13 P2 C19 C24 -34.5(6) . . . . ?
C25 P2 C19 C24 -147.8(5) . . . . ?
S2 P2 C19 C24 90.2(5) . . . . ?
C13 P2 C19 C20 153.2(5) . . . . ?
C25 P2 C19 C20 40.0(6) . . . . ?
S2 P2 C19 C20 -82.1(5) . . . . ?
C24 C19 C20 C21 1.9(10) . . . . ?
P2 C19 C20 C21 174.1(5) . . . . ?
C19 C20 C21 C22 -2.6(11) . . . . ?
C20 C21 C22 C23 1.5(11) . . . . ?
C21 C22 C23 C24 0.4(11) . . . . ?
C20 C19 C24 C23 0.0(10) . . . . ?
P2 C19 C24 C23 -172.3(5) . . . . ?
C22 C23 C24 C19 -1.1(10) . . . . ?
C1 P1 C25 P2 28.1(5) . . . . ?
C7 P1 C25 P2 145.1(4) . . . . ?
S1 P1 C25 P2 -93.5(3) . . . . ?
C1 P1 C25 S3 158.0(3) . . . . ?
C7 P1 C25 S3 -85.0(3) . . . . ?
S1 P1 C25 S3 36.4(3) . . . . ?
C13 P2 C25 P1 48.8(4) . . . . ?
C19 P2 C25 P1 162.1(4) . . . . ?
S2 P2 C25 P1 -76.8(4) . . . . ?
C13 P2 C25 S3 -76.6(4) . . . . ?
C19 P2 C25 S3 36.8(4) . . . . ?
S2 P2 C25 S3 157.8(2) . . . . ?
Ni1 S3 C25 P1 -12.2(4) . . . . ?
Ni1 S3 C25 P2 120.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.115

#===END

_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
####################################################################### 
# 
# 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_jk1605_a
_database_code_depnum_ccdc_archive 'CCDC 1486829'
_audit_update_record             
;
2016-06-27 deposited with the CCDC.
2016-07-19 downloaded from the CCDC.
;
_audit_creation_date             2016-05-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C50 H42 P4 S6 Zn'
_chemical_formula_sum            'C50 H42 P4 S6 Zn'
_chemical_formula_weight         1024.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C50 H42 P4 S6 Zn1'
_chemical_oxdiff_usercomment     'colorless plate'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   10.72456(17)
_cell_length_b                   18.3260(3)
_cell_length_c                   11.6699(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.7455(16)
_cell_angle_gamma                90
_cell_volume                     2288.69(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4394
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.3830
_cell_measurement_theta_min      4.4630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.907
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.409
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 1 -4 0.0158
5 -1 4 0.0138
0 1 0 0.0381
0 -1 0 0.0411
-4 -1 5 0.1459
4 1 -5 0.1499

_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.03
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.0000 1.0000 -4.0000 -0.8836 -0.2715 -0.0248
5.0000 -1.0000 4.0000 0.8836 0.2715 0.0248
-0.0000 1.0000 0.0000 -0.0005 -0.0317 0.0778
0.0000 -1.0000 -0.0000 0.0005 0.0317 -0.0778
-4.0000 -0.9999 5.0000 0.1838 -0.7355 -0.3898
4.0000 0.9999 -5.0000 -0.1838 0.7355 0.3898

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7806
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.952
_diffrn_reflns_theta_min         4.131
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00 -35.00   1.00    1.50    --  -41.65  77.00 -30.00   35
  2  ω    -91.00 -17.00   1.00    1.50    --  -41.65 -57.00  60.00   74
  3  ω   -113.00 -16.00   1.00    1.50    --  -41.65 -57.00 -30.00   97
  4  ω     50.00  86.00   1.00    6.00    --  112.00 -94.00-180.00   36
  5  ω     42.00 108.00   1.00    6.00    --  112.00 -94.00 -60.00   66
  6  ω     84.00 174.00   1.00    6.00    --  112.00  30.00 120.00   90
  7  ω     44.00 130.00   1.00    6.00    --  112.00 -30.00 150.00   86
  8  ω     86.00 178.00   1.00    6.00    --  112.00  30.00-150.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0898172000
_diffrn_orient_matrix_UB_12      -0.0005087000
_diffrn_orient_matrix_UB_13      0.1085080000
_diffrn_orient_matrix_UB_21      0.1040878000
_diffrn_orient_matrix_UB_22      -0.0317260000
_diffrn_orient_matrix_UB_23      -0.0701700000
_diffrn_orient_matrix_UB_31      0.0429603000
_diffrn_orient_matrix_UB_32      0.0778391000
_diffrn_orient_matrix_UB_33      -0.0280311000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4025
_reflns_number_total             4641
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2008 (Burla et al., 2007)'
_refine_diff_density_max         2.037
_refine_diff_density_min         -2.700
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4641
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0571
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²+8.1524P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1369
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Zn1 Zn 0.5000 1.0000 0.0000 0.0733(5) Uani 1 2 d S T P . .
S1 S 0.32169(11) 1.09421(6) 0.08900(8) 0.0364(3) Uani 1 1 d . . . . .
S2 S 0.29152(9) 0.94554(5) -0.14376(8) 0.0294(2) Uani 1 1 d . . . . .
S3 S 0.52688(8) 1.07550(6) -0.15107(7) 0.0308(2) Uani 1 1 d . . . . .
P1 P 0.33712(8) 1.16195(5) -0.03976(7) 0.0224(2) Uani 1 1 d . . . . .
P2 P 0.25993(8) 1.03942(5) -0.22190(7) 0.02006(19) Uani 1 1 d . . . . .
C1 C 0.4700(3) 1.2230(2) -0.0162(3) 0.0234(7) Uani 1 1 d . . . . .
C2 C 0.5309(4) 1.2248(2) 0.0915(3) 0.0307(8) Uani 1 1 d . . . . .
H2 H 0.5057 1.1940 0.1490 0.037 Uiso 1 1 calc R . . . .
C3 C 0.6301(4) 1.2725(3) 0.1140(4) 0.0433(11) Uani 1 1 d . . . . .
H3 H 0.6697 1.2745 0.1873 0.052 Uiso 1 1 calc R . . . .
C4 C 0.6700(4) 1.3168(2) 0.0288(4) 0.0375(10) Uani 1 1 d . . . . .
H4 H 0.7360 1.3490 0.0447 0.045 Uiso 1 1 calc R . . . .
C5 C 0.6129(4) 1.3136(2) -0.0797(5) 0.0409(10) Uani 1 1 d . . . . .
H5 H 0.6410 1.3430 -0.1377 0.049 Uiso 1 1 calc R . . . .
C6 C 0.5126(4) 1.2663(3) -0.1031(4) 0.0385(10) Uani 1 1 d . . . . .
H6 H 0.4742 1.2638 -0.1768 0.046 Uiso 1 1 calc R . . . .
C7 C 0.2009(4) 1.2208(2) -0.0638(4) 0.0330(9) Uani 1 1 d . . . . .
C8 C 0.2003(4) 1.2789(2) -0.1411(5) 0.0464(12) Uani 1 1 d . . . . .
H8 H 0.2706 1.2884 -0.1813 0.056 Uiso 1 1 calc R . . . .
C9 C 0.0951(4) 1.3227(3) -0.1582(7) 0.0625(18) Uani 1 1 d . . . . .
H9 H 0.0952 1.3615 -0.2096 0.075 Uiso 1 1 calc R . . . .
C10 C -0.0093(5) 1.3088(3) -0.0995(7) 0.070(2) Uani 1 1 d . . . . .
H10 H -0.0793 1.3385 -0.1108 0.084 Uiso 1 1 calc R . . . .
C11 C -0.0105(4) 1.2506(4) -0.0235(5) 0.0599(18) Uani 1 1 d . . . . .
H11 H -0.0823 1.2407 0.0143 0.072 Uiso 1 1 calc R . . . .
C12 C 0.0954(4) 1.2068(3) -0.0036(4) 0.0446(12) Uani 1 1 d . . . . .
H12 H 0.0954 1.1687 0.0492 0.054 Uiso 1 1 calc R . . . .
C13 C 0.1010(3) 1.07169(18) -0.2104(3) 0.0177(6) Uani 1 1 d . . . . .
C14 C 0.0599(3) 1.13364(18) -0.2715(3) 0.0200(6) Uani 1 1 d . . . . .
H14 H 0.1128 1.1576 -0.3192 0.024 Uiso 1 1 calc R . . . .
C15 C -0.0606(3) 1.1591(2) -0.2603(3) 0.0223(7) Uani 1 1 d . . . . .
H15 H -0.0881 1.2007 -0.2999 0.027 Uiso 1 1 calc R . . . .
C16 C -0.1403(3) 1.1230(2) -0.1908(3) 0.0247(7) Uani 1 1 d . . . . .
H16 H -0.2207 1.1407 -0.1834 0.030 Uiso 1 1 calc R . . . .
C17 C -0.1005(3) 1.0608(2) -0.1322(3) 0.0243(7) Uani 1 1 d . . . . .
H17 H -0.1547 1.0362 -0.0866 0.029 Uiso 1 1 calc R . . . .
C18 C 0.0209(3) 1.03476(19) -0.1413(3) 0.0221(7) Uani 1 1 d . . . . .
H18 H 0.0480 0.9931 -0.1015 0.027 Uiso 1 1 calc R . . . .
C19 C 0.2721(3) 1.03460(19) -0.3763(3) 0.0198(6) Uani 1 1 d . . . . .
C20 C 0.1747(3) 0.9997(2) -0.4393(3) 0.0243(7) Uani 1 1 d . . . . .
H20 H 0.1071 0.9818 -0.4019 0.029 Uiso 1 1 calc R . . . .
C21 C 0.1778(3) 0.9913(2) -0.5569(3) 0.0263(7) Uani 1 1 d . . . . .
H21 H 0.1122 0.9683 -0.5985 0.032 Uiso 1 1 calc R . . . .
C22 C 0.2793(4) 1.0175(2) -0.6127(3) 0.0260(7) Uani 1 1 d . . . . .
H22 H 0.2819 1.0117 -0.6916 0.031 Uiso 1 1 calc R . . . .
C23 C 0.3757(4) 1.0520(2) -0.5515(3) 0.0269(7) Uani 1 1 d . . . . .
H23 H 0.4434 1.0694 -0.5893 0.032 Uiso 1 1 calc R . . . .
C24 C 0.3730(3) 1.0613(2) -0.4331(3) 0.0251(7) Uani 1 1 d . . . . .
H24 H 0.4382 1.0851 -0.3922 0.030 Uiso 1 1 calc R . . . .
C25 C 0.3702(3) 1.1128(2) -0.1729(3) 0.0236(7) Uani 1 1 d . . . . .
H25 H 0.3714 1.1490 -0.2347 0.028 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 S1 2.8242(11) . ?
Zn1 S1 2.8241(11) 3_675 ?
Zn1 S2 2.8844(10) . ?
Zn1 S3 2.2742(10) . ?
Zn1 S3 2.2742(10) 3_675 ?
S1 P1 1.9643(13) . ?
S2 P2 1.9662(13) . ?
S3 C25 1.816(4) . ?
P1 C1 1.818(4) . ?
P1 C7 1.822(4) . ?
P1 C25 1.850(4) . ?
P2 C13 1.818(3) . ?
P2 C19 1.817(3) . ?
P2 C25 1.856(4) . ?
C1 C2 1.378(5) . ?
C1 C6 1.389(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.390(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.374(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.371(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.395(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.396(7) . ?
C7 C12 1.394(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.389(7) . ?
C9 H9 0.9300 . ?
C9 C10 1.373(9) . ?
C10 H10 0.9300 . ?
C10 C11 1.388(10) . ?
C11 H11 0.9300 . ?
C11 C12 1.398(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.397(5) . ?
C13 C18 1.391(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.389(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.384(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.383(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.397(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.393(5) . ?
C19 C24 1.393(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.384(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.390(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.371(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.395(5) . ?
C24 H24 0.9300 . ?
C25 H25 0.9800 . ?

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
S1 Zn1 S1 180.0 3_675 . ?
S1 Zn1 S2 84.70(3) . . ?
S1 Zn1 S2 95.30(3) 3_675 . ?
S3 Zn1 S1 92.08(3) 3_675 3_675 ?
S3 Zn1 S1 87.92(3) 3_675 . ?
S3 Zn1 S1 87.92(3) . 3_675 ?
S3 Zn1 S1 92.08(3) . . ?
S3 Zn1 S2 83.82(3) . . ?
S3 Zn1 S2 96.18(3) 3_675 . ?
S3 Zn1 S3 180.0 3_675 . ?
P1 S1 Zn1 90.69(4) . . ?
P2 S2 Zn1 94.05(4) . . ?
C25 S3 Zn1 100.05(12) . . ?
C1 P1 S1 112.17(13) . . ?
C1 P1 C7 105.77(17) . . ?
C1 P1 C25 103.59(16) . . ?
C7 P1 S1 112.63(15) . . ?
C7 P1 C25 110.77(17) . . ?
C25 P1 S1 111.41(13) . . ?
C13 P2 S2 112.62(12) . . ?
C13 P2 C25 108.85(16) . . ?
C19 P2 S2 113.33(12) . . ?
C19 P2 C13 102.57(15) . . ?
C19 P2 C25 104.78(16) . . ?
C25 P2 S2 113.82(13) . . ?
C2 C1 P1 118.2(3) . . ?
C2 C1 C6 119.6(3) . . ?
C6 C1 P1 122.2(3) . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 119.9(4) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.4(4) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0(4) . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C5 119.9(4) . . ?
C1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C8 C7 P1 121.4(3) . . ?
C12 C7 P1 118.9(4) . . ?
C12 C7 C8 119.7(4) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.2(5) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.1(6) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 119.9 . . ?
C9 C10 C11 120.3(5) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.4(5) . . ?
C12 C11 H11 119.8 . . ?
C7 C12 C11 119.2(6) . . ?
C7 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C14 C13 P2 119.5(2) . . ?
C18 C13 P2 120.1(3) . . ?
C18 C13 C14 120.4(3) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 119.3(3) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.6(3) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.1(3) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.2(3) . . ?
C18 C17 H17 119.9 . . ?
C13 C18 C17 119.5(3) . . ?
C13 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 P2 116.4(3) . . ?
C20 C19 C24 119.3(3) . . ?
C24 C19 P2 124.3(3) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.6(3) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 120.1 . . ?
C20 C21 C22 119.7(3) . . ?
C22 C21 H21 120.1 . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.2(3) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 119.7 . . ?
C22 C23 C24 120.5(3) . . ?
C24 C23 H23 119.7 . . ?
C19 C24 C23 119.7(3) . . ?
C19 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
S3 C25 P1 106.98(17) . . ?
S3 C25 P2 109.6(2) . . ?
S3 C25 H25 107.5 . . ?
P1 C25 P2 117.28(18) . . ?
P1 C25 H25 107.5 . . ?
P2 C25 H25 107.5 . . ?

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
Zn1 S3 C25 P1 61.69(18) . . . . ?
Zn1 S3 C25 P2 -66.44(17) . . . . ?
S1 P1 C1 C2 -10.6(4) . . . . ?
S1 P1 C1 C6 168.3(3) . . . . ?
S1 P1 C7 C8 171.5(3) . . . . ?
S1 P1 C7 C12 -8.8(3) . . . . ?
S1 P1 C25 S3 -68.38(19) . . . . ?
S1 P1 C25 P2 55.1(2) . . . . ?
S2 P2 C13 C14 -173.3(2) . . . . ?
S2 P2 C13 C18 6.6(3) . . . . ?
S2 P2 C19 C20 73.5(3) . . . . ?
S2 P2 C19 C24 -104.4(3) . . . . ?
S2 P2 C25 S3 40.1(2) . . . . ?
S2 P2 C25 P1 -82.1(2) . . . . ?
P1 C1 C2 C3 -177.7(3) . . . . ?
P1 C1 C6 C5 178.3(3) . . . . ?
P1 C7 C8 C9 179.7(4) . . . . ?
P1 C7 C12 C11 -178.5(3) . . . . ?
P2 C13 C14 C15 -178.5(3) . . . . ?
P2 C13 C18 C17 179.2(3) . . . . ?
P2 C19 C20 C21 -177.9(3) . . . . ?
P2 C19 C24 C23 177.3(3) . . . . ?
C1 P1 C7 C8 48.7(4) . . . . ?
C1 P1 C7 C12 -131.6(3) . . . . ?
C1 P1 C25 S3 52.4(2) . . . . ?
C1 P1 C25 P2 175.9(2) . . . . ?
C1 C2 C3 C4 -1.6(7) . . . . ?
C2 C1 C6 C5 -2.8(7) . . . . ?
C2 C3 C4 C5 -0.6(7) . . . . ?
C3 C4 C5 C6 1.1(7) . . . . ?
C4 C5 C6 C1 0.6(7) . . . . ?
C6 C1 C2 C3 3.4(6) . . . . ?
C7 P1 C1 C2 112.5(3) . . . . ?
C7 P1 C1 C6 -68.6(4) . . . . ?
C7 P1 C25 S3 165.41(19) . . . . ?
C7 P1 C25 P2 -71.1(3) . . . . ?
C7 C8 C9 C10 -0.3(8) . . . . ?
C8 C7 C12 C11 1.2(6) . . . . ?
C8 C9 C10 C11 -0.5(8) . . . . ?
C9 C10 C11 C12 1.7(8) . . . . ?
C10 C11 C12 C7 -2.1(7) . . . . ?
C12 C7 C8 C9 0.0(7) . . . . ?
C13 P2 C19 C20 -48.1(3) . . . . ?
C13 P2 C19 C24 133.9(3) . . . . ?
C13 P2 C25 S3 166.59(16) . . . . ?
C13 P2 C25 P1 44.4(2) . . . . ?
C13 C14 C15 C16 -0.9(5) . . . . ?
C14 C13 C18 C17 -0.9(5) . . . . ?
C14 C15 C16 C17 -0.4(5) . . . . ?
C15 C16 C17 C18 1.1(5) . . . . ?
C16 C17 C18 C13 -0.5(5) . . . . ?
C18 C13 C14 C15 1.6(5) . . . . ?
C19 P2 C13 C14 -51.1(3) . . . . ?
C19 P2 C13 C18 128.8(3) . . . . ?
C19 P2 C25 S3 -84.3(2) . . . . ?
C19 P2 C25 P1 153.6(2) . . . . ?
C19 C20 C21 C22 0.5(6) . . . . ?
C20 C19 C24 C23 -0.6(5) . . . . ?
C20 C21 C22 C23 -0.5(6) . . . . ?
C21 C22 C23 C24 -0.1(6) . . . . ?
C22 C23 C24 C19 0.6(6) . . . . ?
C24 C19 C20 C21 0.1(5) . . . . ?
C25 P1 C1 C2 -130.9(3) . . . . ?
C25 P1 C1 C6 48.0(4) . . . . ?
C25 P1 C7 C8 -62.9(4) . . . . ?
C25 P1 C7 C12 116.8(3) . . . . ?
C25 P2 C13 C14 59.5(3) . . . . ?
C25 P2 C13 C18 -120.6(3) . . . . ?
C25 P2 C19 C20 -161.8(3) . . . . ?
C25 P2 C19 C24 20.3(4) . . . . ?

_shelx_SHELXL_version_number     2014/7

_ins_header                      
;
TITL jk1605_a in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  10.724557  18.326010  11.669916  90.0000  93.7455  90.0000
ZERR    2.00   0.000173   0.000346   0.000206   0.0000   0.0016   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H P S Zn
UNIT 100.00 84.00 8.00 12.00 2.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.382
_oxdiff_exptl_absorpt_empirical_full_min 0.665
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'CH2Cl2, Et2O'
_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Hygroscopic'
