# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1889378'
loop_
_audit_author_name
_audit_author_address
'Moumita Majumdar'
;IISER Pune
India
;
_audit_update_record             
;
2019-01-08 deposited with the CCDC.	2019-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H42 Cl10 F6 Ge2 N2 O6 P2 S2'
_chemical_formula_weight         1458.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.0330(10)
_cell_length_b                   12.4374(11)
_cell_length_c                   13.1345(12)
_cell_angle_alpha                62.303(3)
_cell_angle_beta                 71.710(3)
_cell_angle_gamma                64.929(3)
_cell_volume                     1430.0(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      3.84
_cell_measurement_theta_max      66.87

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_F_000             730
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.38
_exptl_absorpt_coefficient_mu    7.398
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.046
_exptl_absorpt_correction_T_max  0.060
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16149
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.842
_diffrn_reflns_theta_max         66.868
_diffrn_reflns_theta_full        66.868
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             5029
_reflns_number_gt                4500
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²+2.4306P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5029
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1055
_refine_ls_wR_factor_gt          0.1026
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.72682(4) 0.68431(3) 0.36615(3) 0.01211(13) Uani 1 1 d . . . . .
Cl1 Cl 0.68299(8) 0.89860(7) 0.25987(7) 0.01690(19) Uani 1 1 d . . . . .
S1 S 0.39131(8) 0.70515(8) 0.38008(7) 0.01427(19) Uani 1 1 d . . . . .
P1 P 0.82960(8) 0.64754(7) 0.18641(7) 0.00965(18) Uani 1 1 d . . . . .
Cl05 Cl 0.37774(8) 0.69709(8) 0.76501(8) 0.0228(2) Uani 1 1 d . . . . .
Cl4 Cl 0.86665(9) 0.96238(9) 0.41116(8) 0.0258(2) Uani 1 1 d . . . . .
Cl3 Cl 0.65511(9) 0.85917(9) 0.57242(8) 0.0268(2) Uani 1 1 d . . . . .
Cl6 Cl 0.66454(9) 0.54530(9) 0.76248(8) 0.0282(2) Uani 1 1 d . . . . .
F2 F 0.3265(2) 0.8831(2) 0.17573(18) 0.0272(5) Uani 1 1 d . . . . .
F3 F 0.3418(2) 0.9556(2) 0.2896(2) 0.0269(5) Uani 1 1 d . . . . .
F1 F 0.1698(2) 0.8992(2) 0.3205(2) 0.0311(5) Uani 1 1 d . . . . .
O1 O 0.5278(2) 0.6780(2) 0.3160(2) 0.0196(5) Uani 1 1 d . . . . .
O2 O 0.3805(2) 0.7185(2) 0.4857(2) 0.0220(5) Uani 1 1 d . . . . .
O3 O 0.3166(2) 0.6313(2) 0.3859(2) 0.0235(6) Uani 1 1 d . . . . .
N1 N 0.9471(3) 0.6429(3) 0.3651(2) 0.0132(6) Uani 1 1 d . . . . .
C14 C 1.0523(3) 0.4285(3) 0.1790(3) 0.0152(7) Uani 1 1 d . . . . .
H00G H 1.0962 0.4839 0.1196 0.018 Uiso 1 1 calc R U . . .
C22 C 1.0376(3) 0.6830(3) 0.2847(3) 0.0140(7) Uani 1 1 d . . . . .
H00H H 1.1141 0.6731 0.3084 0.017 Uiso 1 1 calc R U . . .
C13 C 0.9217(3) 0.4773(3) 0.2298(3) 0.0120(6) Uani 1 1 d . . . . .
C7 C 0.7180(3) 0.6898(3) 0.0885(3) 0.0130(6) Uani 1 1 d . . . . .
C17 C 0.9201(3) 0.2627(3) 0.3559(3) 0.0172(7) Uani 1 1 d . . . . .
H00K H 0.8760 0.2069 0.4143 0.021 Uiso 1 1 calc R U . . .
C9 C 0.5557(3) 0.8518(3) -0.0403(3) 0.0193(7) Uani 1 1 d . . . . .
H00L H 0.5097 0.9379 -0.0805 0.023 Uiso 1 1 calc R U . . .
C16 C 1.0504(4) 0.2145(3) 0.3053(3) 0.0182(7) Uani 1 1 d . . . . .
H00M H 1.0938 0.1260 0.3306 0.022 Uiso 1 1 calc R U . . .
C23 C 0.9802(3) 0.5723(3) 0.4842(3) 0.0157(7) Uani 1 1 d . . . . .
H00A H 0.9026 0.5990 0.5380 0.019 Uiso 1 1 calc R U . . .
H00B H 1.0546 0.5908 0.4894 0.019 Uiso 1 1 calc R U . . .
C10 C 0.5318(3) 0.7565(4) -0.0500(3) 0.0208(8) Uani 1 1 d . . . . .
H00O H 0.4697 0.7787 -0.0965 0.025 Uiso 1 1 calc R U . . .
C4 C 1.0574(4) 0.8514(4) -0.0837(3) 0.0222(8) Uani 1 1 d . . . . .
H00P H 1.0650 0.8877 -0.1643 0.027 Uiso 1 1 calc R U . . .
C1 C 1.0340(3) 0.7429(3) 0.1590(3) 0.0138(6) Uani 1 1 d . . . . .
C15 C 1.1173(3) 0.2962(3) 0.2174(3) 0.0186(7) Uani 1 1 d . . . . .
H00R H 1.2052 0.2627 0.1843 0.022 Uiso 1 1 calc R U . . .
C21 C 0.3046(3) 0.8692(3) 0.2859(3) 0.0181(7) Uani 1 1 d . . . . .
C8 C 0.6480(3) 0.8196(3) 0.0291(3) 0.0163(7) Uani 1 1 d . . . . .
H00T H 0.6633 0.8837 0.0361 0.020 Uiso 1 1 calc R U . . .
C6 C 0.9506(3) 0.7328(3) 0.1029(3) 0.0126(6) Uani 1 1 d . . . . .
C12 C 0.6940(3) 0.5944(3) 0.0783(3) 0.0163(7) Uani 1 1 d . . . . .
H00V H 0.7404 0.5081 0.1174 0.020 Uiso 1 1 calc R U . . .
C5 C 0.9652(3) 0.7855(3) -0.0173(3) 0.0181(7) Uani 1 1 d . . . . .
H00W H 0.9127 0.7770 -0.0546 0.022 Uiso 1 1 calc R U . . .
C18 C 0.8554(3) 0.3948(3) 0.3190(3) 0.0151(7) Uani 1 1 d . . . . .
H00X H 0.7684 0.4281 0.3537 0.018 Uiso 1 1 calc R U . . .
C3 C 1.1374(4) 0.8623(3) -0.0287(3) 0.0225(8) Uani 1 1 d . . . . .
H00Y H 1.1975 0.9077 -0.0723 0.027 Uiso 1 1 calc R U . . .
C11 C 0.5998(4) 0.6289(4) 0.0091(3) 0.0218(8) Uani 1 1 d . . . . .
H00Z H 0.5828 0.5653 0.0028 0.026 Uiso 1 1 calc R U . . .
C2 C 1.1280(4) 0.8061(3) 0.0903(3) 0.0207(7) Uani 1 1 d . . . . .
H010 H 1.1856 0.8102 0.1260 0.025 Uiso 1 1 calc R U . . .
C20 C 0.5158(4) 0.5902(4) 0.7069(3) 0.0220(8) Uani 1 1 d . . . . .
H01A H 0.4946 0.5139 0.7270 0.026 Uiso 1 1 calc R U . . .
H01B H 0.5307 0.6317 0.6229 0.026 Uiso 1 1 calc R U . . .
C19 C 0.6913(4) 0.9985(3) 0.4631(3) 0.0211(7) Uani 1 1 d . . . . .
H01C H 0.6419 1.0325 0.3993 0.025 Uiso 1 1 calc R U . . .
H01D H 0.6617 1.0639 0.4946 0.025 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 2.258(3) . ?
Ge1 Cl1 2.2713(9) . ?
Ge1 P1 2.4397(9) . ?
S1 O2 1.436(3) . ?
S1 O3 1.438(2) . ?
S1 O1 1.458(2) . ?
S1 C21 1.830(4) . ?
P1 C13 1.806(3) . ?
P1 C7 1.807(3) . ?
P1 C6 1.819(3) . ?
Cl05 C20 1.780(4) . ?
Cl4 C19 1.770(4) . ?
Cl3 C19 1.771(4) . ?
Cl6 C20 1.770(3) . ?
F2 C21 1.328(4) . ?
F3 C21 1.327(4) . ?
F1 C21 1.349(4) . ?
N1 C22 1.277(4) . ?
N1 C23 1.470(4) . ?
C14 C13 1.386(5) . ?
C14 C15 1.390(5) . ?
C14 H00G 0.9300 . ?
C22 C1 1.468(5) . ?
C22 H00H 0.9300 . ?
C13 C18 1.392(5) . ?
C7 C12 1.391(5) . ?
C7 C8 1.400(5) . ?
C17 C16 1.381(5) . ?
C17 C18 1.389(5) . ?
C17 H00K 0.9300 . ?
C9 C10 1.385(5) . ?
C9 C8 1.388(5) . ?
C9 H00L 0.9300 . ?
C16 C15 1.386(5) . ?
C16 H00M 0.9300 . ?
C23 C23 1.533(7) 2_766 ?
C23 H00A 0.9700 . ?
C23 H00B 0.9700 . ?
C10 C11 1.376(5) . ?
C10 H00O 0.9300 . ?
C4 C3 1.382(5) . ?
C4 C5 1.397(5) . ?
C4 H00P 0.9300 . ?
C1 C2 1.397(5) . ?
C1 C6 1.419(4) . ?
C15 H00R 0.9300 . ?
C8 H00T 0.9300 . ?
C6 C5 1.385(5) . ?
C12 C11 1.393(5) . ?
C12 H00V 0.9300 . ?
C5 H00W 0.9300 . ?
C18 H00X 0.9300 . ?
C3 C2 1.373(5) . ?
C3 H00Y 0.9300 . ?
C11 H00Z 0.9300 . ?
C2 H010 0.9300 . ?
C20 H01A 0.9700 . ?
C20 H01B 0.9700 . ?
C19 H01C 0.9700 . ?
C19 H01D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 Cl1 94.75(7) . . ?
N1 Ge1 P1 78.81(7) . . ?
Cl1 Ge1 P1 88.59(3) . . ?
O2 S1 O3 116.09(16) . . ?
O2 S1 O1 114.72(14) . . ?
O3 S1 O1 114.33(15) . . ?
O2 S1 C21 102.85(16) . . ?
O3 S1 C21 103.67(15) . . ?
O1 S1 C21 102.67(15) . . ?
C13 P1 C7 107.70(15) . . ?
C13 P1 C6 107.84(15) . . ?
C7 P1 C6 106.77(15) . . ?
C13 P1 Ge1 105.99(11) . . ?
C7 P1 Ge1 117.60(11) . . ?
C6 P1 Ge1 110.56(11) . . ?
C22 N1 C23 117.1(3) . . ?
C22 N1 Ge1 131.8(2) . . ?
C23 N1 Ge1 110.4(2) . . ?
C13 C14 C15 119.6(3) . . ?
C13 C14 H00G 120.2 . . ?
C15 C14 H00G 120.2 . . ?
N1 C22 C1 127.0(3) . . ?
N1 C22 H00H 116.5 . . ?
C1 C22 H00H 116.5 . . ?
C14 C13 C18 120.5(3) . . ?
C14 C13 P1 122.8(3) . . ?
C18 C13 P1 116.7(2) . . ?
C12 C7 C8 120.0(3) . . ?
C12 C7 P1 120.4(3) . . ?
C8 C7 P1 119.5(2) . . ?
C16 C17 C18 119.7(3) . . ?
C16 C17 H00K 120.2 . . ?
C18 C17 H00K 120.2 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H00L 119.8 . . ?
C8 C9 H00L 119.8 . . ?
C17 C16 C15 120.9(3) . . ?
C17 C16 H00M 119.5 . . ?
C15 C16 H00M 119.5 . . ?
N1 C23 C23 109.0(3) . 2_766 ?
N1 C23 H00A 109.9 . . ?
C23 C23 H00A 109.9 2_766 . ?
N1 C23 H00B 109.9 . . ?
C23 C23 H00B 109.9 2_766 . ?
H00A C23 H00B 108.3 . . ?
C11 C10 C9 120.1(3) . . ?
C11 C10 H00O 119.9 . . ?
C9 C10 H00O 119.9 . . ?
C3 C4 C5 119.6(3) . . ?
C3 C4 H00P 120.2 . . ?
C5 C4 H00P 120.2 . . ?
C2 C1 C6 118.5(3) . . ?
C2 C1 C22 116.2(3) . . ?
C6 C1 C22 125.1(3) . . ?
C16 C15 C14 119.6(3) . . ?
C16 C15 H00R 120.2 . . ?
C14 C15 H00R 120.2 . . ?
F3 C21 F2 108.0(3) . . ?
F3 C21 F1 107.2(3) . . ?
F2 C21 F1 107.2(3) . . ?
F3 C21 S1 112.1(2) . . ?
F2 C21 S1 112.2(2) . . ?
F1 C21 S1 109.9(2) . . ?
C9 C8 C7 119.5(3) . . ?
C9 C8 H00T 120.3 . . ?
C7 C8 H00T 120.3 . . ?
C5 C6 C1 119.0(3) . . ?
C5 C6 P1 119.9(2) . . ?
C1 C6 P1 121.0(2) . . ?
C7 C12 C11 119.5(3) . . ?
C7 C12 H00V 120.2 . . ?
C11 C12 H00V 120.2 . . ?
C6 C5 C4 121.2(3) . . ?
C6 C5 H00W 119.4 . . ?
C4 C5 H00W 119.4 . . ?
C17 C18 C13 119.6(3) . . ?
C17 C18 H00X 120.2 . . ?
C13 C18 H00X 120.2 . . ?
C2 C3 C4 119.9(3) . . ?
C2 C3 H00Y 120.0 . . ?
C4 C3 H00Y 120.0 . . ?
C10 C11 C12 120.5(3) . . ?
C10 C11 H00Z 119.7 . . ?
C12 C11 H00Z 119.7 . . ?
C3 C2 C1 121.7(3) . . ?
C3 C2 H010 119.2 . . ?
C1 C2 H010 119.2 . . ?
Cl6 C20 Cl05 110.5(2) . . ?
Cl6 C20 H01A 109.5 . . ?
Cl05 C20 H01A 109.5 . . ?
Cl6 C20 H01B 109.5 . . ?
Cl05 C20 H01B 109.5 . . ?
H01A C20 H01B 108.1 . . ?
Cl4 C19 Cl3 110.76(19) . . ?
Cl4 C19 H01C 109.5 . . ?
Cl3 C19 H01C 109.5 . . ?
Cl4 C19 H01D 109.5 . . ?
Cl3 C19 H01D 109.5 . . ?
H01C C19 H01D 108.1 . . ?

_refine_diff_density_max         0.736
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.105

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1889380'
loop_
_audit_author_name
_audit_author_address
'Moumita Majumdar'
;IISER Pune
India
;
_audit_update_record             
;
2019-02-20 deposited with the CCDC.	2019-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H23 Cl3 F3 Ge N O3 P S'
_chemical_formula_weight         660.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.8139(5)
_cell_length_b                   17.6150(9)
_cell_length_c                   14.8147(8)
_cell_angle_alpha                90
_cell_angle_beta                 90.808(3)
_cell_angle_gamma                90
_cell_volume                     2821.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4760
_cell_measurement_theta_min      3.90
_cell_measurement_theta_max      66.95

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_F_000             1332
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    5.730
_shelx_estimated_absorpt_T_min   0.254
_shelx_estimated_absorpt_T_max   0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.271
_exptl_absorpt_correction_T_max  0.564
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16690
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_av_R_equivalents  0.1023
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.899
_diffrn_reflns_theta_max         67.221
_diffrn_reflns_theta_full        67.221
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             4915
_reflns_number_gt                3488
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0731P)²+21.8397P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4915
_refine_ls_number_parameters     353
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0733
_refine_ls_wR_factor_ref         0.1893
_refine_ls_wR_factor_gt          0.1698
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.26519(7) 0.60820(4) 0.58018(5) 0.0172(2) Uani 1 1 d . . . A 1
Cl1 Cl 0.23026(16) 0.71504(9) 0.66092(11) 0.0238(4) Uani 1 1 d . . . A 1
P1 P 0.27365(15) 0.53252(9) 0.72283(12) 0.0164(4) Uani 1 1 d . . . A 1
N1 N 0.0684(5) 0.5842(3) 0.5695(4) 0.0149(11) Uani 1 1 d . . . A 1
C1 C 0.3986(6) 0.4645(4) 0.7179(5) 0.0185(14) Uani 1 1 d . . . A 1
C2 C 0.4678(7) 0.4450(4) 0.7946(5) 0.0245(16) Uani 1 1 d . . . A 1
H2 H 0.4512 0.4681 0.8511 0.029 Uiso 1 1 calc R U . A 1
C3 C 0.5612(6) 0.3915(4) 0.7871(5) 0.0253(16) Uani 1 1 d . . . A 1
H3 H 0.6090 0.3776 0.8388 0.030 Uiso 1 1 calc R U . A 1
C4 C 0.5847(7) 0.3583(4) 0.7047(5) 0.0286(17) Uani 1 1 d . . . A 1
H4 H 0.6484 0.3214 0.7001 0.034 Uiso 1 1 calc R U . A 1
C5 C 0.5172(7) 0.3778(4) 0.6294(5) 0.0277(17) Uani 1 1 d . . . A 1
H5 H 0.5340 0.3544 0.5731 0.033 Uiso 1 1 calc R U . A 1
C6 C 0.4241(6) 0.4320(4) 0.6355(5) 0.0224(15) Uani 1 1 d . . . A 1
H6 H 0.3782 0.4465 0.5831 0.027 Uiso 1 1 calc R U . A 1
C7 C 0.2968(6) 0.5905(4) 0.8215(4) 0.0201(15) Uani 1 1 d . . . A 1
C8 C 0.2056(8) 0.6020(5) 0.8857(5) 0.0345(19) Uani 1 1 d . . . A 1
H8 H 0.1277 0.5773 0.8801 0.041 Uiso 1 1 calc R U . A 1
C9 C 0.2309(9) 0.6506(6) 0.9587(6) 0.053(3) Uani 1 1 d . . . A 1
H9 H 0.1686 0.6599 1.0019 0.063 Uiso 1 1 calc R U . A 1
C10 C 0.3437(8) 0.6849(5) 0.9686(6) 0.038(2) Uani 1 1 d . . . A 1
H10 H 0.3604 0.7164 1.0194 0.046 Uiso 1 1 calc R U . A 1
C11 C 0.4314(8) 0.6737(4) 0.9058(5) 0.0337(19) Uani 1 1 d . . . A 1
H11 H 0.5089 0.6988 0.9121 0.040 Uiso 1 1 calc R U . A 1
C12 C 0.4108(7) 0.6268(4) 0.8329(5) 0.0299(18) Uani 1 1 d . . . A 1
H12 H 0.4743 0.6191 0.7902 0.036 Uiso 1 1 calc R U . A 1
C13 C 0.1314(6) 0.4794(4) 0.7400(5) 0.0200(15) Uani 1 1 d . . . A 1
C14 C 0.1380(7) 0.4102(4) 0.7860(6) 0.035(2) Uani 1 1 d . . . A 1
H14 H 0.2160 0.3906 0.8049 0.043 Uiso 1 1 calc R U . A 1
C15 C 0.0313(7) 0.3703(5) 0.8038(6) 0.040(2) Uani 1 1 d . . . A 1
H15 H 0.0360 0.3240 0.8366 0.048 Uiso 1 1 calc R U . A 1
C16 C -0.0818(7) 0.3971(4) 0.7745(6) 0.0341(19) Uani 1 1 d . . . A 1
H16 H -0.1549 0.3694 0.7871 0.041 Uiso 1 1 calc R U . A 1
C17 C -0.0888(6) 0.4647(4) 0.7262(6) 0.0274(17) Uani 1 1 d . . . A 1
H17 H -0.1670 0.4825 0.7050 0.033 Uiso 1 1 calc R U . A 1
C18 C 0.0171(6) 0.5067(4) 0.7086(4) 0.0147(13) Uani 1 1 d . . . A 1
C19 C -0.0005(6) 0.5801(4) 0.6569(5) 0.0210(15) Uani 1 1 d . . . A 1
H19A H -0.0898 0.5869 0.6437 0.025 Uiso 1 1 calc R U . A 1
H19B H 0.0266 0.6227 0.6958 0.025 Uiso 1 1 calc R U . A 1
C20 C 0.0647(6) 0.5122(4) 0.5153(5) 0.0191(14) Uani 1 1 d . . . A 1
H20A H 0.1019 0.4708 0.5519 0.023 Uiso 1 1 calc R U . A 1
H20B H 0.1163 0.5189 0.4612 0.023 Uiso 1 1 calc R U . A 1
C21 C 0.0176(6) 0.6488(4) 0.5147(5) 0.0192(14) Uani 1 1 d . . . A 1
H21A H 0.0648 0.6537 0.4590 0.029 Uiso 1 1 calc R U . A 1
H21B H 0.0243 0.6959 0.5496 0.029 Uiso 1 1 calc R U . A 1
H21C H -0.0694 0.6389 0.4996 0.029 Uiso 1 1 calc R U . A 1
S1 S 0.63718(15) 0.61917(10) 0.62940(12) 0.0236(4) Uani 1 1 d . . . B 1
F1 F 0.6285(7) 0.7577(4) 0.5679(6) 0.103(3) Uani 1 1 d . . . B 1
F2 F 0.7946(5) 0.7309(3) 0.6375(5) 0.0620(17) Uani 1 1 d . . . B 1
F3 F 0.6274(5) 0.7501(3) 0.7113(5) 0.079(2) Uani 1 1 d . . . B 1
O1 O 0.5052(5) 0.6195(3) 0.6148(4) 0.0406(14) Uani 1 1 d . . . B 1
O2 O 0.7094(5) 0.5923(4) 0.5552(4) 0.0444(16) Uani 1 1 d . . . B 1
O3 O 0.6765(5) 0.5910(3) 0.7154(4) 0.0375(14) Uani 1 1 d . . . B 1
C22 C 0.6740(7) 0.7190(5) 0.6370(7) 0.044(2) Uani 1 1 d . . . B 1
C23 C 0.807(2) 0.6382(13) 0.902(2) 0.114(3) Uani 0.5 1 d D U P C 1
H23A H 0.7490 0.6632 0.9441 0.137 Uiso 0.5 1 calc R U P C 1
H23B H 0.7568 0.6178 0.8513 0.137 Uiso 0.5 1 calc R U P C 1
Cl2 Cl 0.9124(8) 0.7122(4) 0.8568(5) 0.0866(18) Uani 0.5 1 d D U P C 1
Cl3 Cl 0.8773(9) 0.5595(6) 0.9605(6) 0.114(2) Uani 0.5 1 d D U P C 1
C23' C 0.863(3) 0.6149(16) 0.973(2) 0.127(3) Uani 0.5 1 d D U P D 2
H23C H 0.9442 0.5912 0.9859 0.152 Uiso 0.5 1 calc R U P D 2
H23D H 0.8410 0.6430 1.0286 0.152 Uiso 0.5 1 calc R U P D 2
Cl2' Cl 0.8906(12) 0.6844(7) 0.8921(8) 0.131(3) Uani 0.5 1 d D U P D 2
Cl3' Cl 0.7599(13) 0.5411(7) 0.9666(8) 0.159(3) Uani 0.5 1 d D U P D 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 2.173(5) . ?
Ge1 Cl1 2.2646(18) . ?
Ge1 P1 2.4993(18) . ?
P1 C7 1.798(7) . ?
P1 C1 1.808(7) . ?
P1 C13 1.822(7) . ?
N1 C21 1.497(8) . ?
N1 C20 1.502(8) . ?
N1 C19 1.503(9) . ?
C1 C6 1.380(10) . ?
C1 C2 1.395(10) . ?
C2 C3 1.388(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.367(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(10) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.394(10) . ?
C7 C12 1.397(10) . ?
C8 C9 1.405(12) . ?
C8 H8 0.9500 . ?
C9 C10 1.367(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.353(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.375(10) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.397(10) . ?
C13 C18 1.400(9) . ?
C14 C15 1.380(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.376(11) . ?
C15 H15 0.9500 . ?
C16 C17 1.392(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.513(9) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C20 1.525(13) 3_566 ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
S1 O3 1.427(6) . ?
S1 O2 1.437(6) . ?
S1 O1 1.440(6) . ?
S1 C22 1.806(9) . ?
F1 C22 1.319(11) . ?
F2 C22 1.321(9) . ?
F3 C22 1.334(11) . ?
C23 Cl3 1.797(18) . ?
C23 Cl2 1.864(18) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23' Cl3' 1.714(18) . ?
C23' Cl2' 1.745(18) . ?
C23' H23C 0.9900 . ?
C23' H23D 0.9900 . ?

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 Ge1 Cl1 91.70(15) . . ?
N1 Ge1 P1 88.95(15) . . ?
Cl1 Ge1 P1 90.06(6) . . ?
C7 P1 C1 108.3(3) . . ?
C7 P1 C13 106.7(3) . . ?
C1 P1 C13 107.4(3) . . ?
C7 P1 Ge1 112.8(2) . . ?
C1 P1 Ge1 109.7(2) . . ?
C13 P1 Ge1 111.8(2) . . ?
C21 N1 C20 110.1(5) . . ?
C21 N1 C19 108.7(5) . . ?
C20 N1 C19 114.2(5) . . ?
C21 N1 Ge1 104.0(4) . . ?
C20 N1 Ge1 102.8(4) . . ?
C19 N1 Ge1 116.3(4) . . ?
C6 C1 C2 120.4(6) . . ?
C6 C1 P1 118.0(5) . . ?
C2 C1 P1 121.5(5) . . ?
C3 C2 C1 119.0(7) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C4 C3 C2 120.1(7) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.8(7) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 119.9(7) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C5 119.7(7) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C8 C7 C12 118.9(7) . . ?
C8 C7 P1 123.0(6) . . ?
C12 C7 P1 118.1(5) . . ?
C7 C8 C9 118.8(8) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 H8 120.6 . . ?
C10 C9 C8 121.1(8) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C11 C10 C9 119.7(8) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 121.3(8) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C11 C12 C7 120.2(7) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
C14 C13 C18 120.1(6) . . ?
C14 C13 P1 118.6(5) . . ?
C18 C13 P1 121.3(5) . . ?
C15 C14 C13 120.0(7) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C16 C15 C14 120.4(7) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 119.9(7) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C18 C17 C16 120.8(7) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C13 118.7(6) . . ?
C17 C18 C19 116.8(6) . . ?
C13 C18 C19 124.5(6) . . ?
N1 C19 C18 114.6(5) . . ?
N1 C19 H19A 108.6 . . ?
C18 C19 H19A 108.6 . . ?
N1 C19 H19B 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
N1 C20 C20 114.4(7) . 3_566 ?
N1 C20 H20A 108.7 . . ?
C20 C20 H20A 108.7 3_566 . ?
N1 C20 H20B 108.7 . . ?
C20 C20 H20B 108.7 3_566 . ?
H20A C20 H20B 107.6 . . ?
N1 C21 H21A 109.5 . . ?
N1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O3 S1 O2 114.2(4) . . ?
O3 S1 O1 114.7(4) . . ?
O2 S1 O1 115.8(4) . . ?
O3 S1 C22 102.7(4) . . ?
O2 S1 C22 104.3(4) . . ?
O1 S1 C22 102.9(4) . . ?
F1 C22 F2 106.3(8) . . ?
F1 C22 F3 106.7(8) . . ?
F2 C22 F3 108.4(8) . . ?
F1 C22 S1 112.0(7) . . ?
F2 C22 S1 111.8(6) . . ?
F3 C22 S1 111.5(6) . . ?
Cl3 C23 Cl2 117.0(13) . . ?
Cl3 C23 H23A 108.0 . . ?
Cl2 C23 H23A 108.0 . . ?
Cl3 C23 H23B 108.0 . . ?
Cl2 C23 H23B 108.0 . . ?
H23A C23 H23B 107.3 . . ?
Cl3' C23' Cl2' 127.6(18) . . ?
Cl3' C23' H23C 105.4 . . ?
Cl2' C23' H23C 105.4 . . ?
Cl3' C23' H23D 105.4 . . ?
Cl2' C23' H23D 105.4 . . ?
H23C C23' H23D 106.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 P1 C1 C6 -158.6(5) . . . . ?
C13 P1 C1 C6 86.5(6) . . . . ?
Ge1 P1 C1 C6 -35.2(6) . . . . ?
C7 P1 C1 C2 21.4(7) . . . . ?
C13 P1 C1 C2 -93.4(6) . . . . ?
Ge1 P1 C1 C2 144.9(5) . . . . ?
C6 C1 C2 C3 -1.1(10) . . . . ?
P1 C1 C2 C3 178.8(5) . . . . ?
C1 C2 C3 C4 0.0(11) . . . . ?
C2 C3 C4 C5 0.4(11) . . . . ?
C3 C4 C5 C6 0.3(11) . . . . ?
C2 C1 C6 C5 1.7(10) . . . . ?
P1 C1 C6 C5 -178.2(5) . . . . ?
C4 C5 C6 C1 -1.3(11) . . . . ?
C1 P1 C7 C8 -127.9(6) . . . . ?
C13 P1 C7 C8 -12.6(7) . . . . ?
Ge1 P1 C7 C8 110.5(6) . . . . ?
C1 P1 C7 C12 53.5(6) . . . . ?
C13 P1 C7 C12 168.7(6) . . . . ?
Ge1 P1 C7 C12 -68.1(6) . . . . ?
C12 C7 C8 C9 1.0(12) . . . . ?
P1 C7 C8 C9 -177.6(7) . . . . ?
C7 C8 C9 C10 -1.7(15) . . . . ?
C8 C9 C10 C11 2.0(15) . . . . ?
C9 C10 C11 C12 -1.7(14) . . . . ?
C10 C11 C12 C7 1.1(13) . . . . ?
C8 C7 C12 C11 -0.8(11) . . . . ?
P1 C7 C12 C11 177.9(6) . . . . ?
C7 P1 C13 C14 -87.0(7) . . . . ?
C1 P1 C13 C14 28.9(7) . . . . ?
Ge1 P1 C13 C14 149.2(6) . . . . ?
C7 P1 C13 C18 92.7(6) . . . . ?
C1 P1 C13 C18 -151.4(6) . . . . ?
Ge1 P1 C13 C18 -31.0(6) . . . . ?
C18 C13 C14 C15 -2.8(13) . . . . ?
P1 C13 C14 C15 176.9(7) . . . . ?
C13 C14 C15 C16 1.8(15) . . . . ?
C14 C15 C16 C17 0.2(15) . . . . ?
C15 C16 C17 C18 -1.3(13) . . . . ?
C16 C17 C18 C13 0.3(11) . . . . ?
C16 C17 C18 C19 -179.1(7) . . . . ?
C14 C13 C18 C17 1.7(11) . . . . ?
P1 C13 C18 C17 -178.0(6) . . . . ?
C14 C13 C18 C19 -179.0(7) . . . . ?
P1 C13 C18 C19 1.3(10) . . . . ?
C21 N1 C19 C18 165.2(5) . . . . ?
C20 N1 C19 C18 41.7(8) . . . . ?
Ge1 N1 C19 C18 -77.9(6) . . . . ?
C17 C18 C19 N1 -121.0(7) . . . . ?
C13 C18 C19 N1 59.6(9) . . . . ?
C21 N1 C20 C20 -60.8(9) . . . 3_566 ?
C19 N1 C20 C20 61.9(9) . . . 3_566 ?
Ge1 N1 C20 C20 -171.2(7) . . . 3_566 ?
O3 S1 C22 F1 -171.1(7) . . . . ?
O2 S1 C22 F1 69.5(7) . . . . ?
O1 S1 C22 F1 -51.7(8) . . . . ?
O3 S1 C22 F2 69.7(8) . . . . ?
O2 S1 C22 F2 -49.6(8) . . . . ?
O1 S1 C22 F2 -170.8(7) . . . . ?
O3 S1 C22 F3 -51.7(7) . . . . ?
O2 S1 C22 F3 -171.1(6) . . . . ?
O1 S1 C22 F3 67.7(7) . . . . ?

_refine_diff_density_max         1.714
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.130

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1889379'
loop_
_audit_author_name
_audit_author_address
'Moumita Majumdar'
;IISER Pune
India
;
_audit_update_record             
;
2019-02-20 deposited with the CCDC.	2019-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H38 Cl2 F6 Ge2 N2 O6 P2 S2'
_chemical_formula_weight         1122.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.9761(12)
_cell_length_b                   13.6739(14)
_cell_length_c                   13.7965(12)
_cell_angle_alpha                85.400(6)
_cell_angle_beta                 86.134(6)
_cell_angle_gamma                70.497(6)
_cell_volume                     2297.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2217
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      66.15

_exptl_crystal_description       needles
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_F_000             1132
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    4.832
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26902
_diffrn_reflns_av_unetI/netI     0.1965
_diffrn_reflns_av_R_equivalents  0.2587
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_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         3.216
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_full        66.597
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             8073
_reflns_number_gt                4100
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0718P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8073
_refine_ls_number_parameters     577
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1784
_refine_ls_R_factor_gt           0.0829
_refine_ls_wR_factor_ref         0.1965
_refine_ls_wR_factor_gt          0.1585
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.4791(6) 0.9295(6) 0.1188(5) 0.0242(19) Uani 1 1 d . . . . .
H1 H 0.5521 0.9255 0.1413 0.029 Uiso 1 1 calc R U . . .
Ge1 Ge 0.36815(9) 1.05352(9) 0.19527(8) 0.0254(3) Uani 1 1 d . . . . .
Ge2 Ge 0.18095(9) 0.30983(10) 0.14630(8) 0.0318(3) Uani 1 1 d . . . . .
S1 S 0.79576(18) 0.87475(19) 0.06630(17) 0.0243(6) Uani 1 1 d . . . . .
Cl1 Cl 0.48767(18) 1.0124(2) 0.31574(17) 0.0307(6) Uani 1 1 d . . . . .
Cl2 Cl 0.31650(19) 0.3283(2) 0.04275(17) 0.0325(6) Uani 1 1 d . . . . .
P2 P 0.24887(19) 0.37486(19) 0.28304(17) 0.0210(5) Uani 1 1 d . . . . .
P1 P 0.26205(18) 0.93698(19) 0.25705(17) 0.0216(6) Uani 1 1 d . . . . .
S2 S 0.85581(19) 0.4304(2) 0.26818(18) 0.0295(6) Uani 1 1 d . . . . .
F6 F 0.8366(5) 0.6215(4) 0.2042(4) 0.0408(15) Uani 1 1 d . . . . .
F2 F 0.8771(5) 0.9259(4) 0.2149(4) 0.0434(16) Uani 1 1 d . . . . .
F3 F 0.9141(4) 0.9957(5) 0.0776(4) 0.0435(16) Uani 1 1 d . . . . .
F1 F 0.7512(5) 1.0536(4) 0.1448(4) 0.0432(16) Uani 1 1 d . . . . .
O1 O 0.7558(5) 0.9317(5) -0.0238(4) 0.0261(15) Uani 1 1 d . . . . .
F5 F 0.8082(5) 0.6011(5) 0.3582(4) 0.0540(18) Uani 1 1 d . . . . .
F4 F 0.6866(5) 0.6017(5) 0.2600(5) 0.0548(19) Uani 1 1 d . . . . .
O2 O 0.7114(5) 0.8560(5) 0.1328(4) 0.0288(16) Uani 1 1 d . . . . .
O3 O 0.8960(5) 0.7875(5) 0.0569(5) 0.0301(16) Uani 1 1 d . . . . .
O4 O 0.8390(5) 0.4140(5) 0.1696(5) 0.0340(17) Uani 1 1 d . . . . .
O6 O 0.9692(5) 0.4151(5) 0.2862(5) 0.0390(19) Uani 1 1 d . . . . .
O5 O 0.7963(5) 0.3898(6) 0.3421(5) 0.043(2) Uani 1 1 d . . . . .
N2 N 0.0833(6) 0.4617(6) 0.1130(5) 0.0252(19) Uani 1 1 d . . . . .
H2 H 0.0136 0.4725 0.1530 0.030 Uiso 1 1 calc R U . . .
C3 C 0.3719(7) 0.8071(7) 0.1132(6) 0.024(2) Uani 1 1 d . . . . .
C29 C 0.3813(7) 0.3876(7) 0.2582(6) 0.020(2) Uani 1 1 d . . . . .
C8 C 0.2679(7) 0.8562(7) 0.1589(6) 0.020(2) Uani 1 1 d . . . . .
C30 C 0.3963(7) 0.4823(8) 0.2450(7) 0.028(2) Uani 1 1 d . . . . .
H30 H 0.3352 0.5433 0.2540 0.034 Uiso 1 1 calc R U . . .
C2 C 0.4739(7) 0.8210(7) 0.1458(7) 0.029(2) Uani 1 1 d . . . . .
H2A H 0.5385 0.7692 0.1157 0.035 Uiso 1 1 calc R U . . .
H2B H 0.4772 0.8077 0.2173 0.035 Uiso 1 1 calc R U . . .
C7 C 0.1760(8) 0.8436(8) 0.1261(6) 0.027(2) Uani 1 1 d . . . . .
H7 H 0.1066 0.8785 0.1560 0.033 Uiso 1 1 calc R U . . .
C27 C 0.1365(7) 0.5287(8) 0.4100(7) 0.029(2) Uani 1 1 d . . . . .
H27 H 0.1686 0.4790 0.4609 0.035 Uiso 1 1 calc R U . . .
C28 C 0.1575(6) 0.5015(7) 0.3142(7) 0.024(2) Uani 1 1 d . . . . .
C15 C 0.1196(7) 1.0116(8) 0.2791(6) 0.024(2) Uani 1 1 d . . . . .
C40 C 0.1829(8) 0.2310(8) 0.4008(7) 0.029(2) Uani 1 1 d . . . . .
H40 H 0.1281 0.2426 0.3548 0.035 Uiso 1 1 calc R U . . .
C11 C 0.3628(7) 0.8181(8) 0.5271(6) 0.023(2) Uani 1 1 d . . . . .
H11 H 0.3837 0.8419 0.5831 0.028 Uiso 1 1 calc R U . . .
C39 C 0.1882(8) 0.1619(7) 0.4785(7) 0.030(2) Uani 1 1 d . . . . .
H39 H 0.1377 0.1248 0.4860 0.036 Uiso 1 1 calc R U . . .
C18 C -0.0959(8) 1.1347(8) 0.3103(7) 0.027(2) Uani 1 1 d . . . . .
H18 H -0.1700 1.1769 0.3211 0.033 Uiso 1 1 calc R U . . .
C9 C 0.3041(7) 0.8495(7) 0.3621(6) 0.023(2) Uani 1 1 d . . . . .
C4 C 0.3776(8) 0.7413(7) 0.0387(6) 0.025(2) Uani 1 1 d . . . . .
H4 H 0.4464 0.7058 0.0082 0.030 Uiso 1 1 calc R U . . .
C35 C 0.2573(7) 0.2845(7) 0.3886(7) 0.024(2) Uani 1 1 d . . . . .
C41 C 0.8375(8) 0.9668(8) 0.1300(7) 0.029(2) Uani 1 1 d . . . . .
C37 C 0.3415(8) 0.1977(8) 0.5355(7) 0.037(3) Uani 1 1 d . . . . .
H37 H 0.3966 0.1856 0.5813 0.044 Uiso 1 1 calc R U . . .
C36 C 0.3358(7) 0.2673(7) 0.4576(7) 0.028(2) Uani 1 1 d . . . . .
H36 H 0.3863 0.3045 0.4504 0.033 Uiso 1 1 calc R U . . .
C23 C 0.1089(7) 0.5747(8) 0.2376(7) 0.027(2) Uani 1 1 d . . . . .
C16 C 0.0713(7) 1.0952(7) 0.2130(7) 0.027(2) Uani 1 1 d . . . . .
H16 H 0.1120 1.1094 0.1571 0.033 Uiso 1 1 calc R U . . .
C14 C 0.3028(8) 0.7488(8) 0.3654(7) 0.032(3) Uani 1 1 d . . . . .
H14 H 0.2820 0.7243 0.3098 0.038 Uiso 1 1 calc R U . . .
C33 C 0.5742(8) 0.3081(9) 0.2186(7) 0.033(3) Uani 1 1 d . . . . .
H33 H 0.6362 0.2477 0.2099 0.040 Uiso 1 1 calc R U . . .
C38 C 0.2673(9) 0.1453(8) 0.5475(7) 0.036(3) Uani 1 1 d . . . . .
H38 H 0.2698 0.0980 0.6023 0.044 Uiso 1 1 calc R U . . .
C5 C 0.2832(9) 0.7275(8) 0.0091(7) 0.035(3) Uani 1 1 d . . . . .
H5 H 0.2884 0.6809 -0.0399 0.042 Uiso 1 1 calc R U . . .
C10 C 0.3349(7) 0.8847(8) 0.4444(6) 0.025(2) Uani 1 1 d . . . . .
H10 H 0.3366 0.9536 0.4437 0.030 Uiso 1 1 calc R U . . .
C34 C 0.4728(7) 0.2977(8) 0.2432(6) 0.028(2) Uani 1 1 d . . . . .
H34 H 0.4650 0.2308 0.2499 0.034 Uiso 1 1 calc R U . . .
C26 C 0.0701(8) 0.6265(9) 0.4326(8) 0.038(3) Uani 1 1 d . . . . .
H26 H 0.0565 0.6451 0.4983 0.045 Uiso 1 1 calc R U . . .
C12 C 0.3604(8) 0.7187(8) 0.5287(7) 0.034(3) Uani 1 1 d . . . . .
H12 H 0.3793 0.6745 0.5861 0.040 Uiso 1 1 calc R U . . .
C17 C -0.0369(8) 1.1571(8) 0.2299(7) 0.030(2) Uani 1 1 d . . . . .
H17 H -0.0700 1.2147 0.1861 0.036 Uiso 1 1 calc R U . . .
C25 C 0.0235(8) 0.6975(8) 0.3569(7) 0.033(3) Uani 1 1 d . . . . .
H25 H -0.0221 0.7656 0.3712 0.040 Uiso 1 1 calc R U . . .
C20 C 0.0589(7) 0.9889(8) 0.3577(7) 0.027(2) Uani 1 1 d . . . . .
H20 H 0.0903 0.9300 0.4007 0.032 Uiso 1 1 calc R U . . .
C22 C 0.1229(7) 0.5485(8) 0.1327(7) 0.031(2) Uani 1 1 d . . . . .
H22A H 0.0828 0.6111 0.0923 0.037 Uiso 1 1 calc R U . . .
H22B H 0.2014 0.5294 0.1125 0.037 Uiso 1 1 calc R U . . .
C19 C -0.0500(7) 1.0533(9) 0.3744(7) 0.035(3) Uani 1 1 d . . . . .
H19 H -0.0913 1.0398 0.4303 0.042 Uiso 1 1 calc R U . . .
C6 C 0.1823(8) 0.7809(8) 0.0503(6) 0.031(2) Uani 1 1 d . . . . .
H6 H 0.1176 0.7748 0.0270 0.037 Uiso 1 1 calc R U . . .
C1 C 0.4896(7) 0.9489(7) 0.0106(7) 0.025(2) Uani 1 1 d . . . . .
H1A H 0.4216 0.9516 -0.0196 0.030 Uiso 1 1 calc R U . . .
H1B H 0.5510 0.8918 -0.0170 0.030 Uiso 1 1 calc R U . . .
C32 C 0.5863(8) 0.4042(9) 0.2065(7) 0.034(3) Uani 1 1 d . . . . .
H32 H 0.6562 0.4102 0.1896 0.041 Uiso 1 1 calc R U . . .
C42 C 0.7920(8) 0.5703(9) 0.2727(7) 0.036(3) Uani 1 1 d . . . . .
C21 C 0.0548(7) 0.4644(9) 0.0102(7) 0.037(3) Uani 1 1 d . . . . .
H21A H 0.1090 0.4855 -0.0328 0.044 Uiso 1 1 calc R U . . .
H21B H 0.0598 0.3935 -0.0055 0.044 Uiso 1 1 calc R U . . .
C13 C 0.3315(9) 0.6817(9) 0.4492(8) 0.045(3) Uani 1 1 d . . . . .
H13 H 0.3308 0.6124 0.4506 0.055 Uiso 1 1 calc R U . . .
C24 C 0.0420(8) 0.6713(8) 0.2627(8) 0.036(3) Uani 1 1 d . . . . .
H24 H 0.0076 0.7213 0.2128 0.043 Uiso 1 1 calc R U . . .
C31 C 0.4968(8) 0.4922(9) 0.2191(8) 0.040(3) Uani 1 1 d . . . . .
H31 H 0.5044 0.5591 0.2100 0.048 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.499(11) . ?
N1 C2 1.523(11) . ?
N1 Ge1 2.125(7) . ?
N1 H1 1.0000 . ?
Ge1 Cl1 2.258(3) . ?
Ge1 P1 2.500(3) . ?
Ge2 N2 2.073(8) . ?
Ge2 Cl2 2.258(3) . ?
Ge2 P2 2.479(3) . ?
S1 O1 1.443(6) . ?
S1 O3 1.448(6) . ?
S1 O2 1.456(6) . ?
S1 C41 1.830(9) . ?
P2 C29 1.792(8) . ?
P2 C28 1.808(9) . ?
P2 C35 1.818(10) . ?
P1 C9 1.795(10) . ?
P1 C8 1.797(9) . ?
P1 C15 1.807(9) . ?
S2 O5 1.427(6) . ?
S2 O4 1.439(7) . ?
S2 O6 1.452(6) . ?
S2 C42 1.817(11) . ?
F6 C42 1.344(11) . ?
F2 C41 1.317(11) . ?
F3 C41 1.337(11) . ?
F1 C41 1.351(10) . ?
F5 C42 1.337(11) . ?
F4 C42 1.310(11) . ?
N2 C21 1.485(11) . ?
N2 C22 1.490(12) . ?
N2 H2 1.0000 . ?
C3 C4 1.402(12) . ?
C3 C8 1.421(11) . ?
C3 C2 1.501(12) . ?
C29 C30 1.369(12) . ?
C29 C34 1.414(12) . ?
C8 C7 1.370(12) . ?
C30 C31 1.376(12) . ?
C30 H30 0.9500 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C7 C6 1.386(12) . ?
C7 H7 0.9500 . ?
C27 C26 1.374(13) . ?
C27 C28 1.388(12) . ?
C27 H27 0.9500 . ?
C28 C23 1.420(13) . ?
C15 C20 1.374(12) . ?
C15 C16 1.401(13) . ?
C40 C39 1.360(13) . ?
C40 C35 1.388(12) . ?
C40 H40 0.9500 . ?
C11 C12 1.369(13) . ?
C11 C10 1.390(12) . ?
C11 H11 0.9500 . ?
C39 C38 1.397(13) . ?
C39 H39 0.9500 . ?
C18 C19 1.359(13) . ?
C18 C17 1.377(12) . ?
C18 H18 0.9500 . ?
C9 C14 1.380(13) . ?
C9 C10 1.399(12) . ?
C4 C5 1.391(12) . ?
C4 H4 0.9500 . ?
C35 C36 1.390(12) . ?
C37 C36 1.366(13) . ?
C37 C38 1.374(14) . ?
C37 H37 0.9500 . ?
C36 H36 0.9500 . ?
C23 C24 1.373(13) . ?
C23 C22 1.503(12) . ?
C16 C17 1.391(12) . ?
C16 H16 0.9500 . ?
C14 C13 1.406(13) . ?
C14 H14 0.9500 . ?
C33 C32 1.370(14) . ?
C33 C34 1.387(12) . ?
C33 H33 0.9500 . ?
C38 H38 0.9500 . ?
C5 C6 1.378(13) . ?
C5 H5 0.9500 . ?
C10 H10 0.9500 . ?
C34 H34 0.9500 . ?
C26 C25 1.389(14) . ?
C26 H26 0.9500 . ?
C12 C13 1.368(14) . ?
C12 H12 0.9500 . ?
C17 H17 0.9500 . ?
C25 C24 1.361(13) . ?
C25 H25 0.9500 . ?
C20 C19 1.408(12) . ?
C20 H20 0.9500 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C19 H19 0.9500 . ?
C6 H6 0.9500 . ?
C1 C1 1.511(17) 2_675 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C32 C31 1.379(14) . ?
C32 H32 0.9500 . ?
C21 C21 1.462(18) 2_565 ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C13 H13 0.9500 . ?
C24 H24 0.9500 . ?
C31 H31 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C2 111.5(7) . . ?
C1 N1 Ge1 116.0(5) . . ?
C2 N1 Ge1 117.0(5) . . ?
C1 N1 H1 103.4 . . ?
C2 N1 H1 103.4 . . ?
Ge1 N1 H1 103.4 . . ?
N1 Ge1 Cl1 88.1(2) . . ?
N1 Ge1 P1 89.6(2) . . ?
Cl1 Ge1 P1 97.18(9) . . ?
N2 Ge2 Cl2 91.4(2) . . ?
N2 Ge2 P2 87.8(2) . . ?
Cl2 Ge2 P2 92.54(9) . . ?
O1 S1 O3 115.3(4) . . ?
O1 S1 O2 114.5(4) . . ?
O3 S1 O2 115.5(4) . . ?
O1 S1 C41 103.5(4) . . ?
O3 S1 C41 103.2(4) . . ?
O2 S1 C41 102.4(4) . . ?
C29 P2 C28 106.6(4) . . ?
C29 P2 C35 108.0(4) . . ?
C28 P2 C35 108.5(4) . . ?
C29 P2 Ge2 113.7(3) . . ?
C28 P2 Ge2 111.3(3) . . ?
C35 P2 Ge2 108.5(3) . . ?
C9 P1 C8 105.7(4) . . ?
C9 P1 C15 106.9(4) . . ?
C8 P1 C15 106.8(4) . . ?
C9 P1 Ge1 120.5(3) . . ?
C8 P1 Ge1 105.5(3) . . ?
C15 P1 Ge1 110.6(3) . . ?
O5 S2 O4 115.9(4) . . ?
O5 S2 O6 116.5(5) . . ?
O4 S2 O6 113.3(4) . . ?
O5 S2 C42 103.6(5) . . ?
O4 S2 C42 102.0(4) . . ?
O6 S2 C42 102.6(4) . . ?
C21 N2 C22 112.9(7) . . ?
C21 N2 Ge2 105.4(6) . . ?
C22 N2 Ge2 119.2(6) . . ?
C21 N2 H2 106.2 . . ?
C22 N2 H2 106.2 . . ?
Ge2 N2 H2 106.2 . . ?
C4 C3 C8 118.0(8) . . ?
C4 C3 C2 120.4(8) . . ?
C8 C3 C2 121.5(8) . . ?
C30 C29 C34 118.1(8) . . ?
C30 C29 P2 122.4(7) . . ?
C34 C29 P2 119.3(7) . . ?
C7 C8 C3 120.1(8) . . ?
C7 C8 P1 122.2(7) . . ?
C3 C8 P1 117.7(7) . . ?
C29 C30 C31 122.4(9) . . ?
C29 C30 H30 118.8 . . ?
C31 C30 H30 118.8 . . ?
C3 C2 N1 112.7(8) . . ?
C3 C2 H2A 109.1 . . ?
N1 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
N1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C8 C7 C6 121.3(9) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C26 C27 C28 121.1(10) . . ?
C26 C27 H27 119.5 . . ?
C28 C27 H27 119.5 . . ?
C27 C28 C23 120.0(9) . . ?
C27 C28 P2 121.6(8) . . ?
C23 C28 P2 118.4(7) . . ?
C20 C15 C16 120.0(9) . . ?
C20 C15 P1 122.2(8) . . ?
C16 C15 P1 117.9(7) . . ?
C39 C40 C35 120.2(9) . . ?
C39 C40 H40 119.9 . . ?
C35 C40 H40 119.9 . . ?
C12 C11 C10 120.6(9) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C40 C39 C38 120.5(9) . . ?
C40 C39 H39 119.8 . . ?
C38 C39 H39 119.8 . . ?
C19 C18 C17 121.1(9) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C14 C9 C10 118.7(9) . . ?
C14 C9 P1 121.5(7) . . ?
C10 C9 P1 119.7(8) . . ?
C5 C4 C3 120.5(8) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C40 C35 C36 118.9(9) . . ?
C40 C35 P2 118.9(8) . . ?
C36 C35 P2 122.2(7) . . ?
F2 C41 F3 108.3(8) . . ?
F2 C41 F1 108.6(7) . . ?
F3 C41 F1 107.4(8) . . ?
F2 C41 S1 111.2(7) . . ?
F3 C41 S1 111.0(6) . . ?
F1 C41 S1 110.2(6) . . ?
C36 C37 C38 119.8(10) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
C37 C36 C35 121.0(9) . . ?
C37 C36 H36 119.5 . . ?
C35 C36 H36 119.5 . . ?
C24 C23 C28 117.4(9) . . ?
C24 C23 C22 119.7(9) . . ?
C28 C23 C22 122.7(9) . . ?
C17 C16 C15 119.4(9) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C9 C14 C13 121.4(9) . . ?
C9 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C32 C33 C34 121.0(10) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C37 C38 C39 119.6(10) . . ?
C37 C38 H38 120.2 . . ?
C39 C38 H38 120.2 . . ?
C6 C5 C4 120.6(9) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C11 C10 C9 119.6(9) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C33 C34 C29 119.3(10) . . ?
C33 C34 H34 120.4 . . ?
C29 C34 H34 120.4 . . ?
C27 C26 C25 118.3(9) . . ?
C27 C26 H26 120.8 . . ?
C25 C26 H26 120.8 . . ?
C13 C12 C11 121.3(10) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C18 C17 C16 119.9(10) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C24 C25 C26 121.2(10) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C15 C20 C19 119.7(10) . . ?
C15 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
N2 C22 C23 113.9(8) . . ?
N2 C22 H22A 108.8 . . ?
C23 C22 H22A 108.8 . . ?
N2 C22 H22B 108.8 . . ?
C23 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C18 C19 C20 119.8(9) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C5 C6 C7 119.4(9) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
N1 C1 C1 108.8(9) . 2_675 ?
N1 C1 H1A 109.9 . . ?
C1 C1 H1A 109.9 2_675 . ?
N1 C1 H1B 109.9 . . ?
C1 C1 H1B 109.9 2_675 . ?
H1A C1 H1B 108.3 . . ?
C33 C32 C31 119.9(9) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
F4 C42 F5 108.4(8) . . ?
F4 C42 F6 107.3(9) . . ?
F5 C42 F6 106.2(8) . . ?
F4 C42 S2 113.0(7) . . ?
F5 C42 S2 110.3(8) . . ?
F6 C42 S2 111.4(7) . . ?
C21 C21 N2 113.2(11) 2_565 . ?
C21 C21 H21A 108.9 2_565 . ?
N2 C21 H21A 108.9 . . ?
C21 C21 H21B 108.9 2_565 . ?
N2 C21 H21B 108.9 . . ?
H21A C21 H21B 107.8 . . ?
C12 C13 C14 118.4(10) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C25 C24 C23 121.9(10) . . ?
C25 C24 H24 119.0 . . ?
C23 C24 H24 119.0 . . ?
C30 C31 C32 119.4(10) . . ?
C30 C31 H31 120.3 . . ?
C32 C31 H31 120.3 . . ?

_refine_diff_density_max         1.074
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.136

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1889434'
loop_
_audit_author_name
_audit_author_address
'Moumita Majumdar'
;IISER Pune
India
;
_audit_update_record             
;
2019-01-08 deposited with the CCDC.	2019-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H38 Cl9 F3 Ga2 N2 O3 P2 S'
_chemical_formula_weight         1228.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.8764(4)
_cell_length_b                   37.6034(12)
_cell_length_c                   12.6639(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.849(2)
_cell_angle_gamma                90
_cell_volume                     5006.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8678
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      66.48

_exptl_crystal_description       colourless
_exptl_crystal_colour            block
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_F_000             2464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    7.177
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.045
_exptl_absorpt_correction_T_max  0.101
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48512
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_av_R_equivalents  0.1643
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.350
_diffrn_reflns_theta_max         66.859
_diffrn_reflns_theta_full        66.859
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             8803
_reflns_number_gt                5713
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1089P)²+14.2295P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00041(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8803
_refine_ls_number_parameters     578
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0746
_refine_ls_wR_factor_ref         0.2193
_refine_ls_wR_factor_gt          0.1899
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ga2 Ga 0.21177(10) 0.50867(3) 0.71032(8) 0.0365(3) Uani 1 1 d . . . . .
Ga1 Ga 0.59239(10) 0.81921(3) 0.49286(8) 0.0361(3) Uani 1 1 d . . . . .
Cl7 Cl 0.2921(2) 0.52150(5) 0.57405(15) 0.0398(5) Uani 1 1 d . . . . .
S1 S 0.90651(19) 0.72898(5) 0.63413(16) 0.0347(4) Uani 1 1 d . . . . .
P2 P 0.47677(19) 0.65048(5) 0.66539(15) 0.0308(4) Uani 1 1 d . . . . .
Cl1 Cl 0.6456(2) 0.81606(6) 0.67057(16) 0.0440(5) Uani 1 1 d . . . . .
P1 P 0.50968(19) 0.61926(5) 0.35165(15) 0.0314(4) Uani 1 1 d . . . . .
Cl5 Cl 0.3412(2) 0.47035(6) 0.81220(17) 0.0466(5) Uani 1 1 d . . . . .
Cl2 Cl 0.3950(2) 0.83292(6) 0.42775(17) 0.0452(5) Uani 1 1 d . . . . .
Cl3 Cl 0.7264(2) 0.84999(6) 0.43124(18) 0.0470(5) Uani 1 1 d . . . . .
Cl4 Cl 0.1944(2) 0.55600(6) 0.80314(17) 0.0488(5) Uani 1 1 d . . . . .
Cl6 Cl 0.0261(2) 0.48410(7) 0.65172(19) 0.0500(6) Uani 1 1 d . . . . .
Cl8 Cl 0.9658(3) 0.54794(8) -0.0520(2) 0.0627(7) Uani 1 1 d . . . . .
Cl9 Cl 0.9887(3) 0.59375(7) 0.1358(2) 0.0710(8) Uani 1 1 d . . . . .
F1 F 1.0639(4) 0.69733(14) 0.5384(4) 0.0430(11) Uani 1 1 d . . . . .
F3 F 1.0163(5) 0.66680(14) 0.6674(4) 0.0467(12) Uani 1 1 d . . . . .
F2 F 0.8803(5) 0.67230(13) 0.5078(4) 0.0459(12) Uani 1 1 d . . . . .
O2 O 0.8043(5) 0.71586(16) 0.6755(5) 0.0398(13) Uani 1 1 d . . . . .
O1 O 0.8681(5) 0.75068(15) 0.5383(4) 0.0384(13) Uani 1 1 d . . . . .
O3 O 1.0144(5) 0.74281(15) 0.7162(4) 0.0384(13) Uani 1 1 d . . . . .
N2 N 0.5068(6) 0.67591(16) 0.4825(5) 0.0290(13) Uani 1 1 d . . . . .
N1 N 0.6115(6) 0.76992(18) 0.4450(5) 0.0351(15) Uani 1 1 d . . . . .
H00A H 0.5860 0.7694 0.3724 0.042 Uiso 1 1 calc R U . . .
H00B H 0.6940 0.7646 0.4637 0.042 Uiso 1 1 calc R U . . .
C1 C 0.5429(7) 0.7412(2) 0.4874(6) 0.0315(16) Uani 1 1 d . . . . .
H00C H 0.4527 0.7465 0.4696 0.038 Uiso 1 1 calc R U . . .
H00D H 0.5738 0.7398 0.5663 0.038 Uiso 1 1 calc R U . . .
C4 C 0.6616(7) 0.6250(2) 0.5643(6) 0.0288(15) Uani 1 1 d . . . . .
C35 C 0.4182(7) 0.5831(2) 0.2831(6) 0.0320(17) Uani 1 1 d . . . . .
C15 C 0.1161(8) 0.6065(2) 0.4330(7) 0.0367(18) Uani 1 1 d . . . . .
H00Q H 0.0441 0.5965 0.3866 0.044 Uiso 1 1 calc R U . . .
C8 C 0.8273(7) 0.5841(2) 0.6423(6) 0.0355(18) Uani 1 1 d . . . . .
H00R H 0.8952 0.5775 0.7001 0.043 Uiso 1 1 calc R U . . .
C5 C 0.6271(8) 0.6045(2) 0.4688(6) 0.0332(17) Uani 1 1 d . . . . .
C41 C 0.9705(7) 0.6897(2) 0.5856(6) 0.0339(17) Uani 1 1 d . . . . .
C25 C 0.5488(7) 0.5535(2) 0.8035(7) 0.0363(18) Uani 1 1 d . . . . .
H00U H 0.5434 0.5300 0.7797 0.044 Uiso 1 1 calc R U . . .
C12 C 0.3352(7) 0.6353(2) 0.5706(6) 0.0321(16) Uani 1 1 d . . . . .
C23 C 0.5247(7) 0.6165(2) 0.7649(6) 0.0299(16) Uani 1 1 d . . . . .
C6 C 0.6943(8) 0.5732(2) 0.4635(6) 0.0356(18) Uani 1 1 d . . . . .
H00X H 0.6715 0.5591 0.4011 0.043 Uiso 1 1 calc R U . . .
C16 C 0.2088(7) 0.6223(2) 0.3895(6) 0.0336(17) Uani 1 1 d . . . . .
H00Y H 0.1971 0.6233 0.3142 0.040 Uiso 1 1 calc R U . . .
C11 C 0.3189(7) 0.6366(2) 0.4587(6) 0.0318(17) Uani 1 1 d . . . . .
C36 C 0.3824(8) 0.5561(2) 0.3453(7) 0.0379(18) Uani 1 1 d . . . . .
H010 H 0.4087 0.5570 0.4211 0.045 Uiso 1 1 calc R U . . .
C24 C 0.5200(7) 0.5810(2) 0.7298(6) 0.0345(17) Uani 1 1 d . . . . .
H011 H 0.4968 0.5760 0.6554 0.041 Uiso 1 1 calc R U . . .
C10 C 0.4177(7) 0.6531(2) 0.4074(6) 0.0311(16) Uani 1 1 d . . . . .
H012 H 0.3721 0.6679 0.3462 0.037 Uiso 1 1 calc R U . . .
C9 C 0.7610(7) 0.6147(2) 0.6498(6) 0.0322(17) Uani 1 1 d . . . . .
H013 H 0.7833 0.6284 0.7129 0.039 Uiso 1 1 calc R U . . .
C2 C 0.5644(7) 0.70583(19) 0.4366(6) 0.0301(16) Uani 1 1 d . . . . .
H01A H 0.5279 0.7069 0.3583 0.036 Uiso 1 1 calc R U . . .
H01B H 0.6551 0.7017 0.4492 0.036 Uiso 1 1 calc R U . . .
C22 C 0.5689(8) 0.7099(2) 0.7871(6) 0.0362(18) Uani 1 1 d . . . . .
H015 H 0.6484 0.6992 0.7992 0.043 Uiso 1 1 calc R U . . .
C21 C 0.5573(8) 0.7437(2) 0.8283(7) 0.0395(19) Uani 1 1 d . . . . .
H016 H 0.6292 0.7556 0.8684 0.047 Uiso 1 1 calc R U . . .
C7 C 0.7948(8) 0.5628(2) 0.5499(7) 0.0391(19) Uani 1 1 d . . . . .
H017 H 0.8392 0.5419 0.5458 0.047 Uiso 1 1 calc R U . . .
C34 C 0.7155(8) 0.6394(2) 0.2729(7) 0.0372(18) Uani 1 1 d . . . . .
H018 H 0.7653 0.6255 0.3285 0.045 Uiso 1 1 calc R U . . .
C13 C 0.2401(7) 0.6197(2) 0.6153(6) 0.0308(16) Uani 1 1 d . . . . .
H019 H 0.2509 0.6190 0.6905 0.037 Uiso 1 1 calc R U . . .
C40 C 0.3793(7) 0.5816(2) 0.1691(6) 0.0358(18) Uani 1 1 d . . . . .
H01C H 0.4038 0.5993 0.1276 0.043 Uiso 1 1 calc R U . . .
C39 C 0.3054(8) 0.5540(2) 0.1185(7) 0.043(2) Uani 1 1 d . . . . .
H01D H 0.2803 0.5531 0.0426 0.052 Uiso 1 1 calc R U . . .
C30 C 0.5108(8) 0.6635(2) 0.1774(6) 0.0375(18) Uani 1 1 d . . . . .
H01E H 0.4237 0.6656 0.1697 0.045 Uiso 1 1 calc R U . . .
C18 C 0.3411(8) 0.7087(2) 0.7092(6) 0.0374(18) Uani 1 1 d . . . . .
H01F H 0.2685 0.6971 0.6696 0.045 Uiso 1 1 calc R U . . .
C32 C 0.6978(10) 0.6784(2) 0.1191(7) 0.045(2) Uani 1 1 d . . . . .
H01G H 0.7365 0.6908 0.0728 0.054 Uiso 1 1 calc R U . . .
C14 C 0.1313(8) 0.6057(2) 0.5452(7) 0.0384(18) Uani 1 1 d . . . . .
H01H H 0.0682 0.5958 0.5735 0.046 Uiso 1 1 calc R U . . .
C17 C 0.4600(8) 0.6921(2) 0.7271(6) 0.0347(17) Uani 1 1 d . . . . .
C29 C 0.5844(8) 0.6421(2) 0.2620(6) 0.0334(17) Uani 1 1 d . . . . .
C19 C 0.3312(9) 0.7422(2) 0.7500(7) 0.041(2) Uani 1 1 d . . . . .
H01I H 0.2523 0.7533 0.7375 0.050 Uiso 1 1 calc R U . . .
C37 C 0.3071(8) 0.5279(2) 0.2932(7) 0.043(2) Uani 1 1 d . . . . .
H01J H 0.2836 0.5098 0.3340 0.052 Uiso 1 1 calc R U . . .
C31 C 0.5664(8) 0.6813(2) 0.1057(7) 0.0399(19) Uani 1 1 d . . . . .
H01K H 0.5170 0.6950 0.0495 0.048 Uiso 1 1 calc R U . . .
C3 C 0.5863(7) 0.6584(2) 0.5791(6) 0.0322(17) Uani 1 1 d . . . . .
H01L H 0.6485 0.6760 0.6169 0.039 Uiso 1 1 calc R U . . .
C33 C 0.7709(9) 0.6570(2) 0.2018(7) 0.045(2) Uani 1 1 d . . . . .
H01M H 0.8577 0.6547 0.2089 0.054 Uiso 1 1 calc R U . . .
C20 C 0.4400(9) 0.7596(2) 0.8100(7) 0.045(2) Uani 1 1 d . . . . .
H01N H 0.4331 0.7822 0.8379 0.054 Uiso 1 1 calc R U . . .
C26 C 0.5866(9) 0.5616(3) 0.9152(8) 0.048(2) Uani 1 1 d . . . . .
H01O H 0.6077 0.5433 0.9663 0.058 Uiso 1 1 calc R U . . .
C28 C 0.5649(8) 0.6237(2) 0.8775(7) 0.041(2) Uani 1 1 d . . . . .
H01P H 0.5724 0.6471 0.9025 0.049 Uiso 1 1 calc R U . . .
C38 C 0.2672(8) 0.5273(2) 0.1785(7) 0.044(2) Uani 1 1 d . . . . .
H01Q H 0.2153 0.5090 0.1430 0.052 Uiso 1 1 calc R U . . .
C27 C 0.5924(9) 0.5964(3) 0.9492(7) 0.047(2) Uani 1 1 d . . . . .
H01R H 0.6159 0.6012 1.0237 0.056 Uiso 1 1 calc R U . . .
C42 C 0.9355(9) 0.5525(3) 0.0778(7) 0.054(2) Uani 1 1 d . . . . .
H01S H 0.8449 0.5503 0.0708 0.065 Uiso 1 1 calc R U . . .
H01T H 0.9784 0.5336 0.1255 0.065 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ga2 Cl4 2.168(2) . ?
Ga2 Cl6 2.172(2) . ?
Ga2 Cl7 2.179(2) . ?
Ga2 Cl5 2.189(2) . ?
Ga1 N1 1.977(7) . ?
Ga1 Cl2 2.156(2) . ?
Ga1 Cl3 2.158(2) . ?
Ga1 Cl1 2.179(2) . ?
S1 O2 1.433(6) . ?
S1 O1 1.433(6) . ?
S1 O3 1.450(5) . ?
S1 C41 1.808(8) . ?
P2 C23 1.776(8) . ?
P2 C17 1.780(8) . ?
P2 C12 1.785(8) . ?
P2 C3 1.836(8) . ?
P1 C35 1.775(8) . ?
P1 C29 1.778(8) . ?
P1 C5 1.780(8) . ?
P1 C10 1.866(8) . ?
Cl8 C42 1.766(10) . ?
Cl9 C42 1.750(11) . ?
F1 C41 1.335(9) . ?
F3 C41 1.341(9) . ?
F2 C41 1.365(9) . ?
N2 C10 1.451(9) . ?
N2 C3 1.461(9) . ?
N2 C2 1.477(9) . ?
N1 C1 1.488(10) . ?
N1 H00A 0.8900 . ?
N1 H00B 0.8900 . ?
C1 C2 1.522(10) . ?
C1 H00C 0.9700 . ?
C1 H00D 0.9700 . ?
C4 C9 1.375(10) . ?
C4 C5 1.402(10) . ?
C4 C3 1.537(11) . ?
C35 C40 1.397(10) . ?
C35 C36 1.398(11) . ?
C15 C14 1.388(11) . ?
C15 C16 1.398(11) . ?
C15 H00Q 0.9300 . ?
C8 C9 1.375(11) . ?
C8 C7 1.386(11) . ?
C8 H00R 0.9300 . ?
C5 C6 1.395(11) . ?
C25 C24 1.374(11) . ?
C25 C26 1.401(12) . ?
C25 H00U 0.9300 . ?
C12 C11 1.383(11) . ?
C12 C13 1.426(10) . ?
C23 C24 1.405(11) . ?
C23 C28 1.407(11) . ?
C6 C7 1.390(11) . ?
C6 H00X 0.9300 . ?
C16 C11 1.398(11) . ?
C16 H00Y 0.9300 . ?
C11 C10 1.523(11) . ?
C36 C37 1.398(12) . ?
C36 H010 0.9300 . ?
C24 H011 0.9300 . ?
C10 H012 0.9800 . ?
C9 H013 0.9300 . ?
C2 H01A 0.9700 . ?
C2 H01B 0.9700 . ?
C22 C21 1.392(12) . ?
C22 C17 1.402(11) . ?
C22 H015 0.9300 . ?
C21 C20 1.373(13) . ?
C21 H016 0.9300 . ?
C7 H017 0.9300 . ?
C34 C33 1.377(12) . ?
C34 C29 1.401(11) . ?
C34 H018 0.9300 . ?
C13 C14 1.389(11) . ?
C13 H019 0.9300 . ?
C40 C39 1.367(12) . ?
C40 H01C 0.9300 . ?
C39 C38 1.385(13) . ?
C39 H01D 0.9300 . ?
C30 C31 1.386(12) . ?
C30 C29 1.411(11) . ?
C30 H01E 0.9300 . ?
C18 C19 1.376(11) . ?
C18 C17 1.401(11) . ?
C18 H01F 0.9300 . ?
C32 C33 1.396(13) . ?
C32 C31 1.400(13) . ?
C32 H01G 0.9300 . ?
C14 H01H 0.9300 . ?
C19 C20 1.394(12) . ?
C19 H01I 0.9300 . ?
C37 C38 1.405(12) . ?
C37 H01J 0.9300 . ?
C31 H01K 0.9300 . ?
C3 H01L 0.9800 . ?
C33 H01M 0.9300 . ?
C20 H01N 0.9300 . ?
C26 C27 1.374(13) . ?
C26 H01O 0.9300 . ?
C28 C27 1.355(12) . ?
C28 H01P 0.9300 . ?
C38 H01Q 0.9300 . ?
C27 H01R 0.9300 . ?
C42 H01S 0.9700 . ?
C42 H01T 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl4 Ga2 Cl6 109.38(10) . . ?
Cl4 Ga2 Cl7 110.87(9) . . ?
Cl6 Ga2 Cl7 110.49(9) . . ?
Cl4 Ga2 Cl5 110.69(10) . . ?
Cl6 Ga2 Cl5 108.81(10) . . ?
Cl7 Ga2 Cl5 106.56(9) . . ?
N1 Ga1 Cl2 106.2(2) . . ?
N1 Ga1 Cl3 105.0(2) . . ?
Cl2 Ga1 Cl3 115.61(10) . . ?
N1 Ga1 Cl1 104.2(2) . . ?
Cl2 Ga1 Cl1 112.51(10) . . ?
Cl3 Ga1 Cl1 112.18(9) . . ?
O2 S1 O1 114.9(3) . . ?
O2 S1 O3 115.0(3) . . ?
O1 S1 O3 114.2(3) . . ?
O2 S1 C41 104.2(4) . . ?
O1 S1 C41 103.4(4) . . ?
O3 S1 C41 103.0(4) . . ?
C23 P2 C17 111.5(4) . . ?
C23 P2 C12 107.1(4) . . ?
C17 P2 C12 114.1(4) . . ?
C23 P2 C3 114.9(4) . . ?
C17 P2 C3 105.9(4) . . ?
C12 P2 C3 103.3(4) . . ?
C35 P1 C29 110.4(4) . . ?
C35 P1 C5 111.2(4) . . ?
C29 P1 C5 109.6(4) . . ?
C35 P1 C10 114.9(4) . . ?
C29 P1 C10 106.8(4) . . ?
C5 P1 C10 103.7(3) . . ?
C10 N2 C3 115.8(6) . . ?
C10 N2 C2 118.1(6) . . ?
C3 N2 C2 116.9(6) . . ?
C1 N1 Ga1 117.9(5) . . ?
C1 N1 H00A 107.8 . . ?
Ga1 N1 H00A 107.8 . . ?
C1 N1 H00B 107.8 . . ?
Ga1 N1 H00B 107.8 . . ?
H00A N1 H00B 107.2 . . ?
N1 C1 C2 109.7(6) . . ?
N1 C1 H00C 109.7 . . ?
C2 C1 H00C 109.7 . . ?
N1 C1 H00D 109.7 . . ?
C2 C1 H00D 109.7 . . ?
H00C C1 H00D 108.2 . . ?
C9 C4 C5 120.4(7) . . ?
C9 C4 C3 118.1(7) . . ?
C5 C4 C3 121.4(7) . . ?
C40 C35 C36 119.9(7) . . ?
C40 C35 P1 121.3(6) . . ?
C36 C35 P1 118.8(6) . . ?
C14 C15 C16 120.2(8) . . ?
C14 C15 H00Q 119.9 . . ?
C16 C15 H00Q 119.9 . . ?
C9 C8 C7 121.1(7) . . ?
C9 C8 H00R 119.4 . . ?
C7 C8 H00R 119.4 . . ?
C6 C5 C4 118.5(7) . . ?
C6 C5 P1 119.7(6) . . ?
C4 C5 P1 121.6(6) . . ?
F1 C41 F3 108.0(6) . . ?
F1 C41 F2 105.6(6) . . ?
F3 C41 F2 107.9(6) . . ?
F1 C41 S1 112.3(6) . . ?
F3 C41 S1 111.1(5) . . ?
F2 C41 S1 111.6(5) . . ?
C24 C25 C26 118.7(8) . . ?
C24 C25 H00U 120.6 . . ?
C26 C25 H00U 120.6 . . ?
C11 C12 C13 120.3(7) . . ?
C11 C12 P2 122.7(6) . . ?
C13 C12 P2 116.9(6) . . ?
C24 C23 C28 118.8(7) . . ?
C24 C23 P2 118.6(6) . . ?
C28 C23 P2 122.6(6) . . ?
C7 C6 C5 121.1(8) . . ?
C7 C6 H00X 119.5 . . ?
C5 C6 H00X 119.5 . . ?
C11 C16 C15 120.3(7) . . ?
C11 C16 H00Y 119.8 . . ?
C15 C16 H00Y 119.8 . . ?
C12 C11 C16 119.6(7) . . ?
C12 C11 C10 122.1(7) . . ?
C16 C11 C10 118.3(7) . . ?
C35 C36 C37 119.9(8) . . ?
C35 C36 H010 120.1 . . ?
C37 C36 H010 120.1 . . ?
C25 C24 C23 121.1(7) . . ?
C25 C24 H011 119.5 . . ?
C23 C24 H011 119.5 . . ?
N2 C10 C11 112.8(6) . . ?
N2 C10 P1 108.5(5) . . ?
C11 C10 P1 112.9(5) . . ?
N2 C10 H012 107.4 . . ?
C11 C10 H012 107.4 . . ?
P1 C10 H012 107.4 . . ?
C4 C9 C8 120.2(7) . . ?
C4 C9 H013 119.9 . . ?
C8 C9 H013 119.9 . . ?
N2 C2 C1 111.9(6) . . ?
N2 C2 H01A 109.2 . . ?
C1 C2 H01A 109.2 . . ?
N2 C2 H01B 109.2 . . ?
C1 C2 H01B 109.2 . . ?
H01A C2 H01B 107.9 . . ?
C21 C22 C17 119.5(8) . . ?
C21 C22 H015 120.2 . . ?
C17 C22 H015 120.2 . . ?
C20 C21 C22 120.3(8) . . ?
C20 C21 H016 119.9 . . ?
C22 C21 H016 119.9 . . ?
C8 C7 C6 118.7(8) . . ?
C8 C7 H017 120.6 . . ?
C6 C7 H017 120.6 . . ?
C33 C34 C29 120.3(8) . . ?
C33 C34 H018 119.8 . . ?
C29 C34 H018 119.8 . . ?
C14 C13 C12 119.2(7) . . ?
C14 C13 H019 120.4 . . ?
C12 C13 H019 120.4 . . ?
C39 C40 C35 120.1(8) . . ?
C39 C40 H01C 120.0 . . ?
C35 C40 H01C 120.0 . . ?
C40 C39 C38 121.0(8) . . ?
C40 C39 H01D 119.5 . . ?
C38 C39 H01D 119.5 . . ?
C31 C30 C29 120.9(8) . . ?
C31 C30 H01E 119.5 . . ?
C29 C30 H01E 119.5 . . ?
C19 C18 C17 120.4(8) . . ?
C19 C18 H01F 119.8 . . ?
C17 C18 H01F 119.8 . . ?
C33 C32 C31 120.2(8) . . ?
C33 C32 H01G 119.9 . . ?
C31 C32 H01G 119.9 . . ?
C15 C14 C13 120.3(8) . . ?
C15 C14 H01H 119.9 . . ?
C13 C14 H01H 119.9 . . ?
C18 C17 C22 119.4(8) . . ?
C18 C17 P2 121.1(6) . . ?
C22 C17 P2 119.3(6) . . ?
C34 C29 C30 118.8(7) . . ?
C34 C29 P1 121.4(6) . . ?
C30 C29 P1 119.8(6) . . ?
C18 C19 C20 119.7(8) . . ?
C18 C19 H01I 120.1 . . ?
C20 C19 H01I 120.1 . . ?
C36 C37 C38 119.2(8) . . ?
C36 C37 H01J 120.4 . . ?
C38 C37 H01J 120.4 . . ?
C30 C31 C32 119.1(8) . . ?
C30 C31 H01K 120.4 . . ?
C32 C31 H01K 120.4 . . ?
N2 C3 C4 119.1(6) . . ?
N2 C3 P2 103.7(5) . . ?
C4 C3 P2 112.8(5) . . ?
N2 C3 H01L 106.9 . . ?
C4 C3 H01L 106.9 . . ?
P2 C3 H01L 106.9 . . ?
C34 C33 C32 120.6(8) . . ?
C34 C33 H01M 119.7 . . ?
C32 C33 H01M 119.7 . . ?
C21 C20 C19 120.7(8) . . ?
C21 C20 H01N 119.7 . . ?
C19 C20 H01N 119.7 . . ?
C27 C26 C25 120.0(8) . . ?
C27 C26 H01O 120.0 . . ?
C25 C26 H01O 120.0 . . ?
C27 C28 C23 119.3(8) . . ?
C27 C28 H01P 120.3 . . ?
C23 C28 H01P 120.3 . . ?
C39 C38 C37 119.9(8) . . ?
C39 C38 H01Q 120.0 . . ?
C37 C38 H01Q 120.0 . . ?
C28 C27 C26 122.0(8) . . ?
C28 C27 H01R 119.0 . . ?
C26 C27 H01R 119.0 . . ?
Cl9 C42 Cl8 110.9(5) . . ?
Cl9 C42 H01S 109.5 . . ?
Cl8 C42 H01S 109.5 . . ?
Cl9 C42 H01T 109.5 . . ?
Cl8 C42 H01T 109.5 . . ?
H01S C42 H01T 108.0 . . ?

_refine_diff_density_max         0.758
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.141

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1889433'
loop_
_audit_author_name
_audit_author_address
'Moumita Majumdar'
;IISER Pune
India
;
_audit_update_record             
;
2019-02-20 deposited with the CCDC.	2019-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H37 F9 N2 O9 P2 S3'
_chemical_formula_weight         1054.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   14.1906(5)
_cell_length_b                   19.4217(7)
_cell_length_c                   16.8932(6)
_cell_angle_alpha                90
_cell_angle_beta                 101.035(2)
_cell_angle_gamma                90
_cell_volume                     4569.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      3.50
_cell_measurement_theta_max      66.65

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_F_000             2160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    2.987
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56035
_diffrn_reflns_av_unetI/netI     0.1140
_diffrn_reflns_av_R_equivalents  0.1711
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.505
_diffrn_reflns_theta_max         66.922
_diffrn_reflns_theta_full        66.922
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             8084
_reflns_number_gt                5331
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1554P)²+9.8049P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8084
_refine_ls_number_parameters     686
_refine_ls_number_restraints     150
_refine_ls_R_factor_all          0.1529
_refine_ls_R_factor_gt           0.1015
_refine_ls_wR_factor_ref         0.2693
_refine_ls_wR_factor_gt          0.2399
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.70326(9) 0.27564(7) 0.53813(8) 0.0098(3) Uani 1 1 d . . . A 5
P2 P 0.97121(9) 0.28041(7) 0.69242(8) 0.0102(3) Uani 1 1 d . . . A 5
N1 N 0.7964(4) 0.4988(2) 0.5247(3) 0.0250(12) Uani 1 1 d . . . A 5
H00A H 0.8496 0.5258 0.5294 0.038 Uiso 1 1 calc R U . A 5
H00B H 0.7451 0.5213 0.4954 0.038 Uiso 1 1 calc R U . A 5
H00C H 0.8062 0.4588 0.4993 0.038 Uiso 1 1 calc R U . A 5
N2 N 0.8310(3) 0.3621(2) 0.6084(3) 0.0124(10) Uani 1 1 d . . . A 5
C1 C 0.7773(4) 0.4831(3) 0.6063(4) 0.0225(14) Uani 1 1 d . . . A 5
H01C H 0.7110 0.4654 0.6014 0.027 Uiso 1 1 calc R U . A 5
H01F H 0.7829 0.5258 0.6388 0.027 Uiso 1 1 calc R U . A 5
C2 C 0.8481(4) 0.4296(3) 0.6486(3) 0.0169(12) Uani 1 1 d . U . A 5
H00D H 0.9145 0.4449 0.6479 0.020 Uiso 1 1 calc R U . A 5
H00E H 0.8410 0.4253 0.7056 0.020 Uiso 1 1 calc R U . A 5
C3 C 0.9151(4) 0.3238(3) 0.5958(3) 0.0119(11) Uani 1 1 d . U . A 5
H00T H 0.9626 0.3576 0.5820 0.014 Uiso 1 1 calc R U . A 5
C4 C 0.7550(4) 0.3219(3) 0.6317(3) 0.0105(11) Uani 1 1 d . . . A 5
H1 H 0.7051 0.3552 0.6424 0.013 Uiso 1 1 calc R U . A 5
C5 C 0.7790(4) 0.2752(3) 0.7057(3) 0.0107(11) Uani 1 1 d . . . A 5
C6 C 0.8721(4) 0.2508(3) 0.7347(3) 0.0117(12) Uani 1 1 d . . . A 5
C7 C 0.8908(4) 0.2064(3) 0.8007(3) 0.0187(13) Uani 1 1 d . . . A 5
H011 H 0.9540 0.1899 0.8198 0.022 Uiso 1 1 calc R U . A 5
C8 C 0.8171(5) 0.1868(3) 0.8379(4) 0.0268(15) Uani 1 1 d . . . A 5
H01J H 0.8298 0.1566 0.8830 0.032 Uiso 1 1 calc R U . A 5
C9 C 0.7251(5) 0.2105(3) 0.8107(4) 0.0238(14) Uani 1 1 d . U . A 5
H010 H 0.6745 0.1968 0.8368 0.029 Uiso 1 1 calc R U . A 5
C10 C 0.7066(4) 0.2549(3) 0.7441(3) 0.0189(13) Uani 1 1 d . U . A 5
H017 H 0.6432 0.2712 0.7253 0.023 Uiso 1 1 calc R U . A 5
C11 C 1.0374(4) 0.3446(3) 0.7575(3) 0.0126(12) Uani 1 1 d . . . A 5
C12 C 1.1103(4) 0.3817(3) 0.7312(3) 0.0186(13) Uani 1 1 d . . . A 5
H00Z H 1.1246 0.3731 0.6794 0.022 Uiso 1 1 calc R U . A 5
C13 C 1.1607(4) 0.4305(3) 0.7804(4) 0.0240(14) Uani 1 1 d . . . A 5
H016 H 1.2120 0.4542 0.7636 0.029 Uiso 1 1 calc R U . A 5
C14 C 1.1376(5) 0.4454(3) 0.8539(4) 0.0269(15) Uani 1 1 d . . . A 5
H019 H 1.1724 0.4798 0.8873 0.032 Uiso 1 1 calc R U . A 5
C15 C 1.0645(5) 0.4108(3) 0.8792(4) 0.0272(15) Uani 1 1 d . . . A 5
H01H H 1.0483 0.4220 0.9297 0.033 Uiso 1 1 calc R U . A 5
C16 C 1.0139(4) 0.3595(3) 0.8319(3) 0.0202(13) Uani 1 1 d . . . A 5
H00X H 0.9641 0.3350 0.8500 0.024 Uiso 1 1 calc R U . A 5
C17 C 1.0441(4) 0.2084(3) 0.6749(3) 0.0154(12) Uani 1 1 d . . . A 5
C18 C 1.1398(4) 0.2178(3) 0.6689(4) 0.0286(15) Uani 1 1 d . . . A 5
H01B H 1.1712 0.2604 0.6834 0.034 Uiso 1 1 calc R U . A 5
C19 C 1.1883(5) 0.1640(4) 0.6414(5) 0.0389(18) Uani 1 1 d . . . A 5
H01R H 1.2537 0.1699 0.6374 0.047 Uiso 1 1 calc R U . A 5
C20 C 1.1438(6) 0.1019(4) 0.6195(4) 0.043(2) Uani 1 1 d . . . A 5
H01T H 1.1779 0.0659 0.5992 0.052 Uiso 1 1 calc R U . A 5
C21 C 1.0497(5) 0.0921(3) 0.6271(4) 0.0317(16) Uani 1 1 d . . . A 5
H01K H 1.0199 0.0486 0.6143 0.038 Uiso 1 1 calc R U . A 5
C22 C 0.9985(4) 0.1453(3) 0.6534(3) 0.0228(14) Uani 1 1 d . . . A 5
H012 H 0.9330 0.1391 0.6569 0.027 Uiso 1 1 calc R U . A 5
C23 C 0.8961(4) 0.2707(3) 0.5292(3) 0.0111(11) Uani 1 1 d . U . A 5
C24 C 0.9716(4) 0.2482(3) 0.4950(3) 0.0204(13) Uani 1 1 d . U . A 5
H015 H 1.0336 0.2677 0.5117 0.025 Uiso 1 1 calc R U . A 5
C25 C 0.9572(5) 0.1975(4) 0.4369(4) 0.0311(16) Uani 1 1 d . . . A 5
H01I H 1.0094 0.1827 0.4133 0.037 Uiso 1 1 calc R U . A 5
C26 C 0.8674(5) 0.1680(3) 0.4123(4) 0.0325(16) Uani 1 1 d . . . A 5
H01M H 0.8586 0.1327 0.3728 0.039 Uiso 1 1 calc R U . A 5
C27 C 0.7923(5) 0.1895(3) 0.4446(4) 0.0260(15) Uani 1 1 d . . . A 5
H01E H 0.7307 0.1694 0.4275 0.031 Uiso 1 1 calc R U . A 5
C28 C 0.8052(4) 0.2416(3) 0.5036(3) 0.0146(12) Uani 1 1 d . . . A 5
C29 C 0.6230(4) 0.2069(3) 0.5524(3) 0.0136(12) Uani 1 1 d . . . A 5
C30 C 0.6621(5) 0.1470(3) 0.5917(3) 0.0236(14) Uani 1 1 d . . . A 5
H01D H 0.7297 0.1422 0.6076 0.028 Uiso 1 1 calc R U . A 5
C31 C 0.6020(5) 0.0952(3) 0.6070(4) 0.0336(17) Uani 1 1 d . . . A 5
H018 H 0.6279 0.0546 0.6341 0.040 Uiso 1 1 calc R U . A 5
C32 C 0.5030(6) 0.1024(3) 0.5826(4) 0.0364(17) Uani 1 1 d . . . A 5
H01Q H 0.4617 0.0664 0.5930 0.044 Uiso 1 1 calc R U . A 5
C33 C 0.4641(5) 0.1613(3) 0.5436(4) 0.0322(16) Uani 1 1 d . . . A 5
H01O H 0.3965 0.1654 0.5269 0.039 Uiso 1 1 calc R U . A 5
C34 C 0.5245(4) 0.2149(3) 0.5287(4) 0.0205(13) Uani 1 1 d . . . A 5
H00Y H 0.4984 0.2560 0.5029 0.025 Uiso 1 1 calc R U . A 5
C35 C 0.6444(4) 0.3396(3) 0.4690(3) 0.0116(11) Uani 1 1 d . U . A 5
C36 C 0.6758(4) 0.3507(3) 0.3963(3) 0.0175(12) Uani 1 1 d . U . A 5
H00U H 0.7264 0.3240 0.3827 0.021 Uiso 1 1 calc R U . A 5
C37 C 0.6316(5) 0.4013(3) 0.3451(4) 0.0277(16) Uani 1 1 d . . . A 5
H014 H 0.6535 0.4100 0.2963 0.033 Uiso 1 1 calc R U . A 5
C38 C 0.5577(5) 0.4391(3) 0.3623(4) 0.0282(16) Uani 1 1 d . . . A 5
H01G H 0.5274 0.4728 0.3252 0.034 Uiso 1 1 calc R U . A 5
C39 C 0.5264(4) 0.4284(3) 0.4346(4) 0.0247(15) Uani 1 1 d . . . A 5
H013 H 0.4751 0.4551 0.4470 0.030 Uiso 1 1 calc R U . A 5
C40 C 0.5696(4) 0.3792(3) 0.4880(3) 0.0201(13) Uani 1 1 d . . . A 5
H01A H 0.5487 0.3723 0.5376 0.024 Uiso 1 1 calc R U . A 5
S1 S 0.68935(11) 0.65068(8) 0.42955(9) 0.0236(4) Uani 1 1 d . . . B 5
O1 O 0.6483(3) 0.5947(3) 0.4682(3) 0.0410(13) Uani 1 1 d . . . B 5
O2 O 0.6780(4) 0.7173(3) 0.4630(3) 0.0560(16) Uani 1 1 d . . . B 5
O3 O 0.7832(4) 0.6367(3) 0.4138(3) 0.0505(15) Uani 1 1 d . . . B 5
C41 C 0.6133(5) 0.6549(4) 0.3298(4) 0.0335(17) Uani 1 1 d . . . B 5
F1 F 0.5226(3) 0.6664(3) 0.3345(3) 0.0717(16) Uani 1 1 d . . . B 5
F2 F 0.6177(4) 0.5967(3) 0.2899(3) 0.0701(15) Uani 1 1 d . . . B 5
F3 F 0.6423(4) 0.7044(3) 0.2858(3) 0.0656(15) Uani 1 1 d . . . B 5
S2 S 0.03778(11) 0.57076(7) 0.59553(8) 0.0201(4) Uani 1 1 d . . . C 5
O4 O 0.1150(3) 0.6003(2) 0.5634(3) 0.0369(12) Uani 1 1 d . . . C 5
O5 O -0.0559(3) 0.5977(2) 0.5608(3) 0.0424(13) Uani 1 1 d . . . C 5
O6 O 0.0415(3) 0.4976(2) 0.6050(3) 0.0305(11) Uani 1 1 d . . . C 5
C42 C 0.0550(6) 0.6041(4) 0.6973(4) 0.048(2) Uani 1 1 d . . . C 5
F4 F 0.1413(4) 0.5883(3) 0.7395(3) 0.0748(17) Uani 1 1 d . . . C 5
F5 F 0.0460(5) 0.6719(3) 0.6982(3) 0.086(2) Uani 1 1 d . . . C 5
F6 F -0.0090(5) 0.5766(4) 0.7360(3) 0.094(2) Uani 1 1 d . . . C 5
S3 S 0.3516(2) 0.53815(14) 0.19170(17) 0.0358(7) Uani 0.7 1 d D U P D 1
O9 O 0.4451(6) 0.5504(6) 0.1633(6) 0.068(3) Uani 0.7 1 d D U P D 1
O7 O 0.3409(6) 0.5772(4) 0.2609(5) 0.0434(19) Uani 0.8 1 d D U P D 1
O8 O 0.3198(7) 0.4666(4) 0.1915(6) 0.056(2) Uani 0.8 1 d D U P D 1
C43 C 0.2684(8) 0.5771(5) 0.1095(6) 0.038(2) Uani 0.7 1 d D U P D 1
F7 F 0.2891(8) 0.6394(5) 0.0906(6) 0.081(3) Uani 0.7 1 d D U P D 1
F8 F 0.1814(5) 0.5810(4) 0.1278(5) 0.069(2) Uani 0.7 1 d D U P D 1
F9 F 0.2558(7) 0.5412(4) 0.0424(5) 0.069(2) Uani 0.7 1 d D U P D 1
S3' S 0.3052(6) 0.5274(4) 0.2034(5) 0.041(2) Uani 0.3 1 d D U P E 2
O9' O 0.2031(10) 0.5426(11) 0.1815(13) 0.063(6) Uani 0.3 1 d D . P E 2
O7' O 0.369(3) 0.564(2) 0.282(3) 0.065(14) Uani 0.2 1 d D U P E 2
O8' O 0.360(3) 0.461(3) 0.198(4) 0.10(2) Uani 0.2 1 d D U P E 2
C43' C 0.337(3) 0.5704(14) 0.116(2) 0.088(12) Uani 0.3 1 d D U P E 2
F7' F 0.3326(16) 0.6382(12) 0.1163(15) 0.077(7) Uani 0.3 1 d D U P E 2
F8' F 0.429(2) 0.5652(17) 0.116(2) 0.134(11) Uani 0.3 1 d D U P E 2
F9' F 0.316(2) 0.5355(16) 0.0478(18) 0.122(10) Uani 0.3 1 d D U P E 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C28 1.788(6) . ?
P1 C35 1.797(5) . ?
P1 C29 1.800(5) . ?
P1 C4 1.844(5) . ?
P2 C6 1.789(5) . ?
P2 C17 1.797(5) . ?
P2 C11 1.803(5) . ?
P2 C3 1.873(5) . ?
N1 C1 1.486(8) . ?
N1 H00A 0.9100 . ?
N1 H00B 0.9100 . ?
N1 H00C 0.9100 . ?
N2 C4 1.446(7) . ?
N2 C3 1.457(7) . ?
N2 C2 1.475(7) . ?
C1 C2 1.524(8) . ?
C1 H01C 0.9900 . ?
C1 H01F 0.9900 . ?
C2 H00D 0.9900 . ?
C2 H00E 0.9900 . ?
C3 C23 1.512(7) . ?
C3 H00T 1.0000 . ?
C4 C5 1.530(7) . ?
C4 H1 1.0000 . ?
C5 C10 1.373(8) . ?
C5 C6 1.402(7) . ?
C6 C7 1.395(7) . ?
C7 C8 1.373(9) . ?
C7 H011 0.9500 . ?
C8 C9 1.379(9) . ?
C8 H01J 0.9500 . ?
C9 C10 1.401(8) . ?
C9 H010 0.9500 . ?
C10 H017 0.9500 . ?
C11 C16 1.391(8) . ?
C11 C12 1.400(8) . ?
C12 C13 1.369(8) . ?
C12 H00Z 0.9500 . ?
C13 C14 1.374(9) . ?
C13 H016 0.9500 . ?
C14 C15 1.371(9) . ?
C14 H019 0.9500 . ?
C15 C16 1.388(9) . ?
C15 H01H 0.9500 . ?
C16 H00X 0.9500 . ?
C17 C18 1.394(9) . ?
C17 C22 1.401(8) . ?
C18 C19 1.379(9) . ?
C18 H01B 0.9500 . ?
C19 C20 1.378(11) . ?
C19 H01R 0.9500 . ?
C20 C21 1.379(11) . ?
C20 H01T 0.9500 . ?
C21 C22 1.385(9) . ?
C21 H01K 0.9500 . ?
C22 H012 0.9500 . ?
C23 C24 1.381(8) . ?
C23 C28 1.398(8) . ?
C24 C25 1.377(9) . ?
C24 H015 0.9500 . ?
C25 C26 1.386(10) . ?
C25 H01I 0.9500 . ?
C26 C27 1.353(9) . ?
C26 H01M 0.9500 . ?
C27 C28 1.407(8) . ?
C27 H01E 0.9500 . ?
C29 C34 1.388(8) . ?
C29 C30 1.401(8) . ?
C30 C31 1.375(9) . ?
C30 H01D 0.9500 . ?
C31 C32 1.393(10) . ?
C31 H018 0.9500 . ?
C32 C33 1.381(10) . ?
C32 H01Q 0.9500 . ?
C33 C34 1.401(8) . ?
C33 H01O 0.9500 . ?
C34 H00Y 0.9500 . ?
C35 C40 1.398(8) . ?
C35 C36 1.400(8) . ?
C36 C37 1.378(8) . ?
C36 H00U 0.9500 . ?
C37 C38 1.357(10) . ?
C37 H014 0.9500 . ?
C38 C39 1.392(9) . ?
C38 H01G 0.9500 . ?
C39 C40 1.375(8) . ?
C39 H013 0.9500 . ?
C40 H01A 0.9500 . ?
S1 O3 1.433(5) . ?
S1 O2 1.433(5) . ?
S1 O1 1.447(5) . ?
S1 C41 1.820(7) . ?
C41 F2 1.323(8) . ?
C41 F1 1.324(8) . ?
C41 F3 1.329(8) . ?
S2 O6 1.430(4) . ?
S2 O4 1.433(5) . ?
S2 O5 1.444(5) . ?
S2 C42 1.810(7) . ?
C42 F5 1.324(9) . ?
C42 F6 1.328(10) . ?
C42 F4 1.330(10) . ?
S3 O7 1.426(8) . ?
S3 O8 1.460(9) . ?
S3 O9 1.514(9) . ?
S3 C43 1.808(10) . ?
C43 F7 1.298(11) . ?
C43 F9 1.315(11) . ?
C43 F8 1.330(11) . ?
S3' O9' 1.455(15) . ?
S3' O8' 1.52(4) . ?
S3' O7' 1.63(4) . ?
S3' C43' 1.82(4) . ?
C43' F8' 1.310(19) . ?
C43' F7' 1.319(19) . ?
C43' F9' 1.326(19) . ?

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
C28 P1 C35 110.4(3) . . ?
C28 P1 C29 110.0(3) . . ?
C35 P1 C29 111.8(2) . . ?
C28 P1 C4 104.2(2) . . ?
C35 P1 C4 106.2(2) . . ?
C29 P1 C4 113.9(2) . . ?
C6 P2 C17 109.7(3) . . ?
C6 P2 C11 109.7(3) . . ?
C17 P2 C11 112.9(3) . . ?
C6 P2 C3 104.9(2) . . ?
C17 P2 C3 111.6(2) . . ?
C11 P2 C3 107.8(2) . . ?
C1 N1 H00A 109.5 . . ?
C1 N1 H00B 109.5 . . ?
H00A N1 H00B 109.5 . . ?
C1 N1 H00C 109.5 . . ?
H00A N1 H00C 109.5 . . ?
H00B N1 H00C 109.5 . . ?
C4 N2 C3 116.0(4) . . ?
C4 N2 C2 114.8(4) . . ?
C3 N2 C2 117.0(4) . . ?
N1 C1 C2 110.7(5) . . ?
N1 C1 H01C 109.5 . . ?
C2 C1 H01C 109.5 . . ?
N1 C1 H01F 109.5 . . ?
C2 C1 H01F 109.5 . . ?
H01C C1 H01F 108.1 . . ?
N2 C2 C1 110.7(4) . . ?
N2 C2 H00D 109.5 . . ?
C1 C2 H00D 109.5 . . ?
N2 C2 H00E 109.5 . . ?
C1 C2 H00E 109.5 . . ?
H00D C2 H00E 108.1 . . ?
N2 C3 C23 115.0(4) . . ?
N2 C3 P2 109.0(3) . . ?
C23 C3 P2 109.1(3) . . ?
N2 C3 H00T 107.8 . . ?
C23 C3 H00T 107.8 . . ?
P2 C3 H00T 107.8 . . ?
N2 C4 C5 118.8(4) . . ?
N2 C4 P1 103.0(3) . . ?
C5 C4 P1 113.7(3) . . ?
N2 C4 H1 106.9 . . ?
C5 C4 H1 106.9 . . ?
P1 C4 H1 106.9 . . ?
C10 C5 C6 118.6(5) . . ?
C10 C5 C4 119.2(5) . . ?
C6 C5 C4 122.2(5) . . ?
C7 C6 C5 120.6(5) . . ?
C7 C6 P2 118.3(4) . . ?
C5 C6 P2 120.9(4) . . ?
C8 C7 C6 119.6(5) . . ?
C8 C7 H011 120.2 . . ?
C6 C7 H011 120.2 . . ?
C7 C8 C9 120.7(5) . . ?
C7 C8 H01J 119.7 . . ?
C9 C8 H01J 119.7 . . ?
C8 C9 C10 119.5(6) . . ?
C8 C9 H010 120.2 . . ?
C10 C9 H010 120.2 . . ?
C5 C10 C9 121.0(5) . . ?
C5 C10 H017 119.5 . . ?
C9 C10 H017 119.5 . . ?
C16 C11 C12 120.0(5) . . ?
C16 C11 P2 120.5(4) . . ?
C12 C11 P2 119.5(4) . . ?
C13 C12 C11 119.7(5) . . ?
C13 C12 H00Z 120.2 . . ?
C11 C12 H00Z 120.2 . . ?
C12 C13 C14 120.5(6) . . ?
C12 C13 H016 119.8 . . ?
C14 C13 H016 119.8 . . ?
C15 C14 C13 120.3(6) . . ?
C15 C14 H019 119.9 . . ?
C13 C14 H019 119.9 . . ?
C14 C15 C16 120.7(6) . . ?
C14 C15 H01H 119.7 . . ?
C16 C15 H01H 119.7 . . ?
C15 C16 C11 118.9(6) . . ?
C15 C16 H00X 120.6 . . ?
C11 C16 H00X 120.6 . . ?
C18 C17 C22 120.3(5) . . ?
C18 C17 P2 120.7(4) . . ?
C22 C17 P2 118.1(4) . . ?
C19 C18 C17 118.8(6) . . ?
C19 C18 H01B 120.6 . . ?
C17 C18 H01B 120.6 . . ?
C20 C19 C18 121.4(7) . . ?
C20 C19 H01R 119.3 . . ?
C18 C19 H01R 119.3 . . ?
C19 C20 C21 119.8(7) . . ?
C19 C20 H01T 120.1 . . ?
C21 C20 H01T 120.1 . . ?
C20 C21 C22 120.3(6) . . ?
C20 C21 H01K 119.9 . . ?
C22 C21 H01K 119.9 . . ?
C21 C22 C17 119.4(6) . . ?
C21 C22 H012 120.3 . . ?
C17 C22 H012 120.3 . . ?
C24 C23 C28 119.1(5) . . ?
C24 C23 C3 119.0(5) . . ?
C28 C23 C3 121.9(5) . . ?
C25 C24 C23 120.2(6) . . ?
C25 C24 H015 119.9 . . ?
C23 C24 H015 119.9 . . ?
C24 C25 C26 120.7(6) . . ?
C24 C25 H01I 119.6 . . ?
C26 C25 H01I 119.6 . . ?
C27 C26 C25 120.2(6) . . ?
C27 C26 H01M 119.9 . . ?
C25 C26 H01M 119.9 . . ?
C26 C27 C28 120.0(6) . . ?
C26 C27 H01E 120.0 . . ?
C28 C27 H01E 120.0 . . ?
C23 C28 C27 119.8(5) . . ?
C23 C28 P1 120.4(4) . . ?
C27 C28 P1 119.5(4) . . ?
C34 C29 C30 121.0(5) . . ?
C34 C29 P1 120.5(4) . . ?
C30 C29 P1 118.5(4) . . ?
C31 C30 C29 119.6(6) . . ?
C31 C30 H01D 120.2 . . ?
C29 C30 H01D 120.2 . . ?
C30 C31 C32 119.8(6) . . ?
C30 C31 H018 120.1 . . ?
C32 C31 H018 120.1 . . ?
C33 C32 C31 120.9(6) . . ?
C33 C32 H01Q 119.6 . . ?
C31 C32 H01Q 119.6 . . ?
C32 C33 C34 119.9(7) . . ?
C32 C33 H01O 120.1 . . ?
C34 C33 H01O 120.1 . . ?
C29 C34 C33 118.9(6) . . ?
C29 C34 H00Y 120.6 . . ?
C33 C34 H00Y 120.6 . . ?
C40 C35 C36 120.0(5) . . ?
C40 C35 P1 120.7(4) . . ?
C36 C35 P1 119.3(4) . . ?
C37 C36 C35 118.5(6) . . ?
C37 C36 H00U 120.7 . . ?
C35 C36 H00U 120.7 . . ?
C38 C37 C36 121.9(6) . . ?
C38 C37 H014 119.0 . . ?
C36 C37 H014 119.0 . . ?
C37 C38 C39 119.8(6) . . ?
C37 C38 H01G 120.1 . . ?
C39 C38 H01G 120.1 . . ?
C40 C39 C38 120.2(6) . . ?
C40 C39 H013 119.9 . . ?
C38 C39 H013 119.9 . . ?
C39 C40 C35 119.6(6) . . ?
C39 C40 H01A 120.2 . . ?
C35 C40 H01A 120.2 . . ?
O3 S1 O2 115.1(4) . . ?
O3 S1 O1 114.2(3) . . ?
O2 S1 O1 114.5(3) . . ?
O3 S1 C41 104.1(3) . . ?
O2 S1 C41 103.5(3) . . ?
O1 S1 C41 103.5(3) . . ?
F2 C41 F1 108.4(6) . . ?
F2 C41 F3 106.4(6) . . ?
F1 C41 F3 108.6(6) . . ?
F2 C41 S1 110.9(5) . . ?
F1 C41 S1 111.3(5) . . ?
F3 C41 S1 111.0(5) . . ?
O6 S2 O4 115.2(3) . . ?
O6 S2 O5 114.6(3) . . ?
O4 S2 O5 114.4(3) . . ?
O6 S2 C42 104.7(3) . . ?
O4 S2 C42 104.1(3) . . ?
O5 S2 C42 101.7(4) . . ?
F5 C42 F6 108.6(7) . . ?
F5 C42 F4 107.7(7) . . ?
F6 C42 F4 106.8(7) . . ?
F5 C42 S2 111.7(5) . . ?
F6 C42 S2 110.1(6) . . ?
F4 C42 S2 111.7(6) . . ?
O7 S3 O8 115.3(6) . . ?
O7 S3 O9 114.4(5) . . ?
O8 S3 O9 116.0(6) . . ?
O7 S3 C43 104.5(5) . . ?
O8 S3 C43 103.9(5) . . ?
O9 S3 C43 100.0(6) . . ?
F7 C43 F9 106.4(9) . . ?
F7 C43 F8 105.6(9) . . ?
F9 C43 F8 104.6(9) . . ?
F7 C43 S3 115.7(8) . . ?
F9 C43 S3 113.6(7) . . ?
F8 C43 S3 110.1(7) . . ?
O9' S3' O8' 131(2) . . ?
O9' S3' O7' 119.3(17) . . ?
O8' S3' O7' 102(3) . . ?
O9' S3' C43' 95.3(15) . . ?
O8' S3' C43' 98(3) . . ?
O7' S3' C43' 106(2) . . ?
F8' C43' F7' 97(3) . . ?
F8' C43' F9' 91(3) . . ?
F7' C43' F9' 121(3) . . ?
F8' C43' S3' 112(3) . . ?
F7' C43' S3' 116(2) . . ?
F9' C43' S3' 115(2) . . ?

_refine_diff_density_max         0.962
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.141

