# 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_5Br
_database_code_depnum_ccdc_archive 'CCDC 1558459'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;

_audit_creation_date             2016-12-01T19:13:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C86 H102 Br4 N4 O P2 Rh2'
_chemical_formula_moiety         '2(C41 H46 Br N2 P Rh), C4 H10 O, 2(Br)'
_chemical_formula_weight         1795.08

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_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                   35.5534(8)
_cell_length_b                   10.8950(3)
_cell_length_c                   26.8665(11)
_cell_angle_alpha                90
_cell_angle_beta                 129.8210(10)
_cell_angle_gamma                90
_cell_volume                     7993.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      1.80
_cell_measurement_reflns_used    9999
_cell_measurement_theta_max      36.29
_cell_measurement_wavelength     0.71073


#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.492
_exptl_crystal_F_000             3656.0
_exptl_crystal_density_method    'not measured'
_exptl_special_details           
;
 ?
;


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.500
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.5561
_exptl_absorpt_correction_T_max  0.7462


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec I\mS Microsource '
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_number            116957
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.292
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             8173
_reflns_number_gt                7764
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0282P)²+20.2649P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8173
_refine_ls_number_parameters     474
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0183
_refine_ls_wR_factor_ref         0.05
_refine_ls_wR_factor_gt          0.0487
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_restrained_S_all      0.91
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.055

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C60A C 0.95046(19) 0.9542(4) 0.7102(3) 0.0344(10) Uani 0.5 1 d . . P A 1
H60A H 0.9544 1.0368 0.7264 0.041 Uiso 0.5 1 calc R U P A 1
H60B H 0.9358 0.9587 0.6649 0.041 Uiso 0.5 1 calc R U P A 1
C61 C 0.92009(9) 0.8799(2) 0.71814(12) 0.0406(5) Uani 1 1 d . . . A 1
H61A H 0.9118 0.8038 0.6952 0.061 Uiso 0.5 1 calc R U P A 1
H61B H 0.8906 0.9239 0.7011 0.061 Uiso 0.5 1 calc R U P A 1
H61C H 0.938 0.8634 0.7633 0.061 Uiso 0.5 1 calc R U P A 1
O1 O 1 0.88782(18) 0.75 0.0335(5) Uani 1 2 d S T P A 1
C60B C 0.9679(2) 0.9579(4) 0.7497(3) 0.0413(11) Uani 0.5 1 d . . P B 2
H60C H 0.9601 1.0327 0.7252 0.05 Uiso 0.5 1 calc R U P B 2
H60D H 0.9823 0.9802 0.7937 0.05 Uiso 0.5 1 calc R U P B 2
H61D H 0.9259 0.821 0.7484 0.048 Uiso 0.5 1 calc R U P B 2
H61E H 0.9116 0.8389 0.6802 0.048 Uiso 0.5 1 calc R U P B 2
H61F H 0.8939 0.9338 0.7053 0.048 Uiso 0.5 1 calc R U P B 2
C1 C 0.14597(5) 1.02454(14) 0.52594(7) 0.0124(3) Uani 1 1 d . . . . .
C2 C 0.13890(6) 1.19294(15) 0.47072(8) 0.0170(3) Uani 1 1 d . . . . .
H2 H 0.1311 1.2719 0.4537 0.02 Uiso 1 1 calc R U . . .
C3 C 0.16107(6) 1.10554(15) 0.46246(8) 0.0164(3) Uani 1 1 d . . . . .
H3 H 0.1716 1.1122 0.4386 0.02 Uiso 1 1 calc R U . . .
C4 C 0.18624(6) 0.88697(14) 0.49784(8) 0.0138(3) Uani 1 1 d . . . . .
H4A H 0.1927 0.8355 0.5321 0.017 Uiso 1 1 calc R U . . .
H4B H 0.2171 0.9021 0.5072 0.017 Uiso 1 1 calc R U . . .
C5 C 0.15148(6) 0.82052(14) 0.43316(8) 0.0140(3) Uani 1 1 d . . . . .
H5A H 0.1423 0.8746 0.3983 0.017 Uiso 1 1 calc R U . . .
H5B H 0.122 0.7971 0.4258 0.017 Uiso 1 1 calc R U . . .
C6 C 0.17706(6) 0.70539(14) 0.43410(8) 0.0142(3) Uani 1 1 d . . . . .
H6A H 0.1926 0.6616 0.4745 0.017 Uiso 1 1 calc R U . . .
H6B H 0.2025 0.7304 0.4326 0.017 Uiso 1 1 calc R U . . .
C11 C 0.10854(6) 1.21322(14) 0.53194(8) 0.0137(3) Uani 1 1 d . . . . .
C12 C 0.05937(6) 1.19721(15) 0.50318(8) 0.0174(3) Uani 1 1 d . . . . .
C13 C 0.04030(6) 1.27180(16) 0.52444(9) 0.0210(4) Uani 1 1 d . . . . .
H13 H 0.0078 1.2616 0.5064 0.025 Uiso 1 1 calc R U . . .
C14 C 0.06834(7) 1.36080(16) 0.57174(9) 0.0212(4) Uani 1 1 d . . . . .
C15 C 0.11697(7) 1.37423(15) 0.59907(8) 0.0190(3) Uani 1 1 d . . . . .
H15 H 0.1361 1.433 0.6312 0.023 Uiso 1 1 calc R U . . .
C16 C 0.13783(6) 1.30197(15) 0.57966(8) 0.0162(3) Uani 1 1 d . . . . .
C17 C 0.02678(7) 1.10732(17) 0.44896(10) 0.0258(4) Uani 1 1 d . . . . .
H17A H 0.0336 1.1097 0.4197 0.039 Uiso 1 1 calc R U . . .
H17B H -0.0069 1.1288 0.426 0.039 Uiso 1 1 calc R U . . .
H17C H 0.0328 1.0261 0.4665 0.039 Uiso 1 1 calc R U . . .
C18 C 0.04598(8) 1.4442(2) 0.59145(11) 0.0326(5) Uani 1 1 d . . . . .
H18A H 0.0391 1.5227 0.5709 0.049 Uiso 1 1 calc R U . . .
H18B H 0.0685 1.4545 0.6377 0.049 Uiso 1 1 calc R U . . .
H18C H 0.0161 1.4085 0.5783 0.049 Uiso 1 1 calc R U . . .
C19 C 0.19001(6) 1.32339(17) 0.60833(9) 0.0217(4) Uani 1 1 d . . . . .
H19A H 0.1906 1.3751 0.5799 0.032 Uiso 1 1 calc R U . . .
H19B H 0.2052 1.2462 0.6136 0.032 Uiso 1 1 calc R U . . .
H19C H 0.2075 1.3625 0.6498 0.032 Uiso 1 1 calc R U . . .
C21 C 0.09984(6) 0.68986(15) 0.29368(8) 0.0149(3) Uani 1 1 d . . . . .
C22 C 0.12475(7) 0.76877(18) 0.28298(9) 0.0260(4) Uani 1 1 d . . . . .
H22 H 0.1583 0.781 0.315 0.031 Uiso 1 1 calc R U . . .
C23 C 0.09899(8) 0.8289(2) 0.22407(10) 0.0358(5) Uani 1 1 d . . . . .
H23 H 0.1155 0.8809 0.2164 0.043 Uiso 1 1 calc R U . . .
C24 C 0.04900(7) 0.81283(18) 0.17640(9) 0.0283(4) Uani 1 1 d . . . . .
H24 H 0.0322 0.8531 0.1369 0.034 Uiso 1 1 calc R U . . .
C25 C 0.02426(7) 0.73666(18) 0.18787(9) 0.0247(4) Uani 1 1 d . . . . .
H25 H -0.0095 0.7272 0.1564 0.03 Uiso 1 1 calc R U . . .
C26 C 0.04970(6) 0.67432(17) 0.24624(8) 0.0205(3) Uani 1 1 d . . . . .
H26 H 0.0331 0.6219 0.2536 0.025 Uiso 1 1 calc R U . . .
C31 C 0.16657(6) 0.48504(15) 0.36041(8) 0.0142(3) Uani 1 1 d . . . . .
C32 C 0.15384(6) 0.46034(16) 0.30040(8) 0.0195(3) Uani 1 1 d . . . . .
H32 H 0.134 0.5146 0.266 0.023 Uiso 1 1 calc R U . . .
C33 C 0.17100(7) 0.35404(17) 0.29229(9) 0.0229(4) Uani 1 1 d . . . . .
H33 H 0.1628 0.3373 0.2524 0.028 Uiso 1 1 calc R U . . .
C34 C 0.20021(6) 0.27327(16) 0.34327(9) 0.0207(3) Uani 1 1 d . . . . .
H34 H 0.2103 0.2004 0.3371 0.025 Uiso 1 1 calc R U . . .
C35 C 0.21454(6) 0.30037(16) 0.40374(9) 0.0197(3) Uani 1 1 d . . . . .
H35 H 0.2354 0.2473 0.4383 0.024 Uiso 1 1 calc R U . . .
C36 C 0.19792(6) 0.40628(15) 0.41281(8) 0.0176(3) Uani 1 1 d . . . . .
H36 H 0.2075 0.4246 0.4533 0.021 Uiso 1 1 calc R U . . .
C41 C 0.09690(6) 0.52468(15) 0.37831(8) 0.0142(3) Uani 1 1 d . . . . .
C42 C 0.06503(6) 0.43471(16) 0.33299(8) 0.0178(3) Uani 1 1 d . . . . .
H42 H 0.0647 0.4166 0.2989 0.021 Uiso 1 1 calc R U . . .
C43 C 0.03395(6) 0.37250(16) 0.33862(9) 0.0207(3) Uani 1 1 d . . . . .
H43 H 0.0127 0.313 0.3084 0.025 Uiso 1 1 calc R U . . .
C44 C 0.03481(6) 0.39972(16) 0.38977(9) 0.0202(3) Uani 1 1 d . . . . .
H44 H 0.0131 0.3605 0.3928 0.024 Uiso 1 1 calc R U . . .
C45 C 0.06766(6) 0.48480(16) 0.43628(8) 0.0199(3) Uani 1 1 d . . . . .
H45 H 0.0688 0.5001 0.4712 0.024 Uiso 1 1 calc R U . . .
C46 C 0.09898(6) 0.54750(15) 0.43104(8) 0.0173(3) Uani 1 1 d . . . . .
H46 H 0.1212 0.6043 0.4625 0.021 Uiso 1 1 calc R U . . .
C51 C 0.16263(6) 0.73794(15) 0.64293(8) 0.0189(3) Uani 1 1 d D . . . .
C52 C 0.21693(7) 0.73048(17) 0.69959(9) 0.0255(4) Uani 1 1 d . . . . .
H52A H 0.228 0.6469 0.7036 0.031 Uiso 1 1 calc R U . . .
H52B H 0.2227 0.7507 0.7391 0.031 Uiso 1 1 calc R U . . .
C53 C 0.24695(6) 0.81747(18) 0.69210(9) 0.0242(4) Uani 1 1 d . . . . .
H53A H 0.2774 0.8368 0.7347 0.029 Uiso 1 1 calc R U . . .
H53B H 0.255 0.7758 0.6681 0.029 Uiso 1 1 calc R U . . .
C54 C 0.22052(6) 0.93584(16) 0.65763(8) 0.0178(3) Uani 1 1 d D . . . .
C55 C 0.19283(6) 1.00687(16) 0.66748(8) 0.0166(3) Uani 1 1 d D . . . .
C56 C 0.18650(6) 0.97820(17) 0.71720(8) 0.0203(3) Uani 1 1 d . . . . .
H56A H 0.1859 1.0542 0.7354 0.024 Uiso 1 1 calc R U . . .
H56B H 0.2142 0.9302 0.7522 0.024 Uiso 1 1 calc R U . . .
C57 C 0.13907(7) 0.90685(16) 0.68644(9) 0.0205(3) Uani 1 1 d . . . . .
H57A H 0.1411 0.8675 0.7204 0.025 Uiso 1 1 calc R U . . .
H57B H 0.1119 0.9641 0.6643 0.025 Uiso 1 1 calc R U . . .
C58 C 0.12913(6) 0.81091(15) 0.63907(8) 0.0176(3) Uani 1 1 d D . . . .
N1 N 0.12973(5) 1.14279(12) 0.50966(6) 0.0134(3) Uani 1 1 d . . . . .
N2 N 0.16521(5) 1.00360(12) 0.49644(6) 0.0127(3) Uani 1 1 d . . . . .
P1 P 0.13563(2) 0.60408(4) 0.36776(2) 0.01200(8) Uani 1 1 d . . . . .
Br1 Br 0.07304(2) 0.79558(2) 0.48394(2) 0.01925(5) Uani 1 1 d . . . . .
Br2 Br 0.23709(2) 0.95426(2) 0.41158(2) 0.02041(5) Uani 1 1 d . . . . .
Rh1 Rh 0.14552(2) 0.90066(2) 0.58190(2) 0.01077(4) Uani 1 1 d . . . . .
H51 H 0.1496(8) 0.6747(17) 0.6115(9) 0.04 Uiso 1 1 d D U . . .
H55 H 0.1881(9) 1.0904(11) 0.6550(12) 0.04 Uiso 1 1 d D U . . .
H54 H 0.2334(8) 0.977(2) 0.6402(11) 0.04 Uiso 1 1 d D U . . .
H58 H 0.0956(4) 0.788(2) 0.6075(9) 0.04 Uiso 1 1 d D U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C60A C61 1.470(5) . ?
C60A O1 1.535(5) . ?
C60A H60A 0.97 . ?
C60A H60B 0.97 . ?
C61 H61A 0.96 . ?
C61 H61B 0.96 . ?
C61 H61C 0.96 . ?
O1 C60A 1.535(5) 2_756 ?
C60B H60C 0.97 . ?
C60B H60D 0.97 . ?
C1 N2 1.357(2) . ?
C1 N1 1.364(2) . ?
C1 Rh1 2.0280(16) . ?
C2 C3 1.342(2) . ?
C2 N1 1.391(2) . ?
C2 H2 0.93 . ?
C3 N2 1.384(2) . ?
C3 H3 0.93 . ?
C4 N2 1.4626(19) . ?
C4 C5 1.523(2) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 C6 1.540(2) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C6 P1 1.7894(16) . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C11 C16 1.398(2) . ?
C11 C12 1.398(2) . ?
C11 N1 1.4465(19) . ?
C12 C13 1.394(2) . ?
C12 C17 1.504(2) . ?
C13 C14 1.388(3) . ?
C13 H13 0.93 . ?
C14 C15 1.387(3) . ?
C14 C18 1.509(2) . ?
C15 C16 1.392(2) . ?
C15 H15 0.93 . ?
C16 C19 1.503(2) . ?
C17 H17A 0.96 . ?
C17 H17B 0.96 . ?
C17 H17C 0.96 . ?
C18 H18A 0.96 . ?
C18 H18B 0.96 . ?
C18 H18C 0.96 . ?
C19 H19A 0.96 . ?
C19 H19B 0.96 . ?
C19 H19C 0.96 . ?
C21 C26 1.386(2) . ?
C21 C22 1.390(2) . ?
C21 P1 1.7917(16) . ?
C22 C23 1.384(3) . ?
C22 H22 0.93 . ?
C23 C24 1.384(3) . ?
C23 H23 0.93 . ?
C24 C25 1.380(3) . ?
C24 H24 0.93 . ?
C25 C26 1.386(2) . ?
C25 H25 0.93 . ?
C26 H26 0.93 . ?
C31 C32 1.394(2) . ?
C31 C36 1.397(2) . ?
C31 P1 1.7915(16) . ?
C32 C33 1.390(2) . ?
C32 H32 0.93 . ?
C33 C34 1.381(3) . ?
C33 H33 0.93 . ?
C34 C35 1.388(2) . ?
C34 H34 0.93 . ?
C35 C36 1.387(2) . ?
C35 H35 0.93 . ?
C36 H36 0.93 . ?
C41 C46 1.393(2) . ?
C41 C42 1.400(2) . ?
C41 P1 1.7957(16) . ?
C42 C43 1.385(2) . ?
C42 H42 0.93 . ?
C43 C44 1.387(3) . ?
C43 H43 0.93 . ?
C44 C45 1.384(3) . ?
C44 H44 0.93 . ?
C45 C46 1.388(2) . ?
C45 H45 0.93 . ?
C46 H46 0.93 . ?
C51 C58 1.380(2) . ?
C51 C52 1.512(3) . ?
C51 Rh1 2.2190(16) . ?
C51 H51 0.949(10) . ?
C52 C53 1.534(3) . ?
C52 H52A 0.97 . ?
C52 H52B 0.97 . ?
C53 C54 1.513(2) . ?
C53 H53A 0.97 . ?
C53 H53B 0.97 . ?
C54 C55 1.404(2) . ?
C54 Rh1 2.1091(16) . ?
C54 H54 0.950(10) . ?
C55 C56 1.522(2) . ?
C55 Rh1 2.1216(16) . ?
C55 H55 0.947(10) . ?
C56 C57 1.532(2) . ?
C56 H56A 0.97 . ?
C56 H56B 0.97 . ?
C57 C58 1.504(2) . ?
C57 H57A 0.97 . ?
C57 H57B 0.97 . ?
C58 Rh1 2.1912(16) . ?
C58 H58 0.951(10) . ?
Br1 Rh1 2.4884(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
C61 C60A O1 105.2(3) . . ?
C61 C60A H60A 110.7 . . ?
O1 C60A H60A 110.7 . . ?
C61 C60A H60B 110.7 . . ?
O1 C60A H60B 110.7 . . ?
H60A C60A H60B 108.8 . . ?
C60A C61 H61A 109.5 . . ?
C60A C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60A C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C60A O1 C60A 123.8(4) . 2_756 ?
H60C C60B H60D 108.4 . . ?
N2 C1 N1 103.86(13) . . ?
N2 C1 Rh1 124.56(11) . . ?
N1 C1 Rh1 131.57(11) . . ?
C3 C2 N1 106.92(14) . . ?
C3 C2 H2 126.5 . . ?
N1 C2 H2 126.5 . . ?
C2 C3 N2 106.60(14) . . ?
C2 C3 H3 126.7 . . ?
N2 C3 H3 126.7 . . ?
N2 C4 C5 110.84(12) . . ?
N2 C4 H4A 109.5 . . ?
C5 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C4 C5 C6 109.23(12) . . ?
C4 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
C4 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.3 . . ?
C5 C6 P1 112.67(11) . . ?
C5 C6 H6A 109.1 . . ?
P1 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
P1 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
C16 C11 C12 121.80(15) . . ?
C16 C11 N1 117.84(14) . . ?
C12 C11 N1 120.23(14) . . ?
C13 C12 C11 117.72(16) . . ?
C13 C12 C17 120.10(15) . . ?
C11 C12 C17 122.12(15) . . ?
C14 C13 C12 122.01(16) . . ?
C14 C13 H13 119 . . ?
C12 C13 H13 119 . . ?
C15 C14 C13 118.64(15) . . ?
C15 C14 C18 120.58(18) . . ?
C13 C14 C18 120.75(17) . . ?
C14 C15 C16 121.65(16) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C15 C16 C11 118.17(15) . . ?
C15 C16 C19 119.95(16) . . ?
C11 C16 C19 121.85(15) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C26 C21 C22 120.00(15) . . ?
C26 C21 P1 122.56(13) . . ?
C22 C21 P1 117.32(13) . . ?
C23 C22 C21 119.11(17) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C24 C23 C22 121.02(18) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C25 C24 C23 119.62(17) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 119.98(17) . . ?
C24 C25 H25 120 . . ?
C26 C25 H25 120 . . ?
C21 C26 C25 120.24(16) . . ?
C21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C32 C31 C36 120.38(15) . . ?
C32 C31 P1 119.99(13) . . ?
C36 C31 P1 118.93(12) . . ?
C33 C32 C31 119.50(16) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 120.15(16) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 120.31(16) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C36 C35 C34 120.28(16) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C35 C36 C31 119.26(15) . . ?
C35 C36 H36 120.4 . . ?
C31 C36 H36 120.4 . . ?
C46 C41 C42 119.72(15) . . ?
C46 C41 P1 121.87(13) . . ?
C42 C41 P1 118.38(12) . . ?
C43 C42 C41 120.37(16) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C42 C43 C44 119.40(16) . . ?
C42 C43 H43 120.3 . . ?
C44 C43 H43 120.3 . . ?
C45 C44 C43 120.54(16) . . ?
C45 C44 H44 119.7 . . ?
C43 C44 H44 119.7 . . ?
C44 C45 C46 120.39(16) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C45 C46 C41 119.46(16) . . ?
C45 C46 H46 120.3 . . ?
C41 C46 H46 120.3 . . ?
C58 C51 C52 126.21(16) . . ?
C58 C51 Rh1 70.68(9) . . ?
C52 C51 Rh1 110.85(11) . . ?
C58 C51 H51 116.5(15) . . ?
C52 C51 H51 115.9(15) . . ?
Rh1 C51 H51 100.1(15) . . ?
C51 C52 C53 112.45(14) . . ?
C51 C52 H52A 109.1 . . ?
C53 C52 H52A 109.1 . . ?
C51 C52 H52B 109.1 . . ?
C53 C52 H52B 109.1 . . ?
H52A C52 H52B 107.8 . . ?
C54 C53 C52 113.29(14) . . ?
C54 C53 H53A 108.9 . . ?
C52 C53 H53A 108.9 . . ?
C54 C53 H53B 108.9 . . ?
C52 C53 H53B 108.9 . . ?
H53A C53 H53B 107.7 . . ?
C55 C54 C53 126.14(15) . . ?
C55 C54 Rh1 71.10(9) . . ?
C53 C54 Rh1 109.97(12) . . ?
C55 C54 H54 116.8(15) . . ?
C53 C54 H54 113.4(15) . . ?
Rh1 C54 H54 108.7(15) . . ?
C54 C55 C56 124.60(15) . . ?
C54 C55 Rh1 70.13(9) . . ?
C56 C55 Rh1 112.26(11) . . ?
C54 C55 H55 116.8(15) . . ?
C56 C55 H55 114.5(15) . . ?
Rh1 C55 H55 107.6(15) . . ?
C55 C56 C57 111.17(14) . . ?
C55 C56 H56A 109.4 . . ?
C57 C56 H56A 109.4 . . ?
C55 C56 H56B 109.4 . . ?
C57 C56 H56B 109.4 . . ?
H56A C56 H56B 108 . . ?
C58 C57 C56 112.98(14) . . ?
C58 C57 H57A 109 . . ?
C56 C57 H57A 109 . . ?
C58 C57 H57B 109 . . ?
C56 C57 H57B 109 . . ?
H57A C57 H57B 107.8 . . ?
C51 C58 C57 127.82(16) . . ?
C51 C58 Rh1 72.87(10) . . ?
C57 C58 Rh1 105.02(11) . . ?
C51 C58 H58 116.4(15) . . ?
C57 C58 H58 114.6(15) . . ?
Rh1 C58 H58 103.5(15) . . ?
C1 N1 C2 110.92(13) . . ?
C1 N1 C11 126.44(13) . . ?
C2 N1 C11 122.53(13) . . ?
C1 N2 C3 111.70(13) . . ?
C1 N2 C4 124.85(13) . . ?
C3 N2 C4 123.41(13) . . ?
C6 P1 C31 112.61(7) . . ?
C6 P1 C21 109.32(8) . . ?
C31 P1 C21 107.74(7) . . ?
C6 P1 C41 111.42(8) . . ?
C31 P1 C41 104.81(7) . . ?
C21 P1 C41 110.84(8) . . ?
C1 Rh1 C54 89.36(6) . . ?
C1 Rh1 C55 93.63(6) . . ?
C54 Rh1 C55 38.77(7) . . ?
C1 Rh1 C58 161.53(6) . . ?
C54 Rh1 C58 98.31(6) . . ?
C55 Rh1 C58 82.30(6) . . ?
C1 Rh1 C51 161.97(6) . . ?
C54 Rh1 C51 81.58(7) . . ?
C55 Rh1 C51 89.03(6) . . ?
C58 Rh1 C51 36.45(6) . . ?
C1 Rh1 Br1 90.94(4) . . ?
C54 Rh1 Br1 156.51(5) . . ?
C55 Rh1 Br1 164.26(5) . . ?
C58 Rh1 Br1 88.62(5) . . ?
C51 Rh1 Br1 91.27(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
C61 C60A O1 C60A -142.3(4) . . . 2_756 ?
N1 C2 C3 N2 -0.09(19) . . . . ?
N2 C4 C5 C6 174.06(13) . . . . ?
C4 C5 C6 P1 167.74(11) . . . . ?
C16 C11 C12 C13 -1.1(2) . . . . ?
N1 C11 C12 C13 -176.91(14) . . . . ?
C16 C11 C12 C17 176.16(16) . . . . ?
N1 C11 C12 C17 0.3(2) . . . . ?
C11 C12 C13 C14 1.0(3) . . . . ?
C17 C12 C13 C14 -176.25(16) . . . . ?
C12 C13 C14 C15 -0.9(3) . . . . ?
C12 C13 C14 C18 177.05(17) . . . . ?
C13 C14 C15 C16 0.8(3) . . . . ?
C18 C14 C15 C16 -177.17(16) . . . . ?
C14 C15 C16 C11 -0.8(2) . . . . ?
C14 C15 C16 C19 177.19(16) . . . . ?
C12 C11 C16 C15 1.0(2) . . . . ?
N1 C11 C16 C15 176.90(14) . . . . ?
C12 C11 C16 C19 -177.00(15) . . . . ?
N1 C11 C16 C19 -1.1(2) . . . . ?
C26 C21 C22 C23 -1.4(3) . . . . ?
P1 C21 C22 C23 174.63(17) . . . . ?
C21 C22 C23 C24 0.9(3) . . . . ?
C22 C23 C24 C25 0.6(4) . . . . ?
C23 C24 C25 C26 -1.7(3) . . . . ?
C22 C21 C26 C25 0.4(3) . . . . ?
P1 C21 C26 C25 -175.43(14) . . . . ?
C24 C25 C26 C21 1.2(3) . . . . ?
C36 C31 C32 C33 2.6(3) . . . . ?
P1 C31 C32 C33 -167.76(14) . . . . ?
C31 C32 C33 C34 0.4(3) . . . . ?
C32 C33 C34 C35 -3.0(3) . . . . ?
C33 C34 C35 C36 2.8(3) . . . . ?
C34 C35 C36 C31 0.1(3) . . . . ?
C32 C31 C36 C35 -2.8(2) . . . . ?
P1 C31 C36 C35 167.63(13) . . . . ?
C46 C41 C42 C43 3.1(2) . . . . ?
P1 C41 C42 C43 -178.99(13) . . . . ?
C41 C42 C43 C44 -0.3(3) . . . . ?
C42 C43 C44 C45 -2.5(3) . . . . ?
C43 C44 C45 C46 2.4(3) . . . . ?
C44 C45 C46 C41 0.4(2) . . . . ?
C42 C41 C46 C45 -3.1(2) . . . . ?
P1 C41 C46 C45 179.02(12) . . . . ?
C58 C51 C52 C53 -93.7(2) . . . . ?
Rh1 C51 C52 C53 -12.92(19) . . . . ?
C51 C52 C53 C54 33.9(2) . . . . ?
C52 C53 C54 C55 42.4(2) . . . . ?
C52 C53 C54 Rh1 -38.35(18) . . . . ?
C53 C54 C55 C56 2.5(3) . . . . ?
Rh1 C54 C55 C56 103.89(16) . . . . ?
C53 C54 C55 Rh1 -101.36(17) . . . . ?
C54 C55 C56 C57 -95.68(19) . . . . ?
Rh1 C55 C56 C57 -15.11(18) . . . . ?
C55 C56 C57 C58 40.4(2) . . . . ?
C52 C51 C58 C57 6.2(3) . . . . ?
Rh1 C51 C58 C57 -95.97(17) . . . . ?
C52 C51 C58 Rh1 102.16(17) . . . . ?
C56 C57 C58 C51 36.2(2) . . . . ?
C56 C57 C58 Rh1 -43.53(16) . . . . ?
N2 C1 N1 C2 0.11(17) . . . . ?
Rh1 C1 N1 C2 178.68(12) . . . . ?
N2 C1 N1 C11 -176.11(14) . . . . ?
Rh1 C1 N1 C11 2.5(2) . . . . ?
C3 C2 N1 C1 -0.01(19) . . . . ?
C3 C2 N1 C11 176.38(14) . . . . ?
C16 C11 N1 C1 103.68(18) . . . . ?
C12 C11 N1 C1 -80.3(2) . . . . ?
C16 C11 N1 C2 -72.1(2) . . . . ?
C12 C11 N1 C2 103.88(18) . . . . ?
N1 C1 N2 C3 -0.17(17) . . . . ?
Rh1 C1 N2 C3 -178.87(11) . . . . ?
N1 C1 N2 C4 -178.06(13) . . . . ?
Rh1 C1 N2 C4 3.2(2) . . . . ?
C2 C3 N2 C1 0.16(19) . . . . ?
C2 C3 N2 C4 178.09(14) . . . . ?
C5 C4 N2 C1 105.02(17) . . . . ?
C5 C4 N2 C3 -72.64(19) . . . . ?
C5 C6 P1 C31 169.48(11) . . . . ?
C5 C6 P1 C21 49.77(13) . . . . ?
C5 C6 P1 C41 -73.07(13) . . . . ?
C32 C31 P1 C6 -131.48(14) . . . . ?
C36 C31 P1 C6 58.06(15) . . . . ?
C32 C31 P1 C21 -10.86(16) . . . . ?
C36 C31 P1 C21 178.68(13) . . . . ?
C32 C31 P1 C41 107.23(14) . . . . ?
C36 C31 P1 C41 -63.23(14) . . . . ?
C26 C21 P1 C6 -135.45(14) . . . . ?
C22 C21 P1 C6 48.61(16) . . . . ?
C26 C21 P1 C31 101.88(15) . . . . ?
C22 C21 P1 C31 -74.06(15) . . . . ?
C26 C21 P1 C41 -12.26(17) . . . . ?
C22 C21 P1 C41 171.80(14) . . . . ?
C46 C41 P1 C6 2.85(16) . . . . ?
C42 C41 P1 C6 -175.04(12) . . . . ?
C46 C41 P1 C31 124.92(14) . . . . ?
C42 C41 P1 C31 -52.98(14) . . . . ?
C46 C41 P1 C21 -119.12(14) . . . . ?
C42 C41 P1 C21 62.99(15) . . . . ?

####################################################################### 
# 
# 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_8OTf
_database_code_depnum_ccdc_archive 'CCDC 1558462'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;

_audit_creation_date             2017-05-04T18:39:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C37 H34 Cl F3 N2 O3 P Pd S'

_chemical_formula_moiety         'C36 H34 Cl N2 P Pd, C F3 O3 S'
_chemical_formula_weight         816.54

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_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                   32.4379(16)
_cell_length_b                   12.1195(6)
_cell_length_c                   24.8212(13)
_cell_angle_alpha                90
_cell_angle_beta                 128.4130(10)
_cell_angle_gamma                90
_cell_volume                     7645.9(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      2.09
_cell_measurement_reflns_used    9999
_cell_measurement_theta_max      36.29
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3320.0

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.6397
_exptl_absorpt_correction_T_max  0.7465

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Incoatec I\mS Microsource '
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_number            112392
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.094
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             7829
_reflns_number_gt                7362
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0295P)²+16.2252P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7829
_refine_ls_number_parameters     455
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.0676
_refine_ls_wR_factor_gt          0.0659
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.064

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
F F 0.0171 0.0103 '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 0.006 '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'
Pd Pd -0.9988 1.0072 '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'

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
C1 C 0.36684(7) 0.35806(14) 0.35660(9) 0.0130(3) Uani 1 1 d . . . . .
C2 C 0.43134(7) 0.39607(16) 0.46944(9) 0.0184(4) Uani 1 1 d . . . . .
H2 H 0.4609 0.4303 0.5098 0.022 Uiso 1 1 calc R U . . .
C3 C 0.40328(7) 0.31125(15) 0.46644(9) 0.0186(4) Uani 1 1 d . . . . .
H3 H 0.4091 0.2739 0.5043 0.022 Uiso 1 1 calc R U . . .
C4 C 0.32622(7) 0.19821(14) 0.37287(9) 0.0147(3) Uani 1 1 d . . . . .
H4A H 0.3448 0.1331 0.4027 0.018 Uiso 1 1 calc R U . . .
H4B H 0.3121 0.1778 0.3256 0.018 Uiso 1 1 calc R U . . .
C5 C 0.28055(7) 0.22772(14) 0.37290(9) 0.0147(3) Uani 1 1 d . . . . .
H5A H 0.2944 0.2651 0.4167 0.018 Uiso 1 1 calc R U . . .
H5B H 0.2628 0.1591 0.3702 0.018 Uiso 1 1 calc R U . . .
C6 C 0.24019(7) 0.30340(14) 0.31247(9) 0.0143(3) Uani 1 1 d . . . . .
H6A H 0.2191 0.2599 0.2694 0.017 Uiso 1 1 calc R U . . .
H6B H 0.2589 0.3618 0.3073 0.017 Uiso 1 1 calc R U . . .
C7 C 0.26217(11) 0.3684(2) 0.13992(12) 0.0473(7) Uani 1 1 d . . . . .
C8A C 0.2785(3) 0.2727(5) 0.1658(3) 0.031(2) Uani 0.423(14) 1 d . . P . .
C8B C 0.3043(3) 0.3021(4) 0.16560(19) 0.0339(19) Uani 0.577(14) 1 d . . P . .
C9 C 0.32711(11) 0.2304(2) 0.21770(12) 0.0455(7) Uani 1 1 d . . . . .
C11 C 0.43266(7) 0.49953(14) 0.38400(8) 0.0141(3) Uani 1 1 d . . . . .
C12 C 0.46253(7) 0.45497(15) 0.36623(9) 0.0167(3) Uani 1 1 d . . . . .
C13 C 0.48634(7) 0.52764(16) 0.34965(9) 0.0185(4) Uani 1 1 d . . . . .
H13 H 0.5064 0.4988 0.3369 0.022 Uiso 1 1 calc R U . . .
C14 C 0.48153(7) 0.64142(15) 0.35127(9) 0.0175(4) Uani 1 1 d . . . . .
C15 C 0.45326(7) 0.68255(15) 0.37208(9) 0.0166(3) Uani 1 1 d . . . . .
H15 H 0.4508 0.7601 0.375 0.02 Uiso 1 1 calc R U . . .
C16 C 0.42841(7) 0.61307(15) 0.38881(9) 0.0155(3) Uani 1 1 d . . . . .
C17 C 0.47008(8) 0.33216(16) 0.36690(11) 0.0248(4) Uani 1 1 d . . . . .
H17A H 0.4371 0.2982 0.328 0.037 Uiso 1 1 calc R U . . .
H17B H 0.4801 0.3011 0.41 0.037 Uiso 1 1 calc R U . . .
H17C H 0.4979 0.3173 0.3631 0.037 Uiso 1 1 calc R U . . .
C18 C 0.50577(8) 0.71862(17) 0.33047(11) 0.0251(4) Uani 1 1 d . . . . .
H18A H 0.534 0.6804 0.334 0.038 Uiso 1 1 calc R U . . .
H18B H 0.5203 0.783 0.3609 0.038 Uiso 1 1 calc R U . . .
H18C H 0.4788 0.7427 0.2829 0.038 Uiso 1 1 calc R U . . .
C19 C 0.39924(8) 0.65976(16) 0.41266(10) 0.0220(4) Uani 1 1 d . . . . .
H19A H 0.4184 0.6424 0.4614 0.033 Uiso 1 1 calc R U . . .
H19B H 0.364 0.6273 0.3857 0.033 Uiso 1 1 calc R U . . .
H19C H 0.3963 0.74 0.4064 0.033 Uiso 1 1 calc R U . . .
C21 C 0.23319(7) 0.46896(14) 0.39221(9) 0.0153(3) Uani 1 1 d . . . . .
C22 C 0.28329(7) 0.50184(15) 0.41580(9) 0.0171(3) Uani 1 1 d . . . . .
H22 H 0.2984 0.4705 0.3966 0.021 Uiso 1 1 calc R U . . .
C23 C 0.31068(7) 0.58053(15) 0.46743(10) 0.0202(4) Uani 1 1 d . . . . .
H23 H 0.3444 0.6042 0.483 0.024 Uiso 1 1 calc R U . . .
C24 C 0.28892(8) 0.62477(15) 0.49636(10) 0.0210(4) Uani 1 1 d . . . . .
H24 H 0.3083 0.6767 0.5328 0.025 Uiso 1 1 calc R U . . .
C25 C 0.23899(8) 0.59340(16) 0.47223(10) 0.0213(4) Uani 1 1 d . . . . .
H25 H 0.2242 0.6245 0.4919 0.026 Uiso 1 1 calc R U . . .
C26 C 0.21053(7) 0.51676(15) 0.41948(10) 0.0191(4) Uani 1 1 d . . . . .
H26 H 0.1759 0.497 0.402 0.023 Uiso 1 1 calc R U . . .
C31 C 0.17435(7) 0.25785(15) 0.35163(9) 0.0155(3) Uani 1 1 d . . . . .
C32 C 0.14896(8) 0.16962(16) 0.30555(10) 0.0227(4) Uani 1 1 d . . . . .
H32 H 0.1447 0.1697 0.2641 0.027 Uiso 1 1 calc R U . . .
C33 C 0.13006(8) 0.08242(17) 0.32046(10) 0.0254(4) Uani 1 1 d . . . . .
H33 H 0.1129 0.0224 0.2893 0.031 Uiso 1 1 calc R U . . .
C34 C 0.13619(8) 0.08277(17) 0.38095(10) 0.0241(4) Uani 1 1 d . . . . .
H34 H 0.1226 0.0235 0.3908 0.029 Uiso 1 1 calc R U . . .
C35 C 0.16181(9) 0.16874(18) 0.42678(11) 0.0288(4) Uani 1 1 d . . . . .
H35 H 0.1662 0.1679 0.4683 0.035 Uiso 1 1 calc R U . . .
C36 C 0.18138(8) 0.25676(16) 0.41286(10) 0.0229(4) Uani 1 1 d . . . . .
H36 H 0.1994 0.3155 0.4449 0.027 Uiso 1 1 calc R U . . .
C41 C 0.14058(7) 0.42510(14) 0.24834(9) 0.0161(3) Uani 1 1 d . . . . .
C42 C 0.14126(7) 0.45217(15) 0.19430(10) 0.0193(4) Uani 1 1 d . . . . .
H42 H 0.1721 0.4405 0.1984 0.023 Uiso 1 1 calc R U . . .
C43 C 0.09615(8) 0.49665(16) 0.13401(10) 0.0243(4) Uani 1 1 d . . . . .
H43 H 0.0961 0.5149 0.0968 0.029 Uiso 1 1 calc R U . . .
C44 C 0.05139(8) 0.51425(16) 0.12846(11) 0.0254(4) Uani 1 1 d . . . . .
H44 H 0.0208 0.5442 0.0872 0.03 Uiso 1 1 calc R U . . .
C45 C 0.05093(8) 0.48860(17) 0.18253(11) 0.0252(4) Uani 1 1 d . . . . .
H45 H 0.0202 0.5016 0.1784 0.03 Uiso 1 1 calc R U . . .
C46 C 0.09544(7) 0.44389(16) 0.24284(10) 0.0204(4) Uani 1 1 d . . . . .
H46 H 0.0953 0.4262 0.28 0.025 Uiso 1 1 calc R U . . .
C100 C 0.10911(9) 0.61255(18) 0.47558(15) 0.0373(6) Uani 1 1 d . . . . .
Cl1 Cl 0.27931(2) 0.54097(3) 0.26270(2) 0.01689(9) Uani 1 1 d . . . . .
F1 F 0.06075(6) 0.65490(12) 0.43910(11) 0.0610(5) Uani 1 1 d . . . . .
F2 F 0.13049(7) 0.61696(16) 0.54225(10) 0.0665(6) Uani 1 1 d . . . . .
F3 F 0.13712(6) 0.67758(12) 0.46649(12) 0.0705(6) Uani 1 1 d . . . . .
N1 N 0.40868(6) 0.42402(12) 0.40195(7) 0.0140(3) Uani 1 1 d . . . . .
N2 N 0.36403(6) 0.28883(12) 0.39710(7) 0.0136(3) Uani 1 1 d . . . . .
O1 O 0.16262(6) 0.44024(12) 0.49700(8) 0.0262(3) Uani 1 1 d . . . . .
O2 O 0.07419(6) 0.41940(12) 0.46169(8) 0.0299(3) Uani 1 1 d . . . . .
O3 O 0.08651(7) 0.48117(18) 0.37955(8) 0.0452(5) Uani 1 1 d . . . . .
P1 P 0.19734(2) 0.36573(4) 0.32646(2) 0.01286(9) Uani 1 1 d . . . . .
Pd1 Pd 0.31449(2) 0.37611(2) 0.25240(2) 0.01474(5) Uani 1 1 d . . . . .
S1 S 0.10805(2) 0.47152(4) 0.45024(2) 0.01763(9) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N2 1.355(2) . ?
C1 N1 1.360(2) . ?
C1 Pd1 2.0404(17) . ?
C2 C3 1.344(3) . ?
C2 N1 1.390(2) . ?
C2 H2 0.95 . ?
C3 N2 1.391(2) . ?
C3 H3 0.95 . ?
C4 N2 1.468(2) . ?
C4 C5 1.524(2) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 C6 1.538(2) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 P1 1.7955(17) . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
C7 C8A 1.271(7) . ?
C7 C8B 1.355(6) . ?
C7 Pd1 2.190(2) . ?
C8A C8B 0.913(7) . ?
C8A C9 1.374(7) . ?
C8A Pd1 2.106(5) . ?
C8B C9 1.337(5) . ?
C8B Pd1 2.161(4) . ?
C9 Pd1 2.113(2) . ?
C11 C16 1.395(2) . ?
C11 C12 1.399(2) . ?
C11 N1 1.439(2) . ?
C12 C13 1.392(3) . ?
C12 C17 1.507(3) . ?
C13 C14 1.391(3) . ?
C13 H13 0.95 . ?
C14 C15 1.395(3) . ?
C14 C18 1.505(3) . ?
C15 C16 1.395(3) . ?
C15 H15 0.95 . ?
C16 C19 1.504(2) . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C21 C26 1.397(2) . ?
C21 C22 1.400(2) . ?
C21 P1 1.7952(18) . ?
C22 C23 1.388(3) . ?
C22 H22 0.95 . ?
C23 C24 1.390(3) . ?
C23 H23 0.95 . ?
C24 C25 1.386(3) . ?
C24 H24 0.95 . ?
C25 C26 1.388(3) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
C31 C36 1.390(3) . ?
C31 C32 1.400(3) . ?
C31 P1 1.7983(18) . ?
C32 C33 1.383(3) . ?
C32 H32 0.95 . ?
C33 C34 1.387(3) . ?
C33 H33 0.95 . ?
C34 C35 1.377(3) . ?
C34 H34 0.95 . ?
C35 C36 1.390(3) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C41 C42 1.394(3) . ?
C41 C46 1.402(3) . ?
C41 P1 1.7975(18) . ?
C42 C43 1.396(3) . ?
C42 H42 0.95 . ?
C43 C44 1.387(3) . ?
C43 H43 0.95 . ?
C44 C45 1.387(3) . ?
C44 H44 0.95 . ?
C45 C46 1.390(3) . ?
C45 H45 0.95 . ?
C46 H46 0.95 . ?
C100 F3 1.324(3) . ?
C100 F1 1.334(3) . ?
C100 F2 1.340(4) . ?
C100 S1 1.814(2) . ?
Cl1 Pd1 2.3922(4) . ?
O1 S1 1.4391(15) . ?
O2 S1 1.4404(14) . ?
O3 S1 1.4342(16) . ?

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
N2 C1 N1 104.03(14) . . ?
N2 C1 Pd1 128.31(13) . . ?
N1 C1 Pd1 127.07(12) . . ?
C3 C2 N1 106.67(16) . . ?
C3 C2 H2 126.7 . . ?
N1 C2 H2 126.7 . . ?
C2 C3 N2 106.60(15) . . ?
C2 C3 H3 126.7 . . ?
N2 C3 H3 126.7 . . ?
N2 C4 C5 112.90(14) . . ?
N2 C4 H4A 109 . . ?
C5 C4 H4A 109 . . ?
N2 C4 H4B 109 . . ?
C5 C4 H4B 109 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 C6 112.21(14) . . ?
C4 C5 H5A 109.2 . . ?
C6 C5 H5A 109.2 . . ?
C4 C5 H5B 109.2 . . ?
C6 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
C5 C6 P1 110.76(11) . . ?
C5 C6 H6A 109.5 . . ?
P1 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
P1 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C8A C7 C8B 40.5(3) . . ?
C8A C7 Pd1 69.2(2) . . ?
C8B C7 Pd1 70.69(18) . . ?
C8B C8A C7 74.7(6) . . ?
C8B C8A C9 68.1(5) . . ?
C7 C8A C9 133.6(7) . . ?
C8B C8A Pd1 81.0(4) . . ?
C7 C8A Pd1 76.4(3) . . ?
C9 C8A Pd1 71.3(2) . . ?
C8A C8B C9 72.5(5) . . ?
C8A C8B C7 64.7(6) . . ?
C9 C8B C7 129.1(6) . . ?
C8A C8B Pd1 74.3(4) . . ?
C9 C8B Pd1 69.84(19) . . ?
C7 C8B Pd1 73.0(2) . . ?
C8B C9 C8A 39.3(3) . . ?
C8B C9 Pd1 73.7(2) . . ?
C8A C9 Pd1 70.7(2) . . ?
C16 C11 C12 122.17(16) . . ?
C16 C11 N1 119.96(16) . . ?
C12 C11 N1 117.75(15) . . ?
C13 C12 C11 118.00(16) . . ?
C13 C12 C17 120.81(16) . . ?
C11 C12 C17 121.16(16) . . ?
C14 C13 C12 121.72(17) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C13 C14 C15 118.46(17) . . ?
C13 C14 C18 120.95(17) . . ?
C15 C14 C18 120.59(17) . . ?
C16 C15 C14 121.93(17) . . ?
C16 C15 H15 119 . . ?
C14 C15 H15 119 . . ?
C15 C16 C11 117.62(16) . . ?
C15 C16 C19 120.73(16) . . ?
C11 C16 C19 121.64(16) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C26 C21 C22 120.19(16) . . ?
C26 C21 P1 119.38(14) . . ?
C22 C21 P1 120.43(13) . . ?
C23 C22 C21 119.49(16) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 120.21(17) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C25 C24 C23 120.21(17) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 C26 120.31(17) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 119.52(17) . . ?
C25 C26 H26 120.2 . . ?
C21 C26 H26 120.2 . . ?
C36 C31 C32 119.98(17) . . ?
C36 C31 P1 124.40(14) . . ?
C32 C31 P1 115.60(14) . . ?
C33 C32 C31 119.93(18) . . ?
C33 C32 H32 120 . . ?
C31 C32 H32 120 . . ?
C32 C33 C34 119.89(19) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C35 C34 C33 120.25(18) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C34 C35 C36 120.65(18) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C31 C36 C35 119.28(18) . . ?
C31 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
C42 C41 C46 120.52(17) . . ?
C42 C41 P1 120.94(14) . . ?
C46 C41 P1 118.54(14) . . ?
C41 C42 C43 119.30(17) . . ?
C41 C42 H42 120.4 . . ?
C43 C42 H42 120.4 . . ?
C44 C43 C42 120.08(19) . . ?
C44 C43 H43 120 . . ?
C42 C43 H43 120 . . ?
C43 C44 C45 120.62(18) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 H44 119.7 . . ?
C44 C45 C46 120.07(18) . . ?
C44 C45 H45 120 . . ?
C46 C45 H45 120 . . ?
C45 C46 C41 119.41(18) . . ?
C45 C46 H46 120.3 . . ?
C41 C46 H46 120.3 . . ?
F3 C100 F1 107.3(2) . . ?
F3 C100 F2 107.7(2) . . ?
F1 C100 F2 108.1(2) . . ?
F3 C100 S1 111.66(18) . . ?
F1 C100 S1 111.49(17) . . ?
F2 C100 S1 110.46(17) . . ?
C1 N1 C2 111.28(14) . . ?
C1 N1 C11 124.81(14) . . ?
C2 N1 C11 123.05(15) . . ?
C1 N2 C3 111.42(14) . . ?
C1 N2 C4 125.69(14) . . ?
C3 N2 C4 122.86(14) . . ?
C21 P1 C6 109.08(8) . . ?
C21 P1 C41 110.65(8) . . ?
C6 P1 C41 110.91(8) . . ?
C21 P1 C31 111.42(8) . . ?
C6 P1 C31 107.41(8) . . ?
C41 P1 C31 107.33(8) . . ?
C1 Pd1 C8A 136.65(17) . . ?
C1 Pd1 C9 101.98(8) . . ?
C8A Pd1 C9 38.00(19) . . ?
C1 Pd1 C8B 135.28(13) . . ?
C8A Pd1 C8B 24.67(18) . . ?
C9 Pd1 C8B 36.43(14) . . ?
C1 Pd1 C7 170.71(9) . . ?
C8A Pd1 C7 34.34(18) . . ?
C9 Pd1 C7 68.77(10) . . ?
C8B Pd1 C7 36.30(15) . . ?
C1 Pd1 Cl1 91.76(5) . . ?
C8A Pd1 Cl1 127.37(17) . . ?
C9 Pd1 Cl1 165.38(7) . . ?
C8B Pd1 Cl1 131.72(11) . . ?
C7 Pd1 Cl1 97.38(7) . . ?
O3 S1 O1 115.37(10) . . ?
O3 S1 O2 115.19(10) . . ?
O1 S1 O2 115.59(9) . . ?
O3 S1 C100 103.72(13) . . ?
O1 S1 C100 102.69(10) . . ?
O2 S1 C100 101.37(10) . . ?


####################################################################### 
# 
# 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_2OTf2
_database_code_depnum_ccdc_archive 'CCDC 1558457'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;

_audit_creation_date             2017-05-04T18:18:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C27 H27 F6 N2 O6 P S2'
_chemical_formula_moiety         'C25 H27 N2 P, 2(C F3 O3 S)'
_chemical_formula_weight         684.59

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.854(2)
_cell_length_b                   12.357(2)
_cell_length_c                   13.259(2)
_cell_angle_alpha                75.729(5)
_cell_angle_beta                 66.227(5)
_cell_angle_gamma                71.854(5)
_cell_volume                     1531.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      1.80
_cell_measurement_reflns_used    9999
_cell_measurement_theta_max      36.29
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             704

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.4319
_exptl_absorpt_correction_T_max  0.7461


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Incoatec I\mS Microsource '
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_number            20616
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.112
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.976
_reflns_Friedel_coverage         0
_reflns_number_total             6127
_reflns_number_gt                4615
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0678P)²+1.3440P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6127
_refine_ls_number_parameters     398
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1478
_refine_ls_wR_factor_gt          0.1298
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.085

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'

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
C1 C 0.3369(3) 0.6713(2) 1.0096(2) 0.0244(6) Uani 1 1 d . . . . .
H011 H 0.3861 0.6115 1.047 0.029 Uiso 1 1 calc R U . . .
C2 C 0.1887(3) 0.7699(3) 0.9278(2) 0.0258(7) Uani 1 1 d . . . . .
H013 H 0.1179 0.7891 0.8994 0.031 Uiso 1 1 calc R U . . .
C3 C 0.2655(3) 0.8400(2) 0.9220(2) 0.0211(6) Uani 1 1 d . . . . .
H00V H 0.2576 0.9164 0.8892 0.025 Uiso 1 1 calc R U . . .
C4 C 0.4567(3) 0.8184(3) 0.9952(2) 0.0239(6) Uani 1 1 d . . . . .
H4A H 0.4719 0.7736 1.0622 0.029 Uiso 1 1 calc R U . . .
H4B H 0.4159 0.8977 1.0087 0.029 Uiso 1 1 calc R U . . .
C5 C 0.5964(3) 0.8120(2) 0.9005(2) 0.0213(6) Uani 1 1 d . . . . .
H5A H 0.6392 0.7325 0.8883 0.026 Uiso 1 1 calc R U . . .
H5B H 0.6564 0.8386 0.9219 0.026 Uiso 1 1 calc R U . . .
C6 C 0.5835(3) 0.8844(2) 0.7920(2) 0.0166(5) Uani 1 1 d . . . . .
H6A H 0.5138 0.9552 0.8101 0.02 Uiso 1 1 calc R U . . .
H6B H 0.5494 0.843 0.7594 0.02 Uiso 1 1 calc R U . . .
C7 C 0.1787(4) 0.5631(3) 1.0079(3) 0.0408(9) Uani 1 1 d . . . . .
H7A H 0.0822 0.587 1.0169 0.061 Uiso 1 1 calc R U . . .
H7B H 0.1891 0.5177 1.0753 0.061 Uiso 1 1 calc R U . . .
H7C H 0.2286 0.5182 0.9477 0.061 Uiso 1 1 calc R U . . .
C8 C 0.5340(3) 0.5129(2) 0.6386(2) 0.0241(6) Uani 1 1 d . . . . .
C9 C 0.2177(3) 0.2988(3) 0.7750(3) 0.0339(8) Uani 1 1 d . . . . .
C21 C 0.6964(3) 0.9919(2) 0.5670(2) 0.0159(5) Uani 1 1 d . . . . .
C22 C 0.5784(3) 1.0830(2) 0.5782(2) 0.0193(6) Uani 1 1 d . . . . .
H22 H 0.5198 1.1029 0.6482 0.023 Uiso 1 1 calc R U . . .
C23 C 0.5496(3) 1.1430(2) 0.4845(2) 0.0224(6) Uani 1 1 d . . . . .
H23 H 0.4724 1.2045 0.4911 0.027 Uiso 1 1 calc R U . . .
C24 C 0.6360(3) 1.1116(2) 0.3807(2) 0.0233(6) Uani 1 1 d . . . . .
H24 H 0.6172 1.1532 0.3177 0.028 Uiso 1 1 calc R U . . .
C25 C 0.7494(3) 1.0194(2) 0.3697(2) 0.0234(6) Uani 1 1 d . . . . .
H25 H 0.805 0.9976 0.2999 0.028 Uiso 1 1 calc R U . . .
C26 C 0.7807(3) 0.9592(2) 0.4629(2) 0.0186(6) Uani 1 1 d . . . . .
H26 H 0.8576 0.8974 0.4558 0.022 Uiso 1 1 calc R U . . .
C31 C 0.8799(3) 0.7975(2) 0.6537(2) 0.0172(6) Uani 1 1 d . . . . .
C32 C 1.0151(3) 0.8052(2) 0.6235(2) 0.0218(6) Uani 1 1 d . . . . .
H32 H 1.033 0.8744 0.6223 0.026 Uiso 1 1 calc R U . . .
C33 C 1.1239(3) 0.7093(3) 0.5949(3) 0.0300(7) Uani 1 1 d . . . . .
H33 H 1.2149 0.7143 0.574 0.036 Uiso 1 1 calc R U . . .
C34 C 1.0963(3) 0.6071(3) 0.5978(3) 0.0362(8) Uani 1 1 d . . . . .
H34 H 1.169 0.5427 0.5793 0.043 Uiso 1 1 calc R U . . .
C35 C 0.9620(3) 0.5991(3) 0.6278(3) 0.0369(8) Uani 1 1 d . . . . .
H35 H 0.9448 0.5294 0.6294 0.044 Uiso 1 1 calc R U . . .
C36 C 0.8518(3) 0.6944(2) 0.6555(3) 0.0257(6) Uani 1 1 d . . . . .
H36 H 0.7611 0.6894 0.675 0.031 Uiso 1 1 calc R U . . .
C41 C 0.7951(3) 1.0174(2) 0.7325(2) 0.0165(5) Uani 1 1 d . . . . .
C42 C 0.8573(3) 0.9733(2) 0.8133(2) 0.0195(6) Uani 1 1 d . . . . .
H42 H 0.8647 0.8967 0.8454 0.023 Uiso 1 1 calc R U . . .
C43 C 0.9074(3) 1.0443(2) 0.8447(2) 0.0215(6) Uani 1 1 d . . . . .
H43 H 0.9487 1.0154 0.8982 0.026 Uiso 1 1 calc R U . . .
C44 C 0.8965(3) 1.1587(2) 0.7970(2) 0.0230(6) Uani 1 1 d . . . . .
H44 H 0.9317 1.2057 0.818 0.028 Uiso 1 1 calc R U . . .
C45 C 0.8336(3) 1.2027(2) 0.7185(2) 0.0243(6) Uani 1 1 d . . . . .
H45 H 0.8249 1.2797 0.6878 0.029 Uiso 1 1 calc R U . . .
C46 C 0.7835(3) 1.1321(2) 0.6856(2) 0.0213(6) Uani 1 1 d . . . . .
H46 H 0.7421 1.1615 0.6321 0.026 Uiso 1 1 calc R U . . .
F1 F 0.4012(2) 0.55447(15) 0.64900(17) 0.0367(5) Uani 1 1 d . . . . .
F2 F 0.6086(2) 0.56738(15) 0.54408(15) 0.0409(5) Uani 1 1 d . . . . .
F3 F 0.5683(2) 0.40197(14) 0.62728(16) 0.0387(5) Uani 1 1 d . . . . .
F4 F 0.0887(2) 0.35024(15) 0.77825(16) 0.0381(5) Uani 1 1 d . . . . .
F5 F 0.2712(3) 0.3794(2) 0.7775(3) 0.0898(10) Uani 1 1 d . . . . .
F6 F 0.2831(3) 0.2599(3) 0.67937(18) 0.1016(13) Uani 1 1 d . . . . .
N1 N 0.2340(3) 0.6653(2) 0.9830(2) 0.0250(5) Uani 1 1 d . . . . .
N2 N 0.3581(2) 0.77659(19) 0.97426(18) 0.0192(5) Uani 1 1 d . . . . .
O1 O 0.5230(2) 0.65753(15) 0.75272(17) 0.0254(5) Uani 1 1 d . . . . .
O2 O 0.7101(2) 0.48520(17) 0.7321(2) 0.0313(5) Uani 1 1 d . . . . .
O3 O 0.4767(2) 0.47217(17) 0.85039(17) 0.0275(5) Uani 1 1 d . . . . .
O4 O 0.3657(2) 0.13623(19) 0.87045(19) 0.0351(6) Uani 1 1 d . . . . .
O5 O 0.1491(3) 0.11104(19) 0.8799(2) 0.0496(7) Uani 1 1 d . . . . .
O6 O 0.1467(2) 0.2448(2) 0.98534(18) 0.0378(6) Uani 1 1 d . . . . .
P1 P 0.73888(7) 0.92137(5) 0.68763(5) 0.01452(17) Uani 1 1 d . . . . .
S1 S 0.56460(7) 0.53406(5) 0.75646(6) 0.01984(17) Uani 1 1 d . . . . .
S2 S 0.22072(8) 0.18507(6) 0.89024(6) 0.02141(18) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N1 1.326(4) . ?
C1 N2 1.328(4) . ?
C1 H011 0.93 . ?
C2 C3 1.347(4) . ?
C2 N1 1.370(4) . ?
C2 H013 0.93 . ?
C3 N2 1.381(3) . ?
C3 H00V 0.93 . ?
C4 N2 1.464(4) . ?
C4 C5 1.523(4) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 C6 1.530(4) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C6 P1 1.804(3) . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C7 N1 1.473(4) . ?
C7 H7A 0.96 . ?
C7 H7B 0.96 . ?
C7 H7C 0.96 . ?
C8 F1 1.332(3) . ?
C8 F3 1.334(3) . ?
C8 F2 1.336(4) . ?
C8 S1 1.815(3) . ?
C9 F6 1.305(4) . ?
C9 F5 1.313(4) . ?
C9 F4 1.333(4) . ?
C9 S2 1.807(3) . ?
C21 C26 1.390(4) . ?
C21 C22 1.401(3) . ?
C21 P1 1.785(3) . ?
C22 C23 1.379(4) . ?
C22 H22 0.93 . ?
C23 C24 1.386(4) . ?
C23 H23 0.93 . ?
C24 C25 1.378(4) . ?
C24 H24 0.93 . ?
C25 C26 1.386(4) . ?
C25 H25 0.93 . ?
C26 H26 0.93 . ?
C31 C32 1.385(4) . ?
C31 C36 1.391(4) . ?
C31 P1 1.792(2) . ?
C32 C33 1.390(4) . ?
C32 H32 0.93 . ?
C33 C34 1.375(5) . ?
C33 H33 0.93 . ?
C34 C35 1.377(5) . ?
C34 H34 0.93 . ?
C35 C36 1.391(4) . ?
C35 H35 0.93 . ?
C36 H36 0.93 . ?
C41 C46 1.389(4) . ?
C41 C42 1.402(4) . ?
C41 P1 1.796(3) . ?
C42 C43 1.379(4) . ?
C42 H42 0.93 . ?
C43 C44 1.388(4) . ?
C43 H43 0.93 . ?
C44 C45 1.381(4) . ?
C44 H44 0.93 . ?
C45 C46 1.388(4) . ?
C45 H45 0.93 . ?
C46 H46 0.93 . ?
O1 S1 1.4442(19) . ?
O2 S1 1.433(2) . ?
O3 S1 1.440(2) . ?
O4 S2 1.436(2) . ?
O5 S2 1.432(2) . ?
O6 S2 1.433(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
N1 C1 N2 109.0(2) . . ?
N1 C1 H011 125.5 . . ?
N2 C1 H011 125.5 . . ?
C3 C2 N1 107.6(3) . . ?
C3 C2 H013 126.2 . . ?
N1 C2 H013 126.2 . . ?
C2 C3 N2 106.8(2) . . ?
C2 C3 H00V 126.6 . . ?
N2 C3 H00V 126.6 . . ?
N2 C4 C5 114.2(2) . . ?
N2 C4 H4A 108.7 . . ?
C5 C4 H4A 108.7 . . ?
N2 C4 H4B 108.7 . . ?
C5 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C4 C5 C6 112.5(2) . . ?
C4 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
C4 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
C5 C6 P1 116.86(19) . . ?
C5 C6 H6A 108.1 . . ?
P1 C6 H6A 108.1 . . ?
C5 C6 H6B 108.1 . . ?
P1 C6 H6B 108.1 . . ?
H6A C6 H6B 107.3 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
F1 C8 F3 107.8(3) . . ?
F1 C8 F2 107.3(2) . . ?
F3 C8 F2 107.6(2) . . ?
F1 C8 S1 111.27(19) . . ?
F3 C8 S1 111.94(19) . . ?
F2 C8 S1 110.7(2) . . ?
F6 C9 F5 109.7(4) . . ?
F6 C9 F4 106.0(3) . . ?
F5 C9 F4 106.3(3) . . ?
F6 C9 S2 111.8(2) . . ?
F5 C9 S2 111.0(3) . . ?
F4 C9 S2 111.7(2) . . ?
C26 C21 C22 120.2(2) . . ?
C26 C21 P1 120.77(19) . . ?
C22 C21 P1 119.0(2) . . ?
C23 C22 C21 119.5(3) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 119.9(3) . . ?
C22 C23 H23 120 . . ?
C24 C23 H23 120 . . ?
C25 C24 C23 120.8(3) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C26 119.9(3) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C25 C26 C21 119.6(2) . . ?
C25 C26 H26 120.2 . . ?
C21 C26 H26 120.2 . . ?
C32 C31 C36 120.5(2) . . ?
C32 C31 P1 120.3(2) . . ?
C36 C31 P1 119.1(2) . . ?
C31 C32 C33 119.9(3) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C34 C33 C32 119.7(3) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C35 120.6(3) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C35 C36 120.5(3) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C31 118.7(3) . . ?
C35 C36 H36 120.6 . . ?
C31 C36 H36 120.6 . . ?
C46 C41 C42 119.9(3) . . ?
C46 C41 P1 121.4(2) . . ?
C42 C41 P1 118.6(2) . . ?
C43 C42 C41 119.5(3) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C42 C43 C44 120.5(3) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C45 C44 C43 120.1(3) . . ?
C45 C44 H44 119.9 . . ?
C43 C44 H44 119.9 . . ?
C44 C45 C46 120.0(3) . . ?
C44 C45 H45 120 . . ?
C46 C45 H45 120 . . ?
C45 C46 C41 120.0(3) . . ?
C45 C46 H46 120 . . ?
C41 C46 H46 120 . . ?
C1 N1 C2 108.4(3) . . ?
C1 N1 C7 125.7(3) . . ?
C2 N1 C7 125.9(3) . . ?
C1 N2 C3 108.2(2) . . ?
C1 N2 C4 124.9(2) . . ?
C3 N2 C4 126.7(2) . . ?
C21 P1 C31 109.73(12) . . ?
C21 P1 C41 109.06(12) . . ?
C31 P1 C41 107.65(12) . . ?
C21 P1 C6 106.56(13) . . ?
C31 P1 C6 112.35(13) . . ?
C41 P1 C6 111.45(12) . . ?
O2 S1 O3 114.35(13) . . ?
O2 S1 O1 114.84(13) . . ?
O3 S1 O1 114.85(13) . . ?
O2 S1 C8 103.94(14) . . ?
O3 S1 C8 103.81(14) . . ?
O1 S1 C8 102.92(12) . . ?
O5 S2 O6 113.94(18) . . ?
O5 S2 O4 114.78(15) . . ?
O6 S2 O4 115.29(13) . . ?
O5 S2 C9 103.51(16) . . ?
O6 S2 C9 103.06(14) . . ?
O4 S2 C9 104.13(15) . . ?

####################################################################### 
# 
# 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_11OTf
_database_code_depnum_ccdc_archive 'CCDC 1558463'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;

_audit_creation_date             2017-06-12T15:31:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C39 H41 Cl0 F3 N3 O3 P Pd S'
_chemical_formula_moiety         'C36 H38 N2 P Pd, C F3 O3 S, C2 H3 N'
_chemical_formula_weight         826.16

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.9799(5)
_cell_length_b                   13.0932(5)
_cell_length_c                   13.5428(5)
_cell_angle_alpha                100.2840(10)
_cell_angle_beta                 104.9000(10)
_cell_angle_gamma                106.0680(10)
_cell_volume                     2058.58(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      1.80
_cell_measurement_reflns_used    9999
_cell_measurement_theta_max      36.29
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.333
_exptl_crystal_F_000             828
_exptl_crystal_density_method    'not measured'


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.5537
_exptl_absorpt_correction_T_max  0.7459

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec I\mS Microsource '
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_number            65531
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.607
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             8425
_reflns_number_gt                7932
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0598P)²+6.5971P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8425
_refine_ls_number_parameters     474
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1317
_refine_ls_wR_factor_gt          0.1286
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0


#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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'
N N 0.0061 0.0033 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.1731(3) -0.0568(3) 0.5751(3) 0.0253(6) Uani 1 1 d . . . . .
C2 C 0.1286(3) -0.2429(3) 0.5292(3) 0.0342(8) Uani 1 1 d . . . . .
H2 H 0.1249 -0.3137 0.5342 0.041 Uiso 1 1 calc R U . . .
C4 C 0.0751(3) -0.0396(3) 0.3973(3) 0.0287(7) Uani 1 1 d . . . . .
H4A H 0.0164 -0.0133 0.4127 0.034 Uiso 1 1 calc R U . . .
H4B H 0.0436 -0.0881 0.3258 0.034 Uiso 1 1 calc R U . . .
C5 C 0.1734(3) 0.0572(3) 0.4030(3) 0.0335(8) Uani 1 1 d . . . . .
H5A H 0.1536 0.0832 0.3404 0.040 Uiso 1 1 calc R U . . .
H5B H 0.2379 0.0335 0.4032 0.040 Uiso 1 1 calc R U . . .
C6 C 0.2067(3) 0.1522(3) 0.5021(3) 0.0303(7) Uani 1 1 d . . . . .
H6 H 0.1408 0.1767 0.4919 0.036 Uiso 1 1 calc R U . . .
C7 C 0.2411(4) 0.0980(4) 0.8136(3) 0.0479(11) Uani 1 1 d . . . . .
C8A C 0.2984(14) 0.2007(7) 0.8159(7) 0.045(4) Uani 0.52(2) 1 d . . P . .
C8B C 0.2241(12) 0.1945(6) 0.8030(6) 0.032(3) Uani 0.48(2) 1 d . . P . .
C9 C 0.2719(5) 0.2695(3) 0.7596(3) 0.0575(13) Uani 1 1 d . . . . .
C11 C 0.2456(3) -0.1458(3) 0.7152(3) 0.0335(8) Uani 1 1 d . . . . .
C12 C 0.3626(3) -0.1183(3) 0.7465(4) 0.0435(10) Uani 1 1 d . . . . .
C13 C 0.4157(4) -0.1253(4) 0.8486(4) 0.0588(14) Uani 1 1 d . . . . .
H13 H 0.4941 -0.1062 0.8726 0.071 Uiso 1 1 calc R U . . .
C14 C 0.3557(5) -0.1592(4) 0.9141(4) 0.0599(14) Uani 1 1 d . . . . .
C15 C 0.2400(5) -0.1855(3) 0.8793(3) 0.0509(11) Uani 1 1 d . . . . .
H15 H 0.1992 -0.2084 0.9234 0.061 Uiso 1 1 calc R U . . .
C16 C 0.1824(4) -0.1790(3) 0.7804(3) 0.0381(8) Uani 1 1 d . . . . .
C17 C 0.4287(4) -0.0841(4) 0.6747(5) 0.0586(13) Uani 1 1 d . . . . .
H17A H 0.4194 -0.1481 0.6212 0.088 Uiso 1 1 calc R U . . .
H17B H 0.5076 -0.0490 0.7155 0.088 Uiso 1 1 calc R U . . .
H17C H 0.4016 -0.0335 0.6415 0.088 Uiso 1 1 calc R U . . .
C18 C 0.4170(7) -0.1678(5) 1.0229(5) 0.097(3) Uani 1 1 d . . . . .
H18A H 0.4024 -0.2441 1.0216 0.145 Uiso 1 1 calc R U . . .
H18B H 0.3902 -0.1335 1.0750 0.145 Uiso 1 1 calc R U . . .
H18C H 0.4970 -0.1312 1.0405 0.145 Uiso 1 1 calc R U . . .
C19 C 0.0565(4) -0.2040(4) 0.7465(4) 0.0482(10) Uani 1 1 d . . . . .
H19A H 0.0295 -0.2165 0.8044 0.072 Uiso 1 1 calc R U . . .
H19B H 0.0203 -0.2689 0.6876 0.072 Uiso 1 1 calc R U . . .
H19C H 0.0392 -0.1428 0.7256 0.072 Uiso 1 1 calc R U . . .
C21 C 0.4588(3) 0.2644(3) 0.5519(3) 0.0323(7) Uani 1 1 d . . . . .
C22 C 0.4835(4) 0.2001(4) 0.6184(4) 0.0497(11) Uani 1 1 d . . . . .
H22 H 0.4258 0.1544 0.6356 0.060 Uiso 1 1 calc R U . . .
C23 C 0.5941(4) 0.2033(5) 0.6598(5) 0.0619(14) Uani 1 1 d . . . . .
H23 H 0.6102 0.1598 0.7047 0.074 Uiso 1 1 calc R U . . .
C24 C 0.6806(4) 0.2710(4) 0.6346(4) 0.0511(11) Uani 1 1 d . . . . .
H24 H 0.7546 0.2728 0.6626 0.061 Uiso 1 1 calc R U . . .
C25 C 0.6566(3) 0.3356(4) 0.5680(4) 0.0426(9) Uani 1 1 d . . . . .
H25 H 0.7146 0.3812 0.5511 0.051 Uiso 1 1 calc R U . . .
C26 C 0.5467(3) 0.3328(3) 0.5265(3) 0.0370(8) Uani 1 1 d . . . . .
H26 H 0.5309 0.3764 0.4815 0.044 Uiso 1 1 calc R U . . .
C3 C 0.0803(3) -0.2152(3) 0.4427(3) 0.0323(7) Uani 1 1 d . . . . .
H3 H 0.0367 -0.2628 0.3760 0.039 Uiso 1 1 calc R U . . .
C31 C 0.3104(3) 0.3924(3) 0.5775(3) 0.0288(7) Uani 1 1 d . . . . .
C32 C 0.4059(3) 0.4734(3) 0.6526(3) 0.0341(8) Uani 1 1 d . . . . .
H32 H 0.4765 0.4650 0.6639 0.041 Uiso 1 1 calc R U . . .
C33 C 0.3959(4) 0.5666(3) 0.7107(3) 0.0434(9) Uani 1 1 d . . . . .
H33 H 0.4600 0.6205 0.7609 0.052 Uiso 1 1 calc R U . . .
C34 C 0.2918(4) 0.5799(3) 0.6945(4) 0.0448(10) Uani 1 1 d . . . . .
H34 H 0.2856 0.6423 0.7343 0.054 Uiso 1 1 calc R U . . .
C35 C 0.1964(4) 0.5005(3) 0.6192(4) 0.0437(9) Uani 1 1 d . . . . .
H35 H 0.1263 0.5100 0.6079 0.052 Uiso 1 1 calc R U . . .
C36 C 0.2052(3) 0.4074(3) 0.5609(3) 0.0363(8) Uani 1 1 d . . . . .
H36 H 0.1409 0.3543 0.5103 0.044 Uiso 1 1 calc R U . . .
C41 C 0.3035(3) 0.2825(3) 0.3685(3) 0.0349(8) Uani 1 1 d . . . . .
C42 C 0.3256(4) 0.2069(4) 0.2976(4) 0.0469(10) Uani 1 1 d . . . . .
H42 H 0.3525 0.1535 0.3205 0.056 Uiso 1 1 calc R U . . .
C43 C 0.3076(4) 0.2110(5) 0.1930(4) 0.0583(13) Uani 1 1 d . . . . .
H43 H 0.3213 0.1596 0.1459 0.070 Uiso 1 1 calc R U . . .
C44 C 0.2699(5) 0.2904(6) 0.1591(4) 0.0693(16) Uani 1 1 d . . . . .
H44 H 0.2584 0.2931 0.0891 0.083 Uiso 1 1 calc R U . . .
C45 C 0.2488(6) 0.3660(6) 0.2283(5) 0.0741(17) Uani 1 1 d . . . . .
H45 H 0.2241 0.4205 0.2051 0.089 Uiso 1 1 calc R U . . .
C46 C 0.2640(4) 0.3618(4) 0.3323(4) 0.0520(11) Uani 1 1 d . . . . .
H46 H 0.2478 0.4123 0.3781 0.062 Uiso 1 1 calc R U . . .
C50 C 0.0583(6) 0.8924(5) 0.0753(4) 0.0722(16) Uani 1 1 d . . . . .
C53 C 0.9736(6) 0.5000(4) 0.7481(6) 0.0693(15) Uani 1 1 d . . . . .
C54 C 1.0204(13) 0.5080(8) 0.8610(7) 0.174(6) Uani 1 1 d . . . . .
H54A H 0.9698 0.4518 0.8797 0.262 Uiso 1 1 calc R U . . .
H54B H 1.0292 0.5793 0.9026 0.262 Uiso 1 1 calc R U . . .
H54C H 1.0928 0.4981 0.8747 0.262 Uiso 1 1 calc R U . . .
N1 N 0.1850(2) -0.1460(2) 0.6098(2) 0.0284(6) Uani 1 1 d . . . . .
N2 N 0.1082(2) -0.1019(2) 0.4720(2) 0.0260(6) Uani 1 1 d . . . . .
N4 N 0.9413(4) 0.4924(4) 0.6636(5) 0.0663(12) Uani 1 1 d . . . . .
P1 P 0.31755(7) 0.26830(7) 0.50182(7) 0.02815(19) Uani 1 1 d . . . . .
Pd1 Pd 0.22585(2) 0.10767(2) 0.65078(2) 0.02522(9) Uani 1 1 d . . . . .
S1 S 0.1140(3) 0.8049(2) 0.13880(16) 0.1138(9) Uani 1 1 d . . . . .
O1 O 0.1357(6) 0.7295(4) 0.0669(4) 0.1008(18) Uani 1 1 d . . . . .
O2 O 0.0399(7) 0.7600(4) 0.1926(4) 0.120(2) Uani 1 1 d . . . . .
O3 O 0.2230(7) 0.8962(7) 0.2148(5) 0.187(5) Uani 1 1 d . . . . .
F1 F 0.0335(4) 0.9629(4) 0.1357(3) 0.0865(11) Uani 1 1 d . . . . .
F2 F 0.1162(5) 0.9393(4) 0.0214(4) 0.1120(17) Uani 1 1 d . . . . .
F3 F -0.0382(6) 0.8334(7) -0.0021(5) 0.200(4) 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
C1 N2 1.354(4) . ?
C1 N1 1.366(4) . ?
C1 Pd1 2.047(3) . ?
C2 C3 1.341(5) . ?
C2 N1 1.385(4) . ?
C2 H2 0.9300 . ?
C4 N2 1.463(4) . ?
C4 C5 1.503(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.530(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 P1 1.782(4) . ?
C6 Pd1 2.168(4) . ?
C6 H6 0.9800 . ?
C7 C8A 1.335(11) . ?
C7 C8B 1.368(10) . ?
C7 Pd1 2.193(4) . ?
C8A C8B 0.912(11) . ?
C8A C9 1.339(11) . ?
C8A Pd1 2.164(8) . ?
C8B C9 1.323(10) . ?
C8B Pd1 2.179(7) . ?
C9 Pd1 2.179(4) . ?
C11 C12 1.388(5) . ?
C11 C16 1.398(6) . ?
C11 N1 1.441(5) . ?
C12 C13 1.408(7) . ?
C12 C17 1.502(7) . ?
C13 C14 1.377(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.373(8) . ?
C14 C18 1.524(7) . ?
C15 C16 1.387(6) . ?
C15 H15 0.9300 . ?
C16 C19 1.501(6) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C21 C22 1.377(6) . ?
C21 C26 1.403(5) . ?
C21 P1 1.802(4) . ?
C22 C23 1.386(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.383(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.379(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.379(6) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C3 N2 1.380(4) . ?
C3 H3 0.9300 . ?
C31 C32 1.391(5) . ?
C31 C36 1.400(5) . ?
C31 P1 1.799(4) . ?
C32 C33 1.386(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.377(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.382(6) . ?
C34 H34 0.9300 . ?
C35 C36 1.379(6) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C41 C46 1.388(6) . ?
C41 C42 1.394(6) . ?
C41 P1 1.816(4) . ?
C42 C43 1.389(7) . ?
C42 H42 0.9300 . ?
C43 C44 1.367(9) . ?
C43 H43 0.9300 . ?
C44 C45 1.372(9) . ?
C44 H44 0.9300 . ?
C45 C46 1.385(7) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C50 F1 1.287(7) . ?
C50 F2 1.288(7) . ?
C50 F3 1.328(8) . ?
C50 S1 1.751(7) . ?
C53 N4 1.089(8) . ?
C53 C54 1.465(11) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
S1 O1 1.398(5) . ?
S1 O2 1.416(6) . ?
S1 O3 1.537(8) . ?

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
N2 C1 N1 103.4(3) . . ?
N2 C1 Pd1 124.1(2) . . ?
N1 C1 Pd1 132.4(3) . . ?
C3 C2 N1 106.9(3) . . ?
C3 C2 H2 126.6 . . ?
N1 C2 H2 126.6 . . ?
N2 C4 C5 112.1(3) . . ?
N2 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
N2 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C4 C5 C6 112.3(3) . . ?
C4 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
C4 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?
C5 C6 P1 110.9(2) . . ?
C5 C6 Pd1 115.9(2) . . ?
P1 C6 Pd1 116.11(18) . . ?
C5 C6 H6 104.0 . . ?
P1 C6 H6 104.0 . . ?
Pd1 C6 H6 104.0 . . ?
C8A C7 C8B 39.4(5) . . ?
C8A C7 Pd1 71.0(4) . . ?
C8B C7 Pd1 71.2(4) . . ?
C8B C8A C7 72.2(10) . . ?
C8B C8A C9 69.0(9) . . ?
C7 C8A C9 132.2(11) . . ?
C8B C8A Pd1 78.8(8) . . ?
C7 C8A Pd1 73.4(4) . . ?
C9 C8A Pd1 72.7(4) . . ?
C8A C8B C9 70.9(9) . . ?
C8A C8B C7 68.3(9) . . ?
C9 C8B C7 130.6(10) . . ?
C8A C8B Pd1 76.9(7) . . ?
C9 C8B Pd1 72.3(4) . . ?
C7 C8B Pd1 72.3(4) . . ?
C8B C9 C8A 40.1(5) . . ?
C8B C9 Pd1 72.3(4) . . ?
C8A C9 Pd1 71.4(4) . . ?
C12 C11 C16 122.4(4) . . ?
C12 C11 N1 119.6(4) . . ?
C16 C11 N1 117.9(3) . . ?
C11 C12 C13 116.6(5) . . ?
C11 C12 C17 121.6(4) . . ?
C13 C12 C17 121.8(4) . . ?
C14 C13 C12 122.4(4) . . ?
C14 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
C15 C14 C13 118.8(4) . . ?
C15 C14 C18 120.9(6) . . ?
C13 C14 C18 120.3(6) . . ?
C14 C15 C16 121.8(5) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C15 C16 C11 117.9(4) . . ?
C15 C16 C19 120.6(4) . . ?
C11 C16 C19 121.5(4) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C21 C26 119.2(4) . . ?
C22 C21 P1 121.7(3) . . ?
C26 C21 P1 119.0(3) . . ?
C21 C22 C23 120.2(4) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C24 C23 C22 120.4(4) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C23 119.8(4) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 120.1(4) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 120.3(4) . . ?
C25 C26 H26 119.9 . . ?
C21 C26 H26 119.9 . . ?
C2 C3 N2 106.5(3) . . ?
C2 C3 H3 126.8 . . ?
N2 C3 H3 126.8 . . ?
C32 C31 C36 119.0(3) . . ?
C32 C31 P1 122.1(3) . . ?
C36 C31 P1 118.9(3) . . ?
C33 C32 C31 120.0(4) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C34 C33 C32 120.5(4) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 120.1(4) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 120.1(4) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C31 120.4(4) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
C46 C41 C42 118.6(4) . . ?
C46 C41 P1 122.1(3) . . ?
C42 C41 P1 119.1(3) . . ?
C43 C42 C41 120.3(5) . . ?
C43 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C44 C43 C42 120.3(5) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 120.0(5) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C44 C45 C46 120.5(5) . . ?
C44 C45 H45 119.7 . . ?
C46 C45 H45 119.7 . . ?
C45 C46 C41 120.2(5) . . ?
C45 C46 H46 119.9 . . ?
C41 C46 H46 119.9 . . ?
F1 C50 F2 111.2(5) . . ?
F1 C50 F3 105.4(7) . . ?
F2 C50 F3 100.0(6) . . ?
F1 C50 S1 114.3(4) . . ?
F2 C50 S1 114.8(5) . . ?
F3 C50 S1 109.9(6) . . ?
N4 C53 C54 177.5(9) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C1 N1 C2 111.2(3) . . ?
C1 N1 C11 127.2(3) . . ?
C2 N1 C11 121.6(3) . . ?
C1 N2 C3 112.1(3) . . ?
C1 N2 C4 125.0(3) . . ?
C3 N2 C4 122.9(3) . . ?
C6 P1 C31 109.46(16) . . ?
C6 P1 C21 115.35(17) . . ?
C31 P1 C21 108.66(17) . . ?
C6 P1 C41 111.52(17) . . ?
C31 P1 C41 106.88(18) . . ?
C21 P1 C41 104.55(17) . . ?
C1 Pd1 C8A 133.4(3) . . ?
C1 Pd1 C6 91.90(13) . . ?
C8A Pd1 C6 134.0(3) . . ?
C1 Pd1 C8B 132.1(2) . . ?
C8A Pd1 C8B 24.3(3) . . ?
C6 Pd1 C8B 130.8(3) . . ?
C1 Pd1 C9 167.37(16) . . ?
C8A Pd1 C9 35.9(3) . . ?
C6 Pd1 C9 99.96(15) . . ?
C8B Pd1 C9 35.4(3) . . ?
C1 Pd1 C7 99.81(15) . . ?
C8A Pd1 C7 35.7(3) . . ?
C6 Pd1 C7 167.25(15) . . ?
C8B Pd1 C7 36.5(3) . . ?
C9 Pd1 C7 68.01(16) . . ?
O1 S1 O2 116.5(3) . . ?
O1 S1 O3 112.5(4) . . ?
O2 S1 O3 112.2(5) . . ?
O1 S1 C50 110.4(3) . . ?
O2 S1 C50 107.3(4) . . ?
O3 S1 C50 95.8(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C4 C5 C6 -74.7(4) . . . . ?
C4 C5 C6 P1 -176.4(2) . . . . ?
C4 C5 C6 Pd1 48.4(4) . . . . ?
Pd1 C7 C8A C8B 83.3(7) . . . . ?
C8B C7 C8A C9 -37.0(11) . . . . ?
Pd1 C7 C8A C9 46.3(10) . . . . ?
C8B C7 C8A Pd1 -83.3(7) . . . . ?
C7 C8A C8B C9 -151.5(5) . . . . ?
Pd1 C8A C8B C9 -75.6(3) . . . . ?
C9 C8A C8B C7 151.5(5) . . . . ?
Pd1 C8A C8B C7 75.9(3) . . . . ?
C7 C8A C8B Pd1 -75.9(3) . . . . ?
C9 C8A C8B Pd1 75.6(3) . . . . ?
Pd1 C7 C8B C8A -82.6(7) . . . . ?
C8A C7 C8B C9 36.4(10) . . . . ?
Pd1 C7 C8B C9 -46.2(8) . . . . ?
C8A C7 C8B Pd1 82.6(7) . . . . ?
C7 C8B C9 C8A -35.8(10) . . . . ?
Pd1 C8B C9 C8A -81.9(7) . . . . ?
C8A C8B C9 Pd1 81.9(7) . . . . ?
C7 C8B C9 Pd1 46.2(8) . . . . ?
C7 C8A C9 C8B 37.8(11) . . . . ?
Pd1 C8A C9 C8B 84.4(7) . . . . ?
C8B C8A C9 Pd1 -84.4(7) . . . . ?
C7 C8A C9 Pd1 -46.5(10) . . . . ?
C16 C11 C12 C13 -0.1(5) . . . . ?
N1 C11 C12 C13 -176.9(3) . . . . ?
C16 C11 C12 C17 179.3(4) . . . . ?
N1 C11 C12 C17 2.5(5) . . . . ?
C11 C12 C13 C14 1.1(6) . . . . ?
C17 C12 C13 C14 -178.3(4) . . . . ?
C12 C13 C14 C15 -1.1(7) . . . . ?
C12 C13 C14 C18 178.6(4) . . . . ?
C13 C14 C15 C16 0.1(7) . . . . ?
C18 C14 C15 C16 -179.6(4) . . . . ?
C14 C15 C16 C11 0.8(6) . . . . ?
C14 C15 C16 C19 -177.6(4) . . . . ?
C12 C11 C16 C15 -0.8(6) . . . . ?
N1 C11 C16 C15 176.0(3) . . . . ?
C12 C11 C16 C19 177.6(4) . . . . ?
N1 C11 C16 C19 -5.6(5) . . . . ?
C26 C21 C22 C23 0.1(7) . . . . ?
P1 C21 C22 C23 -176.7(4) . . . . ?
C21 C22 C23 C24 -0.1(9) . . . . ?
C22 C23 C24 C25 0.0(9) . . . . ?
C23 C24 C25 C26 -0.1(8) . . . . ?
C24 C25 C26 C21 0.2(7) . . . . ?
C22 C21 C26 C25 -0.2(6) . . . . ?
P1 C21 C26 C25 176.8(3) . . . . ?
N1 C2 C3 N2 0.0(4) . . . . ?
C36 C31 C32 C33 0.7(6) . . . . ?
P1 C31 C32 C33 -178.6(3) . . . . ?
C31 C32 C33 C34 0.0(6) . . . . ?
C32 C33 C34 C35 -0.7(7) . . . . ?
C33 C34 C35 C36 0.6(7) . . . . ?
C34 C35 C36 C31 0.1(6) . . . . ?
C32 C31 C36 C35 -0.8(6) . . . . ?
P1 C31 C36 C35 178.6(3) . . . . ?
C46 C41 C42 C43 -0.4(6) . . . . ?
P1 C41 C42 C43 175.4(3) . . . . ?
C41 C42 C43 C44 1.1(7) . . . . ?
C42 C43 C44 C45 -0.4(8) . . . . ?
C43 C44 C45 C46 -0.9(10) . . . . ?
C44 C45 C46 C41 1.5(9) . . . . ?
C42 C41 C46 C45 -0.9(7) . . . . ?
P1 C41 C46 C45 -176.5(4) . . . . ?
N2 C1 N1 C2 0.1(4) . . . . ?
Pd1 C1 N1 C2 176.6(3) . . . . ?
N2 C1 N1 C11 -179.2(3) . . . . ?
Pd1 C1 N1 C11 -2.7(5) . . . . ?
C3 C2 N1 C1 -0.1(4) . . . . ?
C3 C2 N1 C11 179.2(3) . . . . ?
C12 C11 N1 C1 -80.4(5) . . . . ?
C16 C11 N1 C1 102.6(4) . . . . ?
C12 C11 N1 C2 100.3(4) . . . . ?
C16 C11 N1 C2 -76.6(4) . . . . ?
N1 C1 N2 C3 -0.1(4) . . . . ?
Pd1 C1 N2 C3 -177.0(2) . . . . ?
N1 C1 N2 C4 -177.2(3) . . . . ?
Pd1 C1 N2 C4 5.9(4) . . . . ?
C2 C3 N2 C1 0.0(4) . . . . ?
C2 C3 N2 C4 177.2(3) . . . . ?
C5 C4 N2 C1 46.3(4) . . . . ?
C5 C4 N2 C3 -130.5(3) . . . . ?
C5 C6 P1 C31 153.3(3) . . . . ?
Pd1 C6 P1 C31 -71.6(2) . . . . ?
C5 C6 P1 C21 -83.8(3) . . . . ?
Pd1 C6 P1 C21 51.3(2) . . . . ?
C5 C6 P1 C41 35.3(3) . . . . ?
Pd1 C6 P1 C41 170.33(18) . . . . ?
C32 C31 P1 C6 133.3(3) . . . . ?
C36 C31 P1 C6 -46.0(3) . . . . ?
C32 C31 P1 C21 6.5(4) . . . . ?
C36 C31 P1 C21 -172.8(3) . . . . ?
C32 C31 P1 C41 -105.8(3) . . . . ?
C36 C31 P1 C41 74.9(3) . . . . ?
C22 C21 P1 C6 -21.9(4) . . . . ?
C26 C21 P1 C6 161.2(3) . . . . ?
C22 C21 P1 C31 101.4(4) . . . . ?
C26 C21 P1 C31 -75.5(3) . . . . ?
C22 C21 P1 C41 -144.7(4) . . . . ?
C26 C21 P1 C41 38.4(4) . . . . ?
C46 C41 P1 C6 104.2(4) . . . . ?
C42 C41 P1 C6 -71.4(4) . . . . ?
C46 C41 P1 C31 -15.4(4) . . . . ?
C42 C41 P1 C31 169.0(3) . . . . ?
C46 C41 P1 C21 -130.5(4) . . . . ?
C42 C41 P1 C21 53.9(3) . . . . ?
F1 C50 S1 O1 178.5(5) . . . . ?
F2 C50 S1 O1 -51.4(6) . . . . ?
F3 C50 S1 O1 60.3(7) . . . . ?
F1 C50 S1 O2 50.5(6) . . . . ?
F2 C50 S1 O2 -179.3(5) . . . . ?
F3 C50 S1 O2 -67.7(7) . . . . ?
F1 C50 S1 O3 -64.9(6) . . . . ?
F2 C50 S1 O3 65.2(6) . . . . ?
F3 C50 S1 O3 176.9(7) . . . . ?

_refine_diff_density_max         3.621
_refine_diff_density_min         -1.751
_refine_diff_density_rms         0.099




####################################################################### 
# 
# 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_3Br2
_database_code_depnum_ccdc_archive 'CCDC 1558458'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;

_audit_creation_date             2016-06-01T14:29:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C33 H37 Br2 N2 P'
_chemical_formula_moiety         '2(Br), C33 H37 N2 P'
_chemical_formula_weight         652.43

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6755(2)
_cell_length_b                   12.7591(3)
_cell_length_c                   13.7838(3)
_cell_angle_alpha                108.122(2)
_cell_angle_beta                 100.266(2)
_cell_angle_gamma                98.136(2)
_cell_volume                     1555.63(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11178
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.5140
_cell_measurement_theta_min      3.7120

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.393
_exptl_crystal_F_000             668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_colour            colourless
_exptl_crystal_description       block
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.681
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_number            30779
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.001
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_Friedel_coverage         0
_reflns_number_total             6356
_reflns_number_gt                5498
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0344P)²+0.7464P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6356
_refine_ls_number_parameters     346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0243
_refine_ls_wR_factor_ref         0.0652
_refine_ls_wR_factor_gt          0.0609
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_restrained_S_all      1.05
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.06

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.3203(2) 0.35927(16) 0.13584(16) 0.0254(4) Uani 1 1 d . . . . .
H10 H 0.3996 0.4128 0.1817 0.03 Uiso 1 1 calc R U . . .
C2 C 0.0918(3) 0.28051(18) 0.0377(2) 0.0535(8) Uani 1 1 d . . . . .
H12A H 0.0531 0.294 -0.0262 0.064 Uiso 1 1 calc R U . . .
H12B H 0.0131 0.2573 0.0664 0.064 Uiso 1 1 calc R U . . .
C3 C 0.1844(2) 0.19202(17) 0.01712(19) 0.0361(5) Uani 1 1 d . . . . .
H13A H 0.1477 0.128 0.0358 0.043 Uiso 1 1 calc R U . . .
H13B H 0.1894 0.1658 -0.0559 0.043 Uiso 1 1 calc R U . . .
C4 C 0.4588(2) 0.21176(16) 0.09531(15) 0.0248(4) Uani 1 1 d . . . . .
H14A H 0.5346 0.2641 0.0866 0.03 Uiso 1 1 calc R U . . .
H14B H 0.4438 0.1402 0.0388 0.03 Uiso 1 1 calc R U . . .
C5 C 0.50711(19) 0.19501(15) 0.19982(14) 0.0196(4) Uani 1 1 d . . . . .
H15A H 0.4507 0.1258 0.1997 0.023 Uiso 1 1 calc R U . . .
H15B H 0.4941 0.2574 0.2568 0.023 Uiso 1 1 calc R U . . .
C6 C 0.66659(19) 0.18905(15) 0.21457(14) 0.0191(4) Uani 1 1 d . . . . .
H16A H 0.7217 0.2634 0.2265 0.023 Uiso 1 1 calc R U . . .
H16B H 0.6795 0.1386 0.1493 0.023 Uiso 1 1 calc R U . . .
C11 C 0.1631(2) 0.49338(16) 0.14829(16) 0.0252(4) Uani 1 1 d . . . . .
C12 C 0.2096(2) 0.56804(16) 0.09959(16) 0.0253(4) Uani 1 1 d . . . . .
C13 C 0.1870(2) 0.67742(16) 0.13686(16) 0.0261(4) Uani 1 1 d . . . . .
H5 H 0.2195 0.7294 0.107 0.031 Uiso 1 1 calc R U . . .
C14 C 0.1172(2) 0.71067(17) 0.21732(17) 0.0289(4) Uani 1 1 d . . . . .
C15 C 0.0661(2) 0.63227(19) 0.26008(18) 0.0342(5) Uani 1 1 d . . . . .
H7 H 0.0153 0.6533 0.3118 0.041 Uiso 1 1 calc R U . . .
C16 C 0.0892(2) 0.52242(18) 0.22726(19) 0.0320(5) Uani 1 1 d . . . . .
C17 C 0.2823(3) 0.53325(19) 0.0101(2) 0.0428(6) Uani 1 1 d . . . . .
H37A H 0.2283 0.4624 -0.0406 0.064 Uiso 1 1 calc R U . . .
H37B H 0.3777 0.5256 0.0365 0.064 Uiso 1 1 calc R U . . .
H37C H 0.2872 0.5896 -0.0226 0.064 Uiso 1 1 calc R U . . .
C18 C 0.0982(3) 0.83104(19) 0.2570(2) 0.0429(6) Uani 1 1 d . . . . .
H36A H 0.1185 0.8578 0.3324 0.064 Uiso 1 1 calc R U . . .
H36B H 0.0011 0.8341 0.2294 0.064 Uiso 1 1 calc R U . . .
H36C H 0.163 0.8777 0.2345 0.064 Uiso 1 1 calc R U . . .
C19 C 0.0386(3) 0.4408(2) 0.2788(3) 0.0529(7) Uani 1 1 d . . . . .
H38A H -0.0372 0.3814 0.2293 0.079 Uiso 1 1 calc R U . . .
H38B H 0.0035 0.4798 0.338 0.079 Uiso 1 1 calc R U . . .
H38C H 0.1172 0.4094 0.3021 0.079 Uiso 1 1 calc R U . . .
C21 C 0.68010(19) 0.20984(16) 0.43345(14) 0.0206(4) Uani 1 1 d . . . . .
C22 C 0.6300(2) 0.14877(17) 0.49277(16) 0.0271(4) Uani 1 1 d . . . . .
H31 H 0.6336 0.0729 0.4758 0.033 Uiso 1 1 calc R U . . .
C23 C 0.5749(2) 0.2011(2) 0.57693(17) 0.0343(5) Uani 1 1 d . . . . .
H32 H 0.5423 0.1606 0.617 0.041 Uiso 1 1 calc R U . . .
C24 C 0.5684(2) 0.3135(2) 0.60140(17) 0.0346(5) Uani 1 1 d . . . . .
H33 H 0.5305 0.3483 0.6576 0.042 Uiso 1 1 calc R U . . .
C25 C 0.6175(2) 0.37446(18) 0.54302(17) 0.0327(5) Uani 1 1 d . . . . .
H34 H 0.6122 0.45 0.56 0.039 Uiso 1 1 calc R U . . .
C26 C 0.6751(2) 0.32399(17) 0.45902(16) 0.0273(4) Uani 1 1 d . . . . .
H35 H 0.7097 0.3655 0.4204 0.033 Uiso 1 1 calc R U . . .
C31 C 0.93419(19) 0.17854(15) 0.34265(14) 0.0189(4) Uani 1 1 d . . . . .
C32 C 0.9972(2) 0.12396(16) 0.26236(15) 0.0246(4) Uani 1 1 d . . . . .
H23 H 0.9397 0.0741 0.1986 0.03 Uiso 1 1 calc R U . . .
C33 C 1.1451(2) 0.14457(18) 0.27839(17) 0.0300(4) Uani 1 1 d . . . . .
H22 H 1.1876 0.1077 0.2257 0.036 Uiso 1 1 calc R U . . .
C34 C 1.2302(2) 0.22037(18) 0.37327(17) 0.0313(5) Uani 1 1 d . . . . .
H21 H 1.3298 0.2336 0.3841 0.038 Uiso 1 1 calc R U . . .
C35 C 1.1683(2) 0.27642(18) 0.45185(16) 0.0313(5) Uani 1 1 d . . . . .
H20 H 1.226 0.3281 0.5147 0.038 Uiso 1 1 calc R U . . .
C36 C 1.0199(2) 0.25534(16) 0.43679(15) 0.0250(4) Uani 1 1 d . . . . .
H19 H 0.978 0.2926 0.4896 0.03 Uiso 1 1 calc R U . . .
C41 C 0.6945(2) -0.00780(15) 0.28219(14) 0.0204(4) Uani 1 1 d . . . . .
C42 C 0.7751(2) -0.06118(17) 0.33892(17) 0.0291(4) Uani 1 1 d . . . . .
H25 H 0.8499 -0.0188 0.3965 0.035 Uiso 1 1 calc R U . . .
C43 C 0.7428(3) -0.17811(19) 0.30884(19) 0.0360(5) Uani 1 1 d . . . . .
H26 H 0.7954 -0.2139 0.347 0.043 Uiso 1 1 calc R U . . .
C44 C 0.6328(2) -0.24138(17) 0.22248(18) 0.0317(5) Uani 1 1 d . . . . .
H27 H 0.6129 -0.3197 0.2018 0.038 Uiso 1 1 calc R U . . .
C45 C 0.5528(2) -0.18877(17) 0.16706(17) 0.0311(5) Uani 1 1 d . . . . .
H28 H 0.478 -0.2317 0.1096 0.037 Uiso 1 1 calc R U . . .
C46 C 0.5828(2) -0.07154(16) 0.19621(15) 0.0248(4) Uani 1 1 d . . . . .
H29 H 0.5285 -0.0363 0.1584 0.03 Uiso 1 1 calc R U . . .
Br1 Br -0.23712(2) 0.07545(2) -0.03213(2) 0.02507(6) Uani 1 1 d . . . . .
Br2 Br 0.66902(2) 0.49810(2) 0.28024(2) 0.02704(6) Uani 1 1 d . . . . .
N1 N 0.19316(17) 0.38162(13) 0.11468(15) 0.0285(4) Uani 1 1 d . . . . .
N2 N 0.32639(18) 0.25500(13) 0.08685(14) 0.0279(4) Uani 1 1 d . . . . .
P1 P 0.74161(5) 0.14301(4) 0.31880(4) 0.01708(10) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N1 1.305(2) . ?
C1 N2 1.307(2) . ?
C1 H10 0.93 . ?
C2 N1 1.474(3) . ?
C2 C3 1.528(3) . ?
C2 H12A 0.97 . ?
C2 H12B 0.97 . ?
C3 N2 1.481(3) . ?
C3 H13A 0.97 . ?
C3 H13B 0.97 . ?
C4 N2 1.465(2) . ?
C4 C5 1.523(3) . ?
C4 H14A 0.97 . ?
C4 H14B 0.97 . ?
C5 C6 1.536(2) . ?
C5 H15A 0.97 . ?
C5 H15B 0.97 . ?
C6 P1 1.7918(18) . ?
C6 H16A 0.97 . ?
C6 H16B 0.97 . ?
C11 C16 1.391(3) . ?
C11 C12 1.395(3) . ?
C11 N1 1.445(2) . ?
C12 C13 1.393(3) . ?
C12 C17 1.506(3) . ?
C13 C14 1.386(3) . ?
C13 H5 0.93 . ?
C14 C15 1.387(3) . ?
C14 C18 1.512(3) . ?
C15 C16 1.396(3) . ?
C15 H7 0.93 . ?
C16 C19 1.506(3) . ?
C17 H37A 0.96 . ?
C17 H37B 0.96 . ?
C17 H37C 0.96 . ?
C18 H36A 0.96 . ?
C18 H36B 0.96 . ?
C18 H36C 0.96 . ?
C19 H38A 0.96 . ?
C19 H38B 0.96 . ?
C19 H38C 0.96 . ?
C21 C22 1.393(3) . ?
C21 C26 1.398(3) . ?
C21 P1 1.7942(18) . ?
C22 C23 1.384(3) . ?
C22 H31 0.93 . ?
C23 C24 1.381(3) . ?
C23 H32 0.93 . ?
C24 C25 1.378(3) . ?
C24 H33 0.93 . ?
C25 C26 1.390(3) . ?
C25 H34 0.93 . ?
C26 H35 0.93 . ?
C31 C36 1.388(3) . ?
C31 C32 1.401(3) . ?
C31 P1 1.7987(18) . ?
C32 C33 1.383(3) . ?
C32 H23 0.93 . ?
C33 C34 1.388(3) . ?
C33 H22 0.93 . ?
C34 C35 1.384(3) . ?
C34 H21 0.93 . ?
C35 C36 1.388(3) . ?
C35 H20 0.93 . ?
C36 H19 0.93 . ?
C41 C46 1.389(3) . ?
C41 C42 1.396(3) . ?
C41 P1 1.7973(18) . ?
C42 C43 1.390(3) . ?
C42 H25 0.93 . ?
C43 C44 1.381(3) . ?
C43 H26 0.93 . ?
C44 C45 1.374(3) . ?
C44 H27 0.93 . ?
C45 C46 1.395(3) . ?
C45 H28 0.93 . ?
C46 H29 0.93 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 114.04(18) . . ?
N1 C1 H10 123 . . ?
N2 C1 H10 123 . . ?
N1 C2 C3 103.31(17) . . ?
N1 C2 H12A 111.1 . . ?
C3 C2 H12A 111.1 . . ?
N1 C2 H12B 111.1 . . ?
C3 C2 H12B 111.1 . . ?
H12A C2 H12B 109.1 . . ?
N2 C3 C2 102.59(16) . . ?
N2 C3 H13A 111.2 . . ?
C2 C3 H13A 111.2 . . ?
N2 C3 H13B 111.2 . . ?
C2 C3 H13B 111.2 . . ?
H13A C3 H13B 109.2 . . ?
N2 C4 C5 113.13(16) . . ?
N2 C4 H14A 109 . . ?
C5 C4 H14A 109 . . ?
N2 C4 H14B 109 . . ?
C5 C4 H14B 109 . . ?
H14A C4 H14B 107.8 . . ?
C4 C5 C6 107.84(15) . . ?
C4 C5 H15A 110.1 . . ?
C6 C5 H15A 110.1 . . ?
C4 C5 H15B 110.1 . . ?
C6 C5 H15B 110.1 . . ?
H15A C5 H15B 108.5 . . ?
C5 C6 P1 116.84(13) . . ?
C5 C6 H16A 108.1 . . ?
P1 C6 H16A 108.1 . . ?
C5 C6 H16B 108.1 . . ?
P1 C6 H16B 108.1 . . ?
H16A C6 H16B 107.3 . . ?
C16 C11 C12 122.59(18) . . ?
C16 C11 N1 119.18(18) . . ?
C12 C11 N1 118.23(18) . . ?
C13 C12 C11 117.54(19) . . ?
C13 C12 C17 120.53(18) . . ?
C11 C12 C17 121.93(18) . . ?
C14 C13 C12 121.61(19) . . ?
C14 C13 H5 119.2 . . ?
C12 C13 H5 119.2 . . ?
C13 C14 C15 119.05(19) . . ?
C13 C14 C18 119.77(19) . . ?
C15 C14 C18 121.2(2) . . ?
C14 C15 C16 121.5(2) . . ?
C14 C15 H7 119.3 . . ?
C16 C15 H7 119.3 . . ?
C11 C16 C15 117.60(19) . . ?
C11 C16 C19 122.1(2) . . ?
C15 C16 C19 120.2(2) . . ?
C12 C17 H37A 109.5 . . ?
C12 C17 H37B 109.5 . . ?
H37A C17 H37B 109.5 . . ?
C12 C17 H37C 109.5 . . ?
H37A C17 H37C 109.5 . . ?
H37B C17 H37C 109.5 . . ?
C14 C18 H36A 109.5 . . ?
C14 C18 H36B 109.5 . . ?
H36A C18 H36B 109.5 . . ?
C14 C18 H36C 109.5 . . ?
H36A C18 H36C 109.5 . . ?
H36B C18 H36C 109.5 . . ?
C16 C19 H38A 109.5 . . ?
C16 C19 H38B 109.5 . . ?
H38A C19 H38B 109.5 . . ?
C16 C19 H38C 109.5 . . ?
H38A C19 H38C 109.5 . . ?
H38B C19 H38C 109.5 . . ?
C22 C21 C26 120.07(17) . . ?
C22 C21 P1 121.29(14) . . ?
C26 C21 P1 118.53(15) . . ?
C23 C22 C21 119.97(19) . . ?
C23 C22 H31 120 . . ?
C21 C22 H31 120 . . ?
C24 C23 C22 119.9(2) . . ?
C24 C23 H32 120 . . ?
C22 C23 H32 120 . . ?
C25 C24 C23 120.43(19) . . ?
C25 C24 H33 119.8 . . ?
C23 C24 H33 119.8 . . ?
C24 C25 C26 120.6(2) . . ?
C24 C25 H34 119.7 . . ?
C26 C25 H34 119.7 . . ?
C25 C26 C21 119.0(2) . . ?
C25 C26 H35 120.5 . . ?
C21 C26 H35 120.5 . . ?
C36 C31 C32 120.07(17) . . ?
C36 C31 P1 122.51(14) . . ?
C32 C31 P1 117.41(14) . . ?
C33 C32 C31 119.71(18) . . ?
C33 C32 H23 120.1 . . ?
C31 C32 H23 120.1 . . ?
C32 C33 C34 119.86(19) . . ?
C32 C33 H22 120.1 . . ?
C34 C33 H22 120.1 . . ?
C35 C34 C33 120.58(19) . . ?
C35 C34 H21 119.7 . . ?
C33 C34 H21 119.7 . . ?
C34 C35 C36 119.90(19) . . ?
C34 C35 H20 120 . . ?
C36 C35 H20 120 . . ?
C35 C36 C31 119.84(18) . . ?
C35 C36 H19 120.1 . . ?
C31 C36 H19 120.1 . . ?
C46 C41 C42 119.94(18) . . ?
C46 C41 P1 120.82(14) . . ?
C42 C41 P1 119.19(15) . . ?
C43 C42 C41 119.6(2) . . ?
C43 C42 H25 120.2 . . ?
C41 C42 H25 120.2 . . ?
C44 C43 C42 120.3(2) . . ?
C44 C43 H26 119.9 . . ?
C42 C43 H26 119.9 . . ?
C45 C44 C43 120.07(19) . . ?
C45 C44 H27 120 . . ?
C43 C44 H27 120 . . ?
C44 C45 C46 120.6(2) . . ?
C44 C45 H28 119.7 . . ?
C46 C45 H28 119.7 . . ?
C41 C46 C45 119.47(18) . . ?
C41 C46 H29 120.3 . . ?
C45 C46 H29 120.3 . . ?
C1 N1 C11 124.37(16) . . ?
C1 N1 C2 109.97(17) . . ?
C11 N1 C2 124.91(16) . . ?
C1 N2 C4 123.69(17) . . ?
C1 N2 C3 110.06(16) . . ?
C4 N2 C3 126.10(16) . . ?
C6 P1 C21 109.18(8) . . ?
C6 P1 C41 111.57(9) . . ?
C21 P1 C41 110.31(9) . . ?
C6 P1 C31 108.16(8) . . ?
C21 P1 C31 111.63(8) . . ?
C41 P1 C31 105.97(8) . . ?

####################################################################### 
# 
# 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_7prime
_database_code_depnum_ccdc_archive 'CCDC 1558461'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;

_audit_creation_date             2016-06-20T11:12:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C54 H58 Ag2 Br2 N4 O2 P2'
_chemical_formula_moiety         'C54 H58 Ag2 Br2 N4 O2 P2'
_chemical_formula_weight         1232.52

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.1723(2)
_cell_length_b                   9.5115(2)
_cell_length_c                   18.0882(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.3490(10)
_cell_angle_gamma                90
_cell_volume                     2605.88(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      3.37
_cell_measurement_reflns_used    9999
_cell_measurement_theta_max      36.29
_cell_measurement_wavelength     0.71073


#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.571
_exptl_crystal_F_000             1240
_exptl_crystal_density_method    'not measured'

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    2.39
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.5561
_exptl_absorpt_correction_T_max  0.7462

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec I\mS Microsource '
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_number            61683
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.337
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_reflns_Friedel_coverage         0
_reflns_number_total             5321
_reflns_number_gt                4867
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0638P)²+11.5166P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5321
_refine_ls_number_parameters     301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1203
_refine_ls_wR_factor_gt          0.1164
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.119
_refine_diff_density_min         -2.591
_refine_diff_density_rms         0.126

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.1902(2) -0.5661(4) 1.1495(2) 0.0159(7) Uani 1 1 d . . . . .
C2 C 0.2937(2) -0.5668(4) 1.2455(2) 0.0206(8) Uani 1 1 d . . . . .
H2 H 0.319 -0.5644 1.2936 0.025 Uiso 1 1 calc R U . . .
C3 C 0.3362(2) -0.5782(4) 1.1826(2) 0.0204(8) Uani 1 1 d . . . . .
H3 H 0.3969 -0.5854 1.1786 0.024 Uiso 1 1 calc R U . . .
C4 C 0.2916(2) -0.5868(4) 1.04647(19) 0.0157(7) Uani 1 1 d . . . . .
H4A H 0.2371 -0.6032 1.0171 0.019 Uiso 1 1 calc R U . . .
H4B H 0.33 -0.6668 1.0398 0.019 Uiso 1 1 calc R U . . .
C5 C 0.3356(2) -0.4554(4) 1.0181(2) 0.0165(7) Uani 1 1 d . . . . .
H5A H 0.3929 -0.4426 1.0438 0.02 Uiso 1 1 calc R U . . .
H5B H 0.2997 -0.3736 1.0272 0.02 Uiso 1 1 calc R U . . .
C6 C 0.3464(3) -0.4714(4) 0.9346(2) 0.0180(7) Uani 1 1 d . . . . .
H6A H 0.2885 -0.4701 0.9089 0.022 Uiso 1 1 calc R U . . .
H6B H 0.373 -0.562 0.9254 0.022 Uiso 1 1 calc R U . . .
C11 C 0.1343(2) -0.5483(4) 1.2744(2) 0.0173(7) Uani 1 1 d . . . . .
C12 C 0.1078(3) -0.6694(4) 1.3109(2) 0.0221(8) Uani 1 1 d . . . . .
C13 C 0.0395(3) -0.6549(5) 1.3589(2) 0.0280(9) Uani 1 1 d . . . . .
H13 H 0.0218 -0.733 1.3851 0.034 Uiso 1 1 calc R U . . .
C14 C -0.0023(3) -0.5280(6) 1.3685(2) 0.0302(10) Uani 1 1 d . . . . .
C15 C 0.0274(3) -0.4087(5) 1.3318(2) 0.0267(9) Uani 1 1 d . . . . .
H15 H 0 -0.3227 1.3389 0.032 Uiso 1 1 calc R U . . .
C16 C 0.0967(3) -0.4160(4) 1.2851(2) 0.0206(8) Uani 1 1 d . . . . .
C17 C 0.1519(3) -0.8090(5) 1.3005(3) 0.0327(10) Uani 1 1 d . . . . .
H17A H 0.1585 -0.8249 1.2487 0.049 Uiso 1 1 calc R U . . .
H17B H 0.1163 -0.8824 1.3198 0.049 Uiso 1 1 calc R U . . .
H17C H 0.209 -0.8089 1.3264 0.049 Uiso 1 1 calc R U . . .
C18 C -0.0788(3) -0.5170(8) 1.4180(3) 0.0474(14) Uani 1 1 d . . . . .
H18A H -0.0785 -0.5966 1.4507 0.071 Uiso 1 1 calc R U . . .
H18B H -0.1332 -0.5153 1.3882 0.071 Uiso 1 1 calc R U . . .
H18C H -0.0734 -0.4322 1.4467 0.071 Uiso 1 1 calc R U . . .
C19 C 0.1326(3) -0.2867(4) 1.2491(2) 0.0288(9) Uani 1 1 d . . . . .
H19A H 0.1029 -0.2048 1.2663 0.043 Uiso 1 1 calc R U . . .
H19B H 0.1229 -0.2939 1.1963 0.043 Uiso 1 1 calc R U . . .
H19C H 0.1947 -0.279 1.2617 0.043 Uiso 1 1 calc R U . . .
C21 C 0.3606(2) -0.1707(4) 0.91674(18) 0.0144(7) Uani 1 1 d . . . . .
C22 C 0.4133(2) -0.0532(4) 0.9329(2) 0.0191(7) Uani 1 1 d . . . . .
H22 H 0.4744 -0.0602 0.9318 0.023 Uiso 1 1 calc R U . . .
C23 C 0.3749(3) 0.0745(4) 0.9505(2) 0.0250(8) Uani 1 1 d . . . . .
H23 H 0.4101 0.1527 0.9613 0.03 Uiso 1 1 calc R U . . .
C24 C 0.2838(3) 0.0841(4) 0.9521(2) 0.0252(9) Uani 1 1 d . . . . .
H24 H 0.2581 0.1694 0.9637 0.03 Uiso 1 1 calc R U . . .
C25 C 0.2305(3) -0.0325(4) 0.9364(2) 0.0204(8) Uani 1 1 d . . . . .
H25 H 0.1695 -0.0252 0.9377 0.024 Uiso 1 1 calc R U . . .
C26 C 0.2689(2) -0.1597(4) 0.91872(19) 0.0164(7) Uani 1 1 d . . . . .
H26 H 0.2335 -0.2378 0.9082 0.02 Uiso 1 1 calc R U . . .
C31 C 0.4027(3) -0.3546(4) 0.7968(2) 0.0213(8) Uani 1 1 d . . . . .
C32 C 0.4467(4) -0.2568(5) 0.7548(3) 0.0361(11) Uani 1 1 d . . . . .
H32 H 0.4791 -0.1849 0.7783 0.043 Uiso 1 1 calc R U . . .
C33 C 0.4423(4) -0.2667(6) 0.6780(3) 0.0479(14) Uani 1 1 d . . . . .
H33 H 0.472 -0.2014 0.6504 0.057 Uiso 1 1 calc R U . . .
C34 C 0.3942(4) -0.3727(6) 0.6425(3) 0.0464(14) Uani 1 1 d . . . . .
H34 H 0.3904 -0.3776 0.5911 0.056 Uiso 1 1 calc R U . . .
C35 C 0.3517(4) -0.4715(7) 0.6836(3) 0.0517(15) Uani 1 1 d . . . . .
H35 H 0.3202 -0.5441 0.6599 0.062 Uiso 1 1 calc R U . . .
C36 C 0.3562(4) -0.4622(6) 0.7607(3) 0.0421(12) Uani 1 1 d . . . . .
H36 H 0.3275 -0.529 0.7882 0.051 Uiso 1 1 calc R U . . .
N1 N 0.2043(2) -0.5595(3) 1.22427(17) 0.0157(6) Uani 1 1 d . . . . .
N2 N 0.2721(2) -0.5772(3) 1.12471(17) 0.0150(6) Uani 1 1 d . . . . .
O1 O 0.50764(16) -0.3359(3) 0.92557(15) 0.0225(6) Uani 1 1 d . . . . .
P1 P 0.41332(6) -0.33519(10) 0.89681(5) 0.01531(19) Uani 1 1 d . . . . .
Br1 Br -0.09079(3) -0.58916(6) 1.05097(3) 0.04266(16) Uani 1 1 d . . . . .
Ag1 Ag 0.06771(2) -0.55721(3) 1.08921(2) 0.01940(11) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N2 1.350(5) . ?
C1 N1 1.358(5) . ?
C1 Ag1 2.101(4) . ?
C2 C3 1.346(6) . ?
C2 N1 1.390(5) . ?
C2 H2 0.93 . ?
C3 N2 1.387(5) . ?
C3 H3 0.93 . ?
C4 N2 1.465(4) . ?
C4 C5 1.520(5) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 C6 1.537(5) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C6 P1 1.804(4) . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C11 C12 1.398(6) . ?
C11 C16 1.400(5) . ?
C11 N1 1.440(5) . ?
C12 C13 1.397(6) . ?
C12 C17 1.504(6) . ?
C13 C14 1.380(7) . ?
C13 H13 0.93 . ?
C14 C15 1.402(7) . ?
C14 C18 1.511(6) . ?
C15 C16 1.388(6) . ?
C15 H15 0.93 . ?
C16 C19 1.508(6) . ?
C17 H17A 0.96 . ?
C17 H17B 0.96 . ?
C17 H17C 0.96 . ?
C18 H18A 0.96 . ?
C18 H18B 0.96 . ?
C18 H18C 0.96 . ?
C19 H19A 0.96 . ?
C19 H19B 0.96 . ?
C19 H19C 0.96 . ?
C21 C22 1.395(5) . ?
C21 C26 1.398(5) . ?
C21 P1 1.803(4) . ?
C22 C23 1.392(6) . ?
C22 H22 0.93 . ?
C23 C24 1.387(6) . ?
C23 H23 0.93 . ?
C24 C25 1.392(6) . ?
C24 H24 0.93 . ?
C25 C26 1.388(5) . ?
C25 H25 0.93 . ?
C26 H26 0.93 . ?
C31 C36 1.385(7) . ?
C31 C32 1.396(6) . ?
C31 P1 1.816(4) . ?
C32 C33 1.390(7) . ?
C32 H32 0.93 . ?
C33 C34 1.381(9) . ?
C33 H33 0.93 . ?
C34 C35 1.381(9) . ?
C34 H34 0.93 . ?
C35 C36 1.395(7) . ?
C35 H35 0.93 . ?
C36 H36 0.93 . ?
O1 P1 1.494(3) . ?
Br1 Ag1 2.4819(5) . ?
Br1 Ag1 2.9315(6) 3_547 ?
Ag1 Br1 2.9315(6) 3_547 ?

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
N2 C1 N1 103.9(3) . . ?
N2 C1 Ag1 129.3(3) . . ?
N1 C1 Ag1 126.7(3) . . ?
C3 C2 N1 106.2(3) . . ?
C3 C2 H2 126.9 . . ?
N1 C2 H2 126.9 . . ?
C2 C3 N2 106.8(3) . . ?
C2 C3 H3 126.6 . . ?
N2 C3 H3 126.6 . . ?
N2 C4 C5 113.1(3) . . ?
N2 C4 H4A 109 . . ?
C5 C4 H4A 109 . . ?
N2 C4 H4B 109 . . ?
C5 C4 H4B 109 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 C6 109.0(3) . . ?
C4 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
C4 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
C5 C6 P1 113.3(3) . . ?
C5 C6 H6A 108.9 . . ?
P1 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
P1 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
C12 C11 C16 123.0(4) . . ?
C12 C11 N1 118.7(3) . . ?
C16 C11 N1 118.3(3) . . ?
C13 C12 C11 117.1(4) . . ?
C13 C12 C17 121.1(4) . . ?
C11 C12 C17 121.8(4) . . ?
C14 C13 C12 121.9(4) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C13 C14 C15 119.0(4) . . ?
C13 C14 C18 120.7(5) . . ?
C15 C14 C18 120.3(5) . . ?
C16 C15 C14 121.6(4) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C11 117.3(4) . . ?
C15 C16 C19 121.8(4) . . ?
C11 C16 C19 120.9(4) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C21 C26 119.6(3) . . ?
C22 C21 P1 118.8(3) . . ?
C26 C21 P1 121.6(3) . . ?
C23 C22 C21 120.3(3) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C24 C23 C22 119.5(4) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 120.7(4) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C26 C25 C24 119.6(4) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C25 C26 C21 120.2(3) . . ?
C25 C26 H26 119.9 . . ?
C21 C26 H26 119.9 . . ?
C36 C31 C32 118.9(4) . . ?
C36 C31 P1 123.9(3) . . ?
C32 C31 P1 117.2(3) . . ?
C33 C32 C31 120.2(5) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C34 C33 C32 120.5(5) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C35 C34 C33 119.8(4) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C34 C35 C36 119.9(6) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C31 C36 C35 120.8(5) . . ?
C31 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
C1 N1 C2 111.5(3) . . ?
C1 N1 C11 123.5(3) . . ?
C2 N1 C11 124.9(3) . . ?
C1 N2 C3 111.6(3) . . ?
C1 N2 C4 124.6(3) . . ?
C3 N2 C4 123.8(3) . . ?
O1 P1 C21 111.17(17) . . ?
O1 P1 C6 114.46(17) . . ?
C21 P1 C6 106.33(17) . . ?
O1 P1 C31 111.96(17) . . ?
C21 P1 C31 105.84(16) . . ?
C6 P1 C31 106.53(18) . . ?
Ag1 Br1 Ag1 91.158(16) . 3_547 ?
C1 Ag1 Br1 162.37(10) . . ?
C1 Ag1 Br1 108.76(10) . 3_547 ?
Br1 Ag1 Br1 88.844(17) . 3_547 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 0.1(4) . . . . ?
N2 C4 C5 C6 -175.5(3) . . . . ?
C4 C5 C6 P1 -170.7(2) . . . . ?
C16 C11 C12 C13 1.1(6) . . . . ?
N1 C11 C12 C13 -179.7(3) . . . . ?
C16 C11 C12 C17 -177.6(4) . . . . ?
N1 C11 C12 C17 1.6(5) . . . . ?
C11 C12 C13 C14 2.0(6) . . . . ?
C17 C12 C13 C14 -179.3(4) . . . . ?
C12 C13 C14 C15 -3.1(6) . . . . ?
C12 C13 C14 C18 177.1(4) . . . . ?
C13 C14 C15 C16 1.2(6) . . . . ?
C18 C14 C15 C16 -179.0(4) . . . . ?
C14 C15 C16 C11 1.7(6) . . . . ?
C14 C15 C16 C19 -176.2(4) . . . . ?
C12 C11 C16 C15 -2.9(6) . . . . ?
N1 C11 C16 C15 177.9(3) . . . . ?
C12 C11 C16 C19 175.1(4) . . . . ?
N1 C11 C16 C19 -4.1(5) . . . . ?
C26 C21 C22 C23 -0.2(5) . . . . ?
P1 C21 C22 C23 -178.2(3) . . . . ?
C21 C22 C23 C24 0.0(6) . . . . ?
C22 C23 C24 C25 0.2(6) . . . . ?
C23 C24 C25 C26 -0.2(6) . . . . ?
C24 C25 C26 C21 0.0(6) . . . . ?
C22 C21 C26 C25 0.2(5) . . . . ?
P1 C21 C26 C25 178.1(3) . . . . ?
C36 C31 C32 C33 1.1(7) . . . . ?
P1 C31 C32 C33 179.2(4) . . . . ?
C31 C32 C33 C34 0.2(8) . . . . ?
C32 C33 C34 C35 -1.4(8) . . . . ?
C33 C34 C35 C36 1.2(9) . . . . ?
C32 C31 C36 C35 -1.2(8) . . . . ?
P1 C31 C36 C35 -179.2(4) . . . . ?
C34 C35 C36 C31 0.1(9) . . . . ?
N2 C1 N1 C2 -0.2(4) . . . . ?
Ag1 C1 N1 C2 -179.3(3) . . . . ?
N2 C1 N1 C11 -179.3(3) . . . . ?
Ag1 C1 N1 C11 1.6(5) . . . . ?
C3 C2 N1 C1 0.1(4) . . . . ?
C3 C2 N1 C11 179.2(3) . . . . ?
C12 C11 N1 C1 100.5(4) . . . . ?
C16 C11 N1 C1 -80.2(5) . . . . ?
C12 C11 N1 C2 -78.5(5) . . . . ?
C16 C11 N1 C2 100.8(4) . . . . ?
N1 C1 N2 C3 0.3(4) . . . . ?
Ag1 C1 N2 C3 179.3(3) . . . . ?
N1 C1 N2 C4 -179.6(3) . . . . ?
Ag1 C1 N2 C4 -0.6(5) . . . . ?
C2 C3 N2 C1 -0.3(4) . . . . ?
C2 C3 N2 C4 179.6(3) . . . . ?
C5 C4 N2 C1 109.8(4) . . . . ?
C5 C4 N2 C3 -70.1(4) . . . . ?
C22 C21 P1 O1 19.8(3) . . . . ?
C26 C21 P1 O1 -158.1(3) . . . . ?
C22 C21 P1 C6 145.0(3) . . . . ?
C26 C21 P1 C6 -32.9(3) . . . . ?
C22 C21 P1 C31 -102.0(3) . . . . ?
C26 C21 P1 C31 80.1(3) . . . . ?
C5 C6 P1 O1 65.2(3) . . . . ?
C5 C6 P1 C21 -58.0(3) . . . . ?
C5 C6 P1 C31 -170.5(3) . . . . ?
C36 C31 P1 O1 121.7(4) . . . . ?
C32 C31 P1 O1 -56.3(4) . . . . ?
C36 C31 P1 C21 -117.1(4) . . . . ?
C32 C31 P1 C21 65.0(4) . . . . ?
C36 C31 P1 C6 -4.2(4) . . . . ?
C32 C31 P1 C6 177.9(3) . . . . ?

####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1558460'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;

_audit_creation_date             2016-06-20T12:56:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C70 H74 Ag4 Br6 N6 P2'
_chemical_formula_moiety         'C66 H68 Ag4 Br6 N4 P2, 2(C2 H3 N)'
_chemical_formula_weight         1972.17

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7558(4)
_cell_length_b                   12.6715(5)
_cell_length_c                   15.0828(6)
_cell_angle_alpha                92.2450(10)
_cell_angle_beta                 93.8830(10)
_cell_angle_gamma                102.0020(10)
_cell_volume                     1816.89(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      2.41
_cell_measurement_reflns_used    9999
_cell_measurement_theta_max      36.29
_cell_measurement_wavelength     0.71073


#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.803
_exptl_crystal_F_000             964
_exptl_crystal_density_method    'not measured'

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    4.449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.6579
_exptl_absorpt_correction_T_max  0.7462


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec I\mS Microsource '
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_number            69328
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.409
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             7411
_reflns_number_gt                6712
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0162P)²+2.2451P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7411
_refine_ls_number_parameters     401
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0461
_refine_ls_wR_factor_gt          0.0444
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.07

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.1208(2) 0.14819(16) 0.22372(14) 0.0130(4) Uani 1 1 d . . . . .
C2 C -0.0468(2) 0.19443(18) 0.13059(16) 0.0182(5) Uani 1 1 d . . . . .
H2 H -0.0893 0.2199 0.0811 0.022 Uiso 1 1 calc R U . . .
C3 C -0.1094(2) 0.15603(18) 0.20277(16) 0.0183(5) Uani 1 1 d . . . . .
H3 H -0.2038 0.149 0.2129 0.022 Uiso 1 1 calc R U . . .
C4 C -0.0322(2) 0.07365(17) 0.34142(14) 0.0151(4) Uani 1 1 d . . . . .
H4A H -0.0927 0.1083 0.3758 0.018 Uiso 1 1 calc R U . . .
H4B H 0.0558 0.0781 0.3769 0.018 Uiso 1 1 calc R U . . .
C5 C -0.1026(2) -0.04483(17) 0.31918(14) 0.0151(4) Uani 1 1 d . . . . .
H5A H -0.0572 -0.0733 0.2711 0.018 Uiso 1 1 calc R U . . .
H5B H -0.2006 -0.0501 0.2993 0.018 Uiso 1 1 calc R U . . .
C6 C -0.0930(2) -0.11216(16) 0.40079(14) 0.0123(4) Uani 1 1 d . . . . .
H6A H -0.1554 -0.0932 0.4432 0.015 Uiso 1 1 calc R U . . .
H6B H 0.002 -0.0921 0.4287 0.015 Uiso 1 1 calc R U . . .
C7 C 0.5774(3) 0.3055(3) 0.1712(2) 0.0460(8) Uani 1 1 d . . . . .
H7A H 0.5018 0.3435 0.1686 0.069 Uiso 1 1 calc R U . . .
H7B H 0.6237 0.3151 0.23 0.069 Uiso 1 1 calc R U . . .
H7C H 0.5405 0.23 0.1569 0.069 Uiso 1 1 calc R U . . .
C8 C 0.6781(3) 0.34825(19) 0.10705(15) 0.0199(5) Uani 1 1 d . . . . .
C11 C 0.1953(2) 0.21818(18) 0.07932(14) 0.0161(4) Uani 1 1 d . . . . .
C12 C 0.2403(2) 0.32668(19) 0.06323(15) 0.0191(5) Uani 1 1 d . . . . .
C13 C 0.3346(3) 0.3528(2) -0.00206(16) 0.0232(5) Uani 1 1 d . . . . .
H13 H 0.3664 0.4249 -0.0136 0.028 Uiso 1 1 calc R U . . .
C14 C 0.3824(3) 0.2738(2) -0.05031(15) 0.0252(5) Uani 1 1 d . . . . .
C15 C 0.3351(3) 0.1664(2) -0.03191(16) 0.0261(5) Uani 1 1 d . . . . .
H15 H 0.3673 0.1131 -0.0636 0.031 Uiso 1 1 calc R U . . .
C16 C 0.2407(2) 0.1358(2) 0.03261(15) 0.0213(5) Uani 1 1 d . . . . .
C17 C 0.1914(3) 0.4147(2) 0.11469(18) 0.0288(6) Uani 1 1 d . . . . .
H17A H 0.0924 0.4083 0.1011 0.043 Uiso 1 1 calc R U . . .
H17B H 0.2411 0.484 0.0984 0.043 Uiso 1 1 calc R U . . .
H17C H 0.2098 0.4078 0.1773 0.043 Uiso 1 1 calc R U . . .
C18 C 0.4836(3) 0.3042(3) -0.12080(17) 0.0348(7) Uani 1 1 d . . . . .
H18A H 0.4564 0.3601 -0.1546 0.052 Uiso 1 1 calc R U . . .
H18B H 0.4822 0.242 -0.1596 0.052 Uiso 1 1 calc R U . . .
H18C H 0.5768 0.3298 -0.093 0.052 Uiso 1 1 calc R U . . .
C19 C 0.1932(3) 0.0182(2) 0.05034(18) 0.0287(6) Uani 1 1 d . . . . .
H19A H 0.1995 -0.0253 -0.0021 0.043 Uiso 1 1 calc R U . . .
H19B H 0.0975 0.0049 0.066 0.043 Uiso 1 1 calc R U . . .
H19C H 0.2521 0.0002 0.0985 0.043 Uiso 1 1 calc R U . . .
C21 C -0.3225(2) -0.30385(17) 0.36417(14) 0.0122(4) Uani 1 1 d . . . . .
C22 C -0.3808(2) -0.41458(18) 0.35772(16) 0.0179(5) Uani 1 1 d . . . . .
H22 H -0.3228 -0.4642 0.3604 0.022 Uiso 1 1 calc R U . . .
C23 C -0.5256(2) -0.45003(18) 0.34732(16) 0.0211(5) Uani 1 1 d . . . . .
H23 H -0.5648 -0.5236 0.3418 0.025 Uiso 1 1 calc R U . . .
C24 C -0.6118(2) -0.37580(19) 0.34508(15) 0.0189(5) Uani 1 1 d . . . . .
H24 H -0.7088 -0.4 0.3376 0.023 Uiso 1 1 calc R U . . .
C25 C -0.5549(2) -0.26617(18) 0.35387(14) 0.0157(4) Uani 1 1 d . . . . .
H25 H -0.6136 -0.2169 0.3532 0.019 Uiso 1 1 calc R U . . .
C26 C -0.4103(2) -0.22974(17) 0.36360(14) 0.0133(4) Uani 1 1 d . . . . .
H26 H -0.3718 -0.156 0.3697 0.016 Uiso 1 1 calc R U . . .
C31 C -0.0485(2) -0.28582(17) 0.28286(14) 0.0141(4) Uani 1 1 d . . . . .
C32 C -0.1133(2) -0.36247(18) 0.21593(15) 0.0187(5) Uani 1 1 d . . . . .
H32 H -0.2037 -0.4021 0.2209 0.022 Uiso 1 1 calc R U . . .
C33 C -0.0419(3) -0.3793(2) 0.14174(16) 0.0236(5) Uani 1 1 d . . . . .
H33 H -0.0846 -0.4307 0.0972 0.028 Uiso 1 1 calc R U . . .
C34 C 0.0920(3) -0.3201(2) 0.13375(16) 0.0223(5) Uani 1 1 d . . . . .
H34 H 0.1389 -0.3318 0.0838 0.027 Uiso 1 1 calc R U . . .
C35 C 0.1570(2) -0.24336(19) 0.19994(15) 0.0201(5) Uani 1 1 d . . . . .
H35 H 0.2471 -0.2033 0.1942 0.024 Uiso 1 1 calc R U . . .
C36 C 0.0877(2) -0.22660(18) 0.27428(15) 0.0166(5) Uani 1 1 d . . . . .
H36 H 0.1317 -0.1757 0.3189 0.02 Uiso 1 1 calc R U . . .
C41 C -0.0705(2) -0.31585(16) 0.47503(14) 0.0132(4) Uani 1 1 d . . . . .
C42 C -0.1549(2) -0.33624(18) 0.54614(15) 0.0179(5) Uani 1 1 d . . . . .
H42 H -0.2462 -0.3248 0.5417 0.022 Uiso 1 1 calc R U . . .
C43 C -0.1014(3) -0.37361(19) 0.62344(16) 0.0226(5) Uani 1 1 d . . . . .
H43 H -0.1571 -0.3871 0.6711 0.027 Uiso 1 1 calc R U . . .
C44 C 0.0339(3) -0.39094(19) 0.63018(17) 0.0253(5) Uani 1 1 d . . . . .
H44 H 0.0689 -0.4161 0.6823 0.03 Uiso 1 1 calc R U . . .
C45 C 0.1176(3) -0.3710(2) 0.55986(17) 0.0254(5) Uani 1 1 d . . . . .
H45 H 0.2086 -0.383 0.5646 0.03 Uiso 1 1 calc R U . . .
C46 C 0.0660(2) -0.33321(18) 0.48218(16) 0.0200(5) Uani 1 1 d . . . . .
H46 H 0.1224 -0.3195 0.4349 0.024 Uiso 1 1 calc R U . . .
N1 N 0.09383(19) 0.18880(14) 0.14417(12) 0.0142(4) Uani 1 1 d . . . . .
N2 N -0.00548(19) 0.12894(14) 0.25914(12) 0.0142(4) Uani 1 1 d . . . . .
N3 N 0.7554(2) 0.38075(19) 0.05811(15) 0.0313(5) Uani 1 1 d . . . . .
P1 P -0.13591(5) -0.25624(4) 0.37914(4) 0.01086(11) Uani 1 1 d . . . . .
Br1 Br 0.49390(2) 0.27597(2) 0.39564(2) 0.01967(5) Uani 1 1 d . . . . .
Br2 Br 0.50732(2) 0.00894(2) 0.23650(2) 0.01912(5) Uani 1 1 d . . . . .
Ag2 Ag 0.53679(2) 0.07615(2) 0.41038(2) 0.02398(5) Uani 1 1 d . . . . .
Br3 Br 0.71659(2) 0.03939(2) 0.53544(2) 0.01715(5) Uani 1 1 d . . . . .
Ag1 Ag 0.31900(2) 0.12878(2) 0.28058(2) 0.02321(5) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N1 1.355(3) . ?
C1 N2 1.355(3) . ?
C1 Ag1 2.127(2) . ?
C2 C3 1.343(3) . ?
C2 N1 1.390(3) . ?
C2 H2 0.93 . ?
C3 N2 1.386(3) . ?
C3 H3 0.93 . ?
C4 N2 1.461(3) . ?
C4 C5 1.529(3) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 C6 1.534(3) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C6 P1 1.798(2) . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C7 C8 1.464(4) . ?
C7 H7A 0.96 . ?
C7 H7B 0.96 . ?
C7 H7C 0.96 . ?
C8 N3 1.120(3) . ?
C11 C12 1.390(3) . ?
C11 C16 1.399(3) . ?
C11 N1 1.443(3) . ?
C12 C13 1.396(3) . ?
C12 C17 1.509(3) . ?
C13 C14 1.390(4) . ?
C13 H13 0.93 . ?
C14 C15 1.388(4) . ?
C14 C18 1.506(3) . ?
C15 C16 1.396(4) . ?
C15 H15 0.93 . ?
C16 C19 1.506(4) . ?
C17 H17A 0.96 . ?
C17 H17B 0.96 . ?
C17 H17C 0.96 . ?
C18 H18A 0.96 . ?
C18 H18B 0.96 . ?
C18 H18C 0.96 . ?
C19 H19A 0.96 . ?
C19 H19B 0.96 . ?
C19 H19C 0.96 . ?
C21 C26 1.396(3) . ?
C21 C22 1.397(3) . ?
C21 P1 1.791(2) . ?
C22 C23 1.386(3) . ?
C22 H22 0.93 . ?
C23 C24 1.386(3) . ?
C23 H23 0.93 . ?
C24 C25 1.382(3) . ?
C24 H24 0.93 . ?
C25 C26 1.386(3) . ?
C25 H25 0.93 . ?
C26 H26 0.93 . ?
C31 C32 1.394(3) . ?
C31 C36 1.401(3) . ?
C31 P1 1.799(2) . ?
C32 C33 1.390(3) . ?
C32 H32 0.93 . ?
C33 C34 1.379(4) . ?
C33 H33 0.93 . ?
C34 C35 1.388(3) . ?
C34 H34 0.93 . ?
C35 C36 1.379(3) . ?
C35 H35 0.93 . ?
C36 H36 0.93 . ?
C41 C46 1.392(3) . ?
C41 C42 1.395(3) . ?
C41 P1 1.797(2) . ?
C42 C43 1.385(3) . ?
C42 H42 0.93 . ?
C43 C44 1.381(4) . ?
C43 H43 0.93 . ?
C44 C45 1.381(4) . ?
C44 H44 0.93 . ?
C45 C46 1.386(3) . ?
C45 H45 0.93 . ?
C46 H46 0.93 . ?
Br1 Ag2 2.6660(3) . ?
Br1 Ag1 2.7246(3) . ?
Br2 Ag2 2.7032(3) . ?
Br2 Ag1 2.7148(3) . ?
Ag2 Br3 2.6101(3) . ?
Ag2 Br3 2.7900(3) 2_656 ?
Ag2 Ag1 2.9866(3) . ?
Br3 Ag2 2.7900(3) 2_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 103.77(18) . . ?
N1 C1 Ag1 127.16(15) . . ?
N2 C1 Ag1 128.99(15) . . ?
C3 C2 N1 106.70(19) . . ?
C3 C2 H2 126.7 . . ?
N1 C2 H2 126.7 . . ?
C2 C3 N2 106.34(19) . . ?
C2 C3 H3 126.8 . . ?
N2 C3 H3 126.8 . . ?
N2 C4 C5 109.58(17) . . ?
N2 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
N2 C4 H4B 109.8 . . ?
C5 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
C4 C5 C6 110.76(17) . . ?
C4 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
C5 C6 P1 115.61(15) . . ?
C5 C6 H6A 108.4 . . ?
P1 C6 H6A 108.4 . . ?
C5 C6 H6B 108.4 . . ?
P1 C6 H6B 108.4 . . ?
H6A C6 H6B 107.4 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C7 179.8(3) . . ?
C12 C11 C16 122.5(2) . . ?
C12 C11 N1 118.9(2) . . ?
C16 C11 N1 118.6(2) . . ?
C11 C12 C13 117.8(2) . . ?
C11 C12 C17 121.9(2) . . ?
C13 C12 C17 120.3(2) . . ?
C14 C13 C12 121.8(2) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C15 C14 C13 118.5(2) . . ?
C15 C14 C18 120.8(2) . . ?
C13 C14 C18 120.7(2) . . ?
C14 C15 C16 122.0(2) . . ?
C14 C15 H15 119 . . ?
C16 C15 H15 119 . . ?
C15 C16 C11 117.4(2) . . ?
C15 C16 C19 120.0(2) . . ?
C11 C16 C19 122.7(2) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C26 C21 C22 119.88(19) . . ?
C26 C21 P1 119.64(16) . . ?
C22 C21 P1 120.39(16) . . ?
C23 C22 C21 119.6(2) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C22 C23 C24 120.0(2) . . ?
C22 C23 H23 120 . . ?
C24 C23 H23 120 . . ?
C25 C24 C23 120.6(2) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C26 119.9(2) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C25 C26 C21 119.9(2) . . ?
C25 C26 H26 120 . . ?
C21 C26 H26 120 . . ?
C32 C31 C36 119.5(2) . . ?
C32 C31 P1 122.30(17) . . ?
C36 C31 P1 118.18(16) . . ?
C33 C32 C31 119.6(2) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 120.4(2) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 120.3(2) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C36 C35 C34 119.8(2) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 C31 120.3(2) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
C46 C41 C42 119.9(2) . . ?
C46 C41 P1 121.05(17) . . ?
C42 C41 P1 118.78(16) . . ?
C43 C42 C41 119.4(2) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C44 C43 C42 120.4(2) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C43 C44 C45 120.3(2) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C46 120.0(2) . . ?
C44 C45 H45 120 . . ?
C46 C45 H45 120 . . ?
C45 C46 C41 119.9(2) . . ?
C45 C46 H46 120.1 . . ?
C41 C46 H46 120.1 . . ?
C1 N1 C2 111.37(18) . . ?
C1 N1 C11 124.94(18) . . ?
C2 N1 C11 123.64(18) . . ?
C1 N2 C3 111.82(18) . . ?
C1 N2 C4 123.80(18) . . ?
C3 N2 C4 123.95(18) . . ?
C21 P1 C41 108.53(10) . . ?
C21 P1 C6 110.43(10) . . ?
C41 P1 C6 107.37(10) . . ?
C21 P1 C31 112.61(10) . . ?
C41 P1 C31 110.49(10) . . ?
C6 P1 C31 107.29(10) . . ?
Ag2 Br1 Ag1 67.280(8) . . ?
Ag2 Br2 Ag1 66.904(8) . . ?
Br3 Ag2 Br1 119.324(10) . . ?
Br3 Ag2 Br2 128.671(10) . . ?
Br1 Ag2 Br2 99.600(9) . . ?
Br3 Ag2 Br3 101.695(9) . 2_656 ?
Br1 Ag2 Br3 103.911(9) . 2_656 ?
Br2 Ag2 Br3 99.596(9) . 2_656 ?
Br3 Ag2 Ag1 174.582(10) . . ?
Br1 Ag2 Ag1 57.296(7) . . ?
Br2 Ag2 Ag1 56.734(7) . . ?
Br3 Ag2 Ag1 75.915(8) 2_656 . ?
Ag2 Br3 Ag2 78.305(9) . 2_656 ?
C1 Ag1 Br2 135.02(6) . . ?
C1 Ag1 Br1 124.64(6) . . ?
Br2 Ag1 Br1 97.867(9) . . ?
C1 Ag1 Ag2 160.53(6) . . ?
Br2 Ag1 Ag2 56.362(7) . . ?
Br1 Ag1 Ag2 55.424(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
N1 C2 C3 N2 0.6(2) . . . . ?
N2 C4 C5 C6 163.34(17) . . . . ?
C4 C5 C6 P1 -166.85(15) . . . . ?
C16 C11 C12 C13 -0.2(3) . . . . ?
N1 C11 C12 C13 -177.8(2) . . . . ?
C16 C11 C12 C17 -179.4(2) . . . . ?
N1 C11 C12 C17 3.0(3) . . . . ?
C11 C12 C13 C14 0.3(3) . . . . ?
C17 C12 C13 C14 179.6(2) . . . . ?
C12 C13 C14 C15 -0.5(4) . . . . ?
C12 C13 C14 C18 179.6(2) . . . . ?
C13 C14 C15 C16 0.6(4) . . . . ?
C18 C14 C15 C16 -179.6(2) . . . . ?
C14 C15 C16 C11 -0.4(3) . . . . ?
C14 C15 C16 C19 -179.7(2) . . . . ?
C12 C11 C16 C15 0.2(3) . . . . ?
N1 C11 C16 C15 177.8(2) . . . . ?
C12 C11 C16 C19 179.5(2) . . . . ?
N1 C11 C16 C19 -3.0(3) . . . . ?
C26 C21 C22 C23 2.5(3) . . . . ?
P1 C21 C22 C23 179.15(18) . . . . ?
C21 C22 C23 C24 -1.2(4) . . . . ?
C22 C23 C24 C25 -0.5(4) . . . . ?
C23 C24 C25 C26 1.0(3) . . . . ?
C24 C25 C26 C21 0.2(3) . . . . ?
C22 C21 C26 C25 -2.0(3) . . . . ?
P1 C21 C26 C25 -178.68(16) . . . . ?
C36 C31 C32 C33 0.1(3) . . . . ?
P1 C31 C32 C33 177.92(18) . . . . ?
C31 C32 C33 C34 -0.4(4) . . . . ?
C32 C33 C34 C35 0.2(4) . . . . ?
C33 C34 C35 C36 0.4(4) . . . . ?
C34 C35 C36 C31 -0.7(3) . . . . ?
C32 C31 C36 C35 0.4(3) . . . . ?
P1 C31 C36 C35 -177.46(17) . . . . ?
C46 C41 C42 C43 0.1(3) . . . . ?
P1 C41 C42 C43 -174.59(17) . . . . ?
C41 C42 C43 C44 -0.2(3) . . . . ?
C42 C43 C44 C45 0.1(4) . . . . ?
C43 C44 C45 C46 0.2(4) . . . . ?
C44 C45 C46 C41 -0.3(4) . . . . ?
C42 C41 C46 C45 0.2(3) . . . . ?
P1 C41 C46 C45 174.72(18) . . . . ?
N2 C1 N1 C2 -0.1(2) . . . . ?
Ag1 C1 N1 C2 -177.00(15) . . . . ?
N2 C1 N1 C11 -177.40(19) . . . . ?
Ag1 C1 N1 C11 5.7(3) . . . . ?
C3 C2 N1 C1 -0.4(3) . . . . ?
C3 C2 N1 C11 177.0(2) . . . . ?
C12 C11 N1 C1 -111.3(2) . . . . ?
C16 C11 N1 C1 71.0(3) . . . . ?
C12 C11 N1 C2 71.7(3) . . . . ?
C16 C11 N1 C2 -106.0(2) . . . . ?
N1 C1 N2 C3 0.5(2) . . . . ?
Ag1 C1 N2 C3 177.33(15) . . . . ?
N1 C1 N2 C4 173.20(18) . . . . ?
Ag1 C1 N2 C4 -9.9(3) . . . . ?
C2 C3 N2 C1 -0.7(3) . . . . ?
C2 C3 N2 C4 -173.42(19) . . . . ?
C5 C4 N2 C1 -99.0(2) . . . . ?
C5 C4 N2 C3 72.9(3) . . . . ?
C26 C21 P1 C41 122.20(17) . . . . ?
C22 C21 P1 C41 -54.5(2) . . . . ?
C26 C21 P1 C6 4.8(2) . . . . ?
C22 C21 P1 C6 -171.91(17) . . . . ?
C26 C21 P1 C31 -115.15(18) . . . . ?
C22 C21 P1 C31 68.2(2) . . . . ?
C46 C41 P1 C21 152.12(18) . . . . ?
C42 C41 P1 C21 -33.3(2) . . . . ?
C46 C41 P1 C6 -88.51(19) . . . . ?
C42 C41 P1 C6 86.08(19) . . . . ?
C46 C41 P1 C31 28.2(2) . . . . ?
C42 C41 P1 C31 -157.22(17) . . . . ?
C5 C6 P1 C21 -77.92(18) . . . . ?
C5 C6 P1 C41 163.92(16) . . . . ?
C5 C6 P1 C31 45.14(18) . . . . ?
C32 C31 P1 C21 -16.9(2) . . . . ?
C36 C31 P1 C21 160.91(17) . . . . ?
C32 C31 P1 C41 104.62(19) . . . . ?
C36 C31 P1 C41 -77.55(19) . . . . ?
C32 C31 P1 C6 -138.62(18) . . . . ?
C36 C31 P1 C6 39.20(19) . . . . ?

####################################################################### 
# 
# 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_1OTf2
_database_code_depnum_ccdc_archive 'CCDC 1558456'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;

_audit_creation_date             2016-06-20T12:30:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C35 H35 F6 N2 O6 P S2'
_chemical_formula_moiety         'C33 H35 N2 P, 2(C F3 O3 S)'
_chemical_formula_weight         788.74
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7214(4)
_cell_length_b                   13.9079(7)
_cell_length_c                   15.3042(7)
_cell_angle_alpha                68.116(2)
_cell_angle_beta                 87.751(2)
_cell_angle_gamma                70.945(2)
_cell_volume                     1806.84(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      2.47
_cell_measurement_reflns_used    9999
_cell_measurement_theta_max      36.29
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.45
_exptl_crystal_F_000             816
_exptl_crystal_density_method    'not measured'

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.27
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.6702
_exptl_absorpt_correction_T_max  0.7456


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec I\mS Microsource '
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_number            15978
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.469
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.973
_reflns_Friedel_coverage         0
_reflns_number_total             7184
_reflns_number_gt                5510
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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+1.8191P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7184
_refine_ls_number_parameters     472
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1182
_refine_ls_wR_factor_gt          0.1073
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.47
_refine_diff_density_rms         0.07

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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'
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'
O O 0.0106 0.006 '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'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C7 C -0.4426(3) 0.2247(2) 0.6165(2) 0.0296(7) Uani 1 1 d . . . . .
C8 C -0.5186(3) 0.5233(2) 0.26200(18) 0.0200(6) Uani 1 1 d . . . . .
P1 P 0.02223(6) 0.29390(5) 0.34171(4) 0.01337(14) Uani 1 1 d . . . . .
F1 F -0.5463(2) 0.32135(15) 0.58448(18) 0.0641(7) Uani 1 1 d . . . . .
O1 O -0.63150(19) 0.12777(15) 0.67883(13) 0.0279(5) Uani 1 1 d . . . . .
F3 F -0.3885(2) 0.20826(17) 0.70120(13) 0.0475(5) Uani 1 1 d . . . . .
O2 O -0.5530(2) 0.14277(18) 0.52367(14) 0.0339(5) Uani 1 1 d . . . . .
O3 O -0.3894(2) 0.01782(15) 0.66531(15) 0.0296(5) Uani 1 1 d . . . . .
F2 F -0.3353(2) 0.22934(16) 0.56050(13) 0.0455(5) Uani 1 1 d . . . . .
F5 F -0.43459(17) 0.41765(13) 0.28861(13) 0.0355(4) Uani 1 1 d . . . . .
O6 O -0.75262(19) 0.66789(14) 0.15864(13) 0.0240(4) Uani 1 1 d . . . . .
F4 F -0.5576(2) 0.54201(15) 0.33977(11) 0.0383(4) Uani 1 1 d . . . . .
F6 F -0.43572(17) 0.58315(14) 0.22031(13) 0.0351(4) Uani 1 1 d . . . . .
O5 O -0.6121(2) 0.52165(16) 0.10873(13) 0.0307(5) Uani 1 1 d . . . . .
O4 O -0.7484(2) 0.48073(16) 0.24614(14) 0.0309(5) Uani 1 1 d . . . . .
S1 S -0.51166(7) 0.11610(5) 0.62068(5) 0.02001(16) Uani 1 1 d . . . . .
C34 C -0.1970(3) 0.5691(2) 0.06131(19) 0.0304(7) Uani 1 1 d . . . . .
H34 H -0.2389 0.6248 0.0033 0.037 Uiso 1 1 calc R U . . .
C35 C -0.2014(3) 0.4647(2) 0.08156(19) 0.0280(6) Uani 1 1 d . . . . .
H35 H -0.247 0.4506 0.0376 0.034 Uiso 1 1 calc R U . . .
C36 C -0.1379(3) 0.3811(2) 0.16731(18) 0.0210(6) Uani 1 1 d . . . . .
H36 H -0.1408 0.3108 0.1812 0.025 Uiso 1 1 calc R U . . .
C31 C -0.0694(2) 0.4023(2) 0.23293(17) 0.0160(5) Uani 1 1 d . . . . .
C6 C 0.2178(2) 0.2519(2) 0.33749(16) 0.0146(5) Uani 1 1 d . . . . .
H6A H 0.2527 0.3022 0.3527 0.018 Uiso 1 1 calc R U . . .
H6B H 0.2606 0.1796 0.3869 0.018 Uiso 1 1 calc R U . . .
C5 C 0.2756(3) 0.2470(2) 0.24446(16) 0.0162(5) Uani 1 1 d . . . . .
H5A H 0.2489 0.1932 0.2293 0.019 Uiso 1 1 calc R U . . .
H5B H 0.2351 0.3182 0.1932 0.019 Uiso 1 1 calc R U . . .
C4 C 0.4413(3) 0.2140(2) 0.25838(17) 0.0166(5) Uani 1 1 d . . . . .
H4A H 0.4653 0.2694 0.2727 0.02 Uiso 1 1 calc R U . . .
H4B H 0.4786 0.145 0.3124 0.02 Uiso 1 1 calc R U . . .
N2 N 0.5150(2) 0.20154(17) 0.17536(14) 0.0160(4) Uani 1 1 d . . . . .
C1 C 0.5699(3) 0.1073(2) 0.16236(17) 0.0173(5) Uani 1 1 d . . . . .
H1 H 0.5651 0.0395 0.2027 0.021 Uiso 1 1 calc R U . . .
N1 N 0.6330(2) 0.12700(16) 0.08139(14) 0.0161(4) Uani 1 1 d . . . . .
C11 C 0.7102(3) 0.0459(2) 0.04255(17) 0.0162(5) Uani 1 1 d . . . . .
C12 C 0.6529(3) 0.0555(2) -0.04391(17) 0.0184(5) Uani 1 1 d . . . . .
C13 C 0.7324(3) -0.0199(2) -0.08192(18) 0.0207(6) Uani 1 1 d . . . . .
H13 H 0.6977 -0.0153 -0.1396 0.025 Uiso 1 1 calc R U . . .
C14 C 0.8628(3) -0.1024(2) -0.03576(18) 0.0197(5) Uani 1 1 d . . . . .
C18 C 0.9476(3) -0.1831(2) -0.07876(19) 0.0256(6) Uani 1 1 d . . . . .
H18A H 1.046 -0.2183 -0.0494 0.038 Uiso 1 1 calc R U . . .
H18B H 0.9486 -0.1447 -0.1454 0.038 Uiso 1 1 calc R U . . .
H18C H 0.9021 -0.2376 -0.0688 0.038 Uiso 1 1 calc R U . . .
C24 C -0.0921(3) 0.3979(2) 0.59213(19) 0.0252(6) Uani 1 1 d . . . . .
H24 H -0.1173 0.4159 0.6447 0.03 Uiso 1 1 calc R U . . .
C25 C -0.1928(3) 0.4424(2) 0.51416(19) 0.0240(6) Uani 1 1 d . . . . .
H25 H -0.2849 0.4912 0.514 0.029 Uiso 1 1 calc R U . . .
C26 C -0.1572(3) 0.4145(2) 0.43651(18) 0.0190(5) Uani 1 1 d . . . . .
H26 H -0.225 0.4449 0.3841 0.023 Uiso 1 1 calc R U . . .
C21 C -0.0196(3) 0.34085(19) 0.43667(16) 0.0144(5) Uani 1 1 d . . . . .
C3 C 0.5438(3) 0.2841(2) 0.10058(17) 0.0178(5) Uani 1 1 d . . . . .
H3 H 0.5174 0.3578 0.0921 0.021 Uiso 1 1 calc R U . . .
C2 C 0.6176(3) 0.2370(2) 0.04239(17) 0.0182(5) Uani 1 1 d . . . . .
H2 H 0.652 0.2724 -0.0139 0.022 Uiso 1 1 calc R U . . .
C16 C 0.8400(3) -0.0360(2) 0.09181(17) 0.0173(5) Uani 1 1 d . . . . .
C15 C 0.9143(3) -0.1100(2) 0.05059(18) 0.0196(5) Uani 1 1 d . . . . .
H15 H 1.0006 -0.1658 0.0818 0.024 Uiso 1 1 calc R U . . .
C17 C 0.5104(3) 0.1430(2) -0.09375(19) 0.0249(6) Uani 1 1 d . . . . .
H17A H 0.5255 0.2123 -0.1242 0.037 Uiso 1 1 calc R U . . .
H17B H 0.44 0.1486 -0.0485 0.037 Uiso 1 1 calc R U . . .
H17C H 0.4749 0.1237 -0.1403 0.037 Uiso 1 1 calc R U . . .
C19 C 0.9006(3) -0.0451(2) 0.18427(18) 0.0227(6) Uani 1 1 d . . . . .
H19A H 0.8496 -0.0801 0.2344 0.034 Uiso 1 1 calc R U . . .
H19B H 0.8883 0.0271 0.1822 0.034 Uiso 1 1 calc R U . . .
H19C H 1.0027 -0.0881 0.1953 0.034 Uiso 1 1 calc R U . . .
C33 C -0.1311(3) 0.5915(2) 0.1263(2) 0.0285(7) Uani 1 1 d . . . . .
H33 H -0.1298 0.6622 0.1125 0.034 Uiso 1 1 calc R U . . .
C32 C -0.0669(3) 0.5077(2) 0.21238(18) 0.0211(6) Uani 1 1 d . . . . .
H32 H -0.0221 0.5223 0.2563 0.025 Uiso 1 1 calc R U . . .
C41 C -0.0404(3) 0.1796(2) 0.36379(16) 0.0154(5) Uani 1 1 d . . . . .
C46 C -0.1821(3) 0.1895(2) 0.39089(17) 0.0183(5) Uani 1 1 d . . . . .
H46 H -0.2418 0.2545 0.3959 0.022 Uiso 1 1 calc R U . . .
C45 C -0.2330(3) 0.1026(2) 0.41016(17) 0.0207(6) Uani 1 1 d . . . . .
H45 H -0.3266 0.1089 0.4289 0.025 Uiso 1 1 calc R U . . .
C44 C -0.1454(3) 0.0063(2) 0.40176(17) 0.0225(6) Uani 1 1 d . . . . .
H44 H -0.1813 -0.0512 0.4129 0.027 Uiso 1 1 calc R U . . .
C43 C -0.0040(3) -0.0046(2) 0.37667(17) 0.0210(6) Uani 1 1 d . . . . .
H43 H 0.0554 -0.0701 0.3723 0.025 Uiso 1 1 calc R U . . .
C42 C 0.0491(3) 0.0816(2) 0.35805(17) 0.0174(5) Uani 1 1 d . . . . .
H42 H 0.1442 0.0738 0.3418 0.021 Uiso 1 1 calc R U . . .
C22 C 0.0829(3) 0.2981(2) 0.51468(17) 0.0185(5) Uani 1 1 d . . . . .
H22 H 0.1759 0.2504 0.5147 0.022 Uiso 1 1 calc R U . . .
C23 C 0.0458(3) 0.3269(2) 0.59227(18) 0.0222(6) Uani 1 1 d . . . . .
H23 H 0.1139 0.2983 0.6444 0.027 Uiso 1 1 calc R U . . .
S2 S -0.67699(7) 0.55216(5) 0.18492(4) 0.01711(15) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C7 F1 1.314(3) . ?
C7 F2 1.326(3) . ?
C7 F3 1.328(3) . ?
C7 S1 1.823(3) . ?
C8 F6 1.323(3) . ?
C8 F4 1.326(3) . ?
C8 F5 1.337(3) . ?
C8 S2 1.819(3) . ?
P1 C21 1.786(3) . ?
P1 C31 1.791(2) . ?
P1 C41 1.797(3) . ?
P1 C6 1.803(2) . ?
O1 S1 1.4417(19) . ?
O2 S1 1.429(2) . ?
O3 S1 1.4332(19) . ?
O6 S2 1.4357(18) . ?
O5 S2 1.440(2) . ?
O4 S2 1.4328(19) . ?
C34 C35 1.382(4) . ?
C34 C33 1.382(4) . ?
C34 H34 0.93 . ?
C35 C36 1.383(4) . ?
C35 H35 0.93 . ?
C36 C31 1.393(4) . ?
C36 H36 0.93 . ?
C31 C32 1.389(4) . ?
C6 C5 1.527(3) . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C5 C4 1.525(3) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C4 N2 1.473(3) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
N2 C1 1.331(3) . ?
N2 C3 1.383(3) . ?
C1 N1 1.336(3) . ?
C1 H1 0.93 . ?
N1 C2 1.377(3) . ?
N1 C11 1.449(3) . ?
C11 C16 1.398(3) . ?
C11 C12 1.399(4) . ?
C12 C13 1.389(4) . ?
C12 C17 1.507(4) . ?
C13 C14 1.392(4) . ?
C13 H13 0.93 . ?
C14 C15 1.387(4) . ?
C14 C18 1.508(4) . ?
C18 H18A 0.96 . ?
C18 H18B 0.96 . ?
C18 H18C 0.96 . ?
C24 C23 1.381(4) . ?
C24 C25 1.382(4) . ?
C24 H24 0.93 . ?
C25 C26 1.380(4) . ?
C25 H25 0.93 . ?
C26 C21 1.394(3) . ?
C26 H26 0.93 . ?
C21 C22 1.396(3) . ?
C3 C2 1.347(4) . ?
C3 H3 0.93 . ?
C2 H2 0.93 . ?
C16 C15 1.393(4) . ?
C16 C19 1.500(4) . ?
C15 H15 0.93 . ?
C17 H17A 0.96 . ?
C17 H17B 0.96 . ?
C17 H17C 0.96 . ?
C19 H19A 0.96 . ?
C19 H19B 0.96 . ?
C19 H19C 0.96 . ?
C33 C32 1.388(4) . ?
C33 H33 0.93 . ?
C32 H32 0.93 . ?
C41 C42 1.389(3) . ?
C41 C46 1.401(3) . ?
C46 C45 1.381(4) . ?
C46 H46 0.93 . ?
C45 C44 1.382(4) . ?
C45 H45 0.93 . ?
C44 C43 1.388(4) . ?
C44 H44 0.93 . ?
C43 C42 1.387(4) . ?
C43 H43 0.93 . ?
C42 H42 0.93 . ?
C22 C23 1.388(4) . ?
C22 H22 0.93 . ?
C23 H23 0.93 . ?

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
F1 C7 F2 107.9(2) . . ?
F1 C7 F3 107.9(3) . . ?
F2 C7 F3 106.7(2) . . ?
F1 C7 S1 111.1(2) . . ?
F2 C7 S1 111.2(2) . . ?
F3 C7 S1 111.84(19) . . ?
F6 C8 F4 107.5(2) . . ?
F6 C8 F5 107.1(2) . . ?
F4 C8 F5 107.6(2) . . ?
F6 C8 S2 112.66(17) . . ?
F4 C8 S2 111.58(18) . . ?
F5 C8 S2 110.14(18) . . ?
C21 P1 C31 109.65(11) . . ?
C21 P1 C41 108.86(11) . . ?
C31 P1 C41 109.07(12) . . ?
C21 P1 C6 107.85(11) . . ?
C31 P1 C6 110.97(11) . . ?
C41 P1 C6 110.41(12) . . ?
O2 S1 O3 116.22(13) . . ?
O2 S1 O1 114.91(12) . . ?
O3 S1 O1 113.30(11) . . ?
O2 S1 C7 103.63(13) . . ?
O3 S1 C7 103.10(13) . . ?
O1 S1 C7 103.42(13) . . ?
C35 C34 C33 120.7(2) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C34 C35 C36 119.9(3) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C31 120.0(3) . . ?
C35 C36 H36 120 . . ?
C31 C36 H36 120 . . ?
C32 C31 C36 119.8(2) . . ?
C32 C31 P1 119.4(2) . . ?
C36 C31 P1 120.7(2) . . ?
C5 C6 P1 117.09(17) . . ?
C5 C6 H6A 108 . . ?
P1 C6 H6A 108 . . ?
C5 C6 H6B 108 . . ?
P1 C6 H6B 108 . . ?
H6A C6 H6B 107.3 . . ?
C4 C5 C6 106.61(19) . . ?
C4 C5 H5A 110.4 . . ?
C6 C5 H5A 110.4 . . ?
C4 C5 H5B 110.4 . . ?
C6 C5 H5B 110.4 . . ?
H5A C5 H5B 108.6 . . ?
N2 C4 C5 113.4(2) . . ?
N2 C4 H4A 108.9 . . ?
C5 C4 H4A 108.9 . . ?
N2 C4 H4B 108.9 . . ?
C5 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C1 N2 C3 109.0(2) . . ?
C1 N2 C4 125.1(2) . . ?
C3 N2 C4 125.8(2) . . ?
N2 C1 N1 108.2(2) . . ?
N2 C1 H1 125.9 . . ?
N1 C1 H1 125.9 . . ?
C1 N1 C2 108.6(2) . . ?
C1 N1 C11 126.0(2) . . ?
C2 N1 C11 125.3(2) . . ?
C16 C11 C12 123.3(2) . . ?
C16 C11 N1 118.6(2) . . ?
C12 C11 N1 118.1(2) . . ?
C13 C12 C11 117.1(2) . . ?
C13 C12 C17 121.0(2) . . ?
C11 C12 C17 121.9(2) . . ?
C12 C13 C14 121.6(2) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C15 C14 C13 119.3(2) . . ?
C15 C14 C18 120.1(2) . . ?
C13 C14 C18 120.6(2) . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C23 C24 C25 120.3(3) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C26 C25 C24 120.2(2) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C21 120.0(2) . . ?
C25 C26 H26 120 . . ?
C21 C26 H26 120 . . ?
C26 C21 C22 119.5(2) . . ?
C26 C21 P1 120.57(19) . . ?
C22 C21 P1 119.79(18) . . ?
C2 C3 N2 106.6(2) . . ?
C2 C3 H3 126.7 . . ?
N2 C3 H3 126.7 . . ?
C3 C2 N1 107.6(2) . . ?
C3 C2 H2 126.2 . . ?
N1 C2 H2 126.2 . . ?
C15 C16 C11 117.0(2) . . ?
C15 C16 C19 120.2(2) . . ?
C11 C16 C19 122.8(2) . . ?
C14 C15 C16 121.7(2) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C34 C33 C32 119.6(3) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C31 C32 C33 120.1(3) . . ?
C31 C32 H32 120 . . ?
C33 C32 H32 120 . . ?
C42 C41 C46 119.8(2) . . ?
C42 C41 P1 121.94(19) . . ?
C46 C41 P1 118.22(19) . . ?
C45 C46 C41 119.9(2) . . ?
C45 C46 H46 120.1 . . ?
C41 C46 H46 120.1 . . ?
C46 C45 C44 120.3(2) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C45 C44 C43 120.0(2) . . ?
C45 C44 H44 120 . . ?
C43 C44 H44 120 . . ?
C42 C43 C44 120.3(3) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C43 C42 C41 119.7(2) . . ?
C43 C42 H42 120.1 . . ?
C41 C42 H42 120.1 . . ?
C23 C22 C21 119.9(2) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C24 C23 C22 120.0(2) . . ?
C24 C23 H23 120 . . ?
C22 C23 H23 120 . . ?
O4 S2 O6 115.84(12) . . ?
O4 S2 O5 115.22(13) . . ?
O6 S2 O5 114.48(11) . . ?
O4 S2 C8 101.65(12) . . ?
O6 S2 C8 104.13(12) . . ?
O5 S2 C8 102.86(12) . . ?

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
F1 C7 S1 O2 64.0(2) . . . . ?
F2 C7 S1 O2 -56.3(2) . . . . ?
F3 C7 S1 O2 -175.4(2) . . . . ?
F1 C7 S1 O3 -174.5(2) . . . . ?
F2 C7 S1 O3 65.3(2) . . . . ?
F3 C7 S1 O3 -53.8(2) . . . . ?
F1 C7 S1 O1 -56.3(2) . . . . ?
F2 C7 S1 O1 -176.49(19) . . . . ?
F3 C7 S1 O1 64.4(2) . . . . ?
C33 C34 C35 C36 -0.7(4) . . . . ?
C34 C35 C36 C31 -0.1(4) . . . . ?
C35 C36 C31 C32 0.8(4) . . . . ?
C35 C36 C31 P1 -176.6(2) . . . . ?
C21 P1 C31 C32 45.2(2) . . . . ?
C41 P1 C31 C32 164.28(19) . . . . ?
C6 P1 C31 C32 -73.9(2) . . . . ?
C21 P1 C31 C36 -137.4(2) . . . . ?
C41 P1 C31 C36 -18.3(2) . . . . ?
C6 P1 C31 C36 103.6(2) . . . . ?
C21 P1 C6 C5 -159.22(18) . . . . ?
C31 P1 C6 C5 -39.1(2) . . . . ?
C41 P1 C6 C5 81.9(2) . . . . ?
P1 C6 C5 C4 177.88(17) . . . . ?
C6 C5 C4 N2 177.9(2) . . . . ?
C5 C4 N2 C1 -94.0(3) . . . . ?
C5 C4 N2 C3 88.9(3) . . . . ?
C3 N2 C1 N1 0.0(3) . . . . ?
C4 N2 C1 N1 -177.6(2) . . . . ?
N2 C1 N1 C2 0.1(3) . . . . ?
N2 C1 N1 C11 177.8(2) . . . . ?
C1 N1 C11 C16 -65.3(3) . . . . ?
C2 N1 C11 C16 111.9(3) . . . . ?
C1 N1 C11 C12 116.4(3) . . . . ?
C2 N1 C11 C12 -66.4(3) . . . . ?
C16 C11 C12 C13 -1.2(4) . . . . ?
N1 C11 C12 C13 177.0(2) . . . . ?
C16 C11 C12 C17 178.2(2) . . . . ?
N1 C11 C12 C17 -3.6(3) . . . . ?
C11 C12 C13 C14 0.6(4) . . . . ?
C17 C12 C13 C14 -178.8(2) . . . . ?
C12 C13 C14 C15 0.4(4) . . . . ?
C12 C13 C14 C18 -179.7(2) . . . . ?
C23 C24 C25 C26 1.2(4) . . . . ?
C24 C25 C26 C21 0.4(4) . . . . ?
C25 C26 C21 C22 -1.8(4) . . . . ?
C25 C26 C21 P1 174.0(2) . . . . ?
C31 P1 C21 C26 34.9(2) . . . . ?
C41 P1 C21 C26 -84.4(2) . . . . ?
C6 P1 C21 C26 155.8(2) . . . . ?
C31 P1 C21 C22 -149.33(19) . . . . ?
C41 P1 C21 C22 91.4(2) . . . . ?
C6 P1 C21 C22 -28.4(2) . . . . ?
C1 N2 C3 C2 -0.1(3) . . . . ?
C4 N2 C3 C2 177.4(2) . . . . ?
N2 C3 C2 N1 0.2(3) . . . . ?
C1 N1 C2 C3 -0.2(3) . . . . ?
C11 N1 C2 C3 -177.9(2) . . . . ?
C12 C11 C16 C15 0.6(4) . . . . ?
N1 C11 C16 C15 -177.6(2) . . . . ?
C12 C11 C16 C19 179.7(2) . . . . ?
N1 C11 C16 C19 1.5(3) . . . . ?
C13 C14 C15 C16 -1.0(4) . . . . ?
C18 C14 C15 C16 179.1(2) . . . . ?
C11 C16 C15 C14 0.5(4) . . . . ?
C19 C16 C15 C14 -178.7(2) . . . . ?
C35 C34 C33 C32 0.9(4) . . . . ?
C36 C31 C32 C33 -0.7(4) . . . . ?
P1 C31 C32 C33 176.8(2) . . . . ?
C34 C33 C32 C31 -0.2(4) . . . . ?
C21 P1 C41 C42 -130.3(2) . . . . ?
C31 P1 C41 C42 110.1(2) . . . . ?
C6 P1 C41 C42 -12.1(2) . . . . ?
C21 P1 C41 C46 47.3(2) . . . . ?
C31 P1 C41 C46 -72.3(2) . . . . ?
C6 P1 C41 C46 165.55(18) . . . . ?
C42 C41 C46 C45 -1.1(4) . . . . ?
P1 C41 C46 C45 -178.79(19) . . . . ?
C41 C46 C45 C44 -0.8(4) . . . . ?
C46 C45 C44 C43 2.0(4) . . . . ?
C45 C44 C43 C42 -1.3(4) . . . . ?
C44 C43 C42 C41 -0.6(4) . . . . ?
C46 C41 C42 C43 1.8(4) . . . . ?
P1 C41 C42 C43 179.36(19) . . . . ?
C26 C21 C22 C23 1.7(4) . . . . ?
P1 C21 C22 C23 -174.15(19) . . . . ?
C25 C24 C23 C22 -1.3(4) . . . . ?
C21 C22 C23 C24 -0.2(4) . . . . ?
F6 C8 S2 O4 -178.59(19) . . . . ?
F4 C8 S2 O4 -57.5(2) . . . . ?
F5 C8 S2 O4 61.9(2) . . . . ?
F6 C8 S2 O6 -57.9(2) . . . . ?
F4 C8 S2 O6 63.2(2) . . . . ?
F5 C8 S2 O6 -177.39(17) . . . . ?
F6 C8 S2 O5 61.8(2) . . . . ?
F4 C8 S2 O5 -177.10(18) . . . . ?
F5 C8 S2 O5 -57.7(2) . . . . ?

####################################################################### 
# 
# 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_1Br2
_database_code_depnum_ccdc_archive 'CCDC 1558455'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;

_audit_creation_date             2016-06-20T13:36:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C33 H35 Br2 N2 P'
_chemical_formula_moiety         '2(Br), C33 H35 N2 P'
_chemical_formula_weight         650.42

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6720(2)
_cell_length_b                   12.7253(2)
_cell_length_c                   13.8740(2)
_cell_angle_alpha                108.111(2)
_cell_angle_beta                 100.7790(10)
_cell_angle_gamma                98.7350(10)
_cell_volume                     1553.51(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_theta_min      3.4630
_cell_measurement_reflns_used    27482
_cell_measurement_theta_max      32.6430
_cell_measurement_wavelength     0.71073


#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.39
_exptl_crystal_F_000             664
_exptl_crystal_density_method    'not measured'

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    2.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_T_max  1.000



#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_number            69177
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.913
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             6338
_reflns_number_gt                5784
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0560P)²+0.6809P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6338
_refine_ls_number_parameters     346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0912
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.095

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.3348(2) 0.36161(18) 0.12882(18) 0.0253(4) Uani 1 1 d . . . . .
H1 H 0.4147 0.4211 0.1653 0.03 Uiso 1 1 calc R U . . .
C2 C 0.1110(2) 0.26442(19) 0.05137(19) 0.0312(5) Uani 1 1 d . . . . .
H2 H 0.0111 0.2469 0.026 0.037 Uiso 1 1 calc R U . . .
C3 C 0.1980(2) 0.18995(19) 0.04201(19) 0.0305(5) Uani 1 1 d . . . . .
H3 H 0.1694 0.1116 0.009 0.037 Uiso 1 1 calc R U . . .
C4 C 0.4711(2) 0.21001(18) 0.10131(17) 0.0243(4) Uani 1 1 d . . . . .
H4A H 0.5483 0.2632 0.0943 0.029 Uiso 1 1 calc R U . . .
H4B H 0.4564 0.138 0.0452 0.029 Uiso 1 1 calc R U . . .
C5 C 0.5158(2) 0.19407(17) 0.20616(16) 0.0205(4) Uani 1 1 d . . . . .
H5A H 0.4574 0.1245 0.2052 0.025 Uiso 1 1 calc R U . . .
H5B H 0.5025 0.257 0.262 0.025 Uiso 1 1 calc R U . . .
C6 C 0.6756(2) 0.18866(17) 0.22396(16) 0.0199(4) Uani 1 1 d . . . . .
H6A H 0.7322 0.2641 0.2383 0.024 Uiso 1 1 calc R U . . .
H6B H 0.6894 0.1396 0.159 0.024 Uiso 1 1 calc R U . . .
C11 C 0.1561(2) 0.47937(18) 0.13291(18) 0.0247(4) Uani 1 1 d . . . . .
C12 C 0.1987(2) 0.55403(18) 0.08310(17) 0.0250(4) Uani 1 1 d . . . . .
C13 C 0.1672(2) 0.66090(18) 0.11667(18) 0.0269(4) Uani 1 1 d . . . . .
H13 H 0.1953 0.713 0.0857 0.032 Uiso 1 1 calc R U . . .
C14 C 0.0950(2) 0.69163(19) 0.19494(19) 0.0300(5) Uani 1 1 d . . . . .
C15 C 0.0497(3) 0.6124(2) 0.2392(2) 0.0332(5) Uani 1 1 d . . . . .
H15 H -0.0027 0.6315 0.2894 0.04 Uiso 1 1 calc R U . . .
C16 C 0.0810(2) 0.5051(2) 0.2100(2) 0.0312(5) Uani 1 1 d . . . . .
C17 C 0.2743(3) 0.5222(2) -0.0041(2) 0.0353(5) Uani 1 1 d . . . . .
H17A H 0.2653 0.5723 -0.0431 0.053 Uiso 1 1 calc R U . . .
H17B H 0.2311 0.4455 -0.0497 0.053 Uiso 1 1 calc R U . . .
H17C H 0.3747 0.5286 0.0251 0.053 Uiso 1 1 calc R U . . .
C18 C 0.0660(3) 0.8095(2) 0.2312(2) 0.0434(6) Uani 1 1 d . . . . .
H18A H 0.1282 0.859 0.2094 0.065 Uiso 1 1 calc R U . . .
H18B H 0.0846 0.8379 0.3062 0.065 Uiso 1 1 calc R U . . .
H18C H -0.0329 0.8065 0.2011 0.065 Uiso 1 1 calc R U . . .
C19 C 0.0363(3) 0.4226(3) 0.2626(3) 0.0476(7) Uani 1 1 d . . . . .
H19A H -0.0285 0.3555 0.2114 0.071 Uiso 1 1 calc R U . . .
H19B H -0.0113 0.4571 0.315 0.071 Uiso 1 1 calc R U . . .
H19C H 0.1204 0.4028 0.2949 0.071 Uiso 1 1 calc R U . . .
C21 C 0.6910(2) 0.20810(18) 0.44106(16) 0.0226(4) Uani 1 1 d . . . . .
C22 C 0.6439(3) 0.1482(2) 0.50233(18) 0.0295(5) Uani 1 1 d . . . . .
H22 H 0.6479 0.0723 0.4868 0.035 Uiso 1 1 calc R U . . .
C23 C 0.5911(3) 0.2021(2) 0.5863(2) 0.0371(6) Uani 1 1 d . . . . .
H23 H 0.5602 0.1626 0.6275 0.045 Uiso 1 1 calc R U . . .
C24 C 0.5845(3) 0.3153(2) 0.60915(19) 0.0370(6) Uani 1 1 d . . . . .
H24 H 0.5487 0.3512 0.6654 0.044 Uiso 1 1 calc R U . . .
C25 C 0.6310(3) 0.3750(2) 0.54858(19) 0.0343(5) Uani 1 1 d . . . . .
H25 H 0.6255 0.4505 0.5641 0.041 Uiso 1 1 calc R U . . .
C26 C 0.6857(2) 0.32281(19) 0.46500(17) 0.0280(5) Uani 1 1 d . . . . .
H26 H 0.7185 0.3634 0.4252 0.034 Uiso 1 1 calc R U . . .
C31 C 0.9424(2) 0.17264(17) 0.34854(16) 0.0206(4) Uani 1 1 d . . . . .
C32 C 1.0006(2) 0.11371(19) 0.26815(17) 0.0264(4) Uani 1 1 d . . . . .
H32 H 0.9397 0.0612 0.2063 0.032 Uiso 1 1 calc R U . . .
C33 C 1.1489(2) 0.1340(2) 0.28106(19) 0.0319(5) Uani 1 1 d . . . . .
H33 H 1.1881 0.0945 0.2283 0.038 Uiso 1 1 calc R U . . .
C34 C 1.2386(2) 0.2133(2) 0.37299(19) 0.0332(5) Uani 1 1 d . . . . .
H34 H 1.3381 0.2261 0.3819 0.04 Uiso 1 1 calc R U . . .
C35 C 1.1816(2) 0.2738(2) 0.45203(18) 0.0328(5) Uani 1 1 d . . . . .
H35 H 1.2427 0.3278 0.513 0.039 Uiso 1 1 calc R U . . .
C36 C 1.0328(2) 0.25332(19) 0.43970(16) 0.0259(4) Uani 1 1 d . . . . .
H36 H 0.994 0.2936 0.4924 0.031 Uiso 1 1 calc R U . . .
C41 C 0.6952(2) -0.01184(17) 0.28667(16) 0.0207(4) Uani 1 1 d . . . . .
C42 C 0.5853(2) -0.07409(18) 0.19754(17) 0.0251(4) Uani 1 1 d . . . . .
H42 H 0.535 -0.0369 0.1597 0.03 Uiso 1 1 calc R U . . .
C43 C 0.5503(3) -0.19238(19) 0.16472(18) 0.0303(5) Uani 1 1 d . . . . .
H43 H 0.4765 -0.2341 0.1052 0.036 Uiso 1 1 calc R U . . .
C44 C 0.6258(3) -0.24757(19) 0.22119(19) 0.0315(5) Uani 1 1 d . . . . .
H44 H 0.6036 -0.3264 0.1987 0.038 Uiso 1 1 calc R U . . .
C45 C 0.7337(3) -0.1859(2) 0.3106(2) 0.0330(5) Uani 1 1 d . . . . .
H45 H 0.7826 -0.2234 0.3488 0.04 Uiso 1 1 calc R U . . .
C46 C 0.7699(2) -0.0682(2) 0.34395(18) 0.0276(5) Uani 1 1 d . . . . .
H46 H 0.8432 -0.027 0.4039 0.033 Uiso 1 1 calc R U . . .
Br1 Br 0.24534(2) -0.08350(2) 0.02694(2) 0.02458(8) Uani 1 1 d . . . . .
Br2 Br 0.67720(2) 0.49846(2) 0.28801(2) 0.02712(8) Uani 1 1 d . . . . .
N1 N 0.19845(19) 0.37136(15) 0.10574(15) 0.0254(4) Uani 1 1 d . . . . .
N2 N 0.33748(19) 0.25256(15) 0.09090(14) 0.0240(4) Uani 1 1 d . . . . .
P1 P 0.74873(5) 0.13981(4) 0.32633(4) 0.01785(11) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N2 1.329(3) . ?
C1 N1 1.332(3) . ?
C1 H1 0.93 . ?
C2 C3 1.353(3) . ?
C2 N1 1.382(3) . ?
C2 H2 0.93 . ?
C3 N2 1.382(3) . ?
C3 H3 0.93 . ?
C4 N2 1.475(3) . ?
C4 C5 1.523(3) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 C6 1.535(3) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C6 P1 1.792(2) . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C11 C16 1.387(3) . ?
C11 C12 1.395(3) . ?
C11 N1 1.451(3) . ?
C12 C13 1.395(3) . ?
C12 C17 1.510(3) . ?
C13 C14 1.386(3) . ?
C13 H13 0.93 . ?
C14 C15 1.391(3) . ?
C14 C18 1.514(3) . ?
C15 C16 1.396(3) . ?
C15 H15 0.93 . ?
C16 C19 1.509(3) . ?
C17 H17A 0.96 . ?
C17 H17B 0.96 . ?
C17 H17C 0.96 . ?
C18 H18A 0.96 . ?
C18 H18B 0.96 . ?
C18 H18C 0.96 . ?
C19 H19A 0.96 . ?
C19 H19B 0.96 . ?
C19 H19C 0.96 . ?
C21 C22 1.398(3) . ?
C21 C26 1.404(3) . ?
C21 P1 1.795(2) . ?
C22 C23 1.386(3) . ?
C22 H22 0.93 . ?
C23 C24 1.389(4) . ?
C23 H23 0.93 . ?
C24 C25 1.385(4) . ?
C24 H24 0.93 . ?
C25 C26 1.387(3) . ?
C25 H25 0.93 . ?
C26 H26 0.93 . ?
C31 C36 1.387(3) . ?
C31 C32 1.402(3) . ?
C31 P1 1.801(2) . ?
C32 C33 1.386(3) . ?
C32 H32 0.93 . ?
C33 C34 1.385(3) . ?
C33 H33 0.93 . ?
C34 C35 1.389(3) . ?
C34 H34 0.93 . ?
C35 C36 1.391(3) . ?
C35 H35 0.93 . ?
C36 H36 0.93 . ?
C41 C42 1.389(3) . ?
C41 C46 1.401(3) . ?
C41 P1 1.796(2) . ?
C42 C43 1.396(3) . ?
C42 H42 0.93 . ?
C43 C44 1.387(3) . ?
C43 H43 0.93 . ?
C44 C45 1.381(4) . ?
C44 H44 0.93 . ?
C45 C46 1.389(3) . ?
C45 H45 0.93 . ?
C46 H46 0.93 . ?

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
N2 C1 N1 108.53(18) . . ?
N2 C1 H1 125.7 . . ?
N1 C1 H1 125.7 . . ?
C3 C2 N1 107.07(19) . . ?
C3 C2 H2 126.5 . . ?
N1 C2 H2 126.5 . . ?
C2 C3 N2 106.87(19) . . ?
C2 C3 H3 126.6 . . ?
N2 C3 H3 126.6 . . ?
N2 C4 C5 112.10(17) . . ?
N2 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
N2 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C4 C5 C6 107.42(16) . . ?
C4 C5 H5A 110.2 . . ?
C6 C5 H5A 110.2 . . ?
C4 C5 H5B 110.2 . . ?
C6 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
C5 C6 P1 117.62(14) . . ?
C5 C6 H6A 107.9 . . ?
P1 C6 H6A 107.9 . . ?
C5 C6 H6B 107.9 . . ?
P1 C6 H6B 107.9 . . ?
H6A C6 H6B 107.2 . . ?
C16 C11 C12 123.4(2) . . ?
C16 C11 N1 118.50(19) . . ?
C12 C11 N1 118.04(19) . . ?
C13 C12 C11 117.0(2) . . ?
C13 C12 C17 120.54(19) . . ?
C11 C12 C17 122.5(2) . . ?
C14 C13 C12 121.8(2) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C13 C14 C15 118.9(2) . . ?
C13 C14 C18 120.3(2) . . ?
C15 C14 C18 120.8(2) . . ?
C14 C15 C16 121.6(2) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C11 C16 C15 117.2(2) . . ?
C11 C16 C19 122.2(2) . . ?
C15 C16 C19 120.5(2) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C21 C26 120.05(19) . . ?
C22 C21 P1 121.54(17) . . ?
C26 C21 P1 118.30(16) . . ?
C23 C22 C21 119.8(2) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 120.0(2) . . ?
C22 C23 H23 120 . . ?
C24 C23 H23 120 . . ?
C25 C24 C23 120.4(2) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.5(2) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 119.3(2) . . ?
C25 C26 H26 120.4 . . ?
C21 C26 H26 120.4 . . ?
C36 C31 C32 120.13(19) . . ?
C36 C31 P1 122.78(16) . . ?
C32 C31 P1 117.09(15) . . ?
C33 C32 C31 119.9(2) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C34 C33 C32 119.6(2) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C35 120.8(2) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 H34 119.6 . . ?
C34 C35 C36 119.7(2) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C31 C36 C35 119.8(2) . . ?
C31 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
C42 C41 C46 119.75(19) . . ?
C42 C41 P1 120.84(15) . . ?
C46 C41 P1 119.35(16) . . ?
C41 C42 C43 120.1(2) . . ?
C41 C42 H42 120 . . ?
C43 C42 H42 120 . . ?
C44 C43 C42 119.8(2) . . ?
C44 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C45 C44 C43 120.2(2) . . ?
C45 C44 H44 119.9 . . ?
C43 C44 H44 119.9 . . ?
C44 C45 C46 120.5(2) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C45 C46 C41 119.6(2) . . ?
C45 C46 H46 120.2 . . ?
C41 C46 H46 120.2 . . ?
C1 N1 C2 108.65(18) . . ?
C1 N1 C11 123.39(18) . . ?
C2 N1 C11 127.93(18) . . ?
C1 N2 C3 108.88(18) . . ?
C1 N2 C4 123.57(18) . . ?
C3 N2 C4 127.56(18) . . ?
C6 P1 C21 108.89(9) . . ?
C6 P1 C41 111.26(10) . . ?
C21 P1 C41 111.09(10) . . ?
C6 P1 C31 107.52(9) . . ?
C21 P1 C31 112.17(10) . . ?
C41 P1 C31 105.86(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 0.0(3) . . . . ?
N2 C4 C5 C6 -161.65(17) . . . . ?
C4 C5 C6 P1 -166.74(14) . . . . ?
C16 C11 C12 C13 2.3(3) . . . . ?
N1 C11 C12 C13 -174.84(18) . . . . ?
C16 C11 C12 C17 -177.1(2) . . . . ?
N1 C11 C12 C17 5.8(3) . . . . ?
C11 C12 C13 C14 -0.9(3) . . . . ?
C17 C12 C13 C14 178.5(2) . . . . ?
C12 C13 C14 C15 -1.7(3) . . . . ?
C12 C13 C14 C18 178.4(2) . . . . ?
C13 C14 C15 C16 2.9(4) . . . . ?
C18 C14 C15 C16 -177.1(2) . . . . ?
C12 C11 C16 C15 -1.1(3) . . . . ?
N1 C11 C16 C15 176.0(2) . . . . ?
C12 C11 C16 C19 -180.0(2) . . . . ?
N1 C11 C16 C19 -2.8(3) . . . . ?
C14 C15 C16 C11 -1.6(4) . . . . ?
C14 C15 C16 C19 177.3(2) . . . . ?
C26 C21 C22 C23 0.4(3) . . . . ?
P1 C21 C22 C23 -175.74(19) . . . . ?
C21 C22 C23 C24 0.3(4) . . . . ?
C22 C23 C24 C25 -0.3(4) . . . . ?
C23 C24 C25 C26 -0.5(4) . . . . ?
C24 C25 C26 C21 1.2(4) . . . . ?
C22 C21 C26 C25 -1.2(3) . . . . ?
P1 C21 C26 C25 175.11(18) . . . . ?
C36 C31 C32 C33 1.8(3) . . . . ?
P1 C31 C32 C33 -179.08(18) . . . . ?
C31 C32 C33 C34 -0.7(4) . . . . ?
C32 C33 C34 C35 -0.8(4) . . . . ?
C33 C34 C35 C36 1.1(4) . . . . ?
C32 C31 C36 C35 -1.4(3) . . . . ?
P1 C31 C36 C35 179.50(17) . . . . ?
C34 C35 C36 C31 0.0(3) . . . . ?
C46 C41 C42 C43 -0.5(3) . . . . ?
P1 C41 C42 C43 176.60(16) . . . . ?
C41 C42 C43 C44 -0.2(3) . . . . ?
C42 C43 C44 C45 1.1(3) . . . . ?
C43 C44 C45 C46 -1.2(4) . . . . ?
C44 C45 C46 C41 0.5(3) . . . . ?
C42 C41 C46 C45 0.4(3) . . . . ?
P1 C41 C46 C45 -176.80(17) . . . . ?
N2 C1 N1 C2 0.2(3) . . . . ?
N2 C1 N1 C11 -178.27(19) . . . . ?
C3 C2 N1 C1 -0.1(3) . . . . ?
C3 C2 N1 C11 178.2(2) . . . . ?
C16 C11 N1 C1 -109.9(2) . . . . ?
C12 C11 N1 C1 67.4(3) . . . . ?
C16 C11 N1 C2 71.9(3) . . . . ?
C12 C11 N1 C2 -110.8(3) . . . . ?
N1 C1 N2 C3 -0.2(3) . . . . ?
N1 C1 N2 C4 179.63(19) . . . . ?
C2 C3 N2 C1 0.1(3) . . . . ?
C2 C3 N2 C4 -179.7(2) . . . . ?
C5 C4 N2 C1 83.7(3) . . . . ?
C5 C4 N2 C3 -96.5(3) . . . . ?
C5 C6 P1 C21 -45.43(18) . . . . ?
C5 C6 P1 C41 77.33(17) . . . . ?
C5 C6 P1 C31 -167.18(15) . . . . ?
C22 C21 P1 C6 137.26(18) . . . . ?
C26 C21 P1 C6 -38.94(19) . . . . ?
C22 C21 P1 C41 14.4(2) . . . . ?
C26 C21 P1 C41 -161.81(16) . . . . ?
C22 C21 P1 C31 -103.86(19) . . . . ?
C26 C21 P1 C31 79.94(19) . . . . ?
C42 C41 P1 C6 -13.5(2) . . . . ?
C46 C41 P1 C6 163.65(16) . . . . ?
C42 C41 P1 C21 107.99(18) . . . . ?
C46 C41 P1 C21 -74.86(19) . . . . ?
C42 C41 P1 C31 -130.01(17) . . . . ?
C46 C41 P1 C31 47.15(19) . . . . ?
C36 C31 P1 C6 111.65(18) . . . . ?
C32 C31 P1 C6 -67.48(18) . . . . ?
C36 C31 P1 C21 -8.0(2) . . . . ?
C32 C31 P1 C21 172.84(16) . . . . ?
C36 C31 P1 C41 -129.35(18) . . . . ?
C32 C31 P1 C41 51.53(18) . . . . ?

