# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_L1
_database_code_depnum_ccdc_archive 'CCDC 1582379'
_audit_update_record             
;
2017-10-26 deposited with the CCDC.
2017-12-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          '479-481  '
_chemical_formula_moiety         'C27 H30 N7 O P'
_chemical_formula_sum            'C27 H30 N7 O P'
_chemical_formula_weight         499.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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                   8.3136(3)
_cell_length_b                   11.9294(3)
_cell_length_c                   13.9717(4)
_cell_angle_alpha                112.525(2)
_cell_angle_beta                 99.453(2)
_cell_angle_gamma                90.041(2)
_cell_volume                     1259.49(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    130.05(10)
_cell_measurement_reflns_used    10758
_cell_measurement_theta_min      3.0000
_cell_measurement_theta_max      37.2380

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_F_000             528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4000
_exptl_crystal_size_mid          0.3000
_exptl_crystal_size_min          0.2500
_exptl_absorpt_coefficient_mu    0.144
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98200
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      130.05(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 6.3560
_diffrn_reflns_number            19851
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.490
_diffrn_reflns_theta_max         25.495
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4681
_reflns_number_gt                4272
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0470P)²+0.6727P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4681
_refine_ls_number_parameters     333
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0988
_refine_ls_wR_factor_gt          0.0961
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
C2 C 0.53491(17) 1.24416(13) 0.54436(11) 0.0192(3) Uani 1 1 d . . . . .
C4 C 0.68255(16) 1.07816(12) 0.51418(11) 0.0175(3) Uani 1 1 d . . . . .
C5 C 0.67436(17) 1.06243(12) 0.40978(11) 0.0187(3) Uani 1 1 d . . . . .
H5 H 0.7205 0.9980 0.3628 0.022 Uiso 1 1 calc R U . . .
C6 C 0.59371(17) 1.14801(12) 0.37974(11) 0.0180(3) Uani 1 1 d . . . . .
C7 C 0.45674(19) 1.34594(13) 0.61914(12) 0.0242(3) Uani 1 1 d . . . . .
H7A H 0.4692 1.3382 0.6858 0.036 Uiso 1 1 calc R U . . .
H7B H 0.3426 1.3426 0.5911 0.036 Uiso 1 1 calc R U . . .
H7C H 0.5083 1.4223 0.6284 0.036 Uiso 1 1 calc R U . . .
C8 C 0.7886(2) 1.01880(14) 0.66391(11) 0.0252(3) Uani 1 1 d . . . . .
H8A H 0.7516 0.9454 0.6691 0.038 Uiso 1 1 calc R U . . .
H8B H 0.7257 1.0842 0.6999 0.038 Uiso 1 1 calc R U . . .
H8C H 0.9020 1.0382 0.6955 0.038 Uiso 1 1 calc R U . . .
C9 C 0.5571(2) 1.25033(14) 0.25303(12) 0.0262(3) Uani 1 1 d . . . . .
H9A H 0.6538 1.2735 0.2338 0.039 Uiso 1 1 calc R U . . .
H9B H 0.5319 1.3161 0.3134 0.039 Uiso 1 1 calc R U . . .
H9C H 0.4674 1.2318 0.1953 0.039 Uiso 1 1 calc R U . . .
C10 C 0.92140(17) 0.83643(13) 0.51440(11) 0.0196(3) Uani 1 1 d . . . . .
H10 H 0.9411 0.8475 0.5850 0.023 Uiso 1 1 calc R U . . .
C11 C 0.98885(17) 0.73563(12) 0.43652(11) 0.0189(3) Uani 1 1 d . . . . .
C12 C 0.96473(18) 0.71586(13) 0.33012(12) 0.0224(3) Uani 1 1 d . . . . .
H12 H 0.9040 0.7674 0.3049 0.027 Uiso 1 1 calc R U . . .
C13 C 1.03276(19) 0.61837(14) 0.26326(12) 0.0250(3) Uani 1 1 d . . . . .
H13 H 1.0185 0.6030 0.1918 0.030 Uiso 1 1 calc R U . . .
C14 C 1.12288(18) 0.54288(13) 0.30291(12) 0.0239(3) Uani 1 1 d . . . . .
H14 H 1.1710 0.4771 0.2590 0.029 Uiso 1 1 calc R U . . .
C15 C 1.13946(17) 0.56795(13) 0.40958(12) 0.0207(3) Uani 1 1 d . . . . .
C16 C 1.23090(19) 0.49078(13) 0.46036(13) 0.0254(3) Uani 1 1 d . . . . .
H16A H 1.3101 0.5418 0.5209 0.030 Uiso 1 1 calc R U . . .
H16B H 1.1552 0.4502 0.4846 0.030 Uiso 1 1 calc R U . . .
C18 C 0.66174(18) 1.04009(13) 0.11923(11) 0.0217(3) Uani 1 1 d . . . . .
H18 H 0.6254 1.1019 0.0978 0.026 Uiso 1 1 calc R U . . .
C19 C 0.73358(18) 0.93750(13) 0.05001(11) 0.0219(3) Uani 1 1 d . . . . .
C20 C 0.78770(18) 0.93092(14) -0.03861(11) 0.0235(3) Uani 1 1 d . . . . .
C21 C 0.86456(19) 0.81748(15) -0.08928(12) 0.0272(3) Uani 1 1 d . . . . .
C22 C 0.8603(2) 0.73930(15) -0.04103(13) 0.0298(4) Uani 1 1 d . . . . .
H22 H 0.8923 0.6601 -0.0677 0.036 Uiso 1 1 calc R U . . .
C23 C 0.7744(2) 1.02699(15) -0.08365(12) 0.0292(4) Uani 1 1 d . . . . .
H23A H 0.6956 0.9988 -0.1478 0.044 Uiso 1 1 calc R U . . .
H23B H 0.8789 1.0437 -0.0980 0.044 Uiso 1 1 calc R U . . .
H23C H 0.7402 1.0999 -0.0340 0.044 Uiso 1 1 calc R U . . .
C24 C 0.9419(2) 0.79655(17) -0.18391(14) 0.0373(4) Uani 1 1 d . . . . .
H24A H 1.0051 0.7266 -0.1969 0.056 Uiso 1 1 calc R U . . .
H24B H 1.0119 0.8666 -0.1713 0.056 Uiso 1 1 calc R U . . .
H24C H 0.8581 0.7830 -0.2441 0.056 Uiso 1 1 calc R U . . .
C25 C 0.5845(2) 0.72592(14) 0.05655(12) 0.0259(3) Uani 1 1 d . . . . .
C26 C 0.5093(2) 0.64470(15) -0.04287(13) 0.0310(4) Uani 1 1 d . . . . .
H26 H 0.5614 0.6288 -0.1003 0.037 Uiso 1 1 calc R U . . .
C27 C 0.3573(2) 0.58762(16) -0.05658(14) 0.0370(4) Uani 1 1 d . . . . .
H27 H 0.3074 0.5339 -0.1232 0.044 Uiso 1 1 calc R U . . .
C28 C 0.2794(2) 0.61044(16) 0.02869(15) 0.0372(4) Uani 1 1 d . . . . .
H28 H 0.1770 0.5724 0.0193 0.045 Uiso 1 1 calc R U . . .
C29 C 0.3538(2) 0.68970(15) 0.12773(14) 0.0349(4) Uani 1 1 d . . . . .
H29 H 0.3018 0.7047 0.1851 0.042 Uiso 1 1 calc R U . . .
C30 C 0.5053(2) 0.74667(14) 0.14171(13) 0.0305(4) Uani 1 1 d . . . . .
H30 H 0.5552 0.7995 0.2087 0.037 Uiso 1 1 calc R U . . .
N1 N 1.07463(14) 0.66279(11) 0.47604(10) 0.0201(3) Uani 1 1 d . . . . .
N2 N 0.83475(14) 0.90903(10) 0.48357(9) 0.0190(3) Uani 1 1 d . . . . .
N3 N 0.76824(15) 1.00152(11) 0.55408(9) 0.0203(3) Uani 1 1 d . . . . .
N4 N 0.61366(14) 1.16907(10) 0.58279(9) 0.0192(3) Uani 1 1 d . . . . .
N5 N 0.52005(14) 1.23883(10) 0.44556(9) 0.0192(3) Uani 1 1 d . . . . .
N6 N 0.58482(15) 1.14386(11) 0.27816(9) 0.0216(3) Uani 1 1 d . . . . .
N7 N 0.64861(15) 1.04486(11) 0.21121(9) 0.0211(3) Uani 1 1 d . . . . .
O1 O 1.31127(18) 0.40403(12) 0.38803(10) 0.0468(4) Uani 1 1 d . . . . .
H1 H 1.361(3) 0.357(2) 0.416(2) 0.070 Uiso 1 1 d . U . . .
P1 P 0.78565(5) 0.80549(4) 0.08054(3) 0.02563(12) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 N4 1.3317(18) . ?
C2 N5 1.3421(18) . ?
C2 C7 1.4968(19) . ?
C4 N4 1.3446(18) . ?
C4 N3 1.3840(17) . ?
C4 C5 1.3875(19) . ?
C5 C6 1.3802(19) . ?
C5 H5 0.9300 . ?
C6 N5 1.3481(18) . ?
C6 N6 1.3906(18) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N3 1.4484(18) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N6 1.4509(18) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 N2 1.2804(18) . ?
C10 C11 1.464(2) . ?
C10 H10 0.9300 . ?
C11 N1 1.3445(18) . ?
C11 C12 1.393(2) . ?
C12 C13 1.374(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.388(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.386(2) . ?
C14 H14 0.9300 . ?
C15 N1 1.3391(18) . ?
C15 C16 1.501(2) . ?
C16 O1 1.4000(19) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C18 N7 1.2871(19) . ?
C18 C19 1.440(2) . ?
C18 H18 0.9300 . ?
C19 C20 1.360(2) . ?
C19 P1 1.8178(15) . ?
C20 C21 1.469(2) . ?
C20 C23 1.500(2) . ?
C21 C22 1.347(2) . ?
C21 C24 1.500(2) . ?
C22 P1 1.7923(16) . ?
C22 H22 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C30 1.393(2) . ?
C25 C26 1.394(2) . ?
C25 P1 1.8385(17) . ?
C26 C27 1.384(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.385(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.381(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.379(2) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
N2 N3 1.3567(16) . ?
N6 N7 1.3668(17) . ?
O1 H1 0.87(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 C2 N5 126.63(13) . . ?
N4 C2 C7 116.82(12) . . ?
N5 C2 C7 116.54(12) . . ?
N4 C4 N3 116.20(12) . . ?
N4 C4 C5 122.94(12) . . ?
N3 C4 C5 120.83(12) . . ?
C6 C5 C4 116.06(13) . . ?
C6 C5 H5 122.0 . . ?
C4 C5 H5 122.0 . . ?
N5 C6 C5 122.70(13) . . ?
N5 C6 N6 116.58(12) . . ?
C5 C6 N6 120.72(13) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N6 C9 H9A 109.5 . . ?
N6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C11 118.84(13) . . ?
N2 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
N1 C11 C12 122.71(13) . . ?
N1 C11 C10 114.42(12) . . ?
C12 C11 C10 122.87(13) . . ?
C13 C12 C11 118.41(13) . . ?
C13 C12 H12 120.8 . . ?
C11 C12 H12 120.8 . . ?
C12 C13 C14 119.63(14) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 118.38(14) . . ?
C15 C14 H14 120.8 . . ?
C13 C14 H14 120.8 . . ?
N1 C15 C14 122.85(13) . . ?
N1 C15 C16 114.28(13) . . ?
C14 C15 C16 122.87(13) . . ?
O1 C16 C15 109.97(13) . . ?
O1 C16 H16A 109.7 . . ?
C15 C16 H16A 109.7 . . ?
O1 C16 H16B 109.7 . . ?
C15 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
N7 C18 C19 118.97(13) . . ?
N7 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C20 C19 C18 125.81(14) . . ?
C20 C19 P1 111.02(11) . . ?
C18 C19 P1 122.80(11) . . ?
C19 C20 C21 113.29(14) . . ?
C19 C20 C23 125.59(14) . . ?
C21 C20 C23 121.13(13) . . ?
C22 C21 C20 113.35(14) . . ?
C22 C21 C24 125.30(15) . . ?
C20 C21 C24 121.33(15) . . ?
C21 C22 P1 112.19(12) . . ?
C21 C22 H22 123.9 . . ?
P1 C22 H22 123.9 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 118.82(15) . . ?
C30 C25 P1 118.48(12) . . ?
C26 C25 P1 122.70(13) . . ?
C27 C26 C25 120.30(16) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C28 120.13(16) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C29 C28 C27 119.98(17) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C30 C29 C28 120.05(16) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C25 120.70(16) . . ?
C29 C30 H30 119.6 . . ?
C25 C30 H30 119.6 . . ?
C15 N1 C11 118.02(12) . . ?
C10 N2 N3 119.79(12) . . ?
N2 N3 C4 115.54(11) . . ?
N2 N3 C8 121.65(11) . . ?
C4 N3 C8 122.81(12) . . ?
C2 N4 C4 115.80(12) . . ?
C2 N5 C6 115.80(12) . . ?
N7 N6 C6 114.87(11) . . ?
N7 N6 C9 120.38(12) . . ?
C6 N6 C9 122.31(12) . . ?
C18 N7 N6 119.05(12) . . ?
C16 O1 H1 110.5(17) . . ?
C22 P1 C19 89.47(7) . . ?
C22 P1 C25 105.32(7) . . ?
C19 P1 C25 102.44(7) . . ?

_refine_diff_density_max         0.408
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.041

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'Vapour deposition'
_chemical_properties_physical    Heat-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_L1Zn
_database_code_depnum_ccdc_archive 'CCDC 1582380'
_audit_update_record             
;
2017-10-26 deposited with the CCDC.
2017-12-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H30 F6 N7 O7 P1 S2 Zn1'
_chemical_formula_sum            'C29 H30 F6 N7 O7 P1 S2 Zn1'
_chemical_formula_weight         863.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   20.0495(4)
_cell_length_b                   20.1730(4)
_cell_length_c                   17.8536(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.526(2)
_cell_angle_gamma                90
_cell_volume                     7020.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    130.05(10)
_cell_measurement_reflns_used    8461
_cell_measurement_theta_min      2.5300
_cell_measurement_theta_max      28.8780

_exptl_crystal_description       irregular
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_F_000             3520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.953
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      130.05(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3560
_diffrn_reflns_number            26577
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.019
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6545
_reflns_number_gt                5095
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0525P)²+9.4884P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6545
_refine_ls_number_parameters     486
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.1089
_refine_ls_wR_factor_gt          0.0942
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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
C2 C 0.34093(14) -0.01927(14) 0.22437(18) 0.0228(6) Uani 1 1 d . . . . .
C4 C 0.25397(14) 0.01510(14) 0.12350(17) 0.0200(6) Uani 1 1 d . . . . .
C5 C 0.23714(14) -0.04914(14) 0.10402(17) 0.0228(6) Uani 1 1 d . . . . .
H5 H 0.2012 -0.0598 0.0625 0.027 Uiso 1 1 calc R U . . .
C6 C 0.27607(14) -0.09777(14) 0.14903(17) 0.0214(6) Uani 1 1 d . . . . .
C7 C 0.39775(16) -0.00103(15) 0.29101(19) 0.0321(8) Uani 1 1 d . . . . .
H7A H 0.4219 -0.0403 0.3123 0.048 Uiso 1 1 calc R U . . .
H7B H 0.3792 0.0205 0.3296 0.048 Uiso 1 1 calc R U . . .
H7C H 0.4288 0.0285 0.2741 0.048 Uiso 1 1 calc R U . . .
C8 C 0.16811(16) 0.06128(15) 0.00911(18) 0.0289(7) Uani 1 1 d . . . . .
H8A H 0.1234 0.0700 0.0175 0.043 Uiso 1 1 calc R U . . .
H8B H 0.1695 0.0170 -0.0102 0.043 Uiso 1 1 calc R U . . .
H8C H 0.1777 0.0923 -0.0277 0.043 Uiso 1 1 calc R U . . .
C9 C 0.30530(15) -0.21724(14) 0.17400(19) 0.0276(7) Uani 1 1 d . . . . .
H9A H 0.3428 -0.1990 0.2120 0.041 Uiso 1 1 calc R U . . .
H9B H 0.3230 -0.2421 0.1370 0.041 Uiso 1 1 calc R U . . .
H9C H 0.2787 -0.2459 0.1986 0.041 Uiso 1 1 calc R U . . .
C10 C 0.21165(15) 0.18415(14) 0.08381(18) 0.0249(7) Uani 1 1 d . . . . .
H10 H 0.1753 0.1874 0.0408 0.030 Uiso 1 1 calc R U . . .
C11 C 0.24391(15) 0.24209(14) 0.12687(18) 0.0243(7) Uani 1 1 d . . . . .
C12 C 0.22211(17) 0.30678(15) 0.1109(2) 0.0328(8) Uani 1 1 d . . . . .
H12 H 0.1850 0.3162 0.0702 0.039 Uiso 1 1 calc R U . . .
C13 C 0.25668(17) 0.35702(15) 0.1565(2) 0.0337(8) Uani 1 1 d . . . . .
H13 H 0.2429 0.4008 0.1468 0.040 Uiso 1 1 calc R U . . .
C14 C 0.31196(16) 0.34209(15) 0.21686(19) 0.0294(7) Uani 1 1 d . . . . .
H14 H 0.3354 0.3755 0.2481 0.035 Uiso 1 1 calc R U . . .
C15 C 0.33168(15) 0.27605(15) 0.22974(18) 0.0246(7) Uani 1 1 d . . . . .
C16 C 0.39174(15) 0.25332(15) 0.29036(18) 0.0283(7) Uani 1 1 d . . . . .
H16A H 0.4336 0.2592 0.2728 0.034 Uiso 1 1 calc R U . . .
H16B H 0.3953 0.2792 0.3369 0.034 Uiso 1 1 calc R U . . .
C18 C 0.18453(15) -0.23450(15) 0.05863(19) 0.0269(7) Uani 1 1 d . . . . .
H18 H 0.2103 -0.2710 0.0801 0.032 Uiso 1 1 calc R U . . .
C19 C 0.12160(15) -0.24176(15) 0.00068(18) 0.0273(7) Uani 1 1 d . . . . .
C20 C 0.09462(16) -0.29920(16) -0.03331(19) 0.0310(7) Uani 1 1 d . . . . .
C21 C 0.03148(18) -0.28947(18) -0.0942(2) 0.0373(8) Uani 1 1 d . . . . .
C22 C 0.01155(18) -0.22605(19) -0.1024(2) 0.0403(9) Uani 1 1 d . . . . .
H22 H -0.0295 -0.2123 -0.1348 0.048 Uiso 1 1 calc R U . . .
C23 C 0.12355(19) -0.36741(16) -0.0137(2) 0.0396(9) Uani 1 1 d . . . . .
H23A H 0.1688 -0.3639 0.0191 0.059 Uiso 1 1 calc R U . . .
H23B H 0.1258 -0.3903 -0.0601 0.059 Uiso 1 1 calc R U . . .
H23C H 0.0945 -0.3915 0.0125 0.059 Uiso 1 1 calc R U . . .
C24 C -0.0030(2) -0.3466(2) -0.1405(2) 0.0544(11) Uani 1 1 d . . . . .
H24A H -0.0441 -0.3316 -0.1756 0.082 Uiso 1 1 calc R U . . .
H24B H -0.0146 -0.3795 -0.1067 0.082 Uiso 1 1 calc R U . . .
H24C H 0.0273 -0.3657 -0.1690 0.082 Uiso 1 1 calc R U . . .
C25 C 0.02796(15) -0.14382(15) 0.02955(19) 0.0296(7) Uani 1 1 d . . . . .
C26 C -0.01844(16) -0.18469(16) 0.05484(19) 0.0311(7) Uani 1 1 d . . . . .
H26 H -0.0281 -0.2265 0.0332 0.037 Uiso 1 1 calc R U . . .
C27 C -0.05028(17) -0.16403(18) 0.1115(2) 0.0357(8) Uani 1 1 d . . . . .
H27 H -0.0810 -0.1919 0.1278 0.043 Uiso 1 1 calc R U . . .
C28 C -0.03654(17) -0.1022(2) 0.1440(2) 0.0428(9) Uani 1 1 d . . . . .
H28 H -0.0579 -0.0885 0.1823 0.051 Uiso 1 1 calc R U . . .
C29 C 0.00857(19) -0.0608(2) 0.1201(3) 0.0532(11) Uani 1 1 d . . . . .
H29 H 0.0179 -0.0190 0.1421 0.064 Uiso 1 1 calc R U . . .
C30 C 0.04031(18) -0.08151(18) 0.0628(3) 0.0488(11) Uani 1 1 d . . . . .
H30 H 0.0705 -0.0530 0.0464 0.059 Uiso 1 1 calc R U . . .
C31 C 0.12577(19) 0.09067(19) 0.2665(2) 0.0412(9) Uani 1 1 d . . . . .
C32 C 0.41248(18) 0.05840(19) 0.0477(2) 0.0400(9) Uani 1 1 d . . . . .
N1 N 0.29737(12) 0.22808(12) 0.18566(15) 0.0235(6) Uani 1 1 d . . . . .
N2 N 0.23795(12) 0.12829(11) 0.11062(14) 0.0219(5) Uani 1 1 d . . . . .
N3 N 0.21915(12) 0.06813(11) 0.08139(15) 0.0236(6) Uani 1 1 d . . . . .
N4 N 0.30562(11) 0.03135(11) 0.18482(14) 0.0208(5) Uani 1 1 d . . . . .
N5 N 0.32953(12) -0.08301(12) 0.20923(15) 0.0238(6) Uani 1 1 d . . . . .
N6 N 0.26193(12) -0.16354(12) 0.13489(14) 0.0232(5) Uani 1 1 d . . . . .
N7 N 0.20335(12) -0.17490(12) 0.07926(15) 0.0256(6) Uani 1 1 d . . . . .
O1 O 0.38254(11) 0.18498(11) 0.30591(13) 0.0292(5) Uani 1 1 d . . . . .
H1 H 0.4150(18) 0.1703(17) 0.337(2) 0.035 Uiso 1 1 d . U . . .
O11 O 0.25241(11) 0.12310(10) 0.28975(14) 0.0330(5) Uani 1 1 d . . . . .
O12 O 0.21060(13) 0.09072(18) 0.40022(16) 0.0663(9) Uani 1 1 d . . . . .
O13 O 0.22518(18) 0.00804(13) 0.3062(2) 0.0840(12) Uani 1 1 d . . . . .
O21 O 0.41419(10) 0.12538(10) 0.17208(13) 0.0299(5) Uani 1 1 d . . . . .
O22 O 0.38399(12) 0.18318(12) 0.05062(15) 0.0456(7) Uani 1 1 d . . . . .
O23 O 0.50124(11) 0.14653(12) 0.10232(14) 0.0383(6) Uani 1 1 d . . . . .
F11 F 0.12160(12) 0.07760(14) 0.19260(14) 0.0705(8) Uani 1 1 d . . . . .
F12 F 0.08092(12) 0.05222(12) 0.28948(16) 0.0669(7) Uani 1 1 d . . . . .
F13 F 0.10708(10) 0.15234(11) 0.27183(13) 0.0520(6) Uani 1 1 d . . . . .
F21 F 0.43664(13) 0.05726(14) -0.01385(15) 0.0769(9) Uani 1 1 d . . . . .
F22 F 0.44170(13) 0.00934(11) 0.09424(17) 0.0701(8) Uani 1 1 d . . . . .
F23 F 0.34583(10) 0.04566(11) 0.02624(12) 0.0503(6) Uani 1 1 d . . . . .
P1 P 0.07248(4) -0.17012(4) -0.04431(5) 0.0327(2) Uani 1 1 d . . . . .
S1 S 0.21331(5) 0.07546(4) 0.32378(6) 0.0394(2) Uani 1 1 d . . . . .
S2 S 0.42935(4) 0.13727(4) 0.09837(5) 0.02793(19) Uani 1 1 d . . . . .
Zn1 Zn 0.31923(2) 0.12977(2) 0.21447(2) 0.02194(11) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 N5 1.323(4) . ?
C2 N4 1.345(4) . ?
C2 C7 1.488(4) . ?
C4 N4 1.359(4) . ?
C4 C5 1.364(4) . ?
C4 N3 1.397(4) . ?
C5 C6 1.387(4) . ?
C5 H5 0.9300 . ?
C6 N5 1.361(4) . ?
C6 N6 1.368(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N3 1.454(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N6 1.460(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 N2 1.288(4) . ?
C10 C11 1.464(4) . ?
C10 H10 0.9300 . ?
C11 N1 1.343(4) . ?
C11 C12 1.385(4) . ?
C12 C13 1.381(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.386(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.393(4) . ?
C14 H14 0.9300 . ?
C15 N1 1.333(4) . ?
C15 C16 1.491(4) . ?
C16 O1 1.427(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C18 N7 1.288(4) . ?
C18 C19 1.440(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.360(4) . ?
C19 P1 1.826(3) . ?
C20 C21 1.477(5) . ?
C20 C23 1.503(5) . ?
C21 C22 1.338(5) . ?
C21 C24 1.491(5) . ?
C22 P1 1.803(3) . ?
C22 H22 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C30 1.387(5) . ?
C25 C26 1.395(4) . ?
C25 P1 1.835(4) . ?
C26 C27 1.381(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.375(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.371(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.389(6) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 F13 1.309(4) . ?
C31 F12 1.323(4) . ?
C31 F11 1.329(4) . ?
C31 S1 1.838(4) . ?
C32 F21 1.300(4) . ?
C32 F23 1.326(4) . ?
C32 F22 1.336(5) . ?
C32 S2 1.823(4) . ?
N1 Zn1 2.070(2) . ?
N2 N3 1.340(3) . ?
N2 Zn1 2.163(2) . ?
N4 Zn1 2.057(2) . ?
N6 N7 1.368(3) . ?
O1 Zn1 2.133(2) . ?
O1 H1 0.80(4) . ?
O11 S1 1.459(2) . ?
O11 Zn1 2.112(2) . ?
O12 S1 1.412(3) . ?
O13 S1 1.428(3) . ?
O21 S2 1.438(2) . ?
O21 Zn1 2.209(2) . ?
O22 S2 1.431(2) . ?
O23 S2 1.439(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 C2 N4 125.9(3) . . ?
N5 C2 C7 117.9(3) . . ?
N4 C2 C7 116.3(3) . . ?
N4 C4 C5 122.1(3) . . ?
N4 C4 N3 116.1(2) . . ?
C5 C4 N3 121.9(3) . . ?
C4 C5 C6 116.9(3) . . ?
C4 C5 H5 121.6 . . ?
C6 C5 H5 121.6 . . ?
N5 C6 N6 116.7(2) . . ?
N5 C6 C5 122.4(3) . . ?
N6 C6 C5 121.0(3) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N6 C9 H9A 109.5 . . ?
N6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C11 114.3(3) . . ?
N2 C10 H10 122.9 . . ?
C11 C10 H10 122.9 . . ?
N1 C11 C12 121.0(3) . . ?
N1 C11 C10 114.6(2) . . ?
C12 C11 C10 124.4(3) . . ?
C13 C12 C11 118.6(3) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C12 C13 C14 119.9(3) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C15 118.7(3) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
N1 C15 C14 120.6(3) . . ?
N1 C15 C16 115.0(3) . . ?
C14 C15 C16 124.3(3) . . ?
O1 C16 C15 108.6(2) . . ?
O1 C16 H16A 110.0 . . ?
C15 C16 H16A 110.0 . . ?
O1 C16 H16B 110.0 . . ?
C15 C16 H16B 110.0 . . ?
H16A C16 H16B 108.3 . . ?
N7 C18 C19 116.7(3) . . ?
N7 C18 H18 121.7 . . ?
C19 C18 H18 121.7 . . ?
C20 C19 C18 126.7(3) . . ?
C20 C19 P1 111.1(2) . . ?
C18 C19 P1 121.8(2) . . ?
C19 C20 C21 113.5(3) . . ?
C19 C20 C23 125.8(3) . . ?
C21 C20 C23 120.7(3) . . ?
C22 C21 C20 113.0(3) . . ?
C22 C21 C24 126.2(4) . . ?
C20 C21 C24 120.8(3) . . ?
C21 C22 P1 113.0(3) . . ?
C21 C22 H22 123.5 . . ?
P1 C22 H22 123.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 117.6(3) . . ?
C30 C25 P1 120.1(3) . . ?
C26 C25 P1 122.3(3) . . ?
C27 C26 C25 121.1(3) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C28 C27 C26 120.1(3) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C29 C28 C27 120.2(4) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C28 C29 C30 119.7(4) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C25 C30 C29 121.4(4) . . ?
C25 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
F13 C31 F12 107.9(3) . . ?
F13 C31 F11 107.9(3) . . ?
F12 C31 F11 107.6(3) . . ?
F13 C31 S1 111.8(2) . . ?
F12 C31 S1 111.1(3) . . ?
F11 C31 S1 110.4(3) . . ?
F21 C32 F23 107.6(3) . . ?
F21 C32 F22 108.5(3) . . ?
F23 C32 F22 107.6(3) . . ?
F21 C32 S2 111.9(3) . . ?
F23 C32 S2 111.7(2) . . ?
F22 C32 S2 109.5(3) . . ?
C15 N1 C11 121.1(3) . . ?
C15 N1 Zn1 119.9(2) . . ?
C11 N1 Zn1 118.66(19) . . ?
C10 N2 N3 126.5(2) . . ?
C10 N2 Zn1 117.86(19) . . ?
N3 N2 Zn1 115.67(17) . . ?
N2 N3 C4 115.1(2) . . ?
N2 N3 C8 120.5(2) . . ?
C4 N3 C8 124.4(2) . . ?
C2 N4 C4 116.6(2) . . ?
C2 N4 Zn1 125.2(2) . . ?
C4 N4 Zn1 118.05(18) . . ?
C2 N5 C6 116.1(2) . . ?
C6 N6 N7 113.7(2) . . ?
C6 N6 C9 123.8(2) . . ?
N7 N6 C9 122.5(2) . . ?
C18 N7 N6 120.5(3) . . ?
C16 O1 Zn1 115.89(18) . . ?
C16 O1 H1 112(3) . . ?
Zn1 O1 H1 125(3) . . ?
S1 O11 Zn1 142.11(14) . . ?
S2 O21 Zn1 133.65(13) . . ?
C22 P1 C19 88.92(16) . . ?
C22 P1 C25 102.51(16) . . ?
C19 P1 C25 102.46(14) . . ?
O12 S1 O13 117.8(2) . . ?
O12 S1 O11 113.87(18) . . ?
O13 S1 O11 113.74(15) . . ?
O12 S1 C31 104.67(16) . . ?
O13 S1 C31 102.9(2) . . ?
O11 S1 C31 101.22(15) . . ?
O22 S2 O21 114.34(15) . . ?
O22 S2 O23 115.78(15) . . ?
O21 S2 O23 113.61(14) . . ?
O22 S2 C32 104.53(17) . . ?
O21 S2 C32 104.73(16) . . ?
O23 S2 C32 101.83(15) . . ?
N4 Zn1 N1 148.59(10) . . ?
N4 Zn1 O11 92.10(9) . . ?
N1 Zn1 O11 95.17(9) . . ?
N4 Zn1 O1 136.11(9) . . ?
N1 Zn1 O1 75.13(9) . . ?
O11 Zn1 O1 84.18(9) . . ?
N4 Zn1 N2 74.82(9) . . ?
N1 Zn1 N2 74.16(9) . . ?
O11 Zn1 N2 94.69(9) . . ?
O1 Zn1 N2 149.03(8) . . ?
N4 Zn1 O21 86.91(9) . . ?
N1 Zn1 O21 95.90(9) . . ?
O11 Zn1 O21 160.25(9) . . ?
O1 Zn1 O21 82.93(8) . . ?
N2 Zn1 O21 104.04(9) . . ?

_refine_diff_density_max         0.533
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.074

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'Vapour deposition'
####################################################################### 
# 
# 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_L1ZnPd
_database_code_depnum_ccdc_archive 'CCDC 1582381'
_audit_update_record             
;
2017-10-26 deposited with the CCDC.
2017-12-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT602_L1ZnPd              
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info
RESPONSE: The solid state structure of [ZnPdL1Cl3](SO3CF3) ?2C7H8?CH3NO2 contained significant electron density in the asymmetric unit which could not resolved sufficiently. This density was therefore removed by the SQUEEZE procedure of PLATON.  105 electrons were removed from the asymmetric unit of [ZnPdL1Cl3](SO3CF3)?C7H8?CH3NO2 corresponding to one SO3CF3- anion and a CH3NO2 solvent molecule.
;
# Added during the CSD deposition process: Thursday 26 October 2017 10:42 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H30 Cl3 N7 O P Pd Zn, C7 H8, C H3 N O2'
_chemical_formula_sum            'C35 H41 Cl3 N8 O3 P Pd Zn'
_chemical_formula_weight         930.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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                   14.9279(5)
_cell_length_b                   14.9701(5)
_cell_length_c                   21.8728(8)
_cell_angle_alpha                90
_cell_angle_beta                 94.602(4)
_cell_angle_gamma                90
_cell_volume                     4872.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    130.00(14)
_cell_measurement_reflns_used    13204
_cell_measurement_theta_min      2.5900
_cell_measurement_theta_max      27.8460

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_F_000             1892
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.0400
_exptl_absorpt_coefficient_mu    1.096
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.99066
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      130.00(14)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3560
_diffrn_reflns_number            39731
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.191
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9061
_reflns_number_gt                7253
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0767P)²+6.2884P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9061
_refine_ls_number_parameters     479
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1352
_refine_ls_wR_factor_gt          0.1287
_refine_ls_goodness_of_fit_ref   1.029
_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
C2 C 0.7606(3) 0.1748(3) 0.13483(19) 0.0274(9) Uani 1 1 d . . . . .
C4 C 0.6093(3) 0.1874(3) 0.10520(18) 0.0264(9) Uani 1 1 d . . . . .
C5 C 0.6145(3) 0.2793(3) 0.1096(2) 0.0292(9) Uani 1 1 d . . . . .
H5 H 0.5650 0.3154 0.0991 0.035 Uiso 1 1 calc R U . . .
C6 C 0.6968(3) 0.3149(3) 0.13053(19) 0.0265(9) Uani 1 1 d . . . . .
C7 C 0.8415(3) 0.1171(3) 0.1454(2) 0.0352(10) Uani 1 1 d . . . . .
H7A H 0.8475 0.0980 0.1874 0.053 Uiso 1 1 calc R U . . .
H7B H 0.8940 0.1502 0.1365 0.053 Uiso 1 1 calc R U . . .
H7C H 0.8353 0.0658 0.1191 0.053 Uiso 1 1 calc R U . . .
C8 C 0.4436(3) 0.1874(3) 0.0752(2) 0.0384(11) Uani 1 1 d . . . . .
H8A H 0.4157 0.1661 0.0369 0.058 Uiso 1 1 calc R U . . .
H8B H 0.4528 0.2508 0.0728 0.058 Uiso 1 1 calc R U . . .
H8C H 0.4055 0.1747 0.1075 0.058 Uiso 1 1 calc R U . . .
C9 C 0.6335(3) 0.4684(3) 0.1310(3) 0.0402(12) Uani 1 1 d . . . . .
H9A H 0.6458 0.5184 0.1578 0.060 Uiso 1 1 calc R U . . .
H9B H 0.5790 0.4398 0.1409 0.060 Uiso 1 1 calc R U . . .
H9C H 0.6268 0.4889 0.0893 0.060 Uiso 1 1 calc R U . . .
C10 C 0.4654(3) 0.0033(3) 0.07514(19) 0.0293(9) Uani 1 1 d . . . . .
H10 H 0.4085 0.0279 0.0672 0.035 Uiso 1 1 calc R U . . .
C11 C 0.4804(3) -0.0933(3) 0.07470(19) 0.0308(10) Uani 1 1 d . . . . .
C12 C 0.4088(3) -0.1518(3) 0.0627(2) 0.0400(11) Uani 1 1 d . . . . .
H12 H 0.3506 -0.1307 0.0537 0.048 Uiso 1 1 calc R U . . .
C13 C 0.4271(3) -0.2425(3) 0.0646(2) 0.0425(12) Uani 1 1 d . . . . .
H13 H 0.3809 -0.2838 0.0577 0.051 Uiso 1 1 calc R U . . .
C14 C 0.5147(3) -0.2711(3) 0.0770(2) 0.0404(12) Uani 1 1 d . . . . .
H14 H 0.5280 -0.3318 0.0779 0.048 Uiso 1 1 calc R U . . .
C15 C 0.5823(3) -0.2091(3) 0.0881(2) 0.0341(10) Uani 1 1 d . . . . .
C16 C 0.6802(3) -0.2360(3) 0.1009(3) 0.0456(13) Uani 1 1 d . . . . .
H16A H 0.7163 -0.2035 0.0734 0.055 Uiso 1 1 calc R U . . .
H16B H 0.7004 -0.2191 0.1426 0.055 Uiso 1 1 calc R U . . .
C18 C 0.8141(3) 0.5187(3) 0.1563(2) 0.0304(9) Uani 1 1 d . . . . .
H18 H 0.7733 0.5629 0.1430 0.036 Uiso 1 1 calc R U . . .
C19 C 0.9056(3) 0.5381(3) 0.17765(19) 0.0280(9) Uani 1 1 d . . . . .
C20 C 0.9637(3) 0.5969(3) 0.1569(2) 0.0307(9) Uani 1 1 d . . . . .
C21 C 1.0598(3) 0.5724(3) 0.1749(2) 0.0337(10) Uani 1 1 d . . . . .
C22 C 1.0730(3) 0.4949(3) 0.2041(2) 0.0312(10) Uani 1 1 d . . . . .
H22 H 1.1285 0.4687 0.2150 0.037 Uiso 1 1 calc R U . . .
C23 C 0.9410(4) 0.6750(3) 0.1168(2) 0.0443(12) Uani 1 1 d . . . . .
H23A H 0.8773 0.6765 0.1064 0.067 Uiso 1 1 calc R U . . .
H23B H 0.9717 0.6701 0.0801 0.067 Uiso 1 1 calc R U . . .
H23C H 0.9593 0.7289 0.1381 0.067 Uiso 1 1 calc R U . . .
C24 C 1.1343(3) 0.6340(4) 0.1598(3) 0.0488(13) Uani 1 1 d . . . . .
H24A H 1.1912 0.6066 0.1716 0.073 Uiso 1 1 calc R U . . .
H24B H 1.1295 0.6892 0.1816 0.073 Uiso 1 1 calc R U . . .
H24C H 1.1298 0.6456 0.1165 0.073 Uiso 1 1 calc R U . . .
C25 C 0.9557(3) 0.4598(3) 0.3004(2) 0.0304(9) Uani 1 1 d . . . . .
C26 C 1.0258(3) 0.4307(3) 0.3416(2) 0.0393(11) Uani 1 1 d . . . . .
H26 H 1.0789 0.4090 0.3276 0.047 Uiso 1 1 calc R U . . .
C27 C 1.0146(4) 0.4350(4) 0.4035(2) 0.0514(14) Uani 1 1 d . . . . .
H27 H 1.0603 0.4154 0.4317 0.062 Uiso 1 1 calc R U . . .
C28 C 0.9348(4) 0.4688(4) 0.4242(2) 0.0513(14) Uani 1 1 d . . . . .
H28 H 0.9281 0.4719 0.4660 0.062 Uiso 1 1 calc R U . . .
C29 C 0.8675(4) 0.4969(4) 0.3836(3) 0.0582(15) Uani 1 1 d . . . . .
H29 H 0.8147 0.5193 0.3975 0.070 Uiso 1 1 calc R U . . .
C30 C 0.8777(4) 0.4922(4) 0.3212(2) 0.0510(14) Uani 1 1 d . . . . .
H30 H 0.8313 0.5111 0.2933 0.061 Uiso 1 1 calc R U . . .
C31 C 0.7685(5) 0.7687(5) 0.3117(4) 0.086(2) Uani 1 1 d . . . . .
H31A H 0.8329 0.7709 0.3125 0.129 Uiso 1 1 calc R U . . .
H31B H 0.7505 0.7784 0.3524 0.129 Uiso 1 1 calc R U . . .
H31C H 0.7430 0.8142 0.2848 0.129 Uiso 1 1 calc R U . . .
C32 C 0.5175(5) 0.1331(5) 0.2539(3) 0.078(2) Uani 1 1 d . . . . .
H32A H 0.4935 0.1131 0.2910 0.116 Uiso 1 1 calc R U . . .
H32B H 0.5630 0.0921 0.2429 0.116 Uiso 1 1 calc R U . . .
H32C H 0.4702 0.1356 0.2215 0.116 Uiso 1 1 calc R U . . .
C33 C 0.5575(4) 0.2236(4) 0.2638(3) 0.0568(15) Uani 1 1 d . . . . .
C34 C 0.5050(4) 0.2989(5) 0.2637(3) 0.0600(16) Uani 1 1 d . . . . .
H34 H 0.4429 0.2935 0.2570 0.072 Uiso 1 1 calc R U . . .
C35 C 0.5426(4) 0.3817(5) 0.2732(3) 0.0626(16) Uani 1 1 d . . . . .
H35 H 0.5057 0.4319 0.2720 0.075 Uiso 1 1 calc R U . . .
C36 C 0.6341(4) 0.3918(4) 0.2845(3) 0.0637(16) Uani 1 1 d . . . . .
H36 H 0.6592 0.4481 0.2915 0.076 Uiso 1 1 calc R U . . .
C37 C 0.6879(4) 0.3168(5) 0.2853(3) 0.0642(16) Uani 1 1 d . . . . .
H37 H 0.7498 0.3224 0.2930 0.077 Uiso 1 1 calc R U . . .
C38 C 0.6498(4) 0.2329(4) 0.2747(3) 0.0564(15) Uani 1 1 d . . . . .
H38 H 0.6864 0.1827 0.2749 0.068 Uiso 1 1 calc R U . . .
N1 N 0.5661(2) -0.1211(2) 0.08660(16) 0.0309(8) Uani 1 1 d . . . . .
N2 N 0.5354(2) 0.0524(2) 0.08719(16) 0.0277(8) Uani 1 1 d . . . . .
N3 N 0.5303(2) 0.1429(2) 0.08822(16) 0.0279(8) Uani 1 1 d . . . . .
N4 N 0.6831(2) 0.1348(2) 0.11651(16) 0.0271(8) Uani 1 1 d . . . . .
N5 N 0.7702(2) 0.2627(2) 0.14421(15) 0.0256(7) Uani 1 1 d . . . . .
N6 N 0.7074(2) 0.4051(2) 0.13838(17) 0.0296(8) Uani 1 1 d . . . . .
N7 N 0.7928(2) 0.4344(2) 0.15700(17) 0.0300(8) Uani 1 1 d . . . . .
N8 N 0.7362(3) 0.6791(4) 0.2892(3) 0.0622(14) Uani 1 1 d . . . . .
O1 O 0.6944(3) -0.3285(2) 0.09355(17) 0.0516(11) Uani 1 1 d . . . . .
H1 H 0.706(5) -0.335(5) 0.063(3) 0.077 Uiso 1 1 d . U . . .
O2 O 0.7070(3) 0.6305(3) 0.3267(3) 0.0880(16) Uani 1 1 d . . . . .
O3 O 0.7398(6) 0.6616(5) 0.2374(3) 0.157(4) Uani 1 1 d . . . . .
P1 P 0.96594(7) 0.44977(7) 0.21894(5) 0.0284(2) Uani 1 1 d . . . . .
Cl1 Cl 0.99542(7) 0.24463(7) 0.21931(5) 0.0373(3) Uani 1 1 d . . . . .
Cl2 Cl 0.74164(7) -0.02975(7) 0.02199(5) 0.0342(2) Uani 1 1 d . . . . .
Cl3 Cl 0.70803(8) -0.04894(8) 0.20221(5) 0.0397(3) Uani 1 1 d . . . . .
Zn1 Zn 0.66197(3) -0.01074(3) 0.10544(2) 0.02855(14) Uani 1 1 d . . . . .
Pd1 Pd 0.88357(2) 0.33878(2) 0.18061(2) 0.02609(11) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 N4 1.336(5) . ?
C2 N5 1.337(5) . ?
C2 C7 1.488(6) . ?
C4 N4 1.360(5) . ?
C4 N3 1.379(5) . ?
C4 C5 1.381(6) . ?
C5 C6 1.383(6) . ?
C5 H5 0.9300 . ?
C6 N5 1.359(5) . ?
C6 N6 1.369(5) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N3 1.463(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N6 1.454(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 N2 1.287(5) . ?
C10 C11 1.463(6) . ?
C10 H10 0.9300 . ?
C11 N1 1.351(6) . ?
C11 C12 1.390(6) . ?
C12 C13 1.385(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.382(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.378(6) . ?
C14 H14 0.9300 . ?
C15 N1 1.339(6) . ?
C15 C16 1.520(7) . ?
C16 O1 1.412(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C18 N7 1.303(5) . ?
C18 C19 1.437(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.341(6) . ?
C19 P1 1.801(4) . ?
C20 C23 1.484(6) . ?
C20 C21 1.503(6) . ?
C21 C22 1.331(6) . ?
C21 C24 1.503(6) . ?
C22 P1 1.788(4) . ?
C22 H22 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C30 1.373(7) . ?
C25 C26 1.394(6) . ?
C25 P1 1.807(5) . ?
C26 C27 1.379(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.402(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.354(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.386(7) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 N8 1.495(9) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.491(9) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.372(8) . ?
C33 C38 1.385(8) . ?
C34 C35 1.370(9) . ?
C34 H34 0.9300 . ?
C35 C36 1.377(9) . ?
C35 H35 0.9300 . ?
C36 C37 1.379(9) . ?
C36 H36 0.9300 . ?
C37 C38 1.390(9) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
N1 Zn1 2.203(3) . ?
N2 N3 1.358(5) . ?
N2 Zn1 2.122(3) . ?
N4 Zn1 2.211(3) . ?
N5 Pd1 2.140(3) . ?
N6 N7 1.377(5) . ?
N7 Pd1 2.010(3) . ?
N8 O3 1.168(7) . ?
N8 O2 1.204(7) . ?
O1 H1 0.72(7) . ?
P1 Pd1 2.1933(11) . ?
Cl1 Pd1 2.2945(11) . ?
Cl2 Zn1 2.2751(13) . ?
Cl3 Zn1 2.2463(12) . ?

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
N4 C2 N5 124.5(4) . . ?
N4 C2 C7 117.3(4) . . ?
N5 C2 C7 118.2(4) . . ?
N4 C4 N3 115.6(4) . . ?
N4 C4 C5 121.6(4) . . ?
N3 C4 C5 122.7(4) . . ?
C4 C5 C6 116.7(4) . . ?
C4 C5 H5 121.6 . . ?
C6 C5 H5 121.6 . . ?
N5 C6 N6 117.1(3) . . ?
N5 C6 C5 122.0(4) . . ?
N6 C6 C5 120.9(4) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N6 C9 H9A 109.5 . . ?
N6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C11 116.4(4) . . ?
N2 C10 H10 121.8 . . ?
C11 C10 H10 121.8 . . ?
N1 C11 C12 123.0(4) . . ?
N1 C11 C10 116.5(4) . . ?
C12 C11 C10 120.6(4) . . ?
C13 C12 C11 117.7(4) . . ?
C13 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
C14 C13 C12 119.4(4) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C15 C14 C13 119.6(4) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
N1 C15 C14 122.0(4) . . ?
N1 C15 C16 115.8(4) . . ?
C14 C15 C16 122.2(4) . . ?
O1 C16 C15 112.9(4) . . ?
O1 C16 H16A 109.0 . . ?
C15 C16 H16A 109.0 . . ?
O1 C16 H16B 109.0 . . ?
C15 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
N7 C18 C19 114.7(4) . . ?
N7 C18 H18 122.6 . . ?
C19 C18 H18 122.6 . . ?
C20 C19 C18 130.3(4) . . ?
C20 C19 P1 109.9(3) . . ?
C18 C19 P1 116.1(3) . . ?
C19 C20 C23 126.5(4) . . ?
C19 C20 C21 112.4(4) . . ?
C23 C20 C21 121.0(4) . . ?
C22 C21 C24 123.9(4) . . ?
C22 C21 C20 116.1(4) . . ?
C24 C21 C20 120.0(4) . . ?
C21 C22 P1 108.4(3) . . ?
C21 C22 H22 125.8 . . ?
P1 C22 H22 125.8 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 120.6(4) . . ?
C30 C25 P1 119.8(3) . . ?
C26 C25 P1 119.5(4) . . ?
C27 C26 C25 118.4(5) . . ?
C27 C26 H26 120.8 . . ?
C25 C26 H26 120.8 . . ?
C26 C27 C28 120.5(5) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C29 C28 C27 120.4(5) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C28 C29 C30 119.7(5) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C25 C30 C29 120.5(5) . . ?
C25 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
N8 C31 H31A 109.5 . . ?
N8 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N8 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C33 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C38 118.5(6) . . ?
C34 C33 C32 121.6(6) . . ?
C38 C33 C32 119.8(6) . . ?
C35 C34 C33 121.1(6) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C34 C35 C36 120.9(6) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C35 C36 C37 118.8(6) . . ?
C35 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
C36 C37 C38 120.2(6) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C33 C38 C37 120.5(6) . . ?
C33 C38 H38 119.8 . . ?
C37 C38 H38 119.8 . . ?
C15 N1 C11 118.3(4) . . ?
C15 N1 Zn1 128.3(3) . . ?
C11 N1 Zn1 113.3(3) . . ?
C10 N2 N3 121.9(4) . . ?
C10 N2 Zn1 118.7(3) . . ?
N3 N2 Zn1 119.4(2) . . ?
N2 N3 C4 116.0(3) . . ?
N2 N3 C8 120.1(3) . . ?
C4 N3 C8 123.8(3) . . ?
C2 N4 C4 117.6(3) . . ?
C2 N4 Zn1 126.0(3) . . ?
C4 N4 Zn1 116.4(3) . . ?
C2 N5 C6 117.2(3) . . ?
C2 N5 Pd1 130.7(3) . . ?
C6 N5 Pd1 112.1(3) . . ?
C6 N6 N7 116.5(3) . . ?
C6 N6 C9 123.3(3) . . ?
N7 N6 C9 120.1(3) . . ?
C18 N7 N6 121.7(3) . . ?
C18 N7 Pd1 122.2(3) . . ?
N6 N7 Pd1 116.0(2) . . ?
O3 N8 O2 124.9(8) . . ?
O3 N8 C31 118.8(8) . . ?
O2 N8 C31 116.3(6) . . ?
C16 O1 H1 107(6) . . ?
C22 P1 C19 92.9(2) . . ?
C22 P1 C25 107.15(19) . . ?
C19 P1 C25 110.8(2) . . ?
C22 P1 Pd1 134.33(15) . . ?
C19 P1 Pd1 96.98(13) . . ?
C25 P1 Pd1 110.51(14) . . ?
N2 Zn1 N1 75.13(13) . . ?
N2 Zn1 N4 72.49(12) . . ?
N1 Zn1 N4 147.57(13) . . ?
N2 Zn1 Cl3 119.43(10) . . ?
N1 Zn1 Cl3 97.50(10) . . ?
N4 Zn1 Cl3 96.74(10) . . ?
N2 Zn1 Cl2 114.82(10) . . ?
N1 Zn1 Cl2 97.44(10) . . ?
N4 Zn1 Cl2 97.58(10) . . ?
Cl3 Zn1 Cl2 125.72(5) . . ?
N7 Pd1 N5 77.66(13) . . ?
N7 Pd1 P1 84.53(10) . . ?
N5 Pd1 P1 161.41(10) . . ?
N7 Pd1 Cl1 171.12(10) . . ?
N5 Pd1 Cl1 109.93(9) . . ?
P1 Pd1 Cl1 87.43(4) . . ?

_refine_diff_density_max         1.786
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.101

_shelxl_version_number           2013-4

_exptl_crystal_recrystallization_method 'Vapour deposition'
