# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_yy20140326
_database_code_depnum_ccdc_archive 'CCDC 1424116'
_audit_update_record             
;
2015-09-12 deposited with the CCDC.
2015-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H27 Cl3 Ge N P'
_chemical_formula_weight         539.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   12.2706(4)
_cell_length_b                   14.1117(7)
_cell_length_c                   14.6498(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2536.75(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1750
_cell_measurement_theta_min      3.5380
_cell_measurement_theta_max      24.3860

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    1.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5673
_exptl_absorpt_correction_T_max  0.6456
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7161
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4721
_reflns_number_gt                4176
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0263P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(10)
_refine_ls_number_reflns         4721
_refine_ls_number_parameters     275
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.0770
_refine_ls_wR_factor_gt          0.0739
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.84398(3) 0.23349(3) 0.05675(3) 0.02205(11) Uani 1 1 d . . .
Cl2 Cl 0.73189(7) 0.22044(8) -0.05275(7) 0.0383(3) Uani 1 1 d . . .
P1 P 0.68275(7) 0.27978(8) 0.20026(7) 0.0244(2) Uani 1 1 d . . .
Cl3 Cl 0.90370(9) 0.37407(7) 0.04433(8) 0.0382(3) Uani 1 1 d . . .
Cl1 Cl 0.97878(8) 0.14453(8) 0.02746(8) 0.0381(3) Uani 1 1 d . . .
N1 N 0.7909(2) 0.2049(2) 0.1686(2) 0.0203(7) Uani 1 1 d . . .
C63 C 0.9615(3) 0.2315(3) 0.4042(3) 0.0378(11) Uani 1 1 d . . .
H63A H 0.8844 0.2412 0.4189 0.057 Uiso 1 1 calc R . .
H63B H 1.0023 0.2897 0.4173 0.057 Uiso 1 1 calc R . .
H63C H 0.9905 0.1795 0.4413 0.057 Uiso 1 1 calc R . .
C14 C 0.8186(3) 0.4083(3) 0.2878(3) 0.0284(10) Uani 1 1 d . . .
H14A H 0.8544 0.4100 0.2303 0.034 Uiso 1 1 calc R . .
C13 C 0.7307(3) 0.3459(3) 0.3009(3) 0.0267(9) Uani 1 1 d . . .
C5 C 0.9362(3) 0.0333(3) 0.3194(3) 0.0271(10) Uani 1 1 d . . .
H5A H 0.9930 0.0327 0.3634 0.033 Uiso 1 1 calc R . .
C4 C 0.8842(3) -0.0503(3) 0.2987(3) 0.0315(10) Uani 1 1 d . . .
H4A H 0.9041 -0.1074 0.3288 0.038 Uiso 1 1 calc R . .
C61 C 0.9729(3) 0.2068(3) 0.3027(3) 0.0260(9) Uani 1 1 d . . .
H61A H 0.9437 0.2609 0.2661 0.031 Uiso 1 1 calc R . .
C6 C 0.9085(3) 0.1186(3) 0.2781(2) 0.0189(8) Uani 1 1 d . . .
C7 C 0.5804(3) 0.2010(3) 0.2488(3) 0.0270(10) Uani 1 1 d . . .
C18 C 0.6789(3) 0.3474(3) 0.3851(3) 0.0349(11) Uani 1 1 d . . .
H18A H 0.6183 0.3069 0.3955 0.042 Uiso 1 1 calc R . .
C2 C 0.7717(3) 0.0313(3) 0.1882(3) 0.0234(9) Uani 1 1 d . . .
C12 C 0.5955(3) 0.1418(3) 0.3250(3) 0.0351(11) Uani 1 1 d . . .
H12A H 0.6646 0.1388 0.3540 0.042 Uiso 1 1 calc R . .
C21 C 0.6888(3) 0.0226(3) 0.1112(3) 0.0342(11) Uani 1 1 d . . .
H21A H 0.6669 0.0878 0.0920 0.041 Uiso 1 1 calc R . .
C11 C 0.5101(3) 0.0880(4) 0.3576(3) 0.0471(14) Uani 1 1 d . . .
H11A H 0.5208 0.0490 0.4096 0.056 Uiso 1 1 calc R . .
C3 C 0.8030(3) -0.0502(3) 0.2339(3) 0.0301(11) Uani 1 1 d . . .
H3A H 0.7672 -0.1081 0.2199 0.036 Uiso 1 1 calc R . .
C1 C 0.8238(3) 0.1175(3) 0.2126(3) 0.0216(9) Uani 1 1 d . . .
C16 C 0.8019(3) 0.4672(3) 0.4405(3) 0.0386(11) Uani 1 1 d . . .
H16A H 0.8261 0.5080 0.4879 0.046 Uiso 1 1 calc R . .
C62 C 1.0942(3) 0.1938(3) 0.2783(3) 0.0363(11) Uani 1 1 d . . .
H62A H 1.1016 0.1857 0.2121 0.055 Uiso 1 1 calc R . .
H62B H 1.1228 0.1377 0.3095 0.055 Uiso 1 1 calc R . .
H62C H 1.1352 0.2499 0.2976 0.055 Uiso 1 1 calc R . .
C23 C 0.5858(3) -0.0322(4) 0.1385(4) 0.0492(14) Uani 1 1 d . . .
H23A H 0.5535 -0.0030 0.1929 0.074 Uiso 1 1 calc R . .
H23B H 0.6049 -0.0982 0.1519 0.074 Uiso 1 1 calc R . .
H23C H 0.5332 -0.0303 0.0883 0.074 Uiso 1 1 calc R . .
C17 C 0.7142(3) 0.4072(3) 0.4543(3) 0.0405(11) Uani 1 1 d . . .
H17A H 0.6780 0.4069 0.5115 0.049 Uiso 1 1 calc R . .
C15 C 0.8536(4) 0.4668(3) 0.3567(3) 0.0343(10) Uani 1 1 d . . .
H15A H 0.9142 0.5074 0.3467 0.041 Uiso 1 1 calc R . .
C10 C 0.4093(4) 0.0901(4) 0.3159(4) 0.0558(16) Uani 1 1 d . . .
H10A H 0.3512 0.0525 0.3388 0.067 Uiso 1 1 calc R . .
C22 C 0.7425(4) -0.0275(4) 0.0287(3) 0.0483(13) Uani 1 1 d . . .
H22A H 0.8101 0.0054 0.0125 0.072 Uiso 1 1 calc R . .
H22B H 0.6924 -0.0262 -0.0234 0.072 Uiso 1 1 calc R . .
H22C H 0.7589 -0.0934 0.0448 0.072 Uiso 1 1 calc R . .
C8 C 0.4774(3) 0.2027(3) 0.2073(3) 0.0378(12) Uani 1 1 d . . .
H8A H 0.4649 0.2423 0.1559 0.045 Uiso 1 1 calc R . .
C9 C 0.3936(3) 0.1467(4) 0.2410(3) 0.0507(15) Uani 1 1 d . . .
H9A H 0.3245 0.1477 0.2119 0.061 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.808(3) . ?
Ge1 Cl1 2.1203(11) . ?
Ge1 Cl2 2.1210(10) . ?
Ge1 Cl3 2.1227(11) . ?
P1 N1 1.759(3) . ?
P1 C7 1.822(4) . ?
P1 C13 1.841(4) . ?
N1 C1 1.449(5) . ?
C63 C61 1.534(5) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C14 C15 1.373(6) . ?
C14 C13 1.406(5) . ?
C14 H14A 0.9500 . ?
C13 C18 1.388(5) . ?
C5 C4 1.374(6) . ?
C5 C6 1.389(5) . ?
C5 H5A 0.9500 . ?
C4 C3 1.377(6) . ?
C4 H4A 0.9500 . ?
C61 C6 1.518(5) . ?
C61 C62 1.541(5) . ?
C61 H61A 1.0000 . ?
C6 C1 1.415(5) . ?
C7 C8 1.403(5) . ?
C7 C12 1.406(6) . ?
C18 C17 1.388(6) . ?
C18 H18A 0.9500 . ?
C2 C3 1.385(5) . ?
C2 C1 1.420(5) . ?
C2 C21 1.523(5) . ?
C12 C11 1.379(6) . ?
C12 H12A 0.9500 . ?
C21 C23 1.535(6) . ?
C21 C22 1.547(6) . ?
C21 H21A 1.0000 . ?
C11 C10 1.379(6) . ?
C11 H11A 0.9500 . ?
C3 H3A 0.9500 . ?
C16 C15 1.382(6) . ?
C16 C17 1.384(6) . ?
C16 H16A 0.9500 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C17 H17A 0.9500 . ?
C15 H15A 0.9500 . ?
C10 C9 1.370(7) . ?
C10 H10A 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C8 C9 1.387(6) . ?
C8 H8A 0.9500 . ?
C9 H9A 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
N1 Ge1 Cl1 109.41(10) . . ?
N1 Ge1 Cl2 115.62(9) . . ?
Cl1 Ge1 Cl2 107.55(5) . . ?
N1 Ge1 Cl3 114.21(10) . . ?
Cl1 Ge1 Cl3 105.47(5) . . ?
Cl2 Ge1 Cl3 103.90(5) . . ?
N1 P1 C7 104.88(17) . . ?
N1 P1 C13 105.94(15) . . ?
C7 P1 C13 102.53(19) . . ?
C1 N1 P1 127.1(2) . . ?
C1 N1 Ge1 119.5(2) . . ?
P1 N1 Ge1 112.15(16) . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C15 C14 C13 121.1(4) . . ?
C15 C14 H14A 119.4 . . ?
C13 C14 H14A 119.4 . . ?
C18 C13 C14 117.6(4) . . ?
C18 C13 P1 125.0(3) . . ?
C14 C13 P1 117.0(3) . . ?
C4 C5 C6 122.3(4) . . ?
C4 C5 H5A 118.8 . . ?
C6 C5 H5A 118.8 . . ?
C5 C4 C3 119.2(4) . . ?
C5 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
C6 C61 C63 111.6(3) . . ?
C6 C61 C62 110.5(3) . . ?
C63 C61 C62 109.9(3) . . ?
C6 C61 H61A 108.2 . . ?
C63 C61 H61A 108.2 . . ?
C62 C61 H61A 108.2 . . ?
C5 C6 C1 117.7(4) . . ?
C5 C6 C61 118.7(3) . . ?
C1 C6 C61 123.5(3) . . ?
C8 C7 C12 118.2(4) . . ?
C8 C7 P1 116.2(3) . . ?
C12 C7 P1 125.6(3) . . ?
C13 C18 C17 121.0(4) . . ?
C13 C18 H18A 119.5 . . ?
C17 C18 H18A 119.5 . . ?
C3 C2 C1 117.7(4) . . ?
C3 C2 C21 118.4(4) . . ?
C1 C2 C21 123.7(4) . . ?
C11 C12 C7 120.1(4) . . ?
C11 C12 H12A 119.9 . . ?
C7 C12 H12A 119.9 . . ?
C2 C21 C23 113.4(4) . . ?
C2 C21 C22 109.4(3) . . ?
C23 C21 C22 108.9(4) . . ?
C2 C21 H21A 108.4 . . ?
C23 C21 H21A 108.4 . . ?
C22 C21 H21A 108.4 . . ?
C12 C11 C10 121.1(5) . . ?
C12 C11 H11A 119.5 . . ?
C10 C11 H11A 119.5 . . ?
C4 C3 C2 122.3(4) . . ?
C4 C3 H3A 118.8 . . ?
C2 C3 H3A 118.8 . . ?
C6 C1 C2 120.7(4) . . ?
C6 C1 N1 119.8(3) . . ?
C2 C1 N1 119.5(3) . . ?
C15 C16 C17 119.0(4) . . ?
C15 C16 H16A 120.5 . . ?
C17 C16 H16A 120.5 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C16 C17 C18 120.6(4) . . ?
C16 C17 H17A 119.7 . . ?
C18 C17 H17A 119.7 . . ?
C14 C15 C16 120.8(4) . . ?
C14 C15 H15A 119.6 . . ?
C16 C15 H15A 119.6 . . ?
C9 C10 C11 119.5(5) . . ?
C9 C10 H10A 120.2 . . ?
C11 C10 H10A 120.2 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C9 C8 C7 120.2(4) . . ?
C9 C8 H8A 119.9 . . ?
C7 C8 H8A 119.9 . . ?
C10 C9 C8 120.9(4) . . ?
C10 C9 H9A 119.6 . . ?
C8 C9 H9A 119.6 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.067
####################################################################### 
# 
# 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_ljc-140115
_database_code_depnum_ccdc_archive 'CCDC 1424117'
_audit_update_record             
;
2015-09-12 deposited with the CCDC.
2015-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H27 Cl3 Ge N O4 P'
_chemical_formula_weight         639.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   12.5358(9)
_cell_length_b                   13.0789(9)
_cell_length_c                   17.8152(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.189(8)
_cell_angle_gamma                90.00
_cell_volume                     2855.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2859
_cell_measurement_theta_min      3.3330
_cell_measurement_theta_max      26.6070

_exptl_crystal_description       rectangular
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1304
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5960
_exptl_absorpt_correction_T_max  0.7612
_exptl_absorpt_process_details   empirical

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhanced (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 16.1093
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11876
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5595
_reflns_number_gt                4505
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisPro
_computing_cell_refinement       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0378P)²+0.1649P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'refined in a riding mode to the carrier atom'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5595
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0862
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.83596(2) 0.04029(2) 0.215490(17) 0.01860(10) Uani 1 1 d . . .
P1 P 0.70124(6) -0.09079(6) 0.30320(4) 0.01711(17) Uani 1 1 d . . .
Cl1 Cl 0.82770(7) 0.20759(6) 0.19132(5) 0.0354(2) Uani 1 1 d . . .
Cl2 Cl 0.81886(7) 0.01399(7) 0.08835(4) 0.0363(2) Uani 1 1 d . . .
Cl3 Cl 1.00336(6) -0.01805(6) 0.24269(5) 0.0310(2) Uani 1 1 d . . .
O1 O 0.70555(19) -0.04684(18) 0.46986(12) 0.0372(6) Uani 1 1 d . . .
O2 O 0.84399(19) 0.06593(17) 0.48775(11) 0.0338(6) Uani 1 1 d . . .
O3 O 0.83501(18) 0.23432(15) 0.37853(12) 0.0326(5) Uani 1 1 d . . .
O4 O 0.99680(18) 0.15497(18) 0.38826(14) 0.0416(6) Uani 1 1 d . . .
N1 N 0.72803(19) -0.06391(17) 0.21863(13) 0.0179(5) Uani 1 1 d . . .
C1 C 0.7741(2) 0.0089(2) 0.36235(16) 0.0183(6) Uani 1 1 d . . .
C2 C 0.8329(2) 0.0704(2) 0.32699(16) 0.0184(6) Uani 1 1 d . . .
C3 C 0.7694(3) 0.0059(2) 0.44550(17) 0.0226(7) Uani 1 1 d . . .
C4 C 0.9000(3) 0.1568(2) 0.36865(17) 0.0243(7) Uani 1 1 d . . .
C5 C 0.8497(3) 0.0644(3) 0.56993(18) 0.0429(10) Uani 1 1 d . . .
H5A H 0.9047 0.1137 0.5951 0.064 Uiso 1 1 calc R . .
H5B H 0.8700 -0.0043 0.5899 0.064 Uiso 1 1 calc R . .
H5C H 0.7784 0.0828 0.5803 0.064 Uiso 1 1 calc R . .
C6 C 0.8892(4) 0.3229(3) 0.4173(2) 0.0571(12) Uani 1 1 d . . .
H6A H 0.8356 0.3773 0.4178 0.086 Uiso 1 1 calc R . .
H6B H 0.9449 0.3468 0.3902 0.086 Uiso 1 1 calc R . .
H6C H 0.9238 0.3047 0.4702 0.086 Uiso 1 1 calc R . .
C11 C 0.6552(2) -0.1115(2) 0.15267(16) 0.0190(6) Uani 1 1 d . . .
C12 C 0.5586(2) -0.0606(2) 0.11880(16) 0.0224(7) Uani 1 1 d . . .
C13 C 0.4831(3) -0.1124(2) 0.06292(17) 0.0302(8) Uani 1 1 d . . .
H13A H 0.4173 -0.0788 0.0395 0.036 Uiso 1 1 calc R . .
C14 C 0.5009(3) -0.2115(3) 0.04040(18) 0.0338(8) Uani 1 1 d . . .
C15 C 0.6009(3) -0.2553(2) 0.06987(17) 0.0290(7) Uani 1 1 d . . .
H15A H 0.6167 -0.3206 0.0515 0.035 Uiso 1 1 calc R . .
C16 C 0.6801(2) -0.2071(2) 0.12589(16) 0.0220(7) Uani 1 1 d . . .
C17 C 0.5344(3) 0.0472(2) 0.13946(19) 0.0336(8) Uani 1 1 d . . .
H17A H 0.6025 0.0812 0.1640 0.050 Uiso 1 1 calc R . .
H17B H 0.4845 0.0460 0.1750 0.050 Uiso 1 1 calc R . .
H17C H 0.5004 0.0845 0.0928 0.050 Uiso 1 1 calc R . .
C18 C 0.4141(3) -0.2699(3) -0.0160(2) 0.0543(11) Uani 1 1 d . . .
H18A H 0.4252 -0.3436 -0.0076 0.081 Uiso 1 1 calc R . .
H18B H 0.4196 -0.2530 -0.0687 0.081 Uiso 1 1 calc R . .
H18C H 0.3416 -0.2509 -0.0082 0.081 Uiso 1 1 calc R . .
C19 C 0.7897(3) -0.2584(3) 0.1521(2) 0.0358(8) Uani 1 1 d . . .
H19A H 0.8467 -0.2062 0.1648 0.054 Uiso 1 1 calc R . .
H19B H 0.8047 -0.3021 0.1109 0.054 Uiso 1 1 calc R . .
H19C H 0.7887 -0.3001 0.1976 0.054 Uiso 1 1 calc R . .
C31 C 0.7574(2) -0.2094(2) 0.34457(16) 0.0201(6) Uani 1 1 d . . .
C32 C 0.7019(3) -0.2709(2) 0.38712(18) 0.0308(8) Uani 1 1 d . . .
H32A H 0.6287 -0.2554 0.3895 0.037 Uiso 1 1 calc R . .
C33 C 0.7538(3) -0.3550(3) 0.4262(2) 0.0403(9) Uani 1 1 d . . .
H33A H 0.7157 -0.3973 0.4551 0.048 Uiso 1 1 calc R . .
C34 C 0.8593(3) -0.3774(3) 0.4233(2) 0.0367(9) Uani 1 1 d . . .
H34A H 0.8940 -0.4356 0.4497 0.044 Uiso 1 1 calc R . .
C35 C 0.9155(3) -0.3161(2) 0.38224(18) 0.0319(8) Uani 1 1 d . . .
H35A H 0.9889 -0.3322 0.3806 0.038 Uiso 1 1 calc R . .
C36 C 0.8664(2) -0.2315(2) 0.34342(17) 0.0264(7) Uani 1 1 d . . .
H36A H 0.9061 -0.1886 0.3161 0.032 Uiso 1 1 calc R . .
C37 C 0.5575(2) -0.0880(2) 0.29997(16) 0.0207(6) Uani 1 1 d . . .
C38 C 0.4919(2) -0.1660(2) 0.26180(17) 0.0271(7) Uani 1 1 d . . .
H38A H 0.5244 -0.2242 0.2439 0.033 Uiso 1 1 calc R . .
C39 C 0.3800(3) -0.1589(3) 0.25009(19) 0.0370(9) Uani 1 1 d . . .
H39A H 0.3355 -0.2120 0.2238 0.044 Uiso 1 1 calc R . .
C40 C 0.3326(3) -0.0754(3) 0.2762(2) 0.0450(10) Uani 1 1 d . . .
H40A H 0.2553 -0.0705 0.2670 0.054 Uiso 1 1 calc R . .
C41 C 0.3960(3) 0.0013(3) 0.3157(2) 0.0429(9) Uani 1 1 d . . .
H41A H 0.3623 0.0580 0.3347 0.051 Uiso 1 1 calc R . .
C42 C 0.5090(3) -0.0039(3) 0.32772(19) 0.0307(8) Uani 1 1 d . . .
H42A H 0.5528 0.0492 0.3546 0.037 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.930(2) . ?
Ge1 C2 2.033(3) . ?
Ge1 Cl3 2.1890(8) . ?
Ge1 Cl1 2.2282(8) . ?
Ge1 Cl2 2.2560(8) . ?
P1 N1 1.649(2) . ?
P1 C37 1.791(3) . ?
P1 C31 1.796(3) . ?
P1 C1 1.800(3) . ?
O1 C3 1.205(3) . ?
O2 C3 1.327(3) . ?
O2 C5 1.451(4) . ?
O3 C4 1.335(4) . ?
O3 C6 1.443(4) . ?
O4 C4 1.190(4) . ?
N1 C11 1.465(3) . ?
C1 C2 1.336(4) . ?
C1 C3 1.495(4) . ?
C2 C4 1.507(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C11 C16 1.397(4) . ?
C11 C12 1.402(4) . ?
C12 C13 1.396(4) . ?
C12 C17 1.503(4) . ?
C13 C14 1.388(5) . ?
C13 H13A 0.9500 . ?
C14 C15 1.378(4) . ?
C14 C18 1.522(4) . ?
C15 C16 1.400(4) . ?
C15 H15A 0.9500 . ?
C16 C19 1.512(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C31 C32 1.388(4) . ?
C31 C36 1.401(4) . ?
C32 C33 1.389(4) . ?
C32 H32A 0.9500 . ?
C33 C34 1.366(5) . ?
C33 H33A 0.9500 . ?
C34 C35 1.375(4) . ?
C34 H34A 0.9500 . ?
C35 C36 1.379(4) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C37 C38 1.395(4) . ?
C37 C42 1.397(4) . ?
C38 C39 1.377(4) . ?
C38 H38A 0.9500 . ?
C39 C40 1.371(5) . ?
C39 H39A 0.9500 . ?
C40 C41 1.378(5) . ?
C40 H40A 0.9500 . ?
C41 C42 1.389(5) . ?
C41 H41A 0.9500 . ?
C42 H42A 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
N1 Ge1 C2 87.17(10) . . ?
N1 Ge1 Cl3 113.12(7) . . ?
C2 Ge1 Cl3 93.78(8) . . ?
N1 Ge1 Cl1 134.02(7) . . ?
C2 Ge1 Cl1 89.36(8) . . ?
Cl3 Ge1 Cl1 112.85(3) . . ?
N1 Ge1 Cl2 90.16(7) . . ?
C2 Ge1 Cl2 173.21(8) . . ?
Cl3 Ge1 Cl2 93.01(3) . . ?
Cl1 Ge1 Cl2 88.00(3) . . ?
N1 P1 C37 111.33(13) . . ?
N1 P1 C31 114.91(13) . . ?
C37 P1 C31 109.59(14) . . ?
N1 P1 C1 101.80(13) . . ?
C37 P1 C1 112.76(14) . . ?
C31 P1 C1 106.21(13) . . ?
C3 O2 C5 116.3(3) . . ?
C4 O3 C6 115.7(3) . . ?
C11 N1 P1 115.45(18) . . ?
C11 N1 Ge1 126.74(18) . . ?
P1 N1 Ge1 117.15(13) . . ?
C2 C1 C3 128.6(3) . . ?
C2 C1 P1 115.0(2) . . ?
C3 C1 P1 116.1(2) . . ?
C1 C2 C4 121.7(3) . . ?
C1 C2 Ge1 118.0(2) . . ?
C4 C2 Ge1 120.20(19) . . ?
O1 C3 O2 125.2(3) . . ?
O1 C3 C1 122.7(3) . . ?
O2 C3 C1 112.1(3) . . ?
O4 C4 O3 126.1(3) . . ?
O4 C4 C2 123.8(3) . . ?
O3 C4 C2 110.0(2) . . ?
O2 C5 H5A 109.5 . . ?
O2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O3 C6 H6A 109.5 . . ?
O3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C16 C11 C12 120.8(3) . . ?
C16 C11 N1 120.5(3) . . ?
C12 C11 N1 118.6(2) . . ?
C13 C12 C11 118.1(3) . . ?
C13 C12 C17 119.3(3) . . ?
C11 C12 C17 122.7(3) . . ?
C14 C13 C12 122.2(3) . . ?
C14 C13 H13A 118.9 . . ?
C12 C13 H13A 118.9 . . ?
C15 C14 C13 117.9(3) . . ?
C15 C14 C18 120.5(3) . . ?
C13 C14 C18 121.6(3) . . ?
C14 C15 C16 122.3(3) . . ?
C14 C15 H15A 118.8 . . ?
C16 C15 H15A 118.8 . . ?
C11 C16 C15 118.1(3) . . ?
C11 C16 C19 123.0(3) . . ?
C15 C16 C19 118.8(3) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C32 C31 C36 119.4(3) . . ?
C32 C31 P1 121.7(2) . . ?
C36 C31 P1 118.1(2) . . ?
C31 C32 C33 119.8(3) . . ?
C31 C32 H32A 120.1 . . ?
C33 C32 H32A 120.1 . . ?
C34 C33 C32 120.4(3) . . ?
C34 C33 H33A 119.8 . . ?
C32 C33 H33A 119.8 . . ?
C33 C34 C35 120.3(3) . . ?
C33 C34 H34A 119.9 . . ?
C35 C34 H34A 119.9 . . ?
C34 C35 C36 120.6(3) . . ?
C34 C35 H35A 119.7 . . ?
C36 C35 H35A 119.7 . . ?
C35 C36 C31 119.5(3) . . ?
C35 C36 H36A 120.3 . . ?
C31 C36 H36A 120.3 . . ?
C38 C37 C42 119.5(3) . . ?
C38 C37 P1 119.1(2) . . ?
C42 C37 P1 121.0(2) . . ?
C39 C38 C37 120.1(3) . . ?
C39 C38 H38A 119.9 . . ?
C37 C38 H38A 119.9 . . ?
C40 C39 C38 120.2(3) . . ?
C40 C39 H39A 119.9 . . ?
C38 C39 H39A 119.9 . . ?
C39 C40 C41 120.6(3) . . ?
C39 C40 H40A 119.7 . . ?
C41 C40 H40A 119.7 . . ?
C40 C41 C42 120.1(3) . . ?
C40 C41 H41A 119.9 . . ?
C42 C41 H41A 119.9 . . ?
C41 C42 C37 119.4(3) . . ?
C41 C42 H42A 120.3 . . ?
C37 C42 H42A 120.3 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.076
####################################################################### 
# 
# 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_yy-140925
_database_code_depnum_ccdc_archive 'CCDC 1424118'
_audit_update_record             
;
2015-09-12 deposited with the CCDC.
2015-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H42 Ge N O4 P'
_chemical_formula_weight         620.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.5333(6)
_cell_length_b                   10.8401(5)
_cell_length_c                   15.5515(6)
_cell_angle_alpha                80.549(4)
_cell_angle_beta                 86.245(4)
_cell_angle_gamma                68.059(5)
_cell_volume                     1624.71(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5276
_cell_measurement_theta_min      3.5480
_cell_measurement_theta_max      28.6090

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             652
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8611
_exptl_absorpt_correction_T_max  0.8611
_exptl_absorpt_process_details   empirical

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11102
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6372
_reflns_number_gt                5681
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0340P)²+0.6661P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'refined in a riding mode to the carrier atom'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6372
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0781
_refine_ls_wR_factor_gt          0.0760
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.27659(2) 0.286906(19) 0.280437(14) 0.03005(8) Uani 1 1 d . . .
P1 P 0.56934(4) -0.02567(4) 0.22486(3) 0.01639(10) Uani 1 1 d . . .
N1 N 0.61108(15) -0.05953(14) 0.32198(9) 0.0213(3) Uani 1 1 d . . .
O1 O 0.60677(14) 0.19086(16) 0.02669(9) 0.0388(4) Uani 1 1 d . . .
O2 O 0.33170(17) 0.45879(14) 0.09366(10) 0.0416(4) Uani 1 1 d . . .
O3 O 0.74732(14) 0.16737(15) 0.13434(9) 0.0362(3) Uani 1 1 d . . .
O4 O 0.51364(15) 0.43374(14) 0.17106(10) 0.0392(4) Uani 1 1 d . . .
C1 C 0.53539(17) 0.14931(17) 0.17391(11) 0.0186(3) Uani 1 1 d . . .
C2 C 0.43176(18) 0.25783(17) 0.19532(11) 0.0219(4) Uani 1 1 d . . .
C3 C 0.63180(18) 0.17094(16) 0.10241(11) 0.0215(4) Uani 1 1 d . . .
C4 C 0.42011(19) 0.39318(18) 0.14612(12) 0.0260(4) Uani 1 1 d . . .
C5 C 0.8414(2) 0.1985(3) 0.07031(17) 0.0515(6) Uani 1 1 d . . .
H5A H 0.9173 0.2049 0.1001 0.077 Uiso 1 1 calc R . .
H5B H 0.7933 0.2844 0.0337 0.077 Uiso 1 1 calc R . .
H5C H 0.8772 0.1271 0.0338 0.077 Uiso 1 1 calc R . .
C6 C 0.5060(3) 0.5674(2) 0.13096(18) 0.0552(7) Uani 1 1 d . . .
H6A H 0.5744 0.5907 0.1574 0.083 Uiso 1 1 calc R . .
H6B H 0.4145 0.6331 0.1403 0.083 Uiso 1 1 calc R . .
H6C H 0.5240 0.5684 0.0683 0.083 Uiso 1 1 calc R . .
C7 C 0.2480(3) 0.4627(2) 0.31046(17) 0.0480(6) Uani 1 1 d . . .
H7A H 0.1759 0.4848 0.3548 0.072 Uiso 1 1 calc R . .
H7B H 0.2206 0.5308 0.2583 0.072 Uiso 1 1 calc R . .
H7C H 0.3332 0.4612 0.3334 0.072 Uiso 1 1 calc R . .
C8 C 0.1199(2) 0.2990(3) 0.21559(19) 0.0546(7) Uani 1 1 d . . .
H8A H 0.0382 0.3228 0.2528 0.082 Uiso 1 1 calc R . .
H8B H 0.1367 0.2120 0.1971 0.082 Uiso 1 1 calc R . .
H8C H 0.1059 0.3682 0.1641 0.082 Uiso 1 1 calc R . .
C9 C 0.3115(3) 0.1578(2) 0.38574(15) 0.0531(7) Uani 1 1 d . . .
H9A H 0.2808 0.2052 0.4362 0.080 Uiso 1 1 calc R . .
H9B H 0.4099 0.1047 0.3906 0.080 Uiso 1 1 calc R . .
H9C H 0.2617 0.0979 0.3839 0.080 Uiso 1 1 calc R . .
C11 C 0.73879(17) -0.12927(17) 0.36258(10) 0.0198(4) Uani 1 1 d . . .
C12 C 0.81403(19) -0.05785(18) 0.38819(11) 0.0242(4) Uani 1 1 d . . .
C13 C 0.9375(2) -0.1292(2) 0.43165(13) 0.0329(4) Uani 1 1 d . . .
H13A H 0.9886 -0.0815 0.4490 0.039 Uiso 1 1 calc R . .
C14 C 0.9871(2) -0.2683(2) 0.45000(14) 0.0384(5) Uani 1 1 d . . .
H14A H 1.0714 -0.3155 0.4798 0.046 Uiso 1 1 calc R . .
C15 C 0.9136(2) -0.3375(2) 0.42487(13) 0.0341(5) Uani 1 1 d . . .
H15A H 0.9481 -0.4330 0.4377 0.041 Uiso 1 1 calc R . .
C16 C 0.78958(19) -0.27139(18) 0.38096(11) 0.0253(4) Uani 1 1 d . . .
C17 C 0.69384(17) -0.12802(16) 0.15264(11) 0.0188(3) Uani 1 1 d . . .
C18 C 0.83248(18) -0.15378(18) 0.16479(12) 0.0246(4) Uani 1 1 d . . .
H18A H 0.8583 -0.1108 0.2054 0.030 Uiso 1 1 calc R . .
C19 C 0.9324(2) -0.2417(2) 0.11793(13) 0.0321(4) Uani 1 1 d . . .
H19A H 1.0264 -0.2591 0.1267 0.038 Uiso 1 1 calc R . .
C20 C 0.8955(2) -0.3041(2) 0.05840(14) 0.0339(5) Uani 1 1 d . . .
H20A H 0.9641 -0.3641 0.0263 0.041 Uiso 1 1 calc R . .
C21 C 0.7591(2) -0.27917(19) 0.04549(13) 0.0315(4) Uani 1 1 d . . .
H21A H 0.7341 -0.3219 0.0044 0.038 Uiso 1 1 calc R . .
C22 C 0.65816(19) -0.19156(17) 0.09262(11) 0.0234(4) Uani 1 1 d . . .
H22A H 0.5645 -0.1751 0.0837 0.028 Uiso 1 1 calc R . .
C23 C 0.40950(17) -0.04613(18) 0.21249(12) 0.0239(4) Uani 1 1 d . . .
C24 C 0.3603(2) -0.1159(2) 0.28148(15) 0.0372(5) Uani 1 1 d . . .
H24A H 0.4084 -0.1498 0.3351 0.045 Uiso 1 1 calc R . .
C25 C 0.2390(3) -0.1351(3) 0.2701(2) 0.0611(8) Uani 1 1 d . . .
H25A H 0.2039 -0.1822 0.3165 0.073 Uiso 1 1 calc R . .
C26 C 0.1696(3) -0.0860(3) 0.1922(3) 0.0696(10) Uani 1 1 d . . .
H26A H 0.0865 -0.0987 0.1854 0.083 Uiso 1 1 calc R . .
C27 C 0.2193(2) -0.0192(3) 0.1245(2) 0.0555(8) Uani 1 1 d . . .
H27A H 0.1718 0.0124 0.0706 0.067 Uiso 1 1 calc R . .
C28 C 0.33828(19) 0.0025(2) 0.13420(14) 0.0348(5) Uani 1 1 d . . .
H28A H 0.3715 0.0506 0.0874 0.042 Uiso 1 1 calc R . .
C121 C 0.7607(2) 0.09472(19) 0.36938(13) 0.0308(4) Uani 1 1 d . . .
H12A H 0.6896 0.1242 0.3230 0.037 Uiso 1 1 calc R . .
C122 C 0.6914(3) 0.1549(2) 0.45036(18) 0.0550(7) Uani 1 1 d . . .
H12B H 0.6177 0.1221 0.4696 0.082 Uiso 1 1 calc R . .
H12C H 0.6533 0.2532 0.4363 0.082 Uiso 1 1 calc R . .
H12D H 0.7589 0.1279 0.4971 0.082 Uiso 1 1 calc R . .
C123 C 0.8715(3) 0.1492(2) 0.33578(16) 0.0454(6) Uani 1 1 d . . .
H12E H 0.9191 0.1051 0.2864 0.068 Uiso 1 1 calc R . .
H12F H 0.9372 0.1310 0.3824 0.068 Uiso 1 1 calc R . .
H12G H 0.8296 0.2464 0.3169 0.068 Uiso 1 1 calc R . .
C161 C 0.7109(2) -0.35149(18) 0.35505(13) 0.0315(4) Uani 1 1 d . . .
H16A H 0.6389 -0.2895 0.3127 0.038 Uiso 1 1 calc R . .
C162 C 0.6379(3) -0.3997(3) 0.43354(17) 0.0518(6) Uani 1 1 d . . .
H16B H 0.5766 -0.3221 0.4596 0.078 Uiso 1 1 calc R . .
H16C H 0.7057 -0.4604 0.4767 0.078 Uiso 1 1 calc R . .
H16D H 0.5845 -0.4476 0.4148 0.078 Uiso 1 1 calc R . .
C163 C 0.8009(3) -0.4692(2) 0.30955(17) 0.0504(6) Uani 1 1 d . . .
H16E H 0.8442 -0.4355 0.2582 0.076 Uiso 1 1 calc R . .
H16F H 0.7445 -0.5146 0.2915 0.076 Uiso 1 1 calc R . .
H16G H 0.8718 -0.5329 0.3498 0.076 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C9 1.928(2) . ?
Ge1 C8 1.942(3) . ?
Ge1 C7 1.946(2) . ?
Ge1 C2 1.9979(17) . ?
P1 N1 1.5471(15) . ?
P1 C23 1.8045(18) . ?
P1 C17 1.8279(17) . ?
P1 C1 1.8413(17) . ?
N1 C11 1.405(2) . ?
O1 C3 1.191(2) . ?
O2 C4 1.205(2) . ?
O3 C3 1.329(2) . ?
O3 C5 1.448(2) . ?
O4 C4 1.321(2) . ?
O4 C6 1.455(2) . ?
C1 C2 1.344(2) . ?
C1 C3 1.506(2) . ?
C2 C4 1.504(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.410(3) . ?
C11 C16 1.414(2) . ?
C12 C13 1.392(3) . ?
C12 C121 1.518(3) . ?
C13 C14 1.385(3) . ?
C13 H13A 0.9500 . ?
C14 C15 1.373(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.394(3) . ?
C15 H15A 0.9500 . ?
C16 C161 1.517(3) . ?
C17 C22 1.392(2) . ?
C17 C18 1.400(2) . ?
C18 C19 1.388(3) . ?
C18 H18A 0.9500 . ?
C19 C20 1.384(3) . ?
C19 H19A 0.9500 . ?
C20 C21 1.381(3) . ?
C20 H20A 0.9500 . ?
C21 C22 1.394(3) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 C28 1.391(3) . ?
C23 C24 1.395(3) . ?
C24 C25 1.395(3) . ?
C24 H24A 0.9500 . ?
C25 C26 1.379(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.366(4) . ?
C26 H26A 0.9500 . ?
C27 C28 1.381(3) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
C121 C123 1.522(3) . ?
C121 C122 1.529(3) . ?
C121 H12A 1.0000 . ?
C122 H12B 0.9800 . ?
C122 H12C 0.9800 . ?
C122 H12D 0.9800 . ?
C123 H12E 0.9800 . ?
C123 H12F 0.9800 . ?
C123 H12G 0.9800 . ?
C161 C162 1.523(3) . ?
C161 C163 1.527(3) . ?
C161 H16A 1.0000 . ?
C162 H16B 0.9800 . ?
C162 H16C 0.9800 . ?
C162 H16D 0.9800 . ?
C163 H16E 0.9800 . ?
C163 H16F 0.9800 . ?
C163 H16G 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 Ge1 C8 113.54(13) . . ?
C9 Ge1 C7 108.81(11) . . ?
C8 Ge1 C7 109.34(11) . . ?
C9 Ge1 C2 115.53(9) . . ?
C8 Ge1 C2 106.02(9) . . ?
C7 Ge1 C2 102.99(9) . . ?
N1 P1 C23 110.34(9) . . ?
N1 P1 C17 114.77(8) . . ?
C23 P1 C17 107.16(8) . . ?
N1 P1 C1 115.57(8) . . ?
C23 P1 C1 103.38(8) . . ?
C17 P1 C1 104.68(8) . . ?
C11 N1 P1 131.47(12) . . ?
C3 O3 C5 115.34(16) . . ?
C4 O4 C6 115.97(17) . . ?
C2 C1 C3 118.07(15) . . ?
C2 C1 P1 125.18(13) . . ?
C3 C1 P1 116.74(12) . . ?
C1 C2 C4 117.61(16) . . ?
C1 C2 Ge1 134.76(13) . . ?
C4 C2 Ge1 107.62(11) . . ?
O1 C3 O3 124.19(16) . . ?
O1 C3 C1 124.19(16) . . ?
O3 C3 C1 111.61(15) . . ?
O2 C4 O4 124.52(17) . . ?
O2 C4 C2 123.72(18) . . ?
O4 C4 C2 111.66(16) . . ?
O3 C5 H5A 109.5 . . ?
O3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O4 C6 H6A 109.5 . . ?
O4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Ge1 C7 H7A 109.5 . . ?
Ge1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Ge1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Ge1 C8 H8A 109.5 . . ?
Ge1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Ge1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Ge1 C9 H9A 109.5 . . ?
Ge1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Ge1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C11 C12 120.20(15) . . ?
N1 C11 C16 119.92(16) . . ?
C12 C11 C16 119.84(16) . . ?
C13 C12 C11 119.05(17) . . ?
C13 C12 C121 120.42(18) . . ?
C11 C12 C121 120.53(16) . . ?
C14 C13 C12 121.17(19) . . ?
C14 C13 H13A 119.4 . . ?
C12 C13 H13A 119.4 . . ?
C15 C14 C13 119.62(18) . . ?
C15 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
C14 C15 C16 121.66(18) . . ?
C14 C15 H15A 119.2 . . ?
C16 C15 H15A 119.2 . . ?
C15 C16 C11 118.66(18) . . ?
C15 C16 C161 120.04(17) . . ?
C11 C16 C161 121.29(16) . . ?
C22 C17 C18 118.91(15) . . ?
C22 C17 P1 122.91(13) . . ?
C18 C17 P1 117.87(13) . . ?
C19 C18 C17 120.41(17) . . ?
C19 C18 H18A 119.8 . . ?
C17 C18 H18A 119.8 . . ?
C20 C19 C18 120.06(18) . . ?
C20 C19 H19A 120.0 . . ?
C18 C19 H19A 120.0 . . ?
C21 C20 C19 120.15(17) . . ?
C21 C20 H20A 119.9 . . ?
C19 C20 H20A 119.9 . . ?
C20 C21 C22 120.14(18) . . ?
C20 C21 H21A 119.9 . . ?
C22 C21 H21A 119.9 . . ?
C17 C22 C21 120.33(17) . . ?
C17 C22 H22A 119.8 . . ?
C21 C22 H22A 119.8 . . ?
C28 C23 C24 120.10(19) . . ?
C28 C23 P1 120.71(15) . . ?
C24 C23 P1 119.15(16) . . ?
C23 C24 C25 118.6(2) . . ?
C23 C24 H24A 120.7 . . ?
C25 C24 H24A 120.7 . . ?
C26 C25 C24 120.5(3) . . ?
C26 C25 H25A 119.8 . . ?
C24 C25 H25A 119.8 . . ?
C27 C26 C25 120.6(2) . . ?
C27 C26 H26A 119.7 . . ?
C25 C26 H26A 119.7 . . ?
C26 C27 C28 120.2(3) . . ?
C26 C27 H27A 119.9 . . ?
C28 C27 H27A 119.9 . . ?
C27 C28 C23 120.0(2) . . ?
C27 C28 H28A 120.0 . . ?
C23 C28 H28A 120.0 . . ?
C12 C121 C123 112.84(17) . . ?
C12 C121 C122 110.43(17) . . ?
C123 C121 C122 110.48(18) . . ?
C12 C121 H12A 107.6 . . ?
C123 C121 H12A 107.6 . . ?
C122 C121 H12A 107.6 . . ?
C121 C122 H12B 109.5 . . ?
C121 C122 H12C 109.5 . . ?
H12B C122 H12C 109.5 . . ?
C121 C122 H12D 109.5 . . ?
H12B C122 H12D 109.5 . . ?
H12C C122 H12D 109.5 . . ?
C121 C123 H12E 109.5 . . ?
C121 C123 H12F 109.5 . . ?
H12E C123 H12F 109.5 . . ?
C121 C123 H12G 109.5 . . ?
H12E C123 H12G 109.5 . . ?
H12F C123 H12G 109.5 . . ?
C16 C161 C162 110.91(17) . . ?
C16 C161 C163 112.67(18) . . ?
C162 C161 C163 110.87(18) . . ?
C16 C161 H16A 107.4 . . ?
C162 C161 H16A 107.4 . . ?
C163 C161 H16A 107.4 . . ?
C161 C162 H16B 109.5 . . ?
C161 C162 H16C 109.5 . . ?
H16B C162 H16C 109.5 . . ?
C161 C162 H16D 109.5 . . ?
H16B C162 H16D 109.5 . . ?
H16C C162 H16D 109.5 . . ?
C161 C163 H16E 109.5 . . ?
C161 C163 H16F 109.5 . . ?
H16E C163 H16F 109.5 . . ?
C161 C163 H16G 109.5 . . ?
H16E C163 H16G 109.5 . . ?
H16F C163 H16G 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.048
####################################################################### 
# 
# 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_yy-141001
_database_code_depnum_ccdc_archive 'CCDC 1424119'
_audit_update_record             
;
2015-09-12 deposited with the CCDC.
2015-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H40 Ge N O2 P'
_chemical_formula_weight         562.20

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'
P P 0.2955 0.4335 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.4190(2)
_cell_length_b                   21.2619(2)
_cell_length_c                   13.0010(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.5730(10)
_cell_angle_gamma                90.00
_cell_volume                     3121.24(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8042
_cell_measurement_theta_min      4.0270
_cell_measurement_theta_max      60.3030

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184
_exptl_absorpt_coefficient_mu    2.007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5006
_exptl_absorpt_correction_T_max  0.6896
_exptl_absorpt_process_details   empirical

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12237
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.02
_diffrn_reflns_theta_max         60.18
_reflns_number_total             4627
_reflns_number_gt                4439
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0475P)²+0.8557P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'refined in a riding mode to the carrier atom'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4627
_refine_ls_number_parameters     333
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0775
_refine_ls_wR_factor_gt          0.0766
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.868500(17) 0.237858(9) 0.142774(14) 0.03633(9) Uani 1 1 d . . .
P1 P 1.17105(3) 0.165158(19) 0.12453(3) 0.02912(12) Uani 1 1 d . . .
N1 N 1.18230(12) 0.14168(6) 0.23811(10) 0.0338(3) Uani 1 1 d . . .
O1 O 0.74257(12) 0.19112(7) -0.06560(11) 0.0539(4) Uani 1 1 d . . .
O2 O 0.83847(11) 0.10138(6) -0.07990(10) 0.0450(3) Uani 1 1 d . . .
C1 C 1.03056(15) 0.15158(8) 0.04051(12) 0.0321(3) Uani 1 1 d . . .
H1B H 1.0339 0.1236 -0.0160 0.038 Uiso 1 1 calc R . .
C2 C 0.92385(14) 0.17535(7) 0.04712(12) 0.0305(3) Uani 1 1 d . . .
C3 C 0.82525(14) 0.15739(8) -0.03744(12) 0.0326(4) Uani 1 1 d . . .
C4 C 0.75113(17) 0.08502(10) -0.16816(15) 0.0482(5) Uani 1 1 d . . .
H4A H 0.7712 0.0442 -0.1959 0.072 Uiso 1 1 calc R . .
H4B H 0.7501 0.1173 -0.2222 0.072 Uiso 1 1 calc R . .
H4C H 0.6728 0.0825 -0.1462 0.072 Uiso 1 1 calc R . .
C5 C 0.7152(3) 0.20999(17) 0.1700(3) 0.0981(11) Uani 1 1 d . . .
H5A H 0.6940 0.2328 0.2302 0.147 Uiso 1 1 calc R . .
H5B H 0.7180 0.1648 0.1848 0.147 Uiso 1 1 calc R . .
H5C H 0.6558 0.2183 0.1090 0.147 Uiso 1 1 calc R . .
C6 C 0.8546(3) 0.31746(11) 0.0713(2) 0.0742(7) Uani 1 1 d . . .
H6A H 0.8199 0.3486 0.1135 0.111 Uiso 1 1 calc R . .
H6B H 0.8037 0.3126 0.0041 0.111 Uiso 1 1 calc R . .
H6C H 0.9333 0.3317 0.0598 0.111 Uiso 1 1 calc R . .
C7 C 0.9669(3) 0.24591(14) 0.27638(18) 0.0727(8) Uani 1 1 d . . .
H7A H 0.9167 0.2471 0.3313 0.109 Uiso 1 1 calc R . .
H7B H 1.0130 0.2849 0.2780 0.109 Uiso 1 1 calc R . .
H7C H 1.0208 0.2099 0.2876 0.109 Uiso 1 1 calc R . .
C11 C 1.20880(15) 0.08511(7) 0.29100(11) 0.0306(3) Uani 1 1 d . . .
C12 C 1.32727(16) 0.07038(8) 0.33142(13) 0.0375(4) Uani 1 1 d . . .
C13 C 1.34932(18) 0.01794(9) 0.39603(14) 0.0459(4) Uani 1 1 d . . .
H13A H 1.4289 0.0075 0.4229 0.055 Uiso 1 1 calc R . .
C14 C 1.25938(19) -0.01906(9) 0.42198(14) 0.0470(5) Uani 1 1 d . . .
H14A H 1.2766 -0.0537 0.4679 0.056 Uiso 1 1 calc R . .
C15 C 1.14424(17) -0.00527(8) 0.38070(13) 0.0406(4) Uani 1 1 d . . .
H15A H 1.0822 -0.0313 0.3975 0.049 Uiso 1 1 calc R . .
C16 C 1.11667(15) 0.04584(8) 0.31496(12) 0.0326(4) Uani 1 1 d . . .
C17 C 1.19547(16) 0.24878(8) 0.12602(14) 0.0353(4) Uani 1 1 d . . .
C18 C 1.2463(3) 0.27787(10) 0.21607(17) 0.0659(7) Uani 1 1 d . . .
H18A H 1.2666 0.2539 0.2778 0.079 Uiso 1 1 calc R . .
C19 C 1.2681(3) 0.34187(12) 0.2175(2) 0.0897(10) Uani 1 1 d . . .
H19A H 1.3026 0.3616 0.2803 0.108 Uiso 1 1 calc R . .
C20 C 1.2403(3) 0.37657(10) 0.1296(2) 0.0712(7) Uani 1 1 d . . .
H20A H 1.2557 0.4205 0.1309 0.085 Uiso 1 1 calc R . .
C21 C 1.1908(2) 0.34870(10) 0.03993(19) 0.0604(6) Uani 1 1 d . . .
H21A H 1.1720 0.3731 -0.0215 0.072 Uiso 1 1 calc R . .
C22 C 1.16729(17) 0.28456(9) 0.03743(14) 0.0443(4) Uani 1 1 d . . .
H22A H 1.1317 0.2653 -0.0255 0.053 Uiso 1 1 calc R . .
C23 C 1.27493(14) 0.13136(8) 0.04691(12) 0.0338(4) Uani 1 1 d . . .
C24 C 1.26164(15) 0.06866(9) 0.01611(14) 0.0406(4) Uani 1 1 d . . .
H24A H 1.1955 0.0453 0.0316 0.049 Uiso 1 1 calc R . .
C25 C 1.34380(17) 0.04007(10) -0.03671(16) 0.0495(5) Uani 1 1 d . . .
H25A H 1.3337 -0.0026 -0.0578 0.059 Uiso 1 1 calc R . .
C26 C 1.44029(17) 0.07359(11) -0.05871(17) 0.0535(5) Uani 1 1 d . . .
H26A H 1.4964 0.0540 -0.0954 0.064 Uiso 1 1 calc R . .
C27 C 1.45585(17) 0.13516(11) -0.02793(17) 0.0532(5) Uani 1 1 d . . .
H27A H 1.5230 0.1579 -0.0428 0.064 Uiso 1 1 calc R . .
C28 C 1.37377(16) 0.16431(10) 0.02482(15) 0.0438(4) Uani 1 1 d . . .
H28A H 1.3850 0.2069 0.0460 0.053 Uiso 1 1 calc R . .
C121 C 1.43007(17) 0.11105(10) 0.31019(16) 0.0488(5) Uani 1 1 d . . .
H12A H 1.3983 0.1421 0.2553 0.059 Uiso 1 1 calc R . .
C122 C 1.5251(2) 0.07296(15) 0.2683(3) 0.0826(8) Uani 1 1 d . . .
H12B H 1.4906 0.0517 0.2040 0.124 Uiso 1 1 calc R . .
H12C H 1.5574 0.0415 0.3200 0.124 Uiso 1 1 calc R . .
H12D H 1.5887 0.1011 0.2538 0.124 Uiso 1 1 calc R . .
C123 C 1.4810(3) 0.14827(14) 0.4069(2) 0.0797(8) Uani 1 1 d . . .
H12E H 1.4186 0.1743 0.4293 0.120 Uiso 1 1 calc R . .
H12F H 1.5452 0.1754 0.3906 0.120 Uiso 1 1 calc R . .
H12G H 1.5119 0.1191 0.4627 0.120 Uiso 1 1 calc R . .
C161 C 0.98918(16) 0.05864(9) 0.26910(14) 0.0392(4) Uani 1 1 d . . .
H16A H 0.9857 0.1022 0.2397 0.047 Uiso 1 1 calc R . .
C162 C 0.9050(2) 0.05648(13) 0.34976(19) 0.0652(6) Uani 1 1 d . . .
H16B H 0.9314 0.0865 0.4056 0.098 Uiso 1 1 calc R . .
H16C H 0.9046 0.0140 0.3789 0.098 Uiso 1 1 calc R . .
H16D H 0.8249 0.0676 0.3166 0.098 Uiso 1 1 calc R . .
C163 C 0.9494(2) 0.01380(12) 0.17971(19) 0.0644(6) Uani 1 1 d . . .
H16E H 1.0038 0.0168 0.1283 0.097 Uiso 1 1 calc R . .
H16F H 0.8692 0.0250 0.1469 0.097 Uiso 1 1 calc R . .
H16G H 0.9496 -0.0293 0.2063 0.097 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C6 1.926(2) . ?
Ge1 C7 1.930(2) . ?
Ge1 C5 1.930(3) . ?
Ge1 C2 1.9867(16) . ?
P1 N1 1.5458(14) . ?
P1 C17 1.7993(18) . ?
P1 C23 1.8162(17) . ?
P1 C1 1.8242(16) . ?
N1 C11 1.396(2) . ?
O1 C3 1.199(2) . ?
O2 C3 1.331(2) . ?
O2 C4 1.446(2) . ?
C1 C2 1.334(2) . ?
C1 H1B 0.9500 . ?
C2 C3 1.501(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 C12 1.411(2) . ?
C11 C16 1.414(2) . ?
C12 C13 1.396(3) . ?
C12 C121 1.516(3) . ?
C13 C14 1.375(3) . ?
C13 H13A 0.9500 . ?
C14 C15 1.376(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.389(3) . ?
C15 H15A 0.9500 . ?
C16 C161 1.513(3) . ?
C17 C18 1.374(3) . ?
C17 C22 1.378(3) . ?
C18 C19 1.383(3) . ?
C18 H18A 0.9500 . ?
C19 C20 1.358(4) . ?
C19 H19A 0.9500 . ?
C20 C21 1.354(4) . ?
C20 H20A 0.9500 . ?
C21 C22 1.389(3) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 C24 1.394(3) . ?
C23 C28 1.394(3) . ?
C24 C25 1.383(3) . ?
C24 H24A 0.9500 . ?
C25 C26 1.378(3) . ?
C25 H25A 0.9500 . ?
C26 C27 1.373(3) . ?
C26 H26A 0.9500 . ?
C27 C28 1.387(3) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
C121 C122 1.519(4) . ?
C121 C123 1.525(3) . ?
C121 H12A 1.0000 . ?
C122 H12B 0.9800 . ?
C122 H12C 0.9800 . ?
C122 H12D 0.9800 . ?
C123 H12E 0.9800 . ?
C123 H12F 0.9800 . ?
C123 H12G 0.9800 . ?
C161 C163 1.519(3) . ?
C161 C162 1.526(3) . ?
C161 H16A 1.0000 . ?
C162 H16B 0.9800 . ?
C162 H16C 0.9800 . ?
C162 H16D 0.9800 . ?
C163 H16E 0.9800 . ?
C163 H16F 0.9800 . ?
C163 H16G 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 Ge1 C7 110.57(13) . . ?
C6 Ge1 C5 110.30(16) . . ?
C7 Ge1 C5 106.49(15) . . ?
C6 Ge1 C2 107.25(9) . . ?
C7 Ge1 C2 115.20(9) . . ?
C5 Ge1 C2 106.94(10) . . ?
N1 P1 C17 108.55(8) . . ?
N1 P1 C23 115.78(8) . . ?
C17 P1 C23 106.49(8) . . ?
N1 P1 C1 117.48(8) . . ?
C17 P1 C1 106.50(8) . . ?
C23 P1 C1 101.16(7) . . ?
C11 N1 P1 136.86(12) . . ?
C3 O2 C4 115.90(14) . . ?
C2 C1 P1 129.18(13) . . ?
C2 C1 H1B 115.4 . . ?
P1 C1 H1B 115.4 . . ?
C1 C2 C3 116.69(14) . . ?
C1 C2 Ge1 132.29(13) . . ?
C3 C2 Ge1 110.78(11) . . ?
O1 C3 O2 122.81(15) . . ?
O1 C3 C2 122.83(16) . . ?
O2 C3 C2 114.35(14) . . ?
O2 C4 H4A 109.5 . . ?
O2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Ge1 C5 H5A 109.5 . . ?
Ge1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Ge1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Ge1 C6 H6A 109.5 . . ?
Ge1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Ge1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Ge1 C7 H7A 109.5 . . ?
Ge1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Ge1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C11 C12 119.99(15) . . ?
N1 C11 C16 120.24(15) . . ?
C12 C11 C16 119.36(15) . . ?
C13 C12 C11 118.56(16) . . ?
C13 C12 C121 119.34(16) . . ?
C11 C12 C121 122.06(15) . . ?
C14 C13 C12 122.02(18) . . ?
C14 C13 H13A 119.0 . . ?
C12 C13 H13A 119.0 . . ?
C13 C14 C15 119.19(16) . . ?
C13 C14 H14A 120.4 . . ?
C15 C14 H14A 120.4 . . ?
C14 C15 C16 121.50(17) . . ?
C14 C15 H15A 119.2 . . ?
C16 C15 H15A 119.2 . . ?
C15 C16 C11 119.32(16) . . ?
C15 C16 C161 119.98(15) . . ?
C11 C16 C161 120.70(15) . . ?
C18 C17 C22 118.69(18) . . ?
C18 C17 P1 119.94(14) . . ?
C22 C17 P1 121.34(14) . . ?
C17 C18 C19 120.4(2) . . ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 . . ?
C20 C19 C18 120.3(2) . . ?
C20 C19 H19A 119.9 . . ?
C18 C19 H19A 119.9 . . ?
C21 C20 C19 120.1(2) . . ?
C21 C20 H20A 119.9 . . ?
C19 C20 H20A 119.9 . . ?
C20 C21 C22 120.28(19) . . ?
C20 C21 H21A 119.9 . . ?
C22 C21 H21A 119.9 . . ?
C17 C22 C21 120.14(19) . . ?
C17 C22 H22A 119.9 . . ?
C21 C22 H22A 119.9 . . ?
C24 C23 C28 118.57(17) . . ?
C24 C23 P1 119.07(13) . . ?
C28 C23 P1 122.11(14) . . ?
C25 C24 C23 120.68(18) . . ?
C25 C24 H24A 119.7 . . ?
C23 C24 H24A 119.7 . . ?
C26 C25 C24 119.88(19) . . ?
C26 C25 H25A 120.1 . . ?
C24 C25 H25A 120.1 . . ?
C27 C26 C25 120.38(19) . . ?
C27 C26 H26A 119.8 . . ?
C25 C26 H26A 119.8 . . ?
C26 C27 C28 120.16(19) . . ?
C26 C27 H27A 119.9 . . ?
C28 C27 H27A 119.9 . . ?
C27 C28 C23 120.32(18) . . ?
C27 C28 H28A 119.8 . . ?
C23 C28 H28A 119.8 . . ?
C12 C121 C122 112.05(19) . . ?
C12 C121 C123 110.88(18) . . ?
C122 C121 C123 111.5(2) . . ?
C12 C121 H12A 107.4 . . ?
C122 C121 H12A 107.4 . . ?
C123 C121 H12A 107.4 . . ?
C121 C122 H12B 109.5 . . ?
C121 C122 H12C 109.5 . . ?
H12B C122 H12C 109.5 . . ?
C121 C122 H12D 109.5 . . ?
H12B C122 H12D 109.5 . . ?
H12C C122 H12D 109.5 . . ?
C121 C123 H12E 109.5 . . ?
C121 C123 H12F 109.5 . . ?
H12E C123 H12F 109.5 . . ?
C121 C123 H12G 109.5 . . ?
H12E C123 H12G 109.5 . . ?
H12F C123 H12G 109.5 . . ?
C16 C161 C163 110.41(16) . . ?
C16 C161 C162 113.06(16) . . ?
C163 C161 C162 111.08(18) . . ?
C16 C161 H16A 107.3 . . ?
C163 C161 H16A 107.3 . . ?
C162 C161 H16A 107.3 . . ?
C161 C162 H16B 109.5 . . ?
C161 C162 H16C 109.5 . . ?
H16B C162 H16C 109.5 . . ?
C161 C162 H16D 109.5 . . ?
H16B C162 H16D 109.5 . . ?
H16C C162 H16D 109.5 . . ?
C161 C163 H16E 109.5 . . ?
C161 C163 H16F 109.5 . . ?
H16E C163 H16F 109.5 . . ?
C161 C163 H16G 109.5 . . ?
H16E C163 H16G 109.5 . . ?
H16F C163 H16G 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        60.18
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.046
####################################################################### 
# 
# 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_yy-140903
_database_code_depnum_ccdc_archive 'CCDC 1424120'
_audit_update_record             
;
2015-09-12 deposited with the CCDC.
2015-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H84 N2 O8 P2 Sn2'
_chemical_formula_weight         1332.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.0403(5)
_cell_length_b                   18.5444(9)
_cell_length_c                   18.9549(11)
_cell_angle_alpha                119.182(6)
_cell_angle_beta                 102.169(4)
_cell_angle_gamma                93.335(4)
_cell_volume                     3252.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8171
_cell_measurement_theta_min      3.3440
_cell_measurement_theta_max      28.0750

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8806
_exptl_absorpt_correction_T_max  0.8806
_exptl_absorpt_process_details   empirical

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24079
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         26.00
_reflns_number_total             12787
_reflns_number_gt                10721
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0288P)²+1.0080P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'refined in riding mode to the carrier atom'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12787
_refine_ls_number_parameters     739
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.0788
_refine_ls_wR_factor_gt          0.0747
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.464654(19) 0.221173(12) 0.236650(12) 0.02365(6) Uani 1 1 d . . .
P1 P 0.63152(6) 0.27179(4) 0.09735(4) 0.01499(14) Uani 1 1 d . . .
O1 O 0.4328(2) 0.35295(13) 0.03118(13) 0.0334(5) Uani 1 1 d . . .
O2 O 0.32675(19) 0.39006(12) 0.27835(12) 0.0279(5) Uani 1 1 d . . .
O3 O 0.4263(2) 0.44718(12) 0.16121(13) 0.0306(5) Uani 1 1 d . . .
O4 O 0.23638(19) 0.31512(13) 0.13870(13) 0.0305(5) Uani 1 1 d . . .
N1 N 0.5892(2) 0.17870(13) 0.02502(13) 0.0181(5) Uani 1 1 d . . .
C1 C 0.5059(2) 0.32467(15) 0.14053(16) 0.0176(5) Uani 1 1 d . . .
C2 C 0.4453(2) 0.30620(15) 0.18594(16) 0.0181(5) Uani 1 1 d . . .
C3 C 0.4519(3) 0.37537(17) 0.10405(18) 0.0213(6) Uani 1 1 d . . .
C4 C 0.3326(3) 0.34392(16) 0.20734(18) 0.0212(6) Uani 1 1 d . . .
C5 C 0.3535(4) 0.4913(2) 0.1265(2) 0.0504(10) Uani 1 1 d . . .
H5A H 0.3340 0.5408 0.1719 0.076 Uiso 1 1 calc R . .
H5B H 0.2747 0.4536 0.0858 0.076 Uiso 1 1 calc R . .
H5C H 0.4027 0.5091 0.0984 0.076 Uiso 1 1 calc R . .
C6 C 0.1211(3) 0.3454(2) 0.1535(2) 0.0481(9) Uani 1 1 d . . .
H6A H 0.0583 0.3247 0.0995 0.072 Uiso 1 1 calc R . .
H6B H 0.1384 0.4071 0.1848 0.072 Uiso 1 1 calc R . .
H6C H 0.0884 0.3251 0.1861 0.072 Uiso 1 1 calc R . .
C7 C 0.5437(3) 0.11372(18) 0.1702(2) 0.0347(8) Uani 1 1 d . . .
H7A H 0.4990 0.0649 0.1676 0.052 Uiso 1 1 calc R . .
H7B H 0.6332 0.1244 0.1993 0.052 Uiso 1 1 calc R . .
H7C H 0.5353 0.1024 0.1130 0.052 Uiso 1 1 calc R . .
C8 C 0.2692(3) 0.18240(19) 0.2213(2) 0.0363(8) Uani 1 1 d . . .
H8A H 0.2618 0.1468 0.2455 0.054 Uiso 1 1 calc R . .
H8B H 0.2242 0.1506 0.1613 0.054 Uiso 1 1 calc R . .
H8C H 0.2322 0.2321 0.2499 0.054 Uiso 1 1 calc R . .
C9 C 0.5546(3) 0.30210(19) 0.36811(18) 0.0321(7) Uani 1 1 d . . .
H9A H 0.5341 0.2752 0.3987 0.048 Uiso 1 1 calc R . .
H9B H 0.5247 0.3556 0.3885 0.048 Uiso 1 1 calc R . .
H9C H 0.6462 0.3126 0.3773 0.048 Uiso 1 1 calc R . .
C11 C 0.5472(3) 0.14166(15) -0.06264(16) 0.0175(5) Uani 1 1 d . . .
C12 C 0.4170(3) 0.12123(15) -0.10382(17) 0.0206(6) Uani 1 1 d . . .
C13 C 0.3789(3) 0.08295(17) -0.19088(18) 0.0278(7) Uani 1 1 d . . .
H13A H 0.2914 0.0695 -0.2187 0.033 Uiso 1 1 calc R . .
C14 C 0.4645(3) 0.06398(18) -0.23801(19) 0.0333(7) Uani 1 1 d . . .
H14A H 0.4365 0.0385 -0.2974 0.040 Uiso 1 1 calc R . .
C15 C 0.5916(3) 0.08267(17) -0.19758(19) 0.0304(7) Uani 1 1 d . . .
H15A H 0.6506 0.0689 -0.2300 0.036 Uiso 1 1 calc R . .
C16 C 0.6354(3) 0.12114(16) -0.11076(17) 0.0215(6) Uani 1 1 d . . .
C17 C 0.7407(3) 0.27605(17) 0.18515(18) 0.0226(6) Uani 1 1 d . . .
C18 C 0.7632(3) 0.34230(19) 0.26714(18) 0.0309(7) Uani 1 1 d . . .
H18A H 0.7160 0.3861 0.2794 0.037 Uiso 1 1 calc R . .
C19 C 0.8546(3) 0.3447(3) 0.3312(2) 0.0468(9) Uani 1 1 d . . .
H19A H 0.8682 0.3894 0.3874 0.056 Uiso 1 1 calc R . .
C20 C 0.9254(3) 0.2828(3) 0.3139(2) 0.0508(10) Uani 1 1 d . . .
H20A H 0.9885 0.2852 0.3581 0.061 Uiso 1 1 calc R . .
C21 C 0.9054(3) 0.2173(2) 0.2330(2) 0.0431(9) Uani 1 1 d . . .
H21A H 0.9549 0.1748 0.2215 0.052 Uiso 1 1 calc R . .
C22 C 0.8131(3) 0.21294(19) 0.1679(2) 0.0286(7) Uani 1 1 d . . .
H22A H 0.7993 0.1674 0.1120 0.034 Uiso 1 1 calc R . .
C23 C 0.7164(2) 0.34222(15) 0.07457(17) 0.0183(6) Uani 1 1 d . . .
C24 C 0.6789(3) 0.33049(16) -0.00591(17) 0.0208(6) Uani 1 1 d . . .
H24A H 0.6057 0.2903 -0.0457 0.025 Uiso 1 1 calc R . .
C25 C 0.7477(3) 0.37709(17) -0.0283(2) 0.0296(7) Uani 1 1 d . . .
H25A H 0.7216 0.3685 -0.0833 0.035 Uiso 1 1 calc R . .
C26 C 0.8543(3) 0.43614(18) 0.0293(2) 0.0333(8) Uani 1 1 d . . .
H26A H 0.9012 0.4680 0.0137 0.040 Uiso 1 1 calc R . .
C27 C 0.8925(3) 0.44880(18) 0.1092(2) 0.0313(7) Uani 1 1 d . . .
H27A H 0.9653 0.4896 0.1487 0.038 Uiso 1 1 calc R . .
C28 C 0.8241(3) 0.40175(16) 0.13199(18) 0.0227(6) Uani 1 1 d . . .
H28A H 0.8511 0.4103 0.1870 0.027 Uiso 1 1 calc R . .
C121 C 0.3207(3) 0.13826(18) -0.05444(19) 0.0287(7) Uani 1 1 d . . .
H12A H 0.3645 0.1828 0.0049 0.034 Uiso 1 1 calc R . .
C122 C 0.2109(3) 0.1714(2) -0.0856(2) 0.0515(10) Uani 1 1 d . . .
H12B H 0.2439 0.2183 -0.0907 0.077 Uiso 1 1 calc R . .
H12C H 0.1600 0.1908 -0.0455 0.077 Uiso 1 1 calc R . .
H12D H 0.1584 0.1263 -0.1406 0.077 Uiso 1 1 calc R . .
C123 C 0.2727(4) 0.0602(2) -0.0533(2) 0.0498(10) Uani 1 1 d . . .
H12E H 0.3439 0.0427 -0.0288 0.075 Uiso 1 1 calc R . .
H12F H 0.2309 0.0146 -0.1109 0.075 Uiso 1 1 calc R . .
H12G H 0.2124 0.0730 -0.0195 0.075 Uiso 1 1 calc R . .
C161 C 0.7753(3) 0.13782(17) -0.06817(19) 0.0274(7) Uani 1 1 d . . .
H16A H 0.7908 0.1848 -0.0088 0.033 Uiso 1 1 calc R . .
C162 C 0.8120(3) 0.0609(2) -0.0651(2) 0.0412(8) Uani 1 1 d . . .
H16B H 0.7587 0.0452 -0.0376 0.062 Uiso 1 1 calc R . .
H16C H 0.9007 0.0744 -0.0333 0.062 Uiso 1 1 calc R . .
H16D H 0.8001 0.0139 -0.1225 0.062 Uiso 1 1 calc R . .
C163 C 0.8591(3) 0.1657(2) -0.1087(2) 0.0399(8) Uani 1 1 d . . .
H16E H 0.8291 0.2117 -0.1146 0.060 Uiso 1 1 calc R . .
H16F H 0.8555 0.1181 -0.1643 0.060 Uiso 1 1 calc R . .
H16G H 0.9463 0.1850 -0.0732 0.060 Uiso 1 1 calc R . .
Sn2 Sn -0.041884(19) 0.236826(12) 0.725236(13) 0.02548(6) Uani 1 1 d . . .
P2 P 0.15779(6) 0.28699(4) 0.60350(4) 0.01552(14) Uani 1 1 d . . .
O5 O -0.03687(19) 0.36031(12) 0.51441(12) 0.0291(5) Uani 1 1 d . . .
O6 O -0.1766(2) 0.40319(13) 0.75297(13) 0.0339(5) Uani 1 1 d . . .
O7 O -0.05662(19) 0.45640(11) 0.64043(12) 0.0279(5) Uani 1 1 d . . .
O8 O -0.25675(19) 0.32793(12) 0.61254(13) 0.0308(5) Uani 1 1 d . . .
N2 N 0.1329(2) 0.19071(13) 0.54286(14) 0.0195(5) Uani 1 1 d . . .
C31 C 0.0192(2) 0.33495(15) 0.62772(16) 0.0172(5) Uani 1 1 d . . .
C32 C -0.0514(3) 0.31744(16) 0.66912(17) 0.0204(6) Uani 1 1 d . . .
C33 C -0.0263(3) 0.38434(16) 0.58725(18) 0.0211(6) Uani 1 1 d . . .
C34 C -0.1657(3) 0.35623(17) 0.68402(18) 0.0234(6) Uani 1 1 d . . .
C35 C -0.1261(3) 0.4974(2) 0.6009(2) 0.0412(9) Uani 1 1 d . . .
H35A H -0.1501 0.5469 0.6434 0.062 Uiso 1 1 calc R . .
H35B H -0.2023 0.4581 0.5581 0.062 Uiso 1 1 calc R . .
H35C H -0.0729 0.5148 0.5744 0.062 Uiso 1 1 calc R . .
C36 C -0.3724(3) 0.3609(2) 0.6226(2) 0.0484(9) Uani 1 1 d . . .
H36A H -0.4298 0.3416 0.5671 0.073 Uiso 1 1 calc R . .
H36B H -0.3523 0.4225 0.6547 0.073 Uiso 1 1 calc R . .
H36C H -0.4129 0.3407 0.6526 0.073 Uiso 1 1 calc R . .
C37 C -0.2393(3) 0.1914(2) 0.6948(2) 0.0444(9) Uani 1 1 d . . .
H37A H -0.2514 0.1429 0.7020 0.067 Uiso 1 1 calc R . .
H37B H -0.2793 0.1745 0.6363 0.067 Uiso 1 1 calc R . .
H37C H -0.2776 0.2361 0.7321 0.067 Uiso 1 1 calc R . .
C38 C 0.0522(4) 0.13346(19) 0.6762(2) 0.0399(8) Uani 1 1 d . . .
H38A H -0.0014 0.0825 0.6640 0.060 Uiso 1 1 calc R . .
H38B H 0.1319 0.1449 0.7176 0.060 Uiso 1 1 calc R . .
H38C H 0.0693 0.1254 0.6244 0.060 Uiso 1 1 calc R . .
C39 C 0.0313(3) 0.32199(19) 0.85731(19) 0.0378(8) Uani 1 1 d . . .
H39A H 0.0179 0.2931 0.8874 0.057 Uiso 1 1 calc R . .
H39B H -0.0122 0.3699 0.8746 0.057 Uiso 1 1 calc R . .
H39C H 0.1218 0.3421 0.8706 0.057 Uiso 1 1 calc R . .
C41 C 0.1071(3) 0.14161(15) 0.45485(17) 0.0184(6) Uani 1 1 d . . .
C42 C -0.0169(3) 0.11826(15) 0.40247(17) 0.0202(6) Uani 1 1 d . . .
C43 C -0.0371(3) 0.07087(17) 0.31566(18) 0.0278(7) Uani 1 1 d . . .
H43A H -0.1202 0.0561 0.2800 0.033 Uiso 1 1 calc R . .
C44 C 0.0609(3) 0.04487(17) 0.28023(19) 0.0323(7) Uani 1 1 d . . .
H44A H 0.0454 0.0135 0.2209 0.039 Uiso 1 1 calc R . .
C45 C 0.1812(3) 0.06471(17) 0.33151(19) 0.0297(7) Uani 1 1 d . . .
H45A H 0.2477 0.0451 0.3068 0.036 Uiso 1 1 calc R . .
C46 C 0.2080(3) 0.11274(15) 0.41868(18) 0.0213(6) Uani 1 1 d . . .
C47 C 0.2524(3) 0.31256(17) 0.70534(17) 0.0204(6) Uani 1 1 d . . .
C48 C 0.3280(3) 0.25720(19) 0.7123(2) 0.0306(7) Uani 1 1 d . . .
H48A H 0.3264 0.2051 0.6638 0.037 Uiso 1 1 calc R . .
C49 C 0.4055(3) 0.2786(2) 0.7902(2) 0.0418(9) Uani 1 1 d . . .
H49A H 0.4566 0.2408 0.7949 0.050 Uiso 1 1 calc R . .
C50 C 0.4087(3) 0.3540(2) 0.8607(2) 0.0416(9) Uani 1 1 d . . .
H50A H 0.4605 0.3676 0.9140 0.050 Uiso 1 1 calc R . .
C51 C 0.3371(3) 0.4098(2) 0.85422(19) 0.0370(8) Uani 1 1 d . . .
H51A H 0.3419 0.4627 0.9026 0.044 Uiso 1 1 calc R . .
C52 C 0.2579(3) 0.38893(19) 0.77699(17) 0.0292(7) Uani 1 1 d . . .
H52A H 0.2071 0.4271 0.7731 0.035 Uiso 1 1 calc R . .
C53 C 0.2411(2) 0.35109(15) 0.57364(17) 0.0176(5) Uani 1 1 d . . .
C54 C 0.2161(3) 0.32390(16) 0.48812(17) 0.0213(6) Uani 1 1 d . . .
H54A H 0.1582 0.2731 0.4477 0.026 Uiso 1 1 calc R . .
C55 C 0.2761(3) 0.37109(17) 0.46219(19) 0.0269(7) Uani 1 1 d . . .
H55A H 0.2592 0.3524 0.4041 0.032 Uiso 1 1 calc R . .
C56 C 0.3600(3) 0.44474(18) 0.5205(2) 0.0298(7) Uani 1 1 d . . .
H56A H 0.3987 0.4777 0.5026 0.036 Uiso 1 1 calc R . .
C57 C 0.3880(3) 0.47080(18) 0.6045(2) 0.0314(7) Uani 1 1 d . . .
H57A H 0.4482 0.5206 0.6443 0.038 Uiso 1 1 calc R . .
C58 C 0.3281(3) 0.42428(16) 0.63155(18) 0.0240(6) Uani 1 1 d . . .
H58A H 0.3471 0.4429 0.6897 0.029 Uiso 1 1 calc R . .
C421 C -0.1266(3) 0.14081(17) 0.43993(18) 0.0249(6) Uani 1 1 d . . .
H42A H -0.0939 0.1937 0.4959 0.030 Uiso 1 1 calc R . .
C422 C -0.2352(3) 0.1575(2) 0.3886(2) 0.0362(8) Uani 1 1 d . . .
H42B H -0.2967 0.1791 0.4207 0.054 Uiso 1 1 calc R . .
H42C H -0.2762 0.1050 0.3358 0.054 Uiso 1 1 calc R . .
H42D H -0.2025 0.1991 0.3762 0.054 Uiso 1 1 calc R . .
C423 C -0.1748(3) 0.0725(2) 0.4557(2) 0.0397(8) Uani 1 1 d . . .
H42E H -0.1046 0.0630 0.4896 0.059 Uiso 1 1 calc R . .
H42F H -0.2114 0.0202 0.4019 0.059 Uiso 1 1 calc R . .
H42G H -0.2395 0.0905 0.4858 0.059 Uiso 1 1 calc R . .
C461 C 0.3394(3) 0.13288(18) 0.4750(2) 0.0292(7) Uani 1 1 d . . .
H46A H 0.3490 0.1897 0.5257 0.035 Uiso 1 1 calc R . .
C462 C 0.3545(4) 0.0707(2) 0.5059(3) 0.0533(10) Uani 1 1 d . . .
H46B H 0.2896 0.0715 0.5343 0.080 Uiso 1 1 calc R . .
H46C H 0.4382 0.0869 0.5453 0.080 Uiso 1 1 calc R . .
H46D H 0.3454 0.0140 0.4578 0.080 Uiso 1 1 calc R . .
C463 C 0.4451(4) 0.1377(3) 0.4361(3) 0.0607(11) Uani 1 1 d . . .
H46E H 0.4328 0.1767 0.4155 0.091 Uiso 1 1 calc R . .
H46F H 0.4438 0.0817 0.3892 0.091 Uiso 1 1 calc R . .
H46G H 0.5266 0.1577 0.4786 0.091 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 C7 2.130(3) . ?
Sn1 C9 2.141(3) . ?
Sn1 C8 2.147(3) . ?
Sn1 C2 2.210(2) . ?
P1 N1 1.551(2) . ?
P1 C17 1.801(3) . ?
P1 C23 1.830(3) . ?
P1 C1 1.846(3) . ?
O1 C3 1.197(3) . ?
O2 C4 1.212(3) . ?
O3 C3 1.339(3) . ?
O3 C5 1.459(3) . ?
O4 C4 1.334(3) . ?
O4 C6 1.448(4) . ?
N1 C11 1.405(3) . ?
C1 C2 1.345(3) . ?
C1 C3 1.497(4) . ?
C2 C4 1.496(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.412(4) . ?
C11 C16 1.416(4) . ?
C12 C13 1.391(4) . ?
C12 C121 1.509(4) . ?
C13 C14 1.379(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.381(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.389(4) . ?
C15 H15A 0.9500 . ?
C16 C161 1.519(4) . ?
C17 C18 1.388(4) . ?
C17 C22 1.401(4) . ?
C18 C19 1.386(4) . ?
C18 H18A 0.9500 . ?
C19 C20 1.372(5) . ?
C19 H19A 0.9500 . ?
C20 C21 1.372(5) . ?
C20 H20A 0.9500 . ?
C21 C22 1.390(4) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 C24 1.395(4) . ?
C23 C28 1.396(4) . ?
C24 C25 1.386(4) . ?
C24 H24A 0.9500 . ?
C25 C26 1.385(4) . ?
C25 H25A 0.9500 . ?
C26 C27 1.377(4) . ?
C26 H26A 0.9500 . ?
C27 C28 1.395(4) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
C121 C123 1.525(4) . ?
C121 C122 1.528(4) . ?
C121 H12A 1.0000 . ?
C122 H12B 0.9800 . ?
C122 H12C 0.9800 . ?
C122 H12D 0.9800 . ?
C123 H12E 0.9800 . ?
C123 H12F 0.9800 . ?
C123 H12G 0.9800 . ?
C161 C162 1.529(4) . ?
C161 C163 1.531(4) . ?
C161 H16A 1.0000 . ?
C162 H16B 0.9800 . ?
C162 H16C 0.9800 . ?
C162 H16D 0.9800 . ?
C163 H16E 0.9800 . ?
C163 H16F 0.9800 . ?
C163 H16G 0.9800 . ?
Sn2 C38 2.125(3) . ?
Sn2 C39 2.135(3) . ?
Sn2 C37 2.138(3) . ?
Sn2 C32 2.213(3) . ?
P2 N2 1.547(2) . ?
P2 C47 1.800(3) . ?
P2 C53 1.824(3) . ?
P2 C31 1.844(3) . ?
O5 C33 1.202(3) . ?
O6 C34 1.204(3) . ?
O7 C33 1.340(3) . ?
O7 C35 1.453(3) . ?
O8 C34 1.339(3) . ?
O8 C36 1.456(4) . ?
N2 C41 1.408(3) . ?
C31 C32 1.343(4) . ?
C31 C33 1.502(3) . ?
C32 C34 1.499(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C41 C42 1.410(4) . ?
C41 C46 1.425(4) . ?
C42 C43 1.394(4) . ?
C42 C421 1.509(4) . ?
C43 C44 1.380(4) . ?
C43 H43A 0.9500 . ?
C44 C45 1.377(4) . ?
C44 H44A 0.9500 . ?
C45 C46 1.392(4) . ?
C45 H45A 0.9500 . ?
C46 C461 1.510(4) . ?
C47 C52 1.390(4) . ?
C47 C48 1.398(4) . ?
C48 C49 1.388(4) . ?
C48 H48A 0.9500 . ?
C49 C50 1.377(5) . ?
C49 H49A 0.9500 . ?
C50 C51 1.373(5) . ?
C50 H50A 0.9500 . ?
C51 C52 1.388(4) . ?
C51 H51A 0.9500 . ?
C52 H52A 0.9500 . ?
C53 C58 1.386(4) . ?
C53 C54 1.399(4) . ?
C54 C55 1.391(4) . ?
C54 H54A 0.9500 . ?
C55 C56 1.376(4) . ?
C55 H55A 0.9500 . ?
C56 C57 1.374(4) . ?
C56 H56A 0.9500 . ?
C57 C58 1.398(4) . ?
C57 H57A 0.9500 . ?
C58 H58A 0.9500 . ?
C421 C422 1.525(4) . ?
C421 C423 1.528(4) . ?
C421 H42A 1.0000 . ?
C422 H42B 0.9800 . ?
C422 H42C 0.9800 . ?
C422 H42D 0.9800 . ?
C423 H42E 0.9800 . ?
C423 H42F 0.9800 . ?
C423 H42G 0.9800 . ?
C461 C463 1.526(4) . ?
C461 C462 1.528(4) . ?
C461 H46A 1.0000 . ?
C462 H46B 0.9800 . ?
C462 H46C 0.9800 . ?
C462 H46D 0.9800 . ?
C463 H46E 0.9800 . ?
C463 H46F 0.9800 . ?
C463 H46G 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Sn1 C9 117.08(13) . . ?
C7 Sn1 C8 109.70(12) . . ?
C9 Sn1 C8 108.23(13) . . ?
C7 Sn1 C2 116.04(11) . . ?
C9 Sn1 C2 104.84(10) . . ?
C8 Sn1 C2 99.30(11) . . ?
N1 P1 C17 108.63(12) . . ?
N1 P1 C23 115.74(12) . . ?
C17 P1 C23 104.85(12) . . ?
N1 P1 C1 116.01(12) . . ?
C17 P1 C1 104.68(12) . . ?
C23 P1 C1 105.84(11) . . ?
C3 O3 C5 114.8(2) . . ?
C4 O4 C6 115.3(2) . . ?
C11 N1 P1 132.07(17) . . ?
C2 C1 C3 119.6(2) . . ?
C2 C1 P1 124.27(19) . . ?
C3 C1 P1 114.55(18) . . ?
C1 C2 C4 119.8(2) . . ?
C1 C2 Sn1 134.6(2) . . ?
C4 C2 Sn1 105.49(17) . . ?
O1 C3 O3 124.1(2) . . ?
O1 C3 C1 123.0(2) . . ?
O3 C3 C1 112.9(2) . . ?
O2 C4 O4 124.3(3) . . ?
O2 C4 C2 124.2(2) . . ?
O4 C4 C2 111.3(2) . . ?
O3 C5 H5A 109.5 . . ?
O3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O4 C6 H6A 109.5 . . ?
O4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Sn1 C7 H7A 109.5 . . ?
Sn1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Sn1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Sn1 C8 H8A 109.5 . . ?
Sn1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Sn1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Sn1 C9 H9A 109.5 . . ?
Sn1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Sn1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C11 C12 120.6(2) . . ?
N1 C11 C16 119.9(2) . . ?
C12 C11 C16 119.5(2) . . ?
C13 C12 C11 118.9(3) . . ?
C13 C12 C121 120.5(3) . . ?
C11 C12 C121 120.5(2) . . ?
C14 C13 C12 121.9(3) . . ?
C14 C13 H13A 119.0 . . ?
C12 C13 H13A 119.0 . . ?
C13 C14 C15 119.0(3) . . ?
C13 C14 H14A 120.5 . . ?
C15 C14 H14A 120.5 . . ?
C14 C15 C16 121.7(3) . . ?
C14 C15 H15A 119.1 . . ?
C16 C15 H15A 119.1 . . ?
C15 C16 C11 119.0(3) . . ?
C15 C16 C161 120.7(3) . . ?
C11 C16 C161 120.3(2) . . ?
C18 C17 C22 119.2(3) . . ?
C18 C17 P1 122.9(2) . . ?
C22 C17 P1 117.6(2) . . ?
C19 C18 C17 120.1(3) . . ?
C19 C18 H18A 119.9 . . ?
C17 C18 H18A 119.9 . . ?
C20 C19 C18 120.4(3) . . ?
C20 C19 H19A 119.8 . . ?
C18 C19 H19A 119.8 . . ?
C19 C20 C21 120.3(3) . . ?
C19 C20 H20A 119.9 . . ?
C21 C20 H20A 119.9 . . ?
C20 C21 C22 120.4(3) . . ?
C20 C21 H21A 119.8 . . ?
C22 C21 H21A 119.8 . . ?
C21 C22 C17 119.5(3) . . ?
C21 C22 H22A 120.2 . . ?
C17 C22 H22A 120.2 . . ?
C24 C23 C28 118.8(2) . . ?
C24 C23 P1 118.5(2) . . ?
C28 C23 P1 122.4(2) . . ?
C25 C24 C23 120.5(3) . . ?
C25 C24 H24A 119.8 . . ?
C23 C24 H24A 119.8 . . ?
C26 C25 C24 120.2(3) . . ?
C26 C25 H25A 119.9 . . ?
C24 C25 H25A 119.9 . . ?
C27 C26 C25 120.1(3) . . ?
C27 C26 H26A 119.9 . . ?
C25 C26 H26A 119.9 . . ?
C26 C27 C28 120.0(3) . . ?
C26 C27 H27A 120.0 . . ?
C28 C27 H27A 120.0 . . ?
C27 C28 C23 120.4(3) . . ?
C27 C28 H28A 119.8 . . ?
C23 C28 H28A 119.8 . . ?
C12 C121 C123 110.7(2) . . ?
C12 C121 C122 113.2(3) . . ?
C123 C121 C122 110.8(3) . . ?
C12 C121 H12A 107.3 . . ?
C123 C121 H12A 107.3 . . ?
C122 C121 H12A 107.3 . . ?
C121 C122 H12B 109.5 . . ?
C121 C122 H12C 109.5 . . ?
H12B C122 H12C 109.5 . . ?
C121 C122 H12D 109.5 . . ?
H12B C122 H12D 109.5 . . ?
H12C C122 H12D 109.5 . . ?
C121 C123 H12E 109.5 . . ?
C121 C123 H12F 109.5 . . ?
H12E C123 H12F 109.5 . . ?
C121 C123 H12G 109.5 . . ?
H12E C123 H12G 109.5 . . ?
H12F C123 H12G 109.5 . . ?
C16 C161 C162 110.6(2) . . ?
C16 C161 C163 113.1(3) . . ?
C162 C161 C163 110.9(3) . . ?
C16 C161 H16A 107.3 . . ?
C162 C161 H16A 107.3 . . ?
C163 C161 H16A 107.3 . . ?
C161 C162 H16B 109.5 . . ?
C161 C162 H16C 109.5 . . ?
H16B C162 H16C 109.5 . . ?
C161 C162 H16D 109.5 . . ?
H16B C162 H16D 109.5 . . ?
H16C C162 H16D 109.5 . . ?
C161 C163 H16E 109.5 . . ?
C161 C163 H16F 109.5 . . ?
H16E C163 H16F 109.5 . . ?
C161 C163 H16G 109.5 . . ?
H16E C163 H16G 109.5 . . ?
H16F C163 H16G 109.5 . . ?
C38 Sn2 C39 114.13(14) . . ?
C38 Sn2 C37 109.62(14) . . ?
C39 Sn2 C37 110.19(14) . . ?
C38 Sn2 C32 117.77(11) . . ?
C39 Sn2 C32 104.92(11) . . ?
C37 Sn2 C32 99.10(11) . . ?
N2 P2 C47 109.41(12) . . ?
N2 P2 C53 116.23(12) . . ?
C47 P2 C53 105.98(12) . . ?
N2 P2 C31 116.77(12) . . ?
C47 P2 C31 102.59(12) . . ?
C53 P2 C31 104.53(11) . . ?
C33 O7 C35 114.8(2) . . ?
C34 O8 C36 115.2(2) . . ?
C41 N2 P2 131.73(17) . . ?
C32 C31 C33 119.4(2) . . ?
C32 C31 P2 122.63(19) . . ?
C33 C31 P2 117.24(19) . . ?
C31 C32 C34 119.9(2) . . ?
C31 C32 Sn2 134.1(2) . . ?
C34 C32 Sn2 105.95(17) . . ?
O5 C33 O7 124.1(2) . . ?
O5 C33 C31 123.2(2) . . ?
O7 C33 C31 112.7(2) . . ?
O6 C34 O8 124.2(3) . . ?
O6 C34 C32 123.4(3) . . ?
O8 C34 C32 112.2(2) . . ?
O7 C35 H35A 109.5 . . ?
O7 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O7 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O8 C36 H36A 109.5 . . ?
O8 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
O8 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Sn2 C37 H37A 109.5 . . ?
Sn2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
Sn2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Sn2 C38 H38A 109.5 . . ?
Sn2 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Sn2 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Sn2 C39 H39A 109.5 . . ?
Sn2 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
Sn2 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N2 C41 C42 121.1(2) . . ?
N2 C41 C46 119.1(2) . . ?
C42 C41 C46 119.7(2) . . ?
C43 C42 C41 118.9(3) . . ?
C43 C42 C421 120.6(3) . . ?
C41 C42 C421 120.5(2) . . ?
C44 C43 C42 121.5(3) . . ?
C44 C43 H43A 119.2 . . ?
C42 C43 H43A 119.2 . . ?
C45 C44 C43 119.5(3) . . ?
C45 C44 H44A 120.2 . . ?
C43 C44 H44A 120.2 . . ?
C44 C45 C46 121.8(3) . . ?
C44 C45 H45A 119.1 . . ?
C46 C45 H45A 119.1 . . ?
C45 C46 C41 118.4(3) . . ?
C45 C46 C461 121.8(3) . . ?
C41 C46 C461 119.7(2) . . ?
C52 C47 C48 119.0(3) . . ?
C52 C47 P2 121.2(2) . . ?
C48 C47 P2 119.7(2) . . ?
C49 C48 C47 119.8(3) . . ?
C49 C48 H48A 120.1 . . ?
C47 C48 H48A 120.1 . . ?
C50 C49 C48 120.5(3) . . ?
C50 C49 H49A 119.8 . . ?
C48 C49 H49A 119.8 . . ?
C51 C50 C49 120.2(3) . . ?
C51 C50 H50A 119.9 . . ?
C49 C50 H50A 119.9 . . ?
C50 C51 C52 120.0(3) . . ?
C50 C51 H51A 120.0 . . ?
C52 C51 H51A 120.0 . . ?
C51 C52 C47 120.5(3) . . ?
C51 C52 H52A 119.7 . . ?
C47 C52 H52A 119.7 . . ?
C58 C53 C54 119.1(2) . . ?
C58 C53 P2 123.0(2) . . ?
C54 C53 P2 117.9(2) . . ?
C55 C54 C53 120.1(3) . . ?
C55 C54 H54A 120.0 . . ?
C53 C54 H54A 120.0 . . ?
C56 C55 C54 120.2(3) . . ?
C56 C55 H55A 119.9 . . ?
C54 C55 H55A 119.9 . . ?
C57 C56 C55 120.2(3) . . ?
C57 C56 H56A 119.9 . . ?
C55 C56 H56A 119.9 . . ?
C56 C57 C58 120.2(3) . . ?
C56 C57 H57A 119.9 . . ?
C58 C57 H57A 119.9 . . ?
C53 C58 C57 120.1(3) . . ?
C53 C58 H58A 120.0 . . ?
C57 C58 H58A 120.0 . . ?
C42 C421 C422 114.7(2) . . ?
C42 C421 C423 109.9(2) . . ?
C422 C421 C423 110.1(2) . . ?
C42 C421 H42A 107.2 . . ?
C422 C421 H42A 107.2 . . ?
C423 C421 H42A 107.2 . . ?
C421 C422 H42B 109.5 . . ?
C421 C422 H42C 109.5 . . ?
H42B C422 H42C 109.5 . . ?
C421 C422 H42D 109.5 . . ?
H42B C422 H42D 109.5 . . ?
H42C C422 H42D 109.5 . . ?
C421 C423 H42E 109.5 . . ?
C421 C423 H42F 109.5 . . ?
H42E C423 H42F 109.5 . . ?
C421 C423 H42G 109.5 . . ?
H42E C423 H42G 109.5 . . ?
H42F C423 H42G 109.5 . . ?
C46 C461 C463 114.5(3) . . ?
C46 C461 C462 110.5(2) . . ?
C463 C461 C462 110.6(3) . . ?
C46 C461 H46A 107.0 . . ?
C463 C461 H46A 107.0 . . ?
C462 C461 H46A 107.0 . . ?
C461 C462 H46B 109.5 . . ?
C461 C462 H46C 109.5 . . ?
H46B C462 H46C 109.5 . . ?
C461 C462 H46D 109.5 . . ?
H46B C462 H46D 109.5 . . ?
H46C C462 H46D 109.5 . . ?
C461 C463 H46E 109.5 . . ?
C461 C463 H46F 109.5 . . ?
H46E C463 H46F 109.5 . . ?
C461 C463 H46G 109.5 . . ?
H46E C463 H46G 109.5 . . ?
H46F C463 H46G 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.070
####################################################################### 
# 
# 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_yy-140507b
_database_code_depnum_ccdc_archive 'CCDC 1424121'
_audit_update_record             
;
2015-09-12 deposited with the CCDC.
2015-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H74 Cl6 Ge2 N2 O3 P2'
_chemical_formula_weight         1267.01

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'
P P 0.2955 0.4335 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pna2(1)

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

_cell_length_a                   19.2113(2)
_cell_length_b                   9.36270(10)
_cell_length_c                   33.9828(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6112.47(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    14574
_cell_measurement_theta_min      4.7730
_cell_measurement_theta_max      62.1130

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2624
_exptl_absorpt_coefficient_mu    4.457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4693
_exptl_absorpt_correction_T_max  0.8079
_exptl_absorpt_process_details   empirical

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhanced (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34758
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         4.60
_diffrn_reflns_theta_max         62.13
_reflns_number_total             9145
_reflns_number_gt                8559
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisPro
_computing_cell_refinement       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0310P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'refined in a riding mode to the carrier atom'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         9145
_refine_ls_number_parameters     664
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0586
_refine_ls_wR_factor_gt          0.0579
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_restrained_S_all      0.994
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.170284(15) -0.03656(3) 0.284177(9) 0.02303(7) Uani 1 1 d . . .
P1 P 0.26370(3) 0.20906(7) 0.26575(2) 0.01989(14) Uani 1 1 d . . .
Cl1 Cl 0.21324(4) -0.25358(7) 0.29881(2) 0.03753(17) Uani 1 1 d . . .
Cl2 Cl 0.10650(5) -0.12749(8) 0.23755(2) 0.0454(2) Uani 1 1 d . . .
Cl3 Cl 0.11842(4) -0.01769(9) 0.34086(2) 0.04035(18) Uani 1 1 d . . .
N1 N 0.26250(11) 0.0397(2) 0.27840(7) 0.0213(5) Uani 1 1 d . . .
O1 O 0.13697(9) 0.14180(19) 0.26797(6) 0.0253(4) Uani 1 1 d . . .
C1 C 0.17609(13) 0.2613(3) 0.27993(8) 0.0224(6) Uani 1 1 d . . .
H1A H 0.1734 0.2717 0.3092 0.027 Uiso 1 1 calc R . .
C2 C 0.15070(15) 0.3970(3) 0.26037(9) 0.0283(6) Uani 1 1 d . . .
H2A H 0.1858 0.4731 0.2644 0.034 Uiso 1 1 calc R . .
H2B H 0.1465 0.3801 0.2317 0.034 Uiso 1 1 calc R . .
C3 C 0.08173(18) 0.4479(4) 0.27589(12) 0.0466(9) Uani 1 1 d . . .
H3A H 0.0671 0.5332 0.2614 0.070 Uiso 1 1 calc R . .
H3B H 0.0862 0.4712 0.3039 0.070 Uiso 1 1 calc R . .
H3C H 0.0469 0.3725 0.2725 0.070 Uiso 1 1 calc R . .
C11 C 0.32799(14) -0.0294(3) 0.28968(10) 0.0275(6) Uani 1 1 d . . .
C12 C 0.34929(16) -0.0222(3) 0.32874(10) 0.0337(7) Uani 1 1 d . . .
C13 C 0.41313(18) -0.0855(4) 0.33875(14) 0.0500(10) Uani 1 1 d . . .
H13A H 0.4292 -0.0817 0.3652 0.060 Uiso 1 1 calc R . .
C14 C 0.45257(19) -0.1530(4) 0.31045(16) 0.0601(13) Uani 1 1 d . . .
H14A H 0.4959 -0.1946 0.3175 0.072 Uiso 1 1 calc R . .
C15 C 0.43004(19) -0.1607(4) 0.27241(15) 0.0546(12) Uani 1 1 d . . .
H15A H 0.4577 -0.2092 0.2535 0.066 Uiso 1 1 calc R . .
C16 C 0.36732(17) -0.0991(3) 0.26074(11) 0.0383(8) Uani 1 1 d . . .
C17 C 0.33054(14) 0.3117(3) 0.28910(8) 0.0227(6) Uani 1 1 d . . .
C18 C 0.40050(15) 0.2857(3) 0.28106(10) 0.0311(6) Uani 1 1 d . . .
H18A H 0.4135 0.2084 0.2645 0.037 Uiso 1 1 calc R . .
C19 C 0.45076(17) 0.3729(3) 0.29731(11) 0.0378(7) Uani 1 1 d . . .
H19A H 0.4986 0.3551 0.2922 0.045 Uiso 1 1 calc R . .
C20 C 0.43148(16) 0.4865(3) 0.32102(10) 0.0357(7) Uani 1 1 d . . .
H20A H 0.4663 0.5458 0.3323 0.043 Uiso 1 1 calc R . .
C21 C 0.36227(17) 0.5145(3) 0.32849(10) 0.0350(7) Uani 1 1 d . . .
H21A H 0.3496 0.5942 0.3442 0.042 Uiso 1 1 calc R . .
C22 C 0.31105(16) 0.4258(3) 0.31296(9) 0.0282(6) Uani 1 1 d . . .
H22A H 0.2633 0.4429 0.3186 0.034 Uiso 1 1 calc R . .
C23 C 0.26975(14) 0.2414(3) 0.21355(8) 0.0247(6) Uani 1 1 d . . .
C24 C 0.23334(17) 0.1578(3) 0.18702(9) 0.0339(7) Uani 1 1 d . . .
H24A H 0.2092 0.0752 0.1958 0.041 Uiso 1 1 calc R . .
C25 C 0.23220(19) 0.1953(4) 0.14756(9) 0.0423(8) Uani 1 1 d . . .
H25A H 0.2081 0.1366 0.1293 0.051 Uiso 1 1 calc R . .
C26 C 0.26548(18) 0.3164(4) 0.13449(9) 0.0380(7) Uani 1 1 d . . .
H26A H 0.2642 0.3414 0.1074 0.046 Uiso 1 1 calc R . .
C27 C 0.30068(17) 0.4012(3) 0.16103(9) 0.0362(7) Uani 1 1 d . . .
H27A H 0.3233 0.4856 0.1522 0.043 Uiso 1 1 calc R . .
C28 C 0.30329(16) 0.3641(3) 0.20032(9) 0.0315(6) Uani 1 1 d . . .
H28A H 0.3281 0.4226 0.2184 0.038 Uiso 1 1 calc R . .
C121 C 0.30768(19) 0.0461(4) 0.36187(10) 0.0395(8) Uani 1 1 d . . .
H12A H 0.2670 0.0965 0.3499 0.047 Uiso 1 1 calc R . .
C122 C 0.2794(2) -0.0687(4) 0.38983(11) 0.0484(9) Uani 1 1 d . . .
H12B H 0.2534 -0.1401 0.3747 0.073 Uiso 1 1 calc R . .
H12C H 0.2484 -0.0242 0.4092 0.073 Uiso 1 1 calc R . .
H12D H 0.3182 -0.1151 0.4035 0.073 Uiso 1 1 calc R . .
C123 C 0.3500(3) 0.1563(4) 0.38491(12) 0.0596(11) Uani 1 1 d . . .
H12E H 0.3723 0.2226 0.3665 0.089 Uiso 1 1 calc R . .
H12F H 0.3858 0.1074 0.4004 0.089 Uiso 1 1 calc R . .
H12G H 0.3191 0.2095 0.4025 0.089 Uiso 1 1 calc R . .
C161 C 0.3446(2) -0.1123(4) 0.21826(12) 0.0502(9) Uani 1 1 d . . .
H16A H 0.2988 -0.0624 0.2158 0.060 Uiso 1 1 calc R . .
C162 C 0.3949(3) -0.0390(5) 0.19018(15) 0.0737(14) Uani 1 1 d . . .
H16B H 0.3964 0.0634 0.1960 0.111 Uiso 1 1 calc R . .
H16C H 0.3791 -0.0531 0.1630 0.111 Uiso 1 1 calc R . .
H16D H 0.4414 -0.0801 0.1934 0.111 Uiso 1 1 calc R . .
C163 C 0.3330(3) -0.2692(5) 0.20651(17) 0.0799(16) Uani 1 1 d . . .
H16E H 0.3042 -0.3164 0.2265 0.120 Uiso 1 1 calc R . .
H16F H 0.3780 -0.3180 0.2046 0.120 Uiso 1 1 calc R . .
H16G H 0.3093 -0.2732 0.1810 0.120 Uiso 1 1 calc R . .
Ge2 Ge 0.394584(15) 0.55774(3) 0.033280(9) 0.02219(7) Uani 1 1 d . . .
P2 P 0.49213(3) 0.32040(7) 0.053255(19) 0.01838(13) Uani 1 1 d . . .
Cl4 Cl 0.33634(5) 0.66069(8) 0.08078(2) 0.0437(2) Uani 1 1 d . . .
Cl5 Cl 0.43301(4) 0.77268(7) 0.01288(2) 0.03290(16) Uani 1 1 d . . .
Cl6 Cl 0.33831(4) 0.52009(9) -0.02120(2) 0.03865(18) Uani 1 1 d . . .
N2 N 0.48753(11) 0.4865(2) 0.03736(6) 0.0192(4) Uani 1 1 d . . .
O2 O 0.36452(9) 0.38450(19) 0.05460(6) 0.0248(4) Uani 1 1 d . . .
C4 C 0.40295(13) 0.2632(3) 0.04359(7) 0.0214(6) Uani 1 1 d . . .
H4A H 0.3968 0.2447 0.0148 0.026 Uiso 1 1 calc R . .
C5 C 0.38085(15) 0.1313(3) 0.06713(9) 0.0267(6) Uani 1 1 d . . .
H5A H 0.4167 0.0560 0.0643 0.032 Uiso 1 1 calc R . .
H5B H 0.3777 0.1567 0.0954 0.032 Uiso 1 1 calc R . .
C6 C 0.31070(17) 0.0734(3) 0.05325(11) 0.0376(7) Uani 1 1 d . . .
H6A H 0.2991 -0.0129 0.0682 0.056 Uiso 1 1 calc R . .
H6B H 0.3134 0.0503 0.0252 0.056 Uiso 1 1 calc R . .
H6C H 0.2746 0.1458 0.0575 0.056 Uiso 1 1 calc R . .
C31 C 0.55150(14) 0.5535(3) 0.02381(8) 0.0231(6) Uani 1 1 d . . .
C32 C 0.57358(15) 0.5300(3) -0.01515(9) 0.0259(6) Uani 1 1 d . . .
C33 C 0.63938(17) 0.5815(3) -0.02623(10) 0.0350(7) Uani 1 1 d . . .
H33A H 0.6556 0.5660 -0.0523 0.042 Uiso 1 1 calc R . .
C34 C 0.68094(16) 0.6546(3) 0.00032(11) 0.0406(8) Uani 1 1 d . . .
H34A H 0.7259 0.6863 -0.0073 0.049 Uiso 1 1 calc R . .
C35 C 0.65709(16) 0.6810(3) 0.03752(12) 0.0378(8) Uani 1 1 d . . .
H35A H 0.6858 0.7327 0.0553 0.045 Uiso 1 1 calc R . .
C36 C 0.59171(15) 0.6341(3) 0.05026(9) 0.0286(6) Uani 1 1 d . . .
C37 C 0.55549(14) 0.2117(3) 0.02855(8) 0.0222(5) Uani 1 1 d . . .
C38 C 0.62651(14) 0.2396(3) 0.03251(10) 0.0282(6) Uani 1 1 d . . .
H38A H 0.6420 0.3209 0.0468 0.034 Uiso 1 1 calc R . .
C39 C 0.67402(16) 0.1479(3) 0.01547(10) 0.0323(7) Uani 1 1 d . . .
H39A H 0.7224 0.1666 0.0179 0.039 Uiso 1 1 calc R . .
C40 C 0.65144(16) 0.0286(3) -0.00519(10) 0.0320(7) Uani 1 1 d . . .
H40A H 0.6845 -0.0341 -0.0167 0.038 Uiso 1 1 calc R . .
C41 C 0.58141(17) 0.0007(3) -0.00907(9) 0.0313(7) Uani 1 1 d . . .
H41A H 0.5663 -0.0815 -0.0230 0.038 Uiso 1 1 calc R . .
C42 C 0.53299(15) 0.0929(3) 0.00744(8) 0.0255(6) Uani 1 1 d . . .
H42A H 0.4846 0.0750 0.0044 0.031 Uiso 1 1 calc R . .
C43 C 0.50843(14) 0.3088(3) 0.10513(8) 0.0229(6) Uani 1 1 d . . .
C44 C 0.55260(16) 0.2052(3) 0.12040(9) 0.0298(6) Uani 1 1 d . . .
H44A H 0.5757 0.1405 0.1033 0.036 Uiso 1 1 calc R . .
C45 C 0.56284(19) 0.1967(4) 0.16058(10) 0.0413(8) Uani 1 1 d . . .
H45A H 0.5924 0.1247 0.1710 0.050 Uiso 1 1 calc R . .
C46 C 0.53057(19) 0.2919(4) 0.18566(9) 0.0418(8) Uani 1 1 d . . .
H46A H 0.5392 0.2874 0.2132 0.050 Uiso 1 1 calc R . .
C47 C 0.48592(18) 0.3932(4) 0.17069(9) 0.0383(7) Uani 1 1 d . . .
H47A H 0.4632 0.4580 0.1879 0.046 Uiso 1 1 calc R . .
C48 C 0.47411(16) 0.4008(3) 0.13063(8) 0.0309(7) Uani 1 1 d . . .
H48A H 0.4424 0.4693 0.1205 0.037 Uiso 1 1 calc R . .
C321 C 0.52895(17) 0.4584(3) -0.04615(9) 0.0327(7) Uani 1 1 d . . .
H32A H 0.4890 0.4112 -0.0325 0.039 Uiso 1 1 calc R . .
C322 C 0.5682(2) 0.3435(4) -0.06966(10) 0.0471(9) Uani 1 1 d . . .
H32B H 0.5912 0.2775 -0.0514 0.071 Uiso 1 1 calc R . .
H32C H 0.6032 0.3892 -0.0864 0.071 Uiso 1 1 calc R . .
H32D H 0.5352 0.2906 -0.0861 0.071 Uiso 1 1 calc R . .
C323 C 0.4995(2) 0.5707(4) -0.07419(10) 0.0469(9) Uani 1 1 d . . .
H32E H 0.4743 0.6433 -0.0591 0.070 Uiso 1 1 calc R . .
H32F H 0.4676 0.5248 -0.0928 0.070 Uiso 1 1 calc R . .
H32G H 0.5377 0.6159 -0.0887 0.070 Uiso 1 1 calc R . .
C361 C 0.56731(18) 0.6761(3) 0.09105(9) 0.0346(7) Uani 1 1 d . . .
H36A H 0.5199 0.6346 0.0952 0.041 Uiso 1 1 calc R . .
C362 C 0.6153(2) 0.6181(4) 0.12343(12) 0.0534(10) Uani 1 1 d . . .
H36B H 0.6157 0.5135 0.1224 0.080 Uiso 1 1 calc R . .
H36C H 0.5982 0.6495 0.1492 0.080 Uiso 1 1 calc R . .
H36D H 0.6626 0.6544 0.1194 0.080 Uiso 1 1 calc R . .
C363 C 0.5615(2) 0.8392(3) 0.09462(11) 0.0494(9) Uani 1 1 d . . .
H36E H 0.5284 0.8751 0.0750 0.074 Uiso 1 1 calc R . .
H36F H 0.6073 0.8824 0.0901 0.074 Uiso 1 1 calc R . .
H36G H 0.5452 0.8643 0.1211 0.074 Uiso 1 1 calc R . .
O3 O 0.1865(5) 1.4175(9) 0.3819(3) 0.124(3) Uiso 0.661(10) 1 d PD A 2
C51 C 0.1334(5) 1.3541(12) 0.4000(3) 0.102(3) Uiso 0.661(10) 1 d PD A 2
H51A H 0.1499 1.3065 0.4243 0.122 Uiso 0.661(10) 1 calc PR A 2
H51B H 0.1127 1.2807 0.3826 0.122 Uiso 0.661(10) 1 calc PR A 2
C52 C 0.0816(6) 1.4606(12) 0.4097(3) 0.094(3) Uiso 0.661(10) 1 d PD A 2
H52A H 0.0613 1.4423 0.4360 0.113 Uiso 0.661(10) 1 calc PR A 2
H52B H 0.0438 1.4619 0.3900 0.113 Uiso 0.661(10) 1 calc PR A 2
C53 C 0.1249(6) 1.6099(13) 0.4093(4) 0.121(4) Uiso 0.661(10) 1 d PD A 2
H53A H 0.1159 1.6669 0.3853 0.145 Uiso 0.661(10) 1 calc PR A 2
H53B H 0.1161 1.6685 0.4330 0.145 Uiso 0.661(10) 1 calc PR A 2
C54 C 0.2001(9) 1.5404(18) 0.4094(5) 0.153(7) Uiso 0.661(10) 1 d PD A 2
H54A H 0.2358 1.6065 0.3989 0.184 Uiso 0.661(10) 1 calc PR A 2
H54B H 0.2139 1.5074 0.4360 0.184 Uiso 0.661(10) 1 calc PR A 2
O3A O 0.1047(8) 1.5947(16) 0.4464(5) 0.112(5) Uiso 0.339(10) 1 d PD A 1
C51A C 0.1634(12) 1.634(3) 0.4287(7) 0.128(8) Uiso 0.339(10) 1 d PD A 1
H51C H 0.2003 1.6367 0.4490 0.153 Uiso 0.339(10) 1 calc PR A 1
H51D H 0.1569 1.7328 0.4192 0.153 Uiso 0.339(10) 1 calc PR A 1
C52A C 0.1897(8) 1.5517(14) 0.3964(5) 0.055(4) Uiso 0.339(10) 1 d PD A 1
H52C H 0.2409 1.5395 0.3964 0.066 Uiso 0.339(10) 1 calc PR A 1
H52D H 0.1724 1.5824 0.3703 0.066 Uiso 0.339(10) 1 calc PR A 1
C53A C 0.1493(13) 1.426(3) 0.4146(10) 0.144(10) Uiso 0.339(10) 1 d PD A 1
H53C H 0.1667 1.3974 0.4409 0.172 Uiso 0.339(10) 1 calc PR A 1
H53D H 0.1455 1.3422 0.3969 0.172 Uiso 0.339(10) 1 calc PR A 1
C54A C 0.0771(12) 1.526(3) 0.4162(7) 0.117(8) Uiso 0.339(10) 1 d PD A 1
H54C H 0.0700 1.5859 0.3926 0.140 Uiso 0.339(10) 1 calc PR A 1
H54D H 0.0345 1.4712 0.4227 0.140 Uiso 0.339(10) 1 calc PR A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O1 1.8713(18) . ?
Ge1 N1 1.920(2) . ?
Ge1 Cl3 2.1759(8) . ?
Ge1 Cl2 2.1765(8) . ?
Ge1 Cl1 2.2487(8) . ?
P1 N1 1.643(2) . ?
P1 C17 1.789(3) . ?
P1 C23 1.803(3) . ?
P1 C1 1.818(3) . ?
N1 C11 1.466(4) . ?
O1 C1 1.408(3) . ?
C1 C2 1.515(4) . ?
C1 H1A 1.0000 . ?
C2 C3 1.504(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C11 C12 1.390(5) . ?
C11 C16 1.402(5) . ?
C12 C13 1.404(5) . ?
C12 C121 1.522(5) . ?
C13 C14 1.378(7) . ?
C13 H13A 0.9500 . ?
C14 C15 1.365(7) . ?
C14 H14A 0.9500 . ?
C15 C16 1.394(5) . ?
C15 H15A 0.9500 . ?
C16 C161 1.513(6) . ?
C17 C22 1.392(4) . ?
C17 C18 1.393(4) . ?
C18 C19 1.380(5) . ?
C18 H18A 0.9500 . ?
C19 C20 1.384(5) . ?
C19 H19A 0.9500 . ?
C20 C21 1.379(5) . ?
C20 H20A 0.9500 . ?
C21 C22 1.392(4) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 C24 1.384(4) . ?
C23 C28 1.392(4) . ?
C24 C25 1.386(5) . ?
C24 H24A 0.9500 . ?
C25 C26 1.375(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.379(5) . ?
C26 H26A 0.9500 . ?
C27 C28 1.380(4) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
C121 C123 1.530(5) . ?
C121 C122 1.534(5) . ?
C121 H12A 1.0000 . ?
C122 H12B 0.9800 . ?
C122 H12C 0.9800 . ?
C122 H12D 0.9800 . ?
C123 H12E 0.9800 . ?
C123 H12F 0.9800 . ?
C123 H12G 0.9800 . ?
C161 C162 1.521(6) . ?
C161 C163 1.539(5) . ?
C161 H16A 1.0000 . ?
C162 H16B 0.9800 . ?
C162 H16C 0.9800 . ?
C162 H16D 0.9800 . ?
C163 H16E 0.9800 . ?
C163 H16F 0.9800 . ?
C163 H16G 0.9800 . ?
Ge2 O2 1.8679(18) . ?
Ge2 N2 1.911(2) . ?
Ge2 Cl6 2.1726(8) . ?
Ge2 Cl4 2.1878(8) . ?
Ge2 Cl5 2.2529(7) . ?
P2 N2 1.649(2) . ?
P2 C43 1.794(3) . ?
P2 C37 1.795(3) . ?
P2 C4 1.825(3) . ?
N2 C31 1.455(4) . ?
O2 C4 1.406(3) . ?
C4 C5 1.531(4) . ?
C4 H4A 1.0000 . ?
C5 C6 1.527(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C31 C36 1.405(4) . ?
C31 C32 1.408(4) . ?
C32 C33 1.404(4) . ?
C32 C321 1.515(4) . ?
C33 C34 1.386(5) . ?
C33 H33A 0.9500 . ?
C34 C35 1.367(5) . ?
C34 H34A 0.9500 . ?
C35 C36 1.399(5) . ?
C35 H35A 0.9500 . ?
C36 C361 1.515(5) . ?
C37 C42 1.392(4) . ?
C37 C38 1.396(4) . ?
C38 C39 1.380(4) . ?
C38 H38A 0.9500 . ?
C39 C40 1.389(5) . ?
C39 H39A 0.9500 . ?
C40 C41 1.377(5) . ?
C40 H40A 0.9500 . ?
C41 C42 1.387(4) . ?
C41 H41A 0.9500 . ?
C42 H42A 0.9500 . ?
C43 C44 1.389(4) . ?
C43 C48 1.388(4) . ?
C44 C45 1.382(5) . ?
C44 H44A 0.9500 . ?
C45 C46 1.380(5) . ?
C45 H45A 0.9500 . ?
C46 C47 1.376(5) . ?
C46 H46A 0.9500 . ?
C47 C48 1.382(5) . ?
C47 H47A 0.9500 . ?
C48 H48A 0.9500 . ?
C321 C323 1.527(5) . ?
C321 C322 1.538(5) . ?
C321 H32A 1.0000 . ?
C322 H32B 0.9800 . ?
C322 H32C 0.9800 . ?
C322 H32D 0.9800 . ?
C323 H32E 0.9800 . ?
C323 H32F 0.9800 . ?
C323 H32G 0.9800 . ?
C361 C362 1.534(5) . ?
C361 C363 1.536(4) . ?
C361 H36A 1.0000 . ?
C362 H36B 0.9800 . ?
C362 H36C 0.9800 . ?
C362 H36D 0.9800 . ?
C363 H36E 0.9800 . ?
C363 H36F 0.9800 . ?
C363 H36G 0.9800 . ?
O3 C51 1.332(12) . ?
O3 C54 1.505(16) . ?
C51 C52 1.446(14) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.626(15) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.585(17) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
O3A C54A 1.33(2) . ?
O3A C51A 1.33(2) . ?
C51A C52A 1.43(2) . ?
C51A C54A 1.99(3) . ?
C51A C53A 2.02(4) . ?
C51A H51C 0.9900 . ?
C51A H51D 0.9900 . ?
C52A C53A 1.54(2) . ?
C52A H52C 0.9900 . ?
C52A H52D 0.9900 . ?
C53A C54A 1.67(2) . ?
C53A H53C 0.9900 . ?
C53A H53D 0.9900 . ?
C54A H54C 0.9900 . ?
C54A H54D 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
O1 Ge1 N1 87.34(9) . . ?
O1 Ge1 Cl3 91.80(7) . . ?
N1 Ge1 Cl3 118.86(7) . . ?
O1 Ge1 Cl2 86.69(6) . . ?
N1 Ge1 Cl2 126.19(7) . . ?
Cl3 Ge1 Cl2 114.74(4) . . ?
O1 Ge1 Cl1 175.52(7) . . ?
N1 Ge1 Cl1 91.15(7) . . ?
Cl3 Ge1 Cl1 92.62(3) . . ?
Cl2 Ge1 Cl1 90.81(3) . . ?
N1 P1 C17 114.34(12) . . ?
N1 P1 C23 114.87(12) . . ?
C17 P1 C23 107.45(13) . . ?
N1 P1 C1 100.20(12) . . ?
C17 P1 C1 113.73(13) . . ?
C23 P1 C1 105.98(13) . . ?
C11 N1 P1 118.85(17) . . ?
C11 N1 Ge1 126.93(17) . . ?
P1 N1 Ge1 113.50(12) . . ?
C1 O1 Ge1 116.20(15) . . ?
O1 C1 C2 111.6(2) . . ?
O1 C1 P1 101.77(16) . . ?
C2 C1 P1 114.0(2) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
P1 C1 H1A 109.7 . . ?
C3 C2 C1 113.3(3) . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C12 C11 C16 122.3(3) . . ?
C12 C11 N1 118.7(3) . . ?
C16 C11 N1 119.0(3) . . ?
C11 C12 C13 117.9(3) . . ?
C11 C12 C121 124.9(3) . . ?
C13 C12 C121 117.2(3) . . ?
C14 C13 C12 120.3(4) . . ?
C14 C13 H13A 119.8 . . ?
C12 C13 H13A 119.8 . . ?
C15 C14 C13 120.7(3) . . ?
C15 C14 H14A 119.6 . . ?
C13 C14 H14A 119.6 . . ?
C14 C15 C16 121.4(4) . . ?
C14 C15 H15A 119.3 . . ?
C16 C15 H15A 119.3 . . ?
C15 C16 C11 117.3(4) . . ?
C15 C16 C161 119.2(3) . . ?
C11 C16 C161 123.5(3) . . ?
C22 C17 C18 120.5(3) . . ?
C22 C17 P1 118.5(2) . . ?
C18 C17 P1 120.8(2) . . ?
C19 C18 C17 119.5(3) . . ?
C19 C18 H18A 120.2 . . ?
C17 C18 H18A 120.2 . . ?
C18 C19 C20 120.0(3) . . ?
C18 C19 H19A 120.0 . . ?
C20 C19 H19A 120.0 . . ?
C21 C20 C19 120.7(3) . . ?
C21 C20 H20A 119.6 . . ?
C19 C20 H20A 119.6 . . ?
C20 C21 C22 119.9(3) . . ?
C20 C21 H21A 120.0 . . ?
C22 C21 H21A 120.0 . . ?
C17 C22 C21 119.3(3) . . ?
C17 C22 H22A 120.4 . . ?
C21 C22 H22A 120.4 . . ?
C24 C23 C28 119.4(3) . . ?
C24 C23 P1 120.9(2) . . ?
C28 C23 P1 119.1(2) . . ?
C25 C24 C23 119.7(3) . . ?
C25 C24 H24A 120.2 . . ?
C23 C24 H24A 120.2 . . ?
C26 C25 C24 120.9(3) . . ?
C26 C25 H25A 119.5 . . ?
C24 C25 H25A 119.5 . . ?
C25 C26 C27 119.4(3) . . ?
C25 C26 H26A 120.3 . . ?
C27 C26 H26A 120.3 . . ?
C26 C27 C28 120.4(3) . . ?
C26 C27 H27A 119.8 . . ?
C28 C27 H27A 119.8 . . ?
C27 C28 C23 120.2(3) . . ?
C27 C28 H28A 119.9 . . ?
C23 C28 H28A 119.9 . . ?
C12 C121 C123 112.5(3) . . ?
C12 C121 C122 110.5(3) . . ?
C123 C121 C122 110.1(3) . . ?
C12 C121 H12A 107.8 . . ?
C123 C121 H12A 107.8 . . ?
C122 C121 H12A 107.8 . . ?
C121 C122 H12B 109.5 . . ?
C121 C122 H12C 109.5 . . ?
H12B C122 H12C 109.5 . . ?
C121 C122 H12D 109.5 . . ?
H12B C122 H12D 109.5 . . ?
H12C C122 H12D 109.5 . . ?
C121 C123 H12E 109.5 . . ?
C121 C123 H12F 109.5 . . ?
H12E C123 H12F 109.5 . . ?
C121 C123 H12G 109.5 . . ?
H12E C123 H12G 109.5 . . ?
H12F C123 H12G 109.5 . . ?
C16 C161 C162 112.3(4) . . ?
C16 C161 C163 111.5(4) . . ?
C162 C161 C163 111.1(3) . . ?
C16 C161 H16A 107.2 . . ?
C162 C161 H16A 107.2 . . ?
C163 C161 H16A 107.2 . . ?
C161 C162 H16B 109.5 . . ?
C161 C162 H16C 109.5 . . ?
H16B C162 H16C 109.5 . . ?
C161 C162 H16D 109.5 . . ?
H16B C162 H16D 109.5 . . ?
H16C C162 H16D 109.5 . . ?
C161 C163 H16E 109.5 . . ?
C161 C163 H16F 109.5 . . ?
H16E C163 H16F 109.5 . . ?
C161 C163 H16G 109.5 . . ?
H16E C163 H16G 109.5 . . ?
H16F C163 H16G 109.5 . . ?
O2 Ge2 N2 87.58(8) . . ?
O2 Ge2 Cl6 92.05(7) . . ?
N2 Ge2 Cl6 118.05(7) . . ?
O2 Ge2 Cl4 86.46(6) . . ?
N2 Ge2 Cl4 125.31(7) . . ?
Cl6 Ge2 Cl4 116.46(4) . . ?
O2 Ge2 Cl5 175.07(7) . . ?
N2 Ge2 Cl5 91.59(7) . . ?
Cl6 Ge2 Cl5 92.62(3) . . ?
Cl4 Ge2 Cl5 90.06(3) . . ?
N2 P2 C43 112.85(12) . . ?
N2 P2 C37 114.72(12) . . ?
C43 P2 C37 107.88(13) . . ?
N2 P2 C4 99.65(11) . . ?
C43 P2 C4 108.84(12) . . ?
C37 P2 C4 112.70(13) . . ?
C31 N2 P2 117.73(17) . . ?
C31 N2 Ge2 128.01(17) . . ?
P2 N2 Ge2 113.77(12) . . ?
C4 O2 Ge2 115.85(15) . . ?
O2 C4 C5 111.5(2) . . ?
O2 C4 P2 102.00(17) . . ?
C5 C4 P2 113.76(18) . . ?
O2 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
P2 C4 H4A 109.8 . . ?
C6 C5 C4 111.7(2) . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C4 C5 H5B 109.3 . . ?
H5A C5 H5B 107.9 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C36 C31 C32 121.3(3) . . ?
C36 C31 N2 119.6(3) . . ?
C32 C31 N2 119.0(2) . . ?
C33 C32 C31 118.0(3) . . ?
C33 C32 C321 118.4(3) . . ?
C31 C32 C321 123.6(3) . . ?
C34 C33 C32 120.9(3) . . ?
C34 C33 H33A 119.5 . . ?
C32 C33 H33A 119.5 . . ?
C35 C34 C33 119.9(3) . . ?
C35 C34 H34A 120.1 . . ?
C33 C34 H34A 120.1 . . ?
C34 C35 C36 122.0(3) . . ?
C34 C35 H35A 119.0 . . ?
C36 C35 H35A 119.0 . . ?
C35 C36 C31 117.6(3) . . ?
C35 C36 C361 118.7(3) . . ?
C31 C36 C361 123.7(3) . . ?
C42 C37 C38 120.2(3) . . ?
C42 C37 P2 118.9(2) . . ?
C38 C37 P2 120.8(2) . . ?
C39 C38 C37 119.3(3) . . ?
C39 C38 H38A 120.4 . . ?
C37 C38 H38A 120.4 . . ?
C38 C39 C40 120.4(3) . . ?
C38 C39 H39A 119.8 . . ?
C40 C39 H39A 119.8 . . ?
C41 C40 C39 120.4(3) . . ?
C41 C40 H40A 119.8 . . ?
C39 C40 H40A 119.8 . . ?
C40 C41 C42 119.9(3) . . ?
C40 C41 H41A 120.0 . . ?
C42 C41 H41A 120.0 . . ?
C41 C42 C37 119.8(3) . . ?
C41 C42 H42A 120.1 . . ?
C37 C42 H42A 120.1 . . ?
C44 C43 C48 119.3(3) . . ?
C44 C43 P2 121.1(2) . . ?
C48 C43 P2 119.5(2) . . ?
C45 C44 C43 119.7(3) . . ?
C45 C44 H44A 120.1 . . ?
C43 C44 H44A 120.1 . . ?
C46 C45 C44 120.6(3) . . ?
C46 C45 H45A 119.7 . . ?
C44 C45 H45A 119.7 . . ?
C47 C46 C45 119.8(3) . . ?
C47 C46 H46A 120.1 . . ?
C45 C46 H46A 120.1 . . ?
C46 C47 C48 120.1(3) . . ?
C46 C47 H47A 119.9 . . ?
C48 C47 H47A 119.9 . . ?
C47 C48 C43 120.3(3) . . ?
C47 C48 H48A 119.8 . . ?
C43 C48 H48A 119.8 . . ?
C32 C321 C323 109.8(3) . . ?
C32 C321 C322 113.2(3) . . ?
C323 C321 C322 109.8(3) . . ?
C32 C321 H32A 107.9 . . ?
C323 C321 H32A 107.9 . . ?
C322 C321 H32A 107.9 . . ?
C321 C322 H32B 109.5 . . ?
C321 C322 H32C 109.5 . . ?
H32B C322 H32C 109.5 . . ?
C321 C322 H32D 109.5 . . ?
H32B C322 H32D 109.5 . . ?
H32C C322 H32D 109.5 . . ?
C321 C323 H32E 109.5 . . ?
C321 C323 H32F 109.5 . . ?
H32E C323 H32F 109.5 . . ?
C321 C323 H32G 109.5 . . ?
H32E C323 H32G 109.5 . . ?
H32F C323 H32G 109.5 . . ?
C36 C361 C362 112.2(3) . . ?
C36 C361 C363 110.6(3) . . ?
C362 C361 C363 109.8(3) . . ?
C36 C361 H36A 108.0 . . ?
C362 C361 H36A 108.0 . . ?
C363 C361 H36A 108.0 . . ?
C361 C362 H36B 109.5 . . ?
C361 C362 H36C 109.5 . . ?
H36B C362 H36C 109.5 . . ?
C361 C362 H36D 109.5 . . ?
H36B C362 H36D 109.5 . . ?
H36C C362 H36D 109.5 . . ?
C361 C363 H36E 109.5 . . ?
C361 C363 H36F 109.5 . . ?
H36E C363 H36F 109.5 . . ?
C361 C363 H36G 109.5 . . ?
H36E C363 H36G 109.5 . . ?
H36F C363 H36G 109.5 . . ?
C51 O3 C54 100.7(11) . . ?
O3 C51 C52 109.0(9) . . ?
O3 C51 H51A 109.9 . . ?
C52 C51 H51A 109.9 . . ?
O3 C51 H51B 109.9 . . ?
C52 C51 H51B 109.9 . . ?
H51A C51 H51B 108.3 . . ?
C51 C52 C53 103.8(9) . . ?
C51 C52 H52A 111.0 . . ?
C53 C52 H52A 111.0 . . ?
C51 C52 H52B 111.0 . . ?
C53 C52 H52B 111.0 . . ?
H52A C52 H52B 109.0 . . ?
C54 C53 C52 96.5(10) . . ?
C54 C53 H53A 112.5 . . ?
C52 C53 H53A 112.5 . . ?
C54 C53 H53B 112.5 . . ?
C52 C53 H53B 112.5 . . ?
H53A C53 H53B 110.0 . . ?
O3 C54 C53 98.9(11) . . ?
O3 C54 H54A 112.0 . . ?
C53 C54 H54A 112.0 . . ?
O3 C54 H54B 112.0 . . ?
C53 C54 H54B 112.0 . . ?
H54A C54 H54B 109.7 . . ?
C54A O3A C51A 96.9(18) . . ?
O3A C51A C52A 119.9(19) . . ?
O3A C51A C54A 41.4(11) . . ?
C52A C51A C54A 81.8(14) . . ?
O3A C51A C53A 74.3(14) . . ?
C52A C51A C53A 49.4(11) . . ?
C54A C51A C53A 49.3(10) . . ?
O3A C51A H51C 107.3 . . ?
C52A C51A H51C 107.3 . . ?
C54A C51A H51C 139.5 . . ?
C53A C51A H51C 106.8 . . ?
O3A C51A H51D 107.3 . . ?
C52A C51A H51D 107.3 . . ?
C54A C51A H51D 107.6 . . ?
C53A C51A H51D 143.9 . . ?
H51C C51A H51D 106.9 . . ?
C51A C52A C53A 85.7(17) . . ?
C51A C52A H52C 114.4 . . ?
C53A C52A H52C 114.4 . . ?
C51A C52A H52D 114.4 . . ?
C53A C52A H52D 114.4 . . ?
H52C C52A H52D 111.5 . . ?
C52A C53A C54A 90.3(16) . . ?
C52A C53A C51A 44.9(11) . . ?
C54A C53A C51A 64.3(14) . . ?
C52A C53A H53C 113.6 . . ?
C54A C53A H53C 113.6 . . ?
C51A C53A H53C 90.1 . . ?
C52A C53A H53D 113.6 . . ?
C54A C53A H53D 113.6 . . ?
C51A C53A H53D 156.4 . . ?
H53C C53A H53D 110.9 . . ?
O3A C54A C53A 88.0(18) . . ?
O3A C54A C51A 41.7(11) . . ?
C53A C54A C51A 66.4(15) . . ?
O3A C54A H54C 114.0 . . ?
C53A C54A H54C 114.0 . . ?
C51A C54A H54C 89.9 . . ?
O3A C54A H54D 114.0 . . ?
C53A C54A H54D 114.0 . . ?
C51A C54A H54D 154.6 . . ?
H54C C54A H54D 111.2 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        62.13
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.047
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_yy-140702
_database_code_depnum_ccdc_archive 'CCDC 1424122'
_audit_update_record             
;
2015-09-12 deposited with the CCDC.
2015-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H84 Cl6 Ge2 N2 O5 P2'
_chemical_formula_weight         1429.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   13.6361(9)
_cell_length_b                   11.3768(6)
_cell_length_c                   24.1644(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.974(5)
_cell_angle_gamma                90.00
_cell_volume                     3734.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3556
_cell_measurement_theta_min      3.2570
_cell_measurement_theta_max      28.3020

_exptl_crystal_description       'square plate'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1484
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8973
_exptl_absorpt_correction_T_max  0.9467
_exptl_absorpt_process_details   empirical

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11568
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         24.06
_reflns_number_total             5807
_reflns_number_gt                4699
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1130P)²+2.4678P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'refined in a riding mode to the carrier atom'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5807
_refine_ls_number_parameters     410
_refine_ls_number_restraints     150
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0569
_refine_ls_wR_factor_ref         0.1734
_refine_ls_wR_factor_gt          0.1588
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.71198(4) 0.31090(4) 0.13682(2) 0.0401(2) Uani 1 1 d . . .
P1 P 0.76035(8) 0.08472(9) 0.08387(4) 0.0268(3) Uani 1 1 d . . .
Cl1 Cl 0.68848(11) 0.46566(10) 0.08513(6) 0.0593(4) Uani 1 1 d . . .
Cl2 Cl 0.61456(9) 0.28014(12) 0.20145(6) 0.0523(3) Uani 1 1 d . . .
Cl3 Cl 0.81995(8) 0.41090(9) 0.19535(5) 0.0392(3) Uani 1 1 d . . .
O1 O 0.6262(2) 0.2345(3) 0.08387(13) 0.0391(7) Uani 1 1 d . . .
N1 N 0.8050(2) 0.1913(3) 0.12518(13) 0.0265(7) Uani 1 1 d . . .
C1 C 0.6284(3) 0.1111(4) 0.08796(17) 0.0327(9) Uani 1 1 d . . .
H1A H 0.6087 0.0860 0.1251 0.039 Uiso 1 1 calc R . .
C2 C 0.5612(3) 0.0537(4) 0.04182(17) 0.0328(9) Uani 1 1 d . . .
C3 C 0.5179(3) -0.0544(4) 0.05098(19) 0.0402(11) Uani 1 1 d . . .
H3A H 0.5299 -0.0923 0.0859 0.048 Uiso 1 1 calc R . .
C4 C 0.5428(3) 0.1069(4) -0.0090(2) 0.0408(11) Uani 1 1 d . . .
H4A H 0.5722 0.1807 -0.0156 0.049 Uiso 1 1 calc R . .
C11 C 0.9048(3) 0.1810(3) 0.15181(16) 0.0281(9) Uani 1 1 d . . .
C12 C 0.9194(3) 0.1206(4) 0.20281(16) 0.0303(9) Uani 1 1 d . . .
C13 C 1.0159(3) 0.1072(4) 0.22589(18) 0.0375(10) Uani 1 1 d . . .
H13A H 1.0280 0.0646 0.2596 0.045 Uiso 1 1 calc R . .
C14 C 1.0939(3) 0.1537(4) 0.20122(19) 0.0402(11) Uani 1 1 d . . .
H14A H 1.1591 0.1428 0.2177 0.048 Uiso 1 1 calc R . .
C15 C 1.0777(3) 0.2164(4) 0.15250(19) 0.0365(10) Uani 1 1 d . . .
H15A H 1.1319 0.2490 0.1357 0.044 Uiso 1 1 calc R . .
C16 C 0.9828(3) 0.2326(4) 0.12766(17) 0.0313(9) Uani 1 1 d . . .
C21 C 0.7847(3) 0.1020(4) 0.01223(17) 0.0324(9) Uani 1 1 d . . .
C22 C 0.7749(4) 0.2134(4) -0.01262(18) 0.0409(11) Uani 1 1 d . . .
H22A H 0.7619 0.2802 0.0091 0.049 Uiso 1 1 calc R . .
C23 C 0.7842(4) 0.2255(5) -0.0687(2) 0.0517(13) Uani 1 1 d . . .
H23A H 0.7766 0.3007 -0.0856 0.062 Uiso 1 1 calc R . .
C24 C 0.8043(4) 0.1293(5) -0.1005(2) 0.0544(14) Uani 1 1 d . . .
H24A H 0.8120 0.1386 -0.1389 0.065 Uiso 1 1 calc R . .
C25 C 0.8133(4) 0.0195(5) -0.0763(2) 0.0544(14) Uani 1 1 d . . .
H25A H 0.8267 -0.0468 -0.0983 0.065 Uiso 1 1 calc R . .
C26 C 0.8029(4) 0.0053(4) -0.01978(19) 0.0426(11) Uani 1 1 d . . .
H26A H 0.8082 -0.0706 -0.0034 0.051 Uiso 1 1 calc R . .
C27 C 0.8010(3) -0.0584(4) 0.10622(16) 0.0311(9) Uani 1 1 d . . .
C28 C 0.8973(4) -0.0938(4) 0.10054(18) 0.0385(10) Uani 1 1 d . . .
H28A H 0.9431 -0.0406 0.0867 0.046 Uiso 1 1 calc R . .
C29 C 0.9259(4) -0.2082(4) 0.1154(2) 0.0466(12) Uani 1 1 d . . .
H29A H 0.9915 -0.2330 0.1116 0.056 Uiso 1 1 calc R . .
C30 C 0.8596(4) -0.2850(4) 0.1354(2) 0.0488(13) Uani 1 1 d . . .
H30A H 0.8794 -0.3633 0.1444 0.059 Uiso 1 1 calc R . .
C31 C 0.7654(4) -0.2499(4) 0.1425(2) 0.0465(12) Uani 1 1 d . . .
H31A H 0.7205 -0.3035 0.1568 0.056 Uiso 1 1 calc R . .
C32 C 0.7353(4) -0.1350(4) 0.12862(18) 0.0389(10) Uani 1 1 d . . .
H32A H 0.6706 -0.1096 0.1344 0.047 Uiso 1 1 calc R . .
C121 C 0.8366(3) 0.0718(4) 0.23452(17) 0.0348(10) Uani 1 1 d . . .
H12A H 0.7742 0.0743 0.2095 0.042 Uiso 1 1 calc R . .
C122 C 0.8553(4) -0.0552(4) 0.25284(19) 0.0445(11) Uani 1 1 d . . .
H12B H 0.8770 -0.1009 0.2217 0.067 Uiso 1 1 calc R . .
H12C H 0.7945 -0.0892 0.2646 0.067 Uiso 1 1 calc R . .
H12D H 0.9065 -0.0571 0.2839 0.067 Uiso 1 1 calc R . .
C123 C 0.8233(4) 0.1496(5) 0.28568(19) 0.0472(12) Uani 1 1 d . . .
H12E H 0.8155 0.2318 0.2740 0.071 Uiso 1 1 calc R . .
H12F H 0.8813 0.1421 0.3124 0.071 Uiso 1 1 calc R . .
H12G H 0.7646 0.1242 0.3032 0.071 Uiso 1 1 calc R . .
C161 C 0.9692(3) 0.3101(4) 0.07573(18) 0.0371(10) Uani 1 1 d . . .
H16A H 0.8971 0.3157 0.0644 0.045 Uiso 1 1 calc R . .
C162 C 1.0190(4) 0.2567(5) 0.0274(2) 0.0505(12) Uani 1 1 d . . .
H16B H 0.9939 0.1769 0.0203 0.076 Uiso 1 1 calc R . .
H16C H 1.0903 0.2537 0.0369 0.076 Uiso 1 1 calc R . .
H16D H 1.0046 0.3051 -0.0058 0.076 Uiso 1 1 calc R . .
C163 C 1.0075(4) 0.4339(4) 0.0881(2) 0.0511(13) Uani 1 1 d . . .
H16E H 0.9738 0.4675 0.1186 0.077 Uiso 1 1 calc R . .
H16F H 0.9948 0.4830 0.0549 0.077 Uiso 1 1 calc R . .
H16G H 1.0785 0.4310 0.0987 0.077 Uiso 1 1 calc R . .
O2 O 0.5202(3) -0.0236(5) 0.18927(19) 0.0849(13) Uani 1 1 d DU . .
C33 C 0.4171(6) -0.0044(10) 0.1857(4) 0.110(2) Uani 1 1 d DU . .
H33A H 0.3824 -0.0792 0.1916 0.131 Uiso 1 1 calc R . .
H33B H 0.3942 0.0260 0.1484 0.131 Uiso 1 1 calc R . .
C34 C 0.3960(6) 0.0801(9) 0.2279(4) 0.106(2) Uani 1 1 d DU . .
H34A H 0.3323 0.0619 0.2427 0.128 Uiso 1 1 calc R . .
H34B H 0.3927 0.1606 0.2122 0.128 Uiso 1 1 calc R . .
C35 C 0.4787(6) 0.0706(8) 0.2729(3) 0.0937(19) Uani 1 1 d DU . .
H35A H 0.4560 0.0357 0.3071 0.112 Uiso 1 1 calc R . .
H35B H 0.5088 0.1482 0.2817 0.112 Uiso 1 1 calc R . .
C36 C 0.5504(5) -0.0113(7) 0.2461(3) 0.0783(16) Uani 1 1 d DU . .
H36A H 0.6177 0.0219 0.2508 0.094 Uiso 1 1 calc R . .
H36B H 0.5514 -0.0891 0.2645 0.094 Uiso 1 1 calc R . .
O3 O 0.2829(6) 0.2895(8) 0.0803(4) 0.078(2) Uani 0.50 1 d PDU . .
C37 C 0.3222(13) 0.3907(16) 0.1104(6) 0.098(3) Uani 0.50 1 d PDU . .
H37A H 0.3655 0.3666 0.1435 0.118 Uiso 0.50 1 calc PR . .
H37B H 0.2686 0.4406 0.1225 0.118 Uiso 0.50 1 calc PR . .
C38 C 0.3823(10) 0.4577(12) 0.0677(7) 0.082(3) Uani 0.50 1 d PDU . .
H38A H 0.3407 0.5155 0.0459 0.098 Uiso 0.50 1 calc PR . .
H38B H 0.4400 0.4984 0.0865 0.098 Uiso 0.50 1 calc PR . .
C39 C 0.4099(7) 0.3692(11) 0.0354(4) 0.055(2) Uani 0.50 1 d PDU . .
H39A H 0.4689 0.3289 0.0530 0.066 Uiso 0.50 1 calc PR . .
H39B H 0.4249 0.3991 -0.0014 0.066 Uiso 0.50 1 calc PR . .
C40 C 0.3301(11) 0.2938(15) 0.0302(6) 0.088(3) Uani 0.50 1 d PDU . .
H40A H 0.3526 0.2139 0.0209 0.106 Uiso 0.50 1 calc PR . .
H40B H 0.2826 0.3207 -0.0005 0.106 Uiso 0.50 1 calc PR . .


_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 O1 1.871(3) . ?
Ge1 N1 1.898(3) . ?
Ge1 Cl2 2.1648(14) . ?
Ge1 Cl1 2.1664(13) . ?
Ge1 Cl3 2.2586(11) . ?
P1 N1 1.653(3) . ?
P1 C27 1.788(4) . ?
P1 C21 1.802(4) . ?
P1 C1 1.835(4) . ?
O1 C1 1.407(5) . ?
N1 C11 1.458(5) . ?
C1 C2 1.527(5) . ?
C1 H1A 1.0000 . ?
C2 C4 1.373(6) . ?
C2 C3 1.390(6) . ?
C3 C4 1.387(6) 3_655 ?
C3 H3A 0.9500 . ?
C4 C3 1.387(6) 3_655 ?
C4 H4A 0.9500 . ?
C11 C16 1.387(6) . ?
C11 C12 1.410(6) . ?
C12 C13 1.393(6) . ?
C12 C121 1.523(6) . ?
C13 C14 1.370(7) . ?
C13 H13A 0.9500 . ?
C14 C15 1.378(7) . ?
C14 H14A 0.9500 . ?
C15 C16 1.391(6) . ?
C15 H15A 0.9500 . ?
C16 C161 1.532(6) . ?
C21 C26 1.379(6) . ?
C21 C22 1.404(6) . ?
C22 C23 1.378(7) . ?
C22 H22A 0.9500 . ?
C23 C24 1.378(8) . ?
C23 H23A 0.9500 . ?
C24 C25 1.380(8) . ?
C24 H24A 0.9500 . ?
C25 C26 1.394(7) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C27 C32 1.393(6) . ?
C27 C28 1.391(6) . ?
C28 C29 1.397(6) . ?
C28 H28A 0.9500 . ?
C29 C30 1.376(8) . ?
C29 H29A 0.9500 . ?
C30 C31 1.370(8) . ?
C30 H30A 0.9500 . ?
C31 C32 1.402(7) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?
C121 C122 1.527(6) . ?
C121 C123 1.544(6) . ?
C121 H12A 1.0000 . ?
C122 H12B 0.9800 . ?
C122 H12C 0.9800 . ?
C122 H12D 0.9800 . ?
C123 H12E 0.9800 . ?
C123 H12F 0.9800 . ?
C123 H12G 0.9800 . ?
C161 C163 1.522(6) . ?
C161 C162 1.526(7) . ?
C161 H16A 1.0000 . ?
C162 H16B 0.9800 . ?
C162 H16C 0.9800 . ?
C162 H16D 0.9800 . ?
C163 H16E 0.9800 . ?
C163 H16F 0.9800 . ?
C163 H16G 0.9800 . ?
O2 C36 1.407(8) . ?
O2 C33 1.418(9) . ?
C33 C34 1.448(13) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.501(11) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.533(11) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
O3 C40 1.420(16) . ?
O3 C37 1.440(17) . ?
C37 C38 1.569(19) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.348(17) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.383(16) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 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
O1 Ge1 N1 87.23(13) . . ?
O1 Ge1 Cl2 91.83(11) . . ?
N1 Ge1 Cl2 116.80(11) . . ?
O1 Ge1 Cl1 86.05(10) . . ?
N1 Ge1 Cl1 124.38(11) . . ?
Cl2 Ge1 Cl1 118.56(6) . . ?
O1 Ge1 Cl3 175.63(11) . . ?
N1 Ge1 Cl3 92.64(10) . . ?
Cl2 Ge1 Cl3 92.13(5) . . ?
Cl1 Ge1 Cl3 90.43(5) . . ?
N1 P1 C27 113.39(17) . . ?
N1 P1 C21 114.28(19) . . ?
C27 P1 C21 108.14(19) . . ?
N1 P1 C1 99.15(18) . . ?
C27 P1 C1 114.4(2) . . ?
C21 P1 C1 107.30(19) . . ?
C1 O1 Ge1 114.0(2) . . ?
C11 N1 P1 119.2(3) . . ?
C11 N1 Ge1 127.0(2) . . ?
P1 N1 Ge1 113.54(17) . . ?
O1 C1 C2 111.6(3) . . ?
O1 C1 P1 100.0(3) . . ?
C2 C1 P1 114.8(3) . . ?
O1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
P1 C1 H1A 110.0 . . ?
C4 C2 C3 119.0(4) . . ?
C4 C2 C1 121.1(4) . . ?
C3 C2 C1 119.9(4) . . ?
C2 C3 C4 120.0(4) . 3_655 ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 3_655 . ?
C2 C4 C3 121.0(4) . 3_655 ?
C2 C4 H4A 119.5 . . ?
C3 C4 H4A 119.5 3_655 . ?
C16 C11 C12 121.2(4) . . ?
C16 C11 N1 120.0(4) . . ?
C12 C11 N1 118.7(4) . . ?
C13 C12 C11 117.4(4) . . ?
C13 C12 C121 118.3(4) . . ?
C11 C12 C121 124.2(4) . . ?
C14 C13 C12 121.7(4) . . ?
C14 C13 H13A 119.1 . . ?
C12 C13 H13A 119.1 . . ?
C15 C14 C13 119.9(4) . . ?
C15 C14 H14A 120.1 . . ?
C13 C14 H14A 120.1 . . ?
C14 C15 C16 120.8(4) . . ?
C14 C15 H15A 119.6 . . ?
C16 C15 H15A 119.6 . . ?
C11 C16 C15 118.7(4) . . ?
C11 C16 C161 123.1(4) . . ?
C15 C16 C161 118.1(4) . . ?
C26 C21 C22 119.7(4) . . ?
C26 C21 P1 120.6(3) . . ?
C22 C21 P1 119.4(3) . . ?
C23 C22 C21 119.8(5) . . ?
C23 C22 H22A 120.1 . . ?
C21 C22 H22A 120.1 . . ?
C22 C23 C24 120.5(5) . . ?
C22 C23 H23A 119.7 . . ?
C24 C23 H23A 119.7 . . ?
C23 C24 C25 119.8(5) . . ?
C23 C24 H24A 120.1 . . ?
C25 C24 H24A 120.1 . . ?
C24 C25 C26 120.4(5) . . ?
C24 C25 H25A 119.8 . . ?
C26 C25 H25A 119.8 . . ?
C21 C26 C25 119.7(5) . . ?
C21 C26 H26A 120.2 . . ?
C25 C26 H26A 120.2 . . ?
C32 C27 C28 120.1(4) . . ?
C32 C27 P1 119.6(3) . . ?
C28 C27 P1 120.3(3) . . ?
C27 C28 C29 119.3(4) . . ?
C27 C28 H28A 120.3 . . ?
C29 C28 H28A 120.3 . . ?
C30 C29 C28 120.3(5) . . ?
C30 C29 H29A 119.8 . . ?
C28 C29 H29A 119.8 . . ?
C31 C30 C29 120.7(4) . . ?
C31 C30 H30A 119.6 . . ?
C29 C30 H30A 119.6 . . ?
C30 C31 C32 120.0(5) . . ?
C30 C31 H31A 120.0 . . ?
C32 C31 H31A 120.0 . . ?
C27 C32 C31 119.4(5) . . ?
C27 C32 H32A 120.3 . . ?
C31 C32 H32A 120.3 . . ?
C12 C121 C122 112.2(4) . . ?
C12 C121 C123 109.7(4) . . ?
C122 C121 C123 109.8(4) . . ?
C12 C121 H12A 108.3 . . ?
C122 C121 H12A 108.3 . . ?
C123 C121 H12A 108.3 . . ?
C121 C122 H12B 109.5 . . ?
C121 C122 H12C 109.5 . . ?
H12B C122 H12C 109.5 . . ?
C121 C122 H12D 109.5 . . ?
H12B C122 H12D 109.5 . . ?
H12C C122 H12D 109.5 . . ?
C121 C123 H12E 109.5 . . ?
C121 C123 H12F 109.5 . . ?
H12E C123 H12F 109.5 . . ?
C121 C123 H12G 109.5 . . ?
H12E C123 H12G 109.5 . . ?
H12F C123 H12G 109.5 . . ?
C163 C161 C162 110.6(4) . . ?
C163 C161 C16 110.9(4) . . ?
C162 C161 C16 111.6(4) . . ?
C163 C161 H16A 107.9 . . ?
C162 C161 H16A 107.9 . . ?
C16 C161 H16A 107.9 . . ?
C161 C162 H16B 109.5 . . ?
C161 C162 H16C 109.5 . . ?
H16B C162 H16C 109.5 . . ?
C161 C162 H16D 109.5 . . ?
H16B C162 H16D 109.5 . . ?
H16C C162 H16D 109.5 . . ?
C161 C163 H16E 109.5 . . ?
C161 C163 H16F 109.5 . . ?
H16E C163 H16F 109.5 . . ?
C161 C163 H16G 109.5 . . ?
H16E C163 H16G 109.5 . . ?
H16F C163 H16G 109.5 . . ?
C36 O2 C33 104.4(6) . . ?
O2 C33 C34 108.4(7) . . ?
O2 C33 H33A 110.0 . . ?
C34 C33 H33A 110.0 . . ?
O2 C33 H33B 110.0 . . ?
C34 C33 H33B 110.0 . . ?
H33A C33 H33B 108.4 . . ?
C33 C34 C35 106.2(7) . . ?
C33 C34 H34A 110.5 . . ?
C35 C34 H34A 110.5 . . ?
C33 C34 H34B 110.5 . . ?
C35 C34 H34B 110.5 . . ?
H34A C34 H34B 108.7 . . ?
C34 C35 C36 101.9(7) . . ?
C34 C35 H35A 111.4 . . ?
C36 C35 H35A 111.4 . . ?
C34 C35 H35B 111.4 . . ?
C36 C35 H35B 111.4 . . ?
H35A C35 H35B 109.3 . . ?
O2 C36 C35 109.2(6) . . ?
O2 C36 H36A 109.8 . . ?
C35 C36 H36A 109.8 . . ?
O2 C36 H36B 109.8 . . ?
C35 C36 H36B 109.8 . . ?
H36A C36 H36B 108.3 . . ?
C40 O3 C37 103.1(9) . . ?
O3 C37 C38 104.4(11) . . ?
O3 C37 H37A 110.9 . . ?
C38 C37 H37A 110.9 . . ?
O3 C37 H37B 110.9 . . ?
C38 C37 H37B 110.9 . . ?
H37A C37 H37B 108.9 . . ?
C39 C38 C37 101.9(11) . . ?
C39 C38 H38A 111.4 . . ?
C37 C38 H38A 111.4 . . ?
C39 C38 H38B 111.4 . . ?
C37 C38 H38B 111.4 . . ?
H38A C38 H38B 109.2 . . ?
C38 C39 C40 105.0(11) . . ?
C38 C39 H39A 110.8 . . ?
C40 C39 H39A 110.8 . . ?
C38 C39 H39B 110.8 . . ?
C40 C39 H39B 110.8 . . ?
H39A C39 H39B 108.8 . . ?
C39 C40 O3 110.8(11) . . ?
C39 C40 H40A 109.5 . . ?
O3 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
O3 C40 H40B 109.5 . . ?
H40A C40 H40B 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        24.06
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.325
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.109
