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

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

data_exp_1998
_database_code_depnum_ccdc_archive 'CCDC 1410343'
_audit_update_record             
;
2016-03-18 deposited with the CCDC.
2016-08-09 downloaded from the CCDC.
;





_audit_creation_date             2015-02-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014-3

_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C46 H51 Ge N2 O P'
_chemical_formula_sum            'C46 H51 Ge N2 O P'
_chemical_formula_weight         751.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O P Ge'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.91699(11)
_cell_length_b                   19.62321(16)
_cell_length_c                   14.94628(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.7717(7)
_cell_angle_gamma                90
_cell_volume                     4067.62(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14288
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      65.4180
_cell_measurement_theta_min      3.7110
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.930
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20983
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.369
_diffrn_reflns_theta_min         3.726
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -30.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.9338   77.0000 -120.0000 100

#__ type_ start__ end____ width___ exp.time_
  2 omega  -84.00  -35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.9338 -178.0000    0.0000 49

#__ type_ start__ end____ width___ exp.time_
  3 omega    8.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       87.6717  -95.0000   30.0000 101

#__ type_ start__ end____ width___ exp.time_
  4 omega    8.00  110.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       87.6717  -95.0000  150.0000 102

#__ type_ start__ end____ width___ exp.time_
  5 omega   25.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       87.6717  -45.0000    0.0000 73

#__ type_ start__ end____ width___ exp.time_
  6 omega    9.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       87.6717  -15.0000 -150.0000 119

#__ type_ start__ end____ width___ exp.time_
  7 omega   24.00   90.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       87.6717  -30.0000   90.0000 66

#__ type_ start__ end____ width___ exp.time_
  8 omega   76.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       87.6717   45.0000 -150.0000 76

#__ type_ start__ end____ width___ exp.time_
  9 omega   16.00  118.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       87.6717  -77.0000 -120.0000 102
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0232592000
_diffrn_orient_matrix_UB_12      0.0318180000
_diffrn_orient_matrix_UB_13      -0.0899171000
_diffrn_orient_matrix_UB_21      -0.0355912000
_diffrn_orient_matrix_UB_22      0.0697327000
_diffrn_orient_matrix_UB_23      0.0312498000
_diffrn_orient_matrix_UB_31      0.1026046000
_diffrn_orient_matrix_UB_32      0.0169746000
_diffrn_orient_matrix_UB_33      0.0404873000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6414
_reflns_number_total             6846
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         6846
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0251
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0355P)²+2.1496P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0678
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.43470(2) 0.19388(2) 0.74889(2) 0.01467(6) Uani 1 1 d . . . . .
P1 P 0.43085(2) 0.07678(2) 0.74703(2) 0.01680(9) Uani 1 1 d . . . . .
O1 O 0.24249(7) 0.11890(5) 0.74780(7) 0.0218(2) Uani 1 1 d . . . . .
C2 C 0.26570(10) 0.00213(7) 0.75510(9) 0.0150(3) Uani 1 1 d . . . . .
N2 N 0.20628(8) -0.01669(6) 0.81713(8) 0.0165(2) Uani 1 1 d . . . . .
N1 N 0.27700(9) -0.05198(6) 0.70208(8) 0.0172(3) Uani 1 1 d . . . . .
C35 C 0.39757(11) 0.23561(7) 0.86075(10) 0.0187(3) Uani 1 1 d . . . . .
C1 C 0.30539(10) 0.07329(7) 0.74797(9) 0.0163(3) Uani 1 1 d . . . . .
C6 C 0.22515(12) 0.04238(8) 0.96250(10) 0.0238(3) Uani 1 1 d . . . . .
C34 C 0.36267(11) 0.23453(7) 0.64334(10) 0.0176(3) Uani 1 1 d . . . . .
C3 C 0.22341(11) -0.10613(8) 0.73147(11) 0.0215(3) Uani 1 1 d . . . . .
C24 C 0.45892(12) -0.12613(9) 0.71953(11) 0.0289(4) Uani 1 1 d . . . . .
C5 C 0.16860(11) 0.02800(7) 0.88338(10) 0.0188(3) Uani 1 1 d . . . . .
C41 C 0.57065(10) 0.21775(8) 0.74096(9) 0.0189(3) Uani 1 1 d . . . . .
C36 C 0.30432(12) 0.23080(8) 0.88843(10) 0.0220(3) Uani 1 1 d . . . . .
C4 C 0.18036(11) -0.08439(8) 0.80339(11) 0.0213(3) Uani 1 1 d . . . . .
C29 C 0.26415(11) 0.24870(8) 0.64145(10) 0.0209(3) Uani 1 1 d . . . . .
C45 C 0.69783(13) 0.30193(9) 0.73441(11) 0.0295(4) Uani 1 1 d . . . . .
C17 C 0.33308(11) -0.05603(7) 0.62422(10) 0.0189(3) Uani 1 1 d . . . . .
C23 C 0.56345(14) -0.10245(11) 0.74069(14) 0.0377(4) Uani 1 1 d . . . . .
C18 C 0.41714(11) -0.09542(8) 0.63206(10) 0.0220(3) Uani 1 1 d . . . . .
C46 C 0.60095(12) 0.28564(8) 0.73674(11) 0.0244(3) Uani 1 1 d . . . . .
C7 C 0.18530(15) 0.08621(9) 1.02296(11) 0.0346(4) Uani 1 1 d . . . . .
C10 C 0.07615(11) 0.05436(8) 0.86311(10) 0.0235(3) Uani 1 1 d . . . . .
C32 C 0.35661(13) 0.26803(8) 0.48675(11) 0.0274(4) Uani 1 1 d . . . . .
C21 C 0.35047(14) -0.03370(9) 0.47016(11) 0.0315(4) Uani 1 1 d . . . . .
C31 C 0.25896(13) 0.28167(8) 0.48607(11) 0.0269(4) Uani 1 1 d . . . . .
C30 C 0.21292(12) 0.27277(8) 0.56378(11) 0.0244(3) Uani 1 1 d . . . . .
C12 C 0.32494(12) 0.01317(9) 0.98603(11) 0.0271(4) Uani 1 1 d . . . . .
C39 C 0.44249(15) 0.30136(10) 0.99512(13) 0.0390(5) Uani 1 1 d . . . . .
C9 C 0.04005(14) 0.09684(9) 0.92722(12) 0.0341(4) Uani 1 1 d . . . . .
C40 C 0.46648(13) 0.27067(9) 0.91609(11) 0.0294(4) Uani 1 1 d . . . . .
C11 C 0.32359(15) -0.03461(10) 1.06708(14) 0.0369(4) Uani 1 1 d . . . . .
C13 C 0.40009(15) 0.06967(10) 1.00404(13) 0.0351(4) Uani 1 1 d . . . . .
C16 C -0.00031(13) 0.10780(10) 0.72292(13) 0.0306(4) Uani 1 1 d . . . . .
C8 C 0.09425(16) 0.11265(10) 1.00582(12) 0.0399(5) Uani 1 1 d . . . . .
C37 C 0.28049(13) 0.26220(8) 0.96714(11) 0.0283(4) Uani 1 1 d . . . . .
C19 C 0.46499(12) -0.10416(9) 0.55461(11) 0.0286(4) Uani 1 1 d . . . . .
C33 C 0.40804(12) 0.24505(8) 0.56475(10) 0.0223(3) Uani 1 1 d . . . . .
C42 C 0.64096(11) 0.16708(8) 0.74200(10) 0.0216(3) Uani 1 1 d . . . . .
C20 C 0.43172(13) -0.07412(10) 0.47465(12) 0.0334(4) Uani 1 1 d . . . . .
C44 C 0.76617(12) 0.25067(10) 0.73522(11) 0.0308(4) Uani 1 1 d . . . . .
C27 C 0.21024(13) 0.02245(9) 0.53730(12) 0.0296(4) Uani 1 1 d . . . . .
C38 C 0.34952(15) 0.29787(9) 1.01990(12) 0.0347(4) Uani 1 1 d . . . . .
C22 C 0.29859(12) -0.02334(8) 0.54507(10) 0.0234(3) Uani 1 1 d . . . . .
C43 C 0.73756(12) 0.18339(10) 0.73873(11) 0.0281(4) Uani 1 1 d . . . . .
C25 C 0.45287(15) -0.20387(10) 0.71839(15) 0.0362(4) Uani 1 1 d . . . . .
C28 C 0.23319(18) 0.09263(10) 0.50289(17) 0.0453(5) Uani 1 1 d . . . . .
C15 C 0.01711(12) 0.04122(9) 0.77488(11) 0.0267(4) Uani 1 1 d . . . . .
C14 C -0.07773(16) 0.00504(13) 0.79045(18) 0.0478(5) Uani 1 1 d . . . . .
C26 C 0.12954(18) -0.00992(13) 0.4757(2) 0.0608(7) Uani 1 1 d . . . . .
H42 H 0.6221(12) 0.1198(9) 0.7446(11) 0.020(4) Uiso 1 1 d . . . . .
H29 H 0.2296(13) 0.2396(9) 0.6930(12) 0.023(4) Uiso 1 1 d . . . . .
H33 H 0.4757(14) 0.2361(9) 0.5638(11) 0.025(4) Uiso 1 1 d . . . . .
H36 H 0.2579(14) 0.2056(9) 0.8557(12) 0.024(4) Uiso 1 1 d . . . . .
H30 H 0.1439(15) 0.2830(10) 0.5636(13) 0.034(5) Uiso 1 1 d . . . . .
H46 H 0.5542(13) 0.3230(10) 0.7373(12) 0.028(5) Uiso 1 1 d . . . . .
H19 H 0.5236(14) -0.1307(9) 0.5584(12) 0.028(5) Uiso 1 1 d . . . . .
H4 H 0.1406(13) -0.1057(9) 0.8431(12) 0.026(4) Uiso 1 1 d . . . . .
H12 H 0.3441(13) -0.0124(9) 0.9362(13) 0.027(5) Uiso 1 1 d . . . . .
H27 H 0.1867(15) 0.0257(10) 0.5917(15) 0.037(5) Uiso 1 1 d . . . . .
H11A H 0.2764(16) -0.0693(11) 1.0543(14) 0.039(5) Uiso 1 1 d . . . . .
H43 H 0.7834(15) 0.1485(10) 0.7391(13) 0.034(5) Uiso 1 1 d . . . . .
H3 H 0.2204(13) -0.1476(10) 0.7002(12) 0.025(4) Uiso 1 1 d . . . . .
H20 H 0.4662(14) -0.0796(10) 0.4255(14) 0.036(5) Uiso 1 1 d . . . . .
H40 H 0.5332(14) 0.2742(9) 0.9008(12) 0.031(5) Uiso 1 1 d . . . . .
H31 H 0.2240(14) 0.2954(9) 0.4338(13) 0.027(5) Uiso 1 1 d . . . . .
H24 H 0.4226(14) -0.1118(10) 0.7675(13) 0.034(5) Uiso 1 1 d . . . . .
H15 H 0.0536(13) 0.0134(10) 0.7392(12) 0.023(4) Uiso 1 1 d . . . . .
H44 H 0.8331(16) 0.2614(11) 0.7332(14) 0.042(6) Uiso 1 1 d . . . . .
H9 H -0.0235(16) 0.1152(11) 0.9157(14) 0.041(5) Uiso 1 1 d . . . . .
H32 H 0.3895(14) 0.2733(10) 0.4324(14) 0.037(5) Uiso 1 1 d . . . . .
H37 H 0.2149(15) 0.2579(10) 0.9835(13) 0.033(5) Uiso 1 1 d . . . . .
H16A H -0.0373(15) 0.0990(10) 0.6650(14) 0.039(5) Uiso 1 1 d . . . . .
H25A H 0.3886(18) -0.2201(11) 0.7049(15) 0.048(6) Uiso 1 1 d . . . . .
H23A H 0.6057(15) -0.1197(11) 0.6951(14) 0.038(5) Uiso 1 1 d . . . . .
H16B H -0.0362(18) 0.1399(12) 0.7558(15) 0.052(7) Uiso 1 1 d . . . . .
H13A H 0.4077(15) 0.0968(11) 0.9502(15) 0.046(6) Uiso 1 1 d . . . . .
H25B H 0.4900(15) -0.2207(11) 0.6745(14) 0.038(5) Uiso 1 1 d . . . . .
H7 H 0.2223(15) 0.0967(11) 1.0773(15) 0.042(6) Uiso 1 1 d . . . . .
H45 H 0.7157(14) 0.3498(11) 0.7321(13) 0.036(5) Uiso 1 1 d . . . . .
H38 H 0.3323(15) 0.3192(11) 1.0730(15) 0.041(6) Uiso 1 1 d . . . . .
H23B H 0.5875(16) -0.1201(11) 0.7975(16) 0.044(6) Uiso 1 1 d . . . . .
H16C H 0.0599(15) 0.1299(10) 0.7115(13) 0.034(5) Uiso 1 1 d . . . . .
H21 H 0.3292(15) -0.0112(10) 0.4143(14) 0.038(5) Uiso 1 1 d . . . . .
H28A H 0.2479(15) 0.0902(11) 0.4443(16) 0.040(6) Uiso 1 1 d . . . . .
H13B H 0.3785(16) 0.1004(12) 1.0490(15) 0.047(6) Uiso 1 1 d . . . . .
H8 H 0.0680(16) 0.1427(11) 1.0482(15) 0.047(6) Uiso 1 1 d . . . . .
H25C H 0.4790(16) -0.2229(12) 0.7786(16) 0.050(6) Uiso 1 1 d . . . . .
H13C H 0.4629(17) 0.0508(11) 1.0264(15) 0.047(6) Uiso 1 1 d . . . . .
H11B H 0.3858(17) -0.0550(11) 1.0796(14) 0.046(6) Uiso 1 1 d . . . . .
H11C H 0.3076(15) -0.0094(11) 1.1206(15) 0.044(6) Uiso 1 1 d . . . . .
H14A H -0.1116(18) -0.0054(12) 0.7362(17) 0.051(7) Uiso 1 1 d . . . . .
H28B H 0.1771(18) 0.1217(12) 0.5007(15) 0.052(6) Uiso 1 1 d . . . . .
H14B H -0.0647(18) -0.0376(14) 0.8202(17) 0.061(7) Uiso 1 1 d . . . . .
H14C H -0.1179(19) 0.0357(13) 0.8235(17) 0.061(7) Uiso 1 1 d . . . . .
H39 H 0.4917(17) 0.3249(12) 1.0326(16) 0.056(7) Uiso 1 1 d . . . . .
H26A H 0.076(2) 0.0202(13) 0.4684(17) 0.062(7) Uiso 1 1 d . . . . .
H23C H 0.5677(16) -0.0535(14) 0.7436(14) 0.051(6) Uiso 1 1 d . . . . .
H26B H 0.110(2) -0.0519(16) 0.5013(19) 0.079(9) Uiso 1 1 d . . . . .
H28C H 0.288(2) 0.1136(15) 0.5430(19) 0.080(9) Uiso 1 1 d . . . . .
H26C H 0.157(3) -0.0198(19) 0.411(3) 0.120(13) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 P1 2.2987(4) . ?
Ge1 C35 1.9688(14) . ?
Ge1 C34 1.9663(15) . ?
Ge1 C41 1.9623(14) . ?
P1 C1 1.7486(15) . ?
O1 C1 1.2519(18) . ?
C2 N2 1.3444(18) . ?
C2 N1 1.3419(18) . ?
C2 C1 1.5088(19) . ?
N2 C5 1.4529(18) . ?
N2 C4 1.3874(19) . ?
N1 C3 1.3902(19) . ?
N1 C17 1.4562(18) . ?
C35 C36 1.398(2) . ?
C35 C40 1.395(2) . ?
C6 C5 1.394(2) . ?
C6 C7 1.395(2) . ?
C6 C12 1.517(2) . ?
C34 C29 1.397(2) . ?
C34 C33 1.395(2) . ?
C3 C4 1.343(2) . ?
C24 C23 1.535(3) . ?
C24 C18 1.511(2) . ?
C24 C25 1.528(3) . ?
C5 C10 1.396(2) . ?
C41 C46 1.400(2) . ?
C41 C42 1.394(2) . ?
C36 C37 1.392(2) . ?
C29 C30 1.393(2) . ?
C45 C46 1.389(2) . ?
C45 C44 1.384(3) . ?
C17 C18 1.399(2) . ?
C17 C22 1.395(2) . ?
C18 C19 1.393(2) . ?
C7 C8 1.374(3) . ?
C10 C9 1.395(2) . ?
C10 C15 1.517(2) . ?
C32 C31 1.384(3) . ?
C32 C33 1.391(2) . ?
C21 C20 1.378(3) . ?
C21 C22 1.397(2) . ?
C31 C30 1.383(2) . ?
C12 C11 1.533(2) . ?
C12 C13 1.532(3) . ?
C39 C40 1.391(2) . ?
C39 C38 1.377(3) . ?
C9 C8 1.378(3) . ?
C16 C15 1.529(2) . ?
C37 C38 1.382(3) . ?
C19 C20 1.378(3) . ?
C42 C43 1.387(2) . ?
C44 C43 1.381(3) . ?
C27 C22 1.519(2) . ?
C27 C28 1.513(3) . ?
C27 C26 1.529(3) . ?
C15 C14 1.533(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C35 Ge1 P1 114.74(4) . . ?
C34 Ge1 P1 112.70(4) . . ?
C34 Ge1 C35 111.12(6) . . ?
C41 Ge1 P1 105.04(5) . . ?
C41 Ge1 C35 105.93(6) . . ?
C41 Ge1 C34 106.53(6) . . ?
C1 P1 Ge1 93.51(5) . . ?
N2 C2 C1 123.56(12) . . ?
N1 C2 N2 107.40(12) . . ?
N1 C2 C1 128.97(12) . . ?
C2 N2 C5 125.57(12) . . ?
C2 N2 C4 109.16(12) . . ?
C4 N2 C5 125.09(12) . . ?
C2 N1 C3 109.01(12) . . ?
C2 N1 C17 127.74(12) . . ?
C3 N1 C17 123.23(12) . . ?
C36 C35 Ge1 122.62(11) . . ?
C40 C35 Ge1 119.52(12) . . ?
C40 C35 C36 117.86(14) . . ?
O1 C1 P1 132.11(11) . . ?
O1 C1 C2 113.69(12) . . ?
C2 C1 P1 114.11(10) . . ?
C5 C6 C7 116.58(15) . . ?
C5 C6 C12 124.18(14) . . ?
C7 C6 C12 119.24(15) . . ?
C29 C34 Ge1 122.07(11) . . ?
C33 C34 Ge1 119.97(11) . . ?
C33 C34 C29 117.77(14) . . ?
C4 C3 N1 107.28(13) . . ?
C18 C24 C23 110.33(15) . . ?
C18 C24 C25 111.82(15) . . ?
C25 C24 C23 110.79(15) . . ?
C6 C5 N2 119.34(13) . . ?
C6 C5 C10 123.65(14) . . ?
C10 C5 N2 117.00(13) . . ?
C46 C41 Ge1 121.68(12) . . ?
C42 C41 Ge1 120.56(11) . . ?
C42 C41 C46 117.74(14) . . ?
C37 C36 C35 120.83(15) . . ?
C3 C4 N2 107.15(13) . . ?
C30 C29 C34 121.18(15) . . ?
C44 C45 C46 120.03(16) . . ?
C18 C17 N1 117.60(13) . . ?
C22 C17 N1 118.88(13) . . ?
C22 C17 C18 123.45(14) . . ?
C17 C18 C24 123.48(13) . . ?
C19 C18 C24 119.57(14) . . ?
C19 C18 C17 116.92(15) . . ?
C45 C46 C41 121.10(16) . . ?
C8 C7 C6 121.48(17) . . ?
C5 C10 C15 123.26(14) . . ?
C9 C10 C5 116.77(15) . . ?
C9 C10 C15 119.92(15) . . ?
C31 C32 C33 120.34(15) . . ?
C20 C21 C22 121.44(16) . . ?
C30 C31 C32 119.50(15) . . ?
C31 C30 C29 120.11(15) . . ?
C6 C12 C11 110.07(15) . . ?
C6 C12 C13 111.45(14) . . ?
C13 C12 C11 110.90(15) . . ?
C38 C39 C40 120.28(17) . . ?
C8 C9 C10 121.16(16) . . ?
C39 C40 C35 121.02(16) . . ?
C7 C8 C9 120.34(16) . . ?
C38 C37 C36 120.22(16) . . ?
C20 C19 C18 121.24(16) . . ?
C32 C33 C34 121.09(15) . . ?
C43 C42 C41 121.09(15) . . ?
C19 C20 C21 120.24(16) . . ?
C43 C44 C45 119.67(15) . . ?
C22 C27 C26 110.46(16) . . ?
C28 C27 C22 111.82(16) . . ?
C28 C27 C26 109.80(18) . . ?
C39 C38 C37 119.73(16) . . ?
C17 C22 C21 116.64(15) . . ?
C17 C22 C27 123.76(14) . . ?
C21 C22 C27 119.59(15) . . ?
C44 C43 C42 120.36(17) . . ?
C10 C15 C16 110.37(14) . . ?
C10 C15 C14 110.95(16) . . ?
C16 C15 C14 111.76(15) . . ?
_olex2_date_sample_data_collection 2015-06-27
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_test1
_database_code_depnum_ccdc_archive 'CCDC 1410347'
_audit_update_record             
;
2015-09-18 deposited with the CCDC.
2016-08-09 downloaded from the CCDC.
;



_audit_creation_date             2015-02-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H51 N2 O P Si'
_chemical_formula_sum            'C46 H51 N2 O P Si'
_chemical_formula_weight         706.95
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N P O Si'
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'
Si Si 0.2541 0.3302 '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'

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4352(3)
_cell_length_b                   12.6209(7)
_cell_length_c                   17.8147(8)
_cell_angle_alpha                85.360(4)
_cell_angle_beta                 78.369(3)
_cell_angle_gamma                76.089(3)
_cell_volume                     2015.71(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7024
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      65.3490
_cell_measurement_theta_min      4.3470
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10387
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.371
_diffrn_reflns_theta_min         3.610
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.9855
_diffrn_measured_fraction_theta_max 0.9855
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -110.00  -16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474  -57.0000   30.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega  -66.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474   57.0000 -180.0000 95

#__ type_ start__ end____ width___ exp.time_
  3 omega   29.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000   90.0000 74

#__ type_ start__ end____ width___ exp.time_
  4 omega   72.00  160.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932   45.0000   60.0000 88

#__ type_ start__ end____ width___ exp.time_
  5 omega   23.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000 -180.0000 86

#__ type_ start__ end____ width___ exp.time_
  6 omega    8.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000  -30.0000 100

#__ type_ start__ end____ width___ exp.time_
  7 omega   65.00  155.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932   30.0000  150.0000 90

#__ type_ start__ end____ width___ exp.time_
  8 omega  109.00  160.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  125.0000   30.0000 51

#__ type_ start__ end____ width___ exp.time_
  9 omega   21.00   75.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -30.0000  -60.0000 54

#__ type_ start__ end____ width___ exp.time_
 10 omega   14.00   82.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -30.0000  150.0000 68
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0066548000
_diffrn_orient_matrix_UB_12      -0.0735902000
_diffrn_orient_matrix_UB_13      0.0733661000
_diffrn_orient_matrix_UB_21      -0.0362958000
_diffrn_orient_matrix_UB_22      -0.0880489000
_diffrn_orient_matrix_UB_23      -0.0432381000
_diffrn_orient_matrix_UB_31      0.1672524000
_diffrn_orient_matrix_UB_32      -0.0516152000
_diffrn_orient_matrix_UB_33      -0.0234968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6096
_reflns_number_total             6580
_reflns_odcompleteness_completeness 98.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         6580
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0510
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0950P)²+0.6200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1445
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C15(H15), C24(H24), C27(H27), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C7(H7), C9(H9), C20(H20), C8(H8), C41(H41), C19(H19),
 C29(H29), C18(H18), C45(H45), C43(H43), C39(H39), C35(H35), C44(H44), C33(H33),
  C37(H37), C42(H42), C31(H31), C30(H30), C36(H36), C32(H32), C38(H38)
2.c Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C14(H14a,H14b,H14c), C16(H16a,H16b,H16c), C11(H11a,H11b,
 H11c), C23(H23a,H23b,H23c), C28(H28a,H28b,H28c), C26(H26a,H26b,H26c), C13(H13a,
 H13b,H13c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.70008(5) 0.06522(4) 0.29684(3) 0.02693(15) Uani 1 1 d . . . . .
Si1 Si 0.62164(5) 0.28007(4) 0.20591(3) 0.02558(15) Uani 1 1 d . . . . .
N1 N 0.71579(14) -0.22747(11) 0.23031(8) 0.0204(3) Uani 1 1 d . . . . .
N2 N 0.48435(14) -0.16135(11) 0.28339(8) 0.0212(3) Uani 1 1 d . . . . .
C2 C 0.62285(17) -0.13684(13) 0.26654(9) 0.0196(3) Uani 1 1 d . . . . .
O1 O 0.67179(15) 0.14785(10) 0.22000(8) 0.0350(3) Uani 1 1 d . . . . .
C6 C 0.93685(18) -0.23559(14) 0.13064(10) 0.0248(4) Uani 1 1 d . . . . .
C4 C 0.63615(18) -0.30646(14) 0.22684(10) 0.0247(4) Uani 1 1 d . . . . .
H4 H 0.6744 -0.3749 0.2057 0.030 Uiso 1 1 calc R . . . .
C5 C 0.87567(17) -0.24605(13) 0.20797(10) 0.0218(3) Uani 1 1 d . . . . .
C10 C 0.96071(18) -0.27920(14) 0.26508(10) 0.0263(4) Uani 1 1 d . . . . .
C3 C 0.49455(18) -0.26555(14) 0.25954(10) 0.0243(4) Uani 1 1 d . . . . .
H3 H 0.4167 -0.3007 0.2653 0.029 Uiso 1 1 calc R . . . .
C22 C 0.35609(17) -0.09253(14) 0.32878(10) 0.0225(4) Uani 1 1 d . . . . .
C46 C 0.53795(19) 0.30467(15) 0.11783(10) 0.0280(4) Uani 1 1 d . . . . .
C17 C 0.25494(18) -0.01936(14) 0.29073(10) 0.0258(4) Uani 1 1 d . . . . .
C7 C 1.09208(19) -0.26474(15) 0.11013(11) 0.0306(4) Uani 1 1 d . . . . .
H7 H 1.1372 -0.2592 0.0589 0.037 Uiso 1 1 calc R . . . .
C9 C 1.1154(2) -0.30840(16) 0.24118(12) 0.0334(4) Uani 1 1 d . . . . .
H9 H 1.1758 -0.3327 0.2773 0.040 Uiso 1 1 calc R . . . .
C20 C 0.2234(2) -0.02741(16) 0.45099(11) 0.0326(4) Uani 1 1 d . . . . .
H20 H 0.2114 -0.0294 0.5042 0.039 Uiso 1 1 calc R . . . .
C15 C 0.84037(19) -0.19017(15) 0.07148(10) 0.0289(4) Uani 1 1 d . . . . .
H15 H 0.7470 -0.2139 0.0878 0.035 Uiso 1 1 calc R . . . .
C1 C 0.66062(18) -0.04667(14) 0.28523(10) 0.0273(4) Uani 1 1 d . . . . .
C24 C 0.27043(19) -0.01692(16) 0.20428(11) 0.0306(4) Uani 1 1 d . . . . .
H24 H 0.3303 -0.0883 0.1866 0.037 Uiso 1 1 calc R . . . .
C21 C 0.33983(19) -0.10195(15) 0.40851(10) 0.0270(4) Uani 1 1 d . . . . .
C40 C 0.4816(2) 0.34568(16) 0.28921(11) 0.0325(4) Uani 1 1 d . . . . .
C8 C 1.17906(19) -0.30154(16) 0.16474(12) 0.0339(4) Uani 1 1 d . . . . .
H8 H 1.2819 -0.3220 0.1498 0.041 Uiso 1 1 calc R . . . .
C41 C 0.5851(2) 0.23036(17) 0.05863(11) 0.0375(5) Uani 1 1 d . . . . .
H41 H 0.6565 0.1665 0.0639 0.045 Uiso 1 1 calc R . . . .
C19 C 0.1259(2) 0.04928(16) 0.41484(12) 0.0355(4) Uani 1 1 d . . . . .
H19 H 0.0504 0.0996 0.4439 0.043 Uiso 1 1 calc R . . . .
C34 C 0.7846(2) 0.34412(14) 0.19125(12) 0.0317(4) Uani 1 1 d . . . . .
C27 C 0.4406(2) -0.19130(16) 0.44899(10) 0.0333(4) Uani 1 1 d . . . . .
H27 H 0.5024 -0.2422 0.4102 0.040 Uiso 1 1 calc R . . . .
C29 C 0.8076(2) 0.42031(16) 0.13171(13) 0.0387(5) Uani 1 1 d . . . . .
H29 H 0.7439 0.4363 0.0967 0.046 Uiso 1 1 calc R . . . .
C18 C 0.13909(19) 0.05217(16) 0.33610(11) 0.0333(4) Uani 1 1 d . . . . .
H18 H 0.0699 0.1024 0.3130 0.040 Uiso 1 1 calc R . . . .
C45 C 0.4310(2) 0.39889(18) 0.10726(12) 0.0375(4) Uani 1 1 d . . . . .
H45 H 0.3969 0.4489 0.1461 0.045 Uiso 1 1 calc R . . . .
C25 C 0.1215(2) 0.00029(17) 0.17829(12) 0.0364(4) Uani 1 1 d . . . . .
H25A H 0.0682 -0.0519 0.2047 0.055 Uiso 1 1 calc GR . . . .
H25B H 0.1387 -0.0093 0.1240 0.055 Uiso 1 1 calc GR . . . .
H25C H 0.0641 0.0728 0.1899 0.055 Uiso 1 1 calc GR . . . .
C12 C 0.8900(2) -0.28697(16) 0.34890(11) 0.0330(4) Uani 1 1 d . . . . .
H12 H 0.7910 -0.2377 0.3556 0.040 Uiso 1 1 calc R . . . .
C43 C 0.4223(2) 0.3457(2) -0.01740(12) 0.0447(5) Uani 1 1 d . . . . .
H43 H 0.3845 0.3595 -0.0625 0.054 Uiso 1 1 calc R . . . .
C39 C 0.4918(3) 0.44172(18) 0.31844(13) 0.0469(5) Uani 1 1 d . . . . .
H39 H 0.5719 0.4727 0.2978 0.056 Uiso 1 1 calc R . . . .
C35 C 0.3607(2) 0.3010(2) 0.32177(12) 0.0442(5) Uani 1 1 d . . . . .
H35 H 0.3516 0.2364 0.3036 0.053 Uiso 1 1 calc R . . . .
C44 C 0.3738(2) 0.4204(2) 0.04026(13) 0.0473(5) Uani 1 1 d . . . . .
H44 H 0.3033 0.4846 0.0342 0.057 Uiso 1 1 calc R . . . .
C14 C 0.9078(3) -0.2311(2) -0.00896(12) 0.0445(5) Uani 1 1 d . . . . .
H14A H 0.9924 -0.2009 -0.0295 0.067 Uiso 1 1 calc GR . . . .
H14B H 0.8350 -0.2088 -0.0413 0.067 Uiso 1 1 calc GR . . . .
H14C H 0.9384 -0.3093 -0.0069 0.067 Uiso 1 1 calc GR . . . .
C16 C 0.8018(3) -0.06569(18) 0.07037(13) 0.0458(5) Uani 1 1 d . . . . .
H16A H 0.7589 -0.0410 0.1213 0.069 Uiso 1 1 calc GR . . . .
H16B H 0.7318 -0.0382 0.0371 0.069 Uiso 1 1 calc GR . . . .
H16C H 0.8904 -0.0394 0.0519 0.069 Uiso 1 1 calc GR . . . .
C11 C 0.8681(3) -0.4023(2) 0.37124(14) 0.0551(6) Uani 1 1 d . . . . .
H11A H 0.8100 -0.4220 0.3385 0.083 Uiso 1 1 calc GR . . . .
H11B H 0.8172 -0.4043 0.4236 0.083 Uiso 1 1 calc GR . . . .
H11C H 0.9632 -0.4528 0.3657 0.083 Uiso 1 1 calc GR . . . .
C23 C 0.3541(2) 0.0684(2) 0.16633(13) 0.0497(6) Uani 1 1 d . . . . .
H23A H 0.2965 0.1399 0.1808 0.075 Uiso 1 1 calc GR . . . .
H23B H 0.3707 0.0635 0.1116 0.075 Uiso 1 1 calc GR . . . .
H23C H 0.4480 0.0556 0.1826 0.075 Uiso 1 1 calc GR . . . .
C28 C 0.3496(3) -0.25540(18) 0.50789(13) 0.0462(5) Uani 1 1 d . . . . .
H28A H 0.2918 -0.2083 0.5482 0.069 Uiso 1 1 calc GR . . . .
H28B H 0.4153 -0.3154 0.5290 0.069 Uiso 1 1 calc GR . . . .
H28C H 0.2844 -0.2829 0.4835 0.069 Uiso 1 1 calc GR . . . .
C33 C 0.8839(3) 0.3202(2) 0.24113(18) 0.0581(7) Uani 1 1 d . . . . .
H33 H 0.8722 0.2691 0.2811 0.070 Uiso 1 1 calc R . . . .
C37 C 0.2661(4) 0.4485(3) 0.40885(14) 0.0720(10) Uani 1 1 d . . . . .
H37 H 0.1940 0.4832 0.4484 0.086 Uiso 1 1 calc R . . . .
C26 C 0.5447(2) -0.14633(18) 0.48662(12) 0.0412(5) Uani 1 1 d . . . . .
H26A H 0.5997 -0.1049 0.4492 0.062 Uiso 1 1 calc GR . . . .
H26B H 0.6124 -0.2058 0.5069 0.062 Uiso 1 1 calc GR . . . .
H26C H 0.4873 -0.1000 0.5274 0.062 Uiso 1 1 calc GR . . . .
C42 C 0.5258(3) 0.25142(19) -0.00813(12) 0.0449(5) Uani 1 1 d . . . . .
H42 H 0.5570 0.2009 -0.0467 0.054 Uiso 1 1 calc R . . . .
C13 C 0.9759(3) -0.2495(2) 0.40165(13) 0.0536(6) Uani 1 1 d . . . . .
H13A H 1.0711 -0.2993 0.3994 0.080 Uiso 1 1 calc GR . . . .
H13B H 0.9211 -0.2481 0.4533 0.080 Uiso 1 1 calc GR . . . .
H13C H 0.9895 -0.1777 0.3854 0.080 Uiso 1 1 calc GR . . . .
C31 C 1.0189(3) 0.4489(2) 0.1733(2) 0.0718(10) Uani 1 1 d . . . . .
H31 H 1.0964 0.4842 0.1680 0.086 Uiso 1 1 calc R . . . .
C30 C 0.9238(3) 0.4730(2) 0.12346(16) 0.0552(7) Uani 1 1 d . . . . .
H30 H 0.9362 0.5246 0.0838 0.066 Uiso 1 1 calc R . . . .
C36 C 0.2534(3) 0.3529(3) 0.38162(14) 0.0645(9) Uani 1 1 d . . . . .
H36 H 0.1730 0.3227 0.4032 0.077 Uiso 1 1 calc R . . . .
C32 C 1.0012(3) 0.3722(3) 0.2318(2) 0.0807(11) Uani 1 1 d . . . . .
H32 H 1.0679 0.3551 0.2654 0.097 Uiso 1 1 calc R . . . .
C38 C 0.3843(4) 0.4922(2) 0.37797(15) 0.0709(9) Uani 1 1 d . . . . .
H38 H 0.3930 0.5564 0.3969 0.085 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
P1 O1 1.6778(14) . ?
P1 C1 1.5832(18) . ?
Si1 O1 1.6347(13) . ?
Si1 C46 1.8668(19) . ?
Si1 C40 1.8749(19) . ?
Si1 C34 1.8671(19) . ?
N1 C2 1.379(2) . ?
N1 C4 1.397(2) . ?
N1 C5 1.446(2) . ?
N2 C2 1.384(2) . ?
N2 C3 1.390(2) . ?
N2 C22 1.444(2) . ?
C2 C1 1.355(2) . ?
C6 C5 1.391(2) . ?
C6 C7 1.400(2) . ?
C6 C15 1.518(2) . ?
C4 C3 1.339(2) . ?
C5 C10 1.397(2) . ?
C10 C9 1.401(2) . ?
C10 C12 1.513(3) . ?
C22 C17 1.400(2) . ?
C22 C21 1.396(2) . ?
C46 C41 1.400(3) . ?
C46 C45 1.389(3) . ?
C17 C24 1.516(3) . ?
C17 C18 1.397(3) . ?
C7 C8 1.379(3) . ?
C9 C8 1.378(3) . ?
C20 C21 1.395(3) . ?
C20 C19 1.381(3) . ?
C15 C14 1.523(3) . ?
C15 C16 1.524(3) . ?
C24 C25 1.528(2) . ?
C24 C23 1.522(3) . ?
C21 C27 1.525(2) . ?
C40 C39 1.389(3) . ?
C40 C35 1.395(3) . ?
C41 C42 1.394(3) . ?
C19 C18 1.381(3) . ?
C34 C29 1.393(3) . ?
C34 C33 1.384(3) . ?
C27 C28 1.525(3) . ?
C27 C26 1.526(3) . ?
C29 C30 1.391(3) . ?
C45 C44 1.388(3) . ?
C12 C11 1.528(3) . ?
C12 C13 1.525(3) . ?
C43 C44 1.384(3) . ?
C43 C42 1.368(3) . ?
C39 C38 1.387(3) . ?
C35 C36 1.396(3) . ?
C33 C32 1.394(4) . ?
C37 C36 1.376(5) . ?
C37 C38 1.359(5) . ?
C31 C30 1.353(5) . ?
C31 C32 1.376(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 O1 108.44(8) . . ?
O1 Si1 C46 107.25(8) . . ?
O1 Si1 C40 111.41(8) . . ?
O1 Si1 C34 111.27(8) . . ?
C46 Si1 C40 109.53(8) . . ?
C46 Si1 C34 109.20(8) . . ?
C34 Si1 C40 108.16(9) . . ?
C2 N1 C4 110.11(13) . . ?
C2 N1 C5 125.76(13) . . ?
C4 N1 C5 123.66(13) . . ?
C2 N2 C3 109.94(13) . . ?
C2 N2 C22 122.95(14) . . ?
C3 N2 C22 126.57(13) . . ?
N1 C2 N2 104.57(13) . . ?
C1 C2 N1 127.57(14) . . ?
C1 C2 N2 127.77(14) . . ?
Si1 O1 P1 134.51(9) . . ?
C5 C6 C7 116.97(16) . . ?
C5 C6 C15 121.63(14) . . ?
C7 C6 C15 121.35(16) . . ?
C3 C4 N1 107.38(15) . . ?
C6 C5 N1 118.50(15) . . ?
C6 C5 C10 123.51(15) . . ?
C10 C5 N1 117.90(15) . . ?
C5 C10 C9 116.99(16) . . ?
C5 C10 C12 121.94(15) . . ?
C9 C10 C12 121.04(17) . . ?
C4 C3 N2 107.98(14) . . ?
C17 C22 N2 118.47(15) . . ?
C21 C22 N2 118.23(14) . . ?
C21 C22 C17 123.29(15) . . ?
C41 C46 Si1 120.93(15) . . ?
C45 C46 Si1 121.45(14) . . ?
C45 C46 C41 117.58(18) . . ?
C22 C17 C24 121.79(15) . . ?
C18 C17 C22 116.89(16) . . ?
C18 C17 C24 121.31(16) . . ?
C8 C7 C6 120.94(17) . . ?
C8 C9 C10 120.75(18) . . ?
C19 C20 C21 120.65(18) . . ?
C6 C15 C14 114.03(15) . . ?
C6 C15 C16 110.35(16) . . ?
C14 C15 C16 110.35(17) . . ?
C2 C1 P1 172.67(16) . . ?
C17 C24 C25 113.02(15) . . ?
C17 C24 C23 111.16(17) . . ?
C23 C24 C25 110.64(16) . . ?
C22 C21 C27 122.39(15) . . ?
C20 C21 C22 117.22(16) . . ?
C20 C21 C27 120.36(16) . . ?
C39 C40 Si1 121.34(16) . . ?
C39 C40 C35 118.10(19) . . ?
C35 C40 Si1 120.51(16) . . ?
C9 C8 C7 120.76(16) . . ?
C42 C41 C46 120.5(2) . . ?
C18 C19 C20 120.81(17) . . ?
C29 C34 Si1 121.44(15) . . ?
C33 C34 Si1 120.88(17) . . ?
C33 C34 C29 117.6(2) . . ?
C21 C27 C28 111.00(16) . . ?
C21 C27 C26 112.32(16) . . ?
C28 C27 C26 110.38(17) . . ?
C30 C29 C34 121.5(2) . . ?
C19 C18 C17 120.88(17) . . ?
C44 C45 C46 121.8(2) . . ?
C10 C12 C11 110.73(17) . . ?
C10 C12 C13 112.63(17) . . ?
C13 C12 C11 111.58(19) . . ?
C42 C43 C44 120.0(2) . . ?
C38 C39 C40 121.0(3) . . ?
C40 C35 C36 120.2(3) . . ?
C43 C44 C45 119.5(2) . . ?
C34 C33 C32 120.5(3) . . ?
C38 C37 C36 120.0(2) . . ?
C43 C42 C41 120.6(2) . . ?
C30 C31 C32 120.3(2) . . ?
C31 C30 C29 119.7(3) . . ?
C37 C36 C35 120.2(3) . . ?
C31 C32 C33 120.3(3) . . ?
C37 C38 C39 120.5(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_2625
_database_code_depnum_ccdc_archive 'CCDC 1410348'
_audit_update_record             
;
2016-03-18 deposited with the CCDC.
2016-08-09 downloaded from the CCDC.
;



_audit_creation_date             2015-07-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C46 H51 N2 O P Sn'
_chemical_formula_sum            'C46 H51 N2 O P Sn'
_chemical_formula_weight         797.54
_chemical_melting_point          ?
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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.0166(3)
_cell_length_b                   19.8309(6)
_cell_length_c                   14.9450(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.185(2)
_cell_angle_gamma                90
_cell_volume                     4143.07(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10386
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.3490
_cell_measurement_theta_min      4.3470
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.018
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40641
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.654
_diffrn_reflns_theta_min         2.814
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11320
_reflns_number_total             13762
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.361
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         13762
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0442
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0253P)²+2.4179P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0851
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.93092(2) 0.18297(2) 0.75048(2) 0.01663(4) Uani 1 1 d . . . . .
P1 P 0.93920(4) 0.05830(3) 0.74624(4) 0.01989(10) Uani 1 1 d . . . . .
O1 O 0.75988(10) 0.10827(7) 0.76203(10) 0.0222(3) Uani 1 1 d . . . . .
C2 C 0.76866(13) -0.00884(10) 0.75876(12) 0.0160(4) Uani 1 1 d . . . . .
N2 N 0.77858(11) -0.06217(8) 0.70464(11) 0.0184(3) Uani 1 1 d . . . . .
N1 N 0.70602(12) -0.02671(8) 0.81856(11) 0.0177(3) Uani 1 1 d . . . . .
C5 C 0.66381(15) 0.01813(10) 0.88164(13) 0.0202(4) Uani 1 1 d . . . . .
C35 C 1.07774(14) 0.21365(11) 0.73993(13) 0.0224(4) Uani 1 1 d . . . . .
C1 C 0.81558(13) 0.05908(10) 0.75480(12) 0.0165(4) Uani 1 1 d . . . . .
C6 C 0.71435(16) 0.03299(11) 0.96303(14) 0.0249(4) Uani 1 1 d . . . . .
C41 C 0.85077(14) 0.22830(10) 0.63774(13) 0.0196(4) Uani 1 1 d . . . . .
C44 C 0.74492(18) 0.28098(13) 0.48724(16) 0.0321(5) Uani 1 1 d . . . . .
C42 C 0.89584(16) 0.24901(11) 0.56237(14) 0.0242(4) Uani 1 1 d . . . . .
C14 C 0.52222(16) 0.03063(13) 0.76479(15) 0.0281(5) Uani 1 1 d . . . . .
C46 C 0.75144(15) 0.23551(12) 0.63625(15) 0.0239(4) Uani 1 1 d . . . . .
C18 C 0.91652(16) -0.10952(12) 0.63638(15) 0.0272(5) Uani 1 1 d . . . . .
C10 C 0.57305(16) 0.04395(11) 0.85612(14) 0.0248(4) Uani 1 1 d . . . . .
C23 C 0.9510(2) -0.14400(16) 0.72259(18) 0.0427(7) Uani 1 1 d . . . . .
C21 C 0.8657(2) -0.04062(14) 0.47787(16) 0.0360(6) Uani 1 1 d . . . . .
C3 C 0.67746(16) -0.09267(11) 0.80258(15) 0.0241(4) Uani 1 1 d . . . . .
C43 C 0.84332(19) 0.27476(13) 0.48728(16) 0.0314(5) Uani 1 1 d . . . . .
C30 C 0.95889(19) 0.27094(13) 0.91965(16) 0.0331(5) Uani 1 1 d . . . . .
C40 C 1.10695(18) 0.28059(13) 0.73557(17) 0.0324(5) Uani 1 1 d . . . . .
C4 C 0.72176(16) -0.11455(11) 0.73134(15) 0.0245(4) Uani 1 1 d . . . . .
C45 C 0.69920(17) 0.26229(13) 0.56191(16) 0.0302(5) Uani 1 1 d . . . . .
C17 C 0.83743(14) -0.06685(10) 0.62828(13) 0.0197(4) Uani 1 1 d . . . . .
C34 C 0.80045(18) 0.22577(12) 0.90251(16) 0.0284(5) Uani 1 1 d . . . . .
C19 C 0.96814(18) -0.11765(14) 0.56100(17) 0.0345(6) Uani 1 1 d . . . . .
C26 C 0.72750(17) 0.01880(13) 0.54395(15) 0.0295(5) Uani 1 1 d . . . . .
C29 C 0.89158(16) 0.23097(11) 0.87109(13) 0.0228(4) Uani 1 1 d . . . . .
C22 C 0.81065(15) -0.03030(11) 0.55060(14) 0.0242(4) Uani 1 1 d . . . . .
C8 C 0.5793(2) 0.10182(15) 0.99796(17) 0.0421(7) Uani 1 1 d . . . . .
C33 C 0.7775(2) 0.26150(14) 0.97853(18) 0.0395(6) Uani 1 1 d . . . . .
C13 C 0.8118(2) -0.03704(16) 1.0758(2) 0.0424(7) Uani 1 1 d . . . . .
C11 C 0.81357(17) 0.00582(12) 0.99037(15) 0.0287(5) Uani 1 1 d . . . . .
C24 C 1.0525(2) -0.11946(16) 0.7539(2) 0.0670(11) Uani 1 1 d . . . . .
H24A H 1.0967 -0.1335 0.7114 0.100 Uiso 1 1 calc GR . . . .
H24B H 1.0711 -0.1385 0.8116 0.100 Uiso 1 1 calc GR . . . .
H24C H 1.0527 -0.0712 0.7582 0.100 Uiso 1 1 calc GR . . . .
C28 C 0.7461(3) 0.08087(17) 0.4887(3) 0.0566(9) Uani 1 1 d . . . . .
C25 C 0.9506(2) -0.22070(17) 0.7136(2) 0.0444(7) Uani 1 1 d . . . . .
C9 C 0.5314(2) 0.08551(14) 0.91699(17) 0.0376(6) Uani 1 1 d . . . . .
C39 C 1.2037(2) 0.29701(15) 0.73409(18) 0.0395(6) Uani 1 1 d . . . . .
C12 C 0.8864(2) 0.06263(15) 1.0036(2) 0.0390(6) Uani 1 1 d . . . . .
C38 C 1.27154(18) 0.24684(16) 0.73657(18) 0.0401(7) Uani 1 1 d . . . . .
C31 C 0.9354(2) 0.30609(16) 0.99559(19) 0.0469(7) Uani 1 1 d . . . . .
C7 C 0.6697(2) 0.07630(13) 1.02051(16) 0.0364(6) Uani 1 1 d . . . . .
C20 C 0.9427(2) -0.08419(15) 0.48287(17) 0.0387(6) Uani 1 1 d . . . . .
C27 C 0.6364(2) -0.0156(2) 0.5097(4) 0.0676(12) Uani 1 1 d . . . . .
C32 C 0.8450(3) 0.30171(15) 1.02377(19) 0.0469(8) Uani 1 1 d . . . . .
C37 C 1.24466(16) 0.17995(15) 0.74069(17) 0.0337(5) Uani 1 1 d . . . . .
C36 C 1.14829(16) 0.16392(13) 0.74231(14) 0.0251(4) Uani 1 1 d . . . . .
C15 C 0.51192(19) 0.09624(14) 0.71148(19) 0.0344(6) Uani 1 1 d . . . . .
C16 C 0.4252(2) -0.00359(17) 0.7718(2) 0.0456(7) Uani 1 1 d . . . . .
H40 H 1.0619(16) 0.3143(12) 0.7307(15) 0.017(6) Uiso 1 1 d . . . . .
H3 H 0.6370(17) -0.1125(12) 0.8389(15) 0.020(6) Uiso 1 1 d . . . . .
H34 H 0.7532(16) 0.1998(11) 0.8735(15) 0.015(6) Uiso 1 1 d . . . . .
H11 H 0.8343(18) -0.0236(13) 0.9429(16) 0.030(7) Uiso 1 1 d . . . . .
H14 H 0.5592(17) -0.0006(13) 0.7315(15) 0.023(6) Uiso 1 1 d . . . . .
H19 H 1.0217(19) -0.1465(14) 0.5668(17) 0.035(7) Uiso 1 1 d . . . . .
H46 H 0.7197(17) 0.2223(13) 0.6858(16) 0.026(6) Uiso 1 1 d . . . . .
H42 H 0.9628(17) 0.2454(12) 0.5613(15) 0.025(6) Uiso 1 1 d . . . . .
H45 H 0.6316(18) 0.2662(13) 0.5642(16) 0.028(7) Uiso 1 1 d . . . . .
H21 H 0.8461(18) -0.0178(13) 0.4255(17) 0.031(7) Uiso 1 1 d . . . . .
H23 H 0.919(2) -0.1316(16) 0.772(2) 0.055(9) Uiso 1 1 d . . . . .
H33 H 0.719(2) 0.2573(14) 0.9942(17) 0.034(7) Uiso 1 1 d . . . . .
H44 H 0.711(2) 0.2976(15) 0.4371(19) 0.042(8) Uiso 1 1 d . . . . .
H43 H 0.875(2) 0.2851(15) 0.4362(19) 0.042(8) Uiso 1 1 d . . . . .
H20 H 0.9788(19) -0.0891(14) 0.4321(18) 0.035(7) Uiso 1 1 d . . . . .
H9 H 0.471(2) 0.1039(15) 0.9017(18) 0.042(8) Uiso 1 1 d . . . . .
H30 H 1.023(2) 0.2760(14) 0.9014(17) 0.038(8) Uiso 1 1 d . . . . .
H25A H 0.971(2) -0.2439(17) 0.771(2) 0.056(9) Uiso 1 1 d . . . . .
H15A H 0.571(2) 0.1161(14) 0.7051(18) 0.035(7) Uiso 1 1 d . . . . .
H7 H 0.7060(19) 0.0903(14) 1.0743(18) 0.040(8) Uiso 1 1 d . . . . .
H25B H 0.995(2) -0.2348(15) 0.6722(19) 0.043(8) Uiso 1 1 d . . . . .
H36 H 1.133(2) 0.1174(15) 0.7445(19) 0.047(9) Uiso 1 1 d . . . . .
H13A H 0.873(2) -0.0553(16) 1.0908(19) 0.047(8) Uiso 1 1 d . . . . .
H15B H 0.473(2) 0.1284(15) 0.7407(18) 0.039(8) Uiso 1 1 d . . . . .
H16A H 0.386(2) 0.0253(16) 0.806(2) 0.049(9) Uiso 1 1 d . . . . .
H8 H 0.550(2) 0.1305(15) 1.0369(19) 0.048(9) Uiso 1 1 d . . . . .
H13B H 0.795(2) -0.0089(18) 1.126(2) 0.066(11) Uiso 1 1 d . . . . .
H15C H 0.483(2) 0.0878(15) 0.655(2) 0.046(8) Uiso 1 1 d . . . . .
H26 H 0.716(2) 0.0321(15) 0.599(2) 0.046(8) Uiso 1 1 d . . . . .
H37 H 1.295(2) 0.1425(16) 0.7444(19) 0.050(9) Uiso 1 1 d . . . . .
H12A H 0.948(2) 0.0463(16) 1.0247(19) 0.047(8) Uiso 1 1 d . . . . .
H13C H 0.765(2) -0.0744(16) 1.0660(18) 0.042(8) Uiso 1 1 d . . . . .
H31 H 0.985(2) 0.3362(18) 1.027(2) 0.066(10) Uiso 1 1 d . . . . .
H25C H 0.891(3) -0.2335(18) 0.695(2) 0.067(11) Uiso 1 1 d . . . . .
H16B H 0.435(2) -0.0421(17) 0.805(2) 0.051(9) Uiso 1 1 d . . . . .
H38 H 1.336(2) 0.2571(16) 0.734(2) 0.055(9) Uiso 1 1 d . . . . .
H32 H 0.825(3) 0.3255(18) 1.074(2) 0.070(11) Uiso 1 1 d . . . . .
H16C H 0.395(3) -0.0148(18) 0.708(2) 0.074(11) Uiso 1 1 d . . . . .
H12B H 0.896(2) 0.0872(16) 0.948(2) 0.054(9) Uiso 1 1 d . . . . .
H39 H 1.218(2) 0.3461(18) 0.733(2) 0.060(10) Uiso 1 1 d . . . . .
H27A H 0.581(3) 0.0159(19) 0.502(2) 0.076(11) Uiso 1 1 d . . . . .
H12C H 0.864(2) 0.0888(16) 1.047(2) 0.050(9) Uiso 1 1 d . . . . .
H28A H 0.693(2) 0.1115(16) 0.493(2) 0.049(9) Uiso 1 1 d . . . . .
H27B H 0.619(3) -0.057(2) 0.545(2) 0.080(12) Uiso 1 1 d . . . . .
H27C H 0.646(2) -0.0281(17) 0.450(2) 0.051(11) Uiso 1 1 d . . . . .
H28B H 0.754(3) 0.070(2) 0.424(3) 0.085(13) Uiso 1 1 d . . . . .
H4 H 0.7214(18) -0.1537(14) 0.7031(16) 0.027(6) Uiso 1 1 d . . . . .
H28C H 0.799(3) 0.101(2) 0.509(3) 0.082(14) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 P1 2.4761(5) . ?
Sn1 C35 2.163(2) . ?
Sn1 C41 2.1523(19) . ?
Sn1 C29 2.146(2) . ?
P1 C1 1.747(2) . ?
O1 C1 1.259(2) . ?
C2 N2 1.345(2) . ?
C2 N1 1.345(2) . ?
C2 C1 1.502(3) . ?
N2 C4 1.385(3) . ?
N2 C17 1.459(3) . ?
N1 C5 1.453(3) . ?
N1 C3 1.384(3) . ?
C5 C6 1.394(3) . ?
C5 C10 1.398(3) . ?
C35 C40 1.392(3) . ?
C35 C36 1.395(3) . ?
C6 C11 1.519(3) . ?
C6 C7 1.395(3) . ?
C41 C42 1.393(3) . ?
C41 C46 1.398(3) . ?
C44 C43 1.385(4) . ?
C44 C45 1.378(4) . ?
C42 C43 1.393(3) . ?
C14 C10 1.516(3) . ?
C14 C15 1.527(3) . ?
C14 C16 1.530(4) . ?
C46 C45 1.391(3) . ?
C18 C23 1.507(4) . ?
C18 C17 1.393(3) . ?
C18 C19 1.392(3) . ?
C10 C9 1.388(3) . ?
C23 C24 1.544(4) . ?
C23 C25 1.527(4) . ?
C21 C22 1.393(3) . ?
C21 C20 1.380(4) . ?
C3 C4 1.343(3) . ?
C30 C29 1.395(3) . ?
C30 C31 1.392(4) . ?
C40 C39 1.397(4) . ?
C17 C22 1.397(3) . ?
C34 C29 1.397(3) . ?
C34 C33 1.396(3) . ?
C19 C20 1.368(4) . ?
C26 C22 1.516(3) . ?
C26 C28 1.515(4) . ?
C26 C27 1.504(4) . ?
C8 C9 1.379(4) . ?
C8 C7 1.383(4) . ?
C33 C32 1.377(4) . ?
C13 C11 1.536(3) . ?
C11 C12 1.523(4) . ?
C39 C38 1.374(4) . ?
C38 C37 1.382(4) . ?
C31 C32 1.367(5) . ?
C37 C36 1.390(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C35 Sn1 P1 103.44(6) . . ?
C41 Sn1 P1 114.82(5) . . ?
C41 Sn1 C35 105.70(8) . . ?
C29 Sn1 P1 118.68(6) . . ?
C29 Sn1 C35 103.92(8) . . ?
C29 Sn1 C41 108.71(8) . . ?
C1 P1 Sn1 86.59(7) . . ?
N2 C2 C1 128.08(17) . . ?
N1 C2 N2 107.07(17) . . ?
N1 C2 C1 124.84(17) . . ?
C2 N2 C4 109.24(17) . . ?
C2 N2 C17 127.57(17) . . ?
C4 N2 C17 123.19(17) . . ?
C2 N1 C5 125.88(17) . . ?
C2 N1 C3 109.21(17) . . ?
C3 N1 C5 124.35(17) . . ?
C6 C5 N1 119.38(18) . . ?
C6 C5 C10 123.7(2) . . ?
C10 C5 N1 116.90(18) . . ?
C40 C35 Sn1 123.80(17) . . ?
C40 C35 C36 117.7(2) . . ?
C36 C35 Sn1 118.40(16) . . ?
O1 C1 P1 129.63(15) . . ?
O1 C1 C2 114.54(16) . . ?
C2 C1 P1 115.75(14) . . ?
C5 C6 C11 123.83(19) . . ?
C5 C6 C7 116.4(2) . . ?
C7 C6 C11 119.7(2) . . ?
C42 C41 Sn1 120.96(15) . . ?
C42 C41 C46 117.83(19) . . ?
C46 C41 Sn1 121.16(15) . . ?
C45 C44 C43 119.9(2) . . ?
C41 C42 C43 121.0(2) . . ?
C10 C14 C15 110.0(2) . . ?
C10 C14 C16 112.1(2) . . ?
C15 C14 C16 111.3(2) . . ?
C45 C46 C41 121.2(2) . . ?
C17 C18 C23 123.6(2) . . ?
C19 C18 C23 119.1(2) . . ?
C19 C18 C17 117.2(2) . . ?
C5 C10 C14 122.7(2) . . ?
C9 C10 C5 117.2(2) . . ?
C9 C10 C14 120.1(2) . . ?
C18 C23 C24 110.3(3) . . ?
C18 C23 C25 112.2(2) . . ?
C25 C23 C24 109.7(2) . . ?
C20 C21 C22 121.7(2) . . ?
C4 C3 N1 107.31(19) . . ?
C44 C43 C42 120.0(2) . . ?
C31 C30 C29 121.2(3) . . ?
C35 C40 C39 120.8(3) . . ?
C3 C4 N2 107.16(19) . . ?
C44 C45 C46 120.1(2) . . ?
C18 C17 N2 117.55(18) . . ?
C18 C17 C22 123.5(2) . . ?
C22 C17 N2 118.96(18) . . ?
C33 C34 C29 120.5(2) . . ?
C20 C19 C18 121.1(2) . . ?
C28 C26 C22 113.3(2) . . ?
C27 C26 C22 111.1(2) . . ?
C27 C26 C28 111.0(3) . . ?
C30 C29 Sn1 118.93(17) . . ?
C30 C29 C34 117.9(2) . . ?
C34 C29 Sn1 123.17(16) . . ?
C21 C22 C17 116.2(2) . . ?
C21 C22 C26 120.7(2) . . ?
C17 C22 C26 123.12(19) . . ?
C9 C8 C7 120.4(2) . . ?
C32 C33 C34 120.2(3) . . ?
C6 C11 C13 110.5(2) . . ?
C6 C11 C12 111.3(2) . . ?
C12 C11 C13 110.7(2) . . ?
C8 C9 C10 120.9(2) . . ?
C38 C39 C40 120.1(3) . . ?
C39 C38 C37 120.4(2) . . ?
C32 C31 C30 119.9(3) . . ?
C8 C7 C6 121.3(2) . . ?
C19 C20 C21 120.3(2) . . ?
C31 C32 C33 120.3(3) . . ?
C38 C37 C36 119.3(3) . . ?
C37 C36 C35 121.7(2) . . ?
_olex2_date_sample_data_collection 2015-06-27
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_2095
_database_code_depnum_ccdc_archive 'CCDC 1425914'
_audit_update_record             
;
2015-09-18 deposited with the CCDC.
2016-08-09 downloaded from the CCDC.
;





_audit_creation_date             2015-02-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C45 H51 N2 P Sn, C4 H10 O'
_chemical_formula_sum            'C49 H61 N2 O P Sn'
_chemical_formula_weight         843.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N P Sn'
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'
Sn Sn 0.0259 5.4591 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.64809(19)
_cell_length_b                   11.6076(2)
_cell_length_c                   19.4163(3)
_cell_angle_alpha                91.4216(14)
_cell_angle_beta                 92.8956(14)
_cell_angle_gamma                110.2887(17)
_cell_volume                     2245.77(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    25345
_cell_measurement_temperature    292.34(10)
_cell_measurement_theta_max      65.4140
_cell_measurement_theta_min      4.0370
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.127
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35617
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.388
_diffrn_reflns_theta_min         4.065
_diffrn_ambient_temperature      292.34(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -110.00  -17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474  -57.0000 -120.0000 93

#__ type_ start__ end____ width___ exp.time_
  2 omega  -92.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474  125.0000   30.0000 82

#__ type_ start__ end____ width___ exp.time_
  3 omega  -50.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474   38.0000   30.0000 81

#__ type_ start__ end____ width___ exp.time_
  4 omega   28.00   90.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -45.0000   90.0000 62

#__ type_ start__ end____ width___ exp.time_
  5 omega   23.00  122.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932 -125.0000  150.0000 99

#__ type_ start__ end____ width___ exp.time_
  6 omega   65.00  146.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932   45.0000  -30.0000 81

#__ type_ start__ end____ width___ exp.time_
  7 omega   47.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -77.0000 -180.0000 73

#__ type_ start__ end____ width___ exp.time_
  8 omega   15.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -30.0000  -30.0000 76

#__ type_ start__ end____ width___ exp.time_
  9 omega   29.00  101.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000    0.0000 72

#__ type_ start__ end____ width___ exp.time_
 10 omega   15.00  121.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -15.0000  150.0000 106

#__ type_ start__ end____ width___ exp.time_
 11 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4974  -57.0000  -60.0000 97

#__ type_ start__ end____ width___ exp.time_
 12 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4974  -57.0000  150.0000 97

#__ type_ start__ end____ width___ exp.time_
 13 omega -115.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4974  -77.0000   60.0000 105

#__ type_ start__ end____ width___ exp.time_
 14 omega   61.00  158.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.1682   61.0000 -180.0000 97

#__ type_ start__ end____ width___ exp.time_
 15 omega   61.00  158.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.1682   61.0000 -120.0000 97

#__ type_ start__ end____ width___ exp.time_
 16 omega   61.00  158.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.1682   61.0000   30.0000 97

#__ type_ start__ end____ width___ exp.time_
 17 omega   57.00  162.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.1682   77.0000  -30.0000 105

#__ type_ start__ end____ width___ exp.time_
 18 omega   57.00  162.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.1682   77.0000   60.0000 105

#__ type_ start__ end____ width___ exp.time_
 19 omega   61.00  158.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.1682   61.0000  120.0000 97

#__ type_ start__ end____ width___ exp.time_
 20 omega -115.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4974  -77.0000  150.0000 105

#__ type_ start__ end____ width___ exp.time_
 21 omega   10.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4974   77.0000    0.0000 105

#__ type_ start__ end____ width___ exp.time_
 22 omega   23.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4974 -125.0000  -90.0000 74

#__ type_ start__ end____ width___ exp.time_
 23 omega   61.00  158.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.1682   61.0000  150.0000 97

#__ type_ start__ end____ width___ exp.time_
 24 omega   61.00  158.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.1682   61.0000 -150.0000 97

#__ type_ start__ end____ width___ exp.time_
 25 omega   94.00  160.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.1682  125.0000   60.0000 66

#__ type_ start__ end____ width___ exp.time_
 26 omega   57.00  142.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.1682   77.0000   30.0000 85

#__ type_ start__ end____ width___ exp.time_
 27 omega   57.00  162.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.1682   77.0000  -90.0000 105
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0501825000
_diffrn_orient_matrix_UB_12      -0.0096021000
_diffrn_orient_matrix_UB_13      -0.0722169000
_diffrn_orient_matrix_UB_21      0.0261444000
_diffrn_orient_matrix_UB_22      0.1377953000
_diffrn_orient_matrix_UB_23      -0.0086567000
_diffrn_orient_matrix_UB_31      0.1438267000
_diffrn_orient_matrix_UB_32      0.0313563000
_diffrn_orient_matrix_UB_33      0.0321589000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7316
_reflns_number_total             7579
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.584
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7579
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0341
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0587P)²+3.6116P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0952
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C102) = Uanis(C103) = Uanis(C100) = Uanis(C101) = Uanis(O104)
3.a Free rotating group:
 O104(C103,C102,C101,C100)
3.b Ternary CH refined with riding coordinates:
 C25(H25), C10(H10), C22(H22), C13(H13)
3.c Secondary CH2 refined with riding coordinates:
 C102(H10D,H10E), C101(H10F,H10G)
3.d Aromatic/amide H refined with riding coordinates:
 C33(H33), C35(H35), C41(H41), C39(H39), C2(H2), C19(H19), C20(H20), C3(H3),
 C45(H45), C29(H29), C8(H8), C32(H32), C18(H18), C31(H31), C7(H7), C44(H44),
 C38(H38), C6(H6), C42(H42), C37(H37), C43(H43), C30(H30), C36(H36)
3.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C27(H27A,H27B,
 H27C), C23(H23A,H23B,H23C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C14(H14A,
 H14B,H14C), C103(H10A,H10B,H10C), C100(H10H,H10I,H10J)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.59645(2) 0.08682(2) 0.31716(2) 0.01892(8) Uani 1 1 d . . . . .
P1 P 0.64901(7) 0.10681(7) 0.19509(4) 0.02160(16) Uani 1 1 d . . . . .
C28 C 0.3809(3) 0.0085(3) 0.30021(17) 0.0274(6) Uani 1 1 d . . . . .
N1 N 0.9339(2) 0.2466(2) 0.22684(12) 0.0188(5) Uani 1 1 d . . . . .
C34 C 0.6258(3) 0.2334(3) 0.39347(15) 0.0241(6) Uani 1 1 d . . . . .
N2 N 0.8763(2) 0.1535(2) 0.12594(11) 0.0193(5) Uani 1 1 d . . . . .
C40 C 0.6547(3) -0.0526(3) 0.36599(15) 0.0246(6) Uani 1 1 d . . . . .
C1 C 0.8247(3) 0.1710(2) 0.18715(14) 0.0179(5) Uani 1 1 d . . . . .
C33 C 0.3008(4) -0.0693(3) 0.3462(2) 0.0436(9) Uani 1 1 d . . . . .
H33 H 0.3414 -0.0899 0.3865 0.052 Uiso 1 1 calc R . . . .
C16 C 0.9348(3) 0.3168(3) 0.28960(14) 0.0201(6) Uani 1 1 d . . . . .
C35 C 0.5686(3) 0.3228(3) 0.38136(17) 0.0291(7) Uani 1 1 d . . . . .
H35 H 0.5192 0.3199 0.3388 0.035 Uiso 1 1 calc R . . . .
C21 C 0.8913(3) 0.4175(3) 0.28376(15) 0.0228(6) Uani 1 1 d . . . . .
C25 C 1.0477(3) 0.1868(3) 0.35625(15) 0.0262(6) Uani 1 1 d . . . . .
H25 H 1.0113 0.1295 0.3149 0.031 Uiso 1 1 calc R . . . .
C41 C 0.6217(3) -0.0867(3) 0.43290(17) 0.0331(7) Uani 1 1 d . . . . .
H41 H 0.5748 -0.0455 0.4584 0.040 Uiso 1 1 calc R . . . .
C39 C 0.6956(3) 0.2390(3) 0.45683(16) 0.0293(7) Uani 1 1 d . . . . .
H39 H 0.7352 0.1789 0.4663 0.035 Uiso 1 1 calc R . . . .
C17 C 0.9938(3) 0.2917(3) 0.35071(15) 0.0221(6) Uani 1 1 d . . . . .
C9 C 0.7741(3) -0.0380(3) 0.05724(15) 0.0240(6) Uani 1 1 d . . . . .
C4 C 0.7973(3) 0.0878(3) 0.06553(14) 0.0212(6) Uani 1 1 d . . . . .
C2 C 1.0498(3) 0.2747(3) 0.18996(15) 0.0243(6) Uani 1 1 d . . . . .
H2 H 1.1379 0.3254 0.2060 0.029 Uiso 1 1 calc R . . . .
C19 C 0.9656(3) 0.4717(3) 0.40343(16) 0.0287(7) Uani 1 1 d . . . . .
H19 H 0.9763 0.5251 0.4429 0.034 Uiso 1 1 calc R . . . .
C20 C 0.9073(3) 0.4935(3) 0.34275(16) 0.0270(6) Uani 1 1 d . . . . .
H20 H 0.8774 0.5617 0.3409 0.032 Uiso 1 1 calc R . . . .
C3 C 1.0132(3) 0.2166(3) 0.12791(15) 0.0238(6) Uani 1 1 d . . . . .
H3 H 1.0707 0.2184 0.0918 0.029 Uiso 1 1 calc R . . . .
C45 C 0.7225(3) -0.1152(3) 0.32961(18) 0.0327(7) Uani 1 1 d . . . . .
H45 H 0.7454 -0.0940 0.2838 0.039 Uiso 1 1 calc R . . . .
C5 C 0.7497(3) 0.1529(3) 0.01759(15) 0.0261(6) Uani 1 1 d . . . . .
C29 C 0.3167(4) 0.0382(4) 0.24239(18) 0.0410(8) Uani 1 1 d . . . . .
H29 H 0.3689 0.0927 0.2105 0.049 Uiso 1 1 calc R . . . .
C26 C 1.0057(3) 0.1135(3) 0.42096(17) 0.0310(7) Uani 1 1 d . . . . .
H26A H 1.0466 0.1663 0.4622 0.047 Uiso 1 1 calc GR . . . .
H26B H 1.0359 0.0428 0.4199 0.047 Uiso 1 1 calc GR . . . .
H26C H 0.9078 0.0846 0.4222 0.047 Uiso 1 1 calc GR . . . .
C10 C 0.8295(3) -0.1066(3) 0.10879(16) 0.0281(7) Uani 1 1 d . . . . .
H10 H 0.8741 -0.0482 0.1487 0.034 Uiso 1 1 calc R . . . .
C22 C 0.8399(4) 0.4513(3) 0.21591(16) 0.0302(7) Uani 1 1 d . . . . .
H22 H 0.8188 0.3786 0.1829 0.036 Uiso 1 1 calc R . . . .
C8 C 0.6972(3) -0.0995(3) -0.00155(16) 0.0322(7) Uani 1 1 d . . . . .
H8 H 0.6799 -0.1849 -0.0091 0.039 Uiso 1 1 calc R . . . .
C32 C 0.1614(4) -0.1181(4) 0.3342(3) 0.0580(12) Uani 1 1 d . . . . .
H32 H 0.1080 -0.1716 0.3662 0.070 Uiso 1 1 calc R . . . .
C12 C 0.7186(4) -0.2140(3) 0.13622(19) 0.0440(9) Uani 1 1 d . . . . .
H12A H 0.6508 -0.1847 0.1549 0.066 Uiso 1 1 calc GR . . . .
H12B H 0.7565 -0.2512 0.1728 0.066 Uiso 1 1 calc GR . . . .
H12C H 0.6770 -0.2756 0.0986 0.066 Uiso 1 1 calc GR . . . .
C24 C 0.9494(5) 0.5575(4) 0.1859(2) 0.0551(11) Uani 1 1 d . . . . .
H24A H 0.9707 0.6313 0.2164 0.083 Uiso 1 1 calc GR . . . .
H24B H 0.9179 0.5737 0.1401 0.083 Uiso 1 1 calc GR . . . .
H24C H 1.0300 0.5359 0.1820 0.083 Uiso 1 1 calc GR . . . .
C18 C 1.0088(3) 0.3727(3) 0.40753(16) 0.0274(6) Uani 1 1 d . . . . .
H18 H 1.0495 0.3594 0.4498 0.033 Uiso 1 1 calc R . . . .
C31 C 0.1014(4) -0.0884(4) 0.2761(3) 0.0559(11) Uani 1 1 d . . . . .
H31 H 0.0068 -0.1222 0.2677 0.067 Uiso 1 1 calc R . . . .
C13 C 0.7810(3) 0.2906(3) 0.02543(17) 0.0304(7) Uani 1 1 d . . . . .
H13 H 0.8417 0.3214 0.0680 0.036 Uiso 1 1 calc R . . . .
C7 C 0.6457(4) -0.0380(3) -0.04898(17) 0.0362(8) Uani 1 1 d . . . . .
H7 H 0.5917 -0.0819 -0.0882 0.043 Uiso 1 1 calc R . . . .
C44 C 0.7570(4) -0.2084(3) 0.3595(2) 0.0444(9) Uani 1 1 d . . . . .
H44 H 0.8035 -0.2503 0.3342 0.053 Uiso 1 1 calc R . . . .
C38 C 0.7081(3) 0.3315(3) 0.50637(18) 0.0367(8) Uani 1 1 d . . . . .
H38 H 0.7548 0.3335 0.5496 0.044 Uiso 1 1 calc R . . . .
C27 C 1.2015(3) 0.2365(3) 0.35568(18) 0.0345(7) Uani 1 1 d . . . . .
H27A H 1.2281 0.2789 0.3129 0.052 Uiso 1 1 calc GR . . . .
H27B H 1.2352 0.1681 0.3585 0.052 Uiso 1 1 calc GR . . . .
H27C H 1.2393 0.2943 0.3953 0.052 Uiso 1 1 calc GR . . . .
C23 C 0.7123(4) 0.4802(4) 0.2214(2) 0.0483(10) Uani 1 1 d . . . . .
H23A H 0.6421 0.4087 0.2382 0.072 Uiso 1 1 calc GR . . . .
H23B H 0.6829 0.4995 0.1759 0.072 Uiso 1 1 calc GR . . . .
H23C H 0.7294 0.5509 0.2538 0.072 Uiso 1 1 calc GR . . . .
C6 C 0.6720(3) 0.0862(3) -0.03987(16) 0.0337(7) Uani 1 1 d . . . . .
H6 H 0.6367 0.1272 -0.0732 0.040 Uiso 1 1 calc R . . . .
C15 C 0.6546(4) 0.3223(3) 0.0348(2) 0.0408(8) Uani 1 1 d . . . . .
H15A H 0.5925 0.2924 -0.0060 0.061 Uiso 1 1 calc GR . . . .
H15B H 0.6792 0.4117 0.0408 0.061 Uiso 1 1 calc GR . . . .
H15C H 0.6111 0.2831 0.0757 0.061 Uiso 1 1 calc GR . . . .
C42 C 0.6560(4) -0.1798(3) 0.4628(2) 0.0439(9) Uani 1 1 d . . . . .
H42 H 0.6330 -0.2017 0.5085 0.053 Uiso 1 1 calc R . . . .
C37 C 0.6526(4) 0.4204(3) 0.49270(19) 0.0401(9) Uani 1 1 d . . . . .
H37 H 0.6627 0.4846 0.5262 0.048 Uiso 1 1 calc R . . . .
C43 C 0.7237(4) -0.2404(3) 0.4261(2) 0.0467(10) Uani 1 1 d . . . . .
H43 H 0.7474 -0.3041 0.4465 0.056 Uiso 1 1 calc R . . . .
C30 C 0.1783(4) -0.0103(4) 0.2305(2) 0.0528(11) Uani 1 1 d . . . . .
H30 H 0.1369 0.0108 0.1906 0.063 Uiso 1 1 calc R . . . .
C11 C 0.9357(4) -0.1493(4) 0.0776(2) 0.0439(9) Uani 1 1 d . . . . .
H11A H 0.8937 -0.2106 0.0400 0.066 Uiso 1 1 calc GR . . . .
H11B H 0.9765 -0.1859 0.1133 0.066 Uiso 1 1 calc GR . . . .
H11C H 1.0051 -0.0787 0.0596 0.066 Uiso 1 1 calc GR . . . .
C36 C 0.5826(4) 0.4162(3) 0.4304(2) 0.0375(8) Uani 1 1 d . . . . .
H36 H 0.5440 0.4771 0.4211 0.045 Uiso 1 1 calc R . . . .
C14 C 0.8556(4) 0.3563(4) -0.0357(2) 0.0419(9) Uani 1 1 d . . . . .
H14A H 0.9397 0.3403 -0.0385 0.063 Uiso 1 1 calc GR . . . .
H14B H 0.8753 0.4450 -0.0293 0.063 Uiso 1 1 calc GR . . . .
H14C H 0.7996 0.3258 -0.0785 0.063 Uiso 1 1 calc GR . . . .
O104 O 1.3401(3) 0.5145(3) 0.20662(17) 0.1140(10) Uani 1 1 d . . . A -1
C103 C 1.3538(6) 0.4090(5) 0.1016(2) 0.1140(10) Uani 1 1 d G . . A -1
H10A H 1.4017 0.4178 0.0591 0.171 Uiso 1 1 calc GR . . A -1
H10B H 1.2571 0.3830 0.0898 0.171 Uiso 1 1 calc GR . . A -1
H10C H 1.3728 0.3472 0.1296 0.171 Uiso 1 1 calc GR . . A -1
C102 C 1.3999(6) 0.5315(4) 0.1422(2) 0.1140(10) Uani 1 1 d G . . A -1
H10D H 1.4989 0.5629 0.1498 0.137 Uiso 1 1 calc R . . A -1
H10E H 1.3732 0.5923 0.1161 0.137 Uiso 1 1 calc R . . A -1
C101 C 1.3767(6) 0.6240(3) 0.2489(2) 0.1140(10) Uani 1 1 d G . . A -1
H10F H 1.3496 0.6867 0.2248 0.137 Uiso 1 1 calc R . . A -1
H10G H 1.4752 0.6572 0.2586 0.137 Uiso 1 1 calc R . . A -1
C100 C 1.3071(6) 0.5949(5) 0.3160(2) 0.1140(10) Uani 1 1 d G . . A -1
H10H H 1.2097 0.5642 0.3060 0.171 Uiso 1 1 calc GR . . A -1
H10I H 1.3331 0.6697 0.3459 0.171 Uiso 1 1 calc GR . . A -1
H10J H 1.3336 0.5321 0.3392 0.171 Uiso 1 1 calc GR . . 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
Sn1 P1 2.4608(7) . ?
Sn1 C28 2.160(3) . ?
Sn1 C34 2.155(3) . ?
Sn1 C40 2.148(3) . ?
P1 C1 1.774(3) . ?
C28 C33 1.386(5) . ?
C28 C29 1.397(5) . ?
N1 C1 1.373(4) . ?
N1 C16 1.447(4) . ?
N1 C2 1.401(4) . ?
C34 C35 1.393(4) . ?
C34 C39 1.393(5) . ?
N2 C1 1.374(4) . ?
N2 C4 1.441(4) . ?
N2 C3 1.384(4) . ?
C40 C41 1.394(4) . ?
C40 C45 1.393(5) . ?
C33 C32 1.398(6) . ?
C16 C21 1.404(4) . ?
C16 C17 1.398(4) . ?
C35 C36 1.388(5) . ?
C21 C20 1.395(4) . ?
C21 C22 1.514(4) . ?
C25 C17 1.520(4) . ?
C25 C26 1.532(4) . ?
C25 C27 1.537(4) . ?
C41 C42 1.386(5) . ?
C39 C38 1.390(5) . ?
C17 C18 1.398(4) . ?
C9 C4 1.398(4) . ?
C9 C10 1.514(4) . ?
C9 C8 1.394(4) . ?
C4 C5 1.395(4) . ?
C2 C3 1.337(4) . ?
C19 C20 1.374(5) . ?
C19 C18 1.380(5) . ?
C45 C44 1.388(5) . ?
C5 C13 1.518(4) . ?
C5 C6 1.396(4) . ?
C29 C30 1.387(5) . ?
C10 C12 1.519(5) . ?
C10 C11 1.527(5) . ?
C22 C24 1.525(5) . ?
C22 C23 1.516(5) . ?
C8 C7 1.383(5) . ?
C32 C31 1.378(7) . ?
C31 C30 1.370(7) . ?
C13 C15 1.531(5) . ?
C13 C14 1.530(5) . ?
C7 C6 1.374(5) . ?
C44 C43 1.384(6) . ?
C38 C37 1.381(5) . ?
C42 C43 1.379(6) . ?
C37 C36 1.378(6) . ?
O104 C102 1.4195 . ?
O104 C101 1.4192 . ?
C103 C102 1.5177 . ?
C101 C100 1.5184 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C28 Sn1 P1 97.26(9) . . ?
C34 Sn1 P1 127.25(8) . . ?
C34 Sn1 C28 103.34(11) . . ?
C40 Sn1 P1 112.98(8) . . ?
C40 Sn1 C28 105.38(12) . . ?
C40 Sn1 C34 107.42(11) . . ?
C1 P1 Sn1 110.99(9) . . ?
C33 C28 Sn1 122.2(3) . . ?
C33 C28 C29 117.5(3) . . ?
C29 C28 Sn1 120.3(2) . . ?
C1 N1 C16 127.9(2) . . ?
C1 N1 C2 110.2(2) . . ?
C2 N1 C16 120.1(2) . . ?
C35 C34 Sn1 119.9(2) . . ?
C39 C34 Sn1 122.0(2) . . ?
C39 C34 C35 118.0(3) . . ?
C1 N2 C4 124.7(2) . . ?
C1 N2 C3 110.9(2) . . ?
C3 N2 C4 124.2(2) . . ?
C41 C40 Sn1 121.9(2) . . ?
C45 C40 Sn1 119.9(2) . . ?
C45 C40 C41 118.2(3) . . ?
N1 C1 P1 136.5(2) . . ?
N1 C1 N2 104.2(2) . . ?
N2 C1 P1 119.2(2) . . ?
C28 C33 C32 121.1(4) . . ?
C21 C16 N1 117.3(2) . . ?
C17 C16 N1 119.1(3) . . ?
C17 C16 C21 123.0(3) . . ?
C36 C35 C34 121.1(3) . . ?
C16 C21 C22 122.8(3) . . ?
C20 C21 C16 117.1(3) . . ?
C20 C21 C22 119.8(3) . . ?
C17 C25 C26 112.8(3) . . ?
C17 C25 C27 110.1(3) . . ?
C26 C25 C27 109.5(3) . . ?
C42 C41 C40 121.2(3) . . ?
C38 C39 C34 120.9(3) . . ?
C16 C17 C25 123.2(3) . . ?
C18 C17 C16 116.9(3) . . ?
C18 C17 C25 119.8(3) . . ?
C4 C9 C10 122.5(3) . . ?
C8 C9 C4 117.1(3) . . ?
C8 C9 C10 120.4(3) . . ?
C9 C4 N2 118.2(3) . . ?
C5 C4 N2 118.6(3) . . ?
C5 C4 C9 123.2(3) . . ?
C3 C2 N1 107.2(3) . . ?
C20 C19 C18 120.5(3) . . ?
C19 C20 C21 121.2(3) . . ?
C2 C3 N2 107.5(2) . . ?
C44 C45 C40 120.8(3) . . ?
C4 C5 C13 122.7(3) . . ?
C4 C5 C6 117.2(3) . . ?
C6 C5 C13 120.1(3) . . ?
C30 C29 C28 121.5(4) . . ?
C9 C10 C12 111.5(3) . . ?
C9 C10 C11 111.1(3) . . ?
C12 C10 C11 111.0(3) . . ?
C21 C22 C24 110.2(3) . . ?
C21 C22 C23 113.2(3) . . ?
C23 C22 C24 111.1(3) . . ?
C7 C8 C9 121.0(3) . . ?
C31 C32 C33 119.9(4) . . ?
C19 C18 C17 121.3(3) . . ?
C30 C31 C32 120.0(4) . . ?
C5 C13 C15 112.0(3) . . ?
C5 C13 C14 111.0(3) . . ?
C14 C13 C15 110.8(3) . . ?
C6 C7 C8 120.5(3) . . ?
C43 C44 C45 120.1(4) . . ?
C37 C38 C39 120.0(3) . . ?
C7 C6 C5 121.1(3) . . ?
C43 C42 C41 119.8(3) . . ?
C36 C37 C38 120.0(3) . . ?
C42 C43 C44 120.0(3) . . ?
C31 C30 C29 120.0(4) . . ?
C37 C36 C35 120.0(3) . . ?
C101 O104 C102 113.4 . . ?
O104 C102 C103 108.8 . . ?
O104 C101 C100 108.8 . . ?

_olex2_date_sample_data_collection 2015-07-25
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_2172
_database_code_depnum_ccdc_archive 'CCDC 1425915'
_audit_update_record             
;
2015-09-18 deposited with the CCDC.
2016-08-09 downloaded from the CCDC.
;





_audit_creation_date             2015-02-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014-3

_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C45 H51 Ge N2 P'
_chemical_formula_sum            'C45 H51 Ge N2 P'
_chemical_formula_weight         723.43
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O P Ge'
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'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   24.06280(20)
_cell_length_b                   12.81520(9)
_cell_length_c                   25.4632(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.7933(7)
_cell_angle_gamma                90
_cell_volume                     7824.60(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    22361
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      65.3780
_cell_measurement_theta_min      3.8520
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.928
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42736
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.405
_diffrn_reflns_theta_min         3.687
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -50.00   31.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474   38.0000  -90.0000 81

#__ type_ start__ end____ width___ exp.time_
  2 omega  -48.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474   38.0000   30.0000 78

#__ type_ start__ end____ width___ exp.time_
  3 omega  -50.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2474   38.0000  150.0000 80

#__ type_ start__ end____ width___ exp.time_
  4 omega    8.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000  -30.0000 101

#__ type_ start__ end____ width___ exp.time_
  5 omega   19.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -61.0000  -30.0000 44

#__ type_ start__ end____ width___ exp.time_
  6 omega   75.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -61.0000  -30.0000 41

#__ type_ start__ end____ width___ exp.time_
  7 omega   60.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000 -150.0000 49

#__ type_ start__ end____ width___ exp.time_
  8 omega   19.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -95.0000 -150.0000 28

#__ type_ start__ end____ width___ exp.time_
  9 omega   43.00  167.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932   15.0000 -180.0000 124

#__ type_ start__ end____ width___ exp.time_
 10 omega   14.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -30.0000 -180.0000 77

#__ type_ start__ end____ width___ exp.time_
 11 omega   69.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932   45.0000   60.0000 73

#__ type_ start__ end____ width___ exp.time_
 12 omega   22.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7932  -77.0000  120.0000 74
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0316032000
_diffrn_orient_matrix_UB_12      -0.1042334000
_diffrn_orient_matrix_UB_13      -0.0070364000
_diffrn_orient_matrix_UB_21      0.0554438000
_diffrn_orient_matrix_UB_22      -0.0597503000
_diffrn_orient_matrix_UB_23      0.0099265000
_diffrn_orient_matrix_UB_31      -0.0075041000
_diffrn_orient_matrix_UB_32      -0.0023832000
_diffrn_orient_matrix_UB_33      0.0594956000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11618
_reflns_number_total             13144
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         13144
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0275
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0420P)²+3.2880P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0770
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C71(H71), C23(H23), C68(H68), C59(H59), C11(H11), C26(H26), C14(H14), C56(H56)
2.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C3(H3), C47(H47), C45(H45), C18(H18), C2(H2), C51(H51), C84(H84),
 C29(H29), C35(H35), C52(H52), C20(H20), C34(H34), C33(H33), C41(H41), C36(H36),
  C8(H8), C63(H63), C53(H53), C65(H65), C37(H37), C78(H78), C42(H42), C64(H64),
 C19(H19), C80(H80), C6(H6), C38(H38), C30(H30), C7(H7), C31(H31), C90(H90),
 C32(H32), C77(H77), C44(H44), C82(H82), C89(H89), C88(H88), C86(H86), C83(H83),
  C81(H81), C75(H75), C74(H74), C43(H43), C87(H87), C76(H76)
2.c Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C10(H10a,H10b,H10c), C12(H12a,H12b,H12c), C24(H24a,H24b,
 H24c), C27(H27a,H27b,H27c), C72(H72a,H72b,H72c), C58(H58a,H58b,H58c), C13(H13a,
 H13b,H13c), C25(H25a,H25b,H25c), C70(H70a,H70b,H70c), C60(H60a,H60b,H60c),
 C55(H55a,H55b,H55c), C15(H15a,H15b,H15c), C67(H67a,H67b,H67c), C57(H57a,H57b,
 H57c), C69(H69a,H69b,H69c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.85653(2) 0.89516(2) 0.21595(2) 0.02245(6) Uani 1 1 d . . . . .
Ge2 Ge 0.84244(2) 0.54485(2) 0.71125(2) 0.02609(6) Uani 1 1 d . . . . .
P1 P 0.87371(2) 0.73972(3) 0.17654(2) 0.02331(9) Uani 1 1 d . . . . .
P2 P 0.86675(2) 0.69635(3) 0.67149(2) 0.02530(9) Uani 1 1 d . . . . .
N1 N 0.83550(5) 0.66699(10) 0.07802(5) 0.0220(3) Uani 1 1 d . . . . .
C48 C 0.84122(7) 0.74397(13) 0.51792(6) 0.0287(4) Uani 1 1 d . . . . .
H48 H 0.8309 0.7879 0.4897 0.034 Uiso 1 1 calc R . . . .
N4 N 0.83869(5) 0.76676(10) 0.57078(5) 0.0226(3) Uani 1 1 d . . . . .
N2 N 0.87093(5) 0.82190(10) 0.06995(5) 0.0219(3) Uani 1 1 d . . . . .
C1 C 0.85835(6) 0.74967(11) 0.10733(6) 0.0204(3) Uani 1 1 d . . . . .
C3 C 0.85613(7) 0.78367(13) 0.01972(6) 0.0272(4) Uani 1 1 d . . . . .
H3 H 0.8604 0.8183 -0.0118 0.033 Uiso 1 1 calc R . . . .
N3 N 0.87167(5) 0.60958(10) 0.56605(5) 0.0221(3) Uani 1 1 d . . . . .
C21 C 0.75946(7) 0.54989(12) 0.09808(6) 0.0245(3) Uani 1 1 d . . . . .
C46 C 0.85756(6) 0.68335(12) 0.60171(6) 0.0207(3) Uani 1 1 d . . . . .
C61 C 0.90241(7) 0.51366(13) 0.57709(6) 0.0242(3) Uani 1 1 d . . . . .
C39 C 0.87174(7) 0.85081(12) 0.29008(6) 0.0245(3) Uani 1 1 d . . . . .
C47 C 0.86131(7) 0.64716(13) 0.51489(6) 0.0288(4) Uani 1 1 d . . . . .
H47 H 0.8673 0.6113 0.4841 0.035 Uiso 1 1 calc R . . . .
C17 C 0.85672(7) 0.49279(13) 0.11421(7) 0.0279(4) Uani 1 1 d . . . . .
C45 C 0.74141(7) 0.90200(14) 0.16601(7) 0.0331(4) Uani 1 1 d . . . . .
H45 H 0.7550 0.8634 0.1390 0.040 Uiso 1 1 calc R . . . .
C40 C 0.77751(7) 0.93350(12) 0.20850(6) 0.0260(3) Uani 1 1 d . . . . .
C5 C 0.96562(7) 0.89047(14) 0.08398(7) 0.0306(4) Uani 1 1 d . . . . .
C18 C 0.83750(8) 0.39718(13) 0.13116(7) 0.0334(4) Uani 1 1 d . . . . .
H18 H 0.8631 0.3456 0.1421 0.040 Uiso 1 1 calc R . . . .
C50 C 0.76952(7) 0.89451(13) 0.59518(7) 0.0283(4) Uani 1 1 d . . . . .
C2 C 0.83468(7) 0.68839(13) 0.02466(6) 0.0282(4) Uani 1 1 d . . . . .
H2 H 0.8216 0.6445 -0.0027 0.034 Uiso 1 1 calc R . . . .
C28 C 0.90206(7) 1.02212(13) 0.21388(6) 0.0265(3) Uani 1 1 d . . . . .
C16 C 0.81681(7) 0.56830(12) 0.09820(6) 0.0233(3) Uani 1 1 d . . . . .
C71 C 0.81331(7) 0.41280(13) 0.54952(7) 0.0291(4) Uani 1 1 d . . . . .
H71 H 0.7964 0.4810 0.5552 0.035 Uiso 1 1 calc R . . . .
C51 C 0.75851(8) 0.99355(13) 0.61420(7) 0.0337(4) Uani 1 1 d . . . . .
H51 H 0.7218 1.0131 0.6181 0.040 Uiso 1 1 calc R . . . .
C84 C 0.85733(11) 0.31810(15) 0.71661(7) 0.0466(5) Uani 1 1 d . . . . .
H84 H 0.8186 0.3156 0.7145 0.056 Uiso 1 1 calc R . . . .
C29 C 0.87985(8) 1.11975(13) 0.22428(7) 0.0339(4) Uani 1 1 d . . . . .
H29 H 0.8416 1.1264 0.2262 0.041 Uiso 1 1 calc R . . . .
C85 C 0.85374(8) 0.59402(14) 0.78477(7) 0.0333(4) Uani 1 1 d . . . . .
C49 C 0.82525(7) 0.86884(12) 0.59024(6) 0.0236(3) Uani 1 1 d . . . . .
C73 C 0.76219(8) 0.51519(13) 0.69909(7) 0.0318(4) Uani 1 1 d . . . . .
C23 C 0.71539(7) 0.62909(13) 0.07968(7) 0.0300(4) Uani 1 1 d . . . . .
H23 H 0.7343 0.6938 0.0710 0.036 Uiso 1 1 calc R . . . .
C35 C 0.92010(7) 0.87237(15) 0.37660(7) 0.0342(4) Uani 1 1 d . . . . .
H35 H 0.9445 0.9105 0.3994 0.041 Uiso 1 1 calc R . . . .
C52 C 0.80113(8) 1.06337(13) 0.62744(7) 0.0358(4) Uani 1 1 d . . . . .
H52 H 0.7930 1.1287 0.6408 0.043 Uiso 1 1 calc R . . . .
C20 C 0.74259(7) 0.45231(13) 0.11534(7) 0.0292(4) Uani 1 1 d . . . . .
H20 H 0.7048 0.4377 0.1156 0.035 Uiso 1 1 calc R . . . .
C66 C 0.96006(7) 0.52002(15) 0.59055(7) 0.0310(4) Uani 1 1 d . . . . .
C34 C 0.90832(7) 0.90604(13) 0.32500(6) 0.0282(4) Uani 1 1 d . . . . .
H34 H 0.9251 0.9664 0.3136 0.034 Uiso 1 1 calc R . . . .
C4 C 0.90818(7) 0.91050(13) 0.07809(6) 0.0246(3) Uani 1 1 d . . . . .
C33 C 0.95944(8) 1.01557(15) 0.21095(7) 0.0353(4) Uani 1 1 d . . . . .
H33 H 0.9755 0.9516 0.2039 0.042 Uiso 1 1 calc R . . . .
C68 C 0.99122(7) 0.62306(16) 0.59408(8) 0.0380(4) Uani 1 1 d . . . . .
H68 H 0.9633 0.6790 0.5919 0.046 Uiso 1 1 calc R . . . .
C79 C 0.88438(8) 0.41354(14) 0.71237(7) 0.0349(4) Uani 1 1 d . . . . .
C62 C 0.87428(7) 0.41879(13) 0.56939(6) 0.0267(3) Uani 1 1 d . . . . .
C59 C 0.72205(8) 0.81991(14) 0.58073(9) 0.0418(5) Uani 1 1 d . . . . .
H59 H 0.7381 0.7529 0.5713 0.050 Uiso 1 1 calc R . . . .
C41 C 0.75537(8) 0.99020(14) 0.24867(7) 0.0325(4) Uani 1 1 d . . . . .
H41 H 0.7789 1.0118 0.2775 0.039 Uiso 1 1 calc R . . . .
C36 C 0.89594(8) 0.78320(15) 0.39408(7) 0.0352(4) Uani 1 1 d . . . . .
H36 H 0.9046 0.7601 0.4284 0.042 Uiso 1 1 calc R . . . .
C9 C 0.88580(7) 1.01120(13) 0.07420(6) 0.0286(4) Uani 1 1 d . . . . .
C8 C 0.92342(9) 1.09443(15) 0.07915(7) 0.0390(4) Uani 1 1 d . . . . .
H8 H 0.9100 1.1625 0.0775 0.047 Uiso 1 1 calc R . . . .
C22 C 0.67686(8) 0.65328(15) 0.12283(9) 0.0450(5) Uani 1 1 d . . . . .
H22A H 0.6567 0.5914 0.1309 0.068 Uiso 1 1 calc GR . . . .
H22B H 0.6510 0.7069 0.1108 0.068 Uiso 1 1 calc GR . . . .
H22C H 0.6987 0.6768 0.1539 0.068 Uiso 1 1 calc GR . . . .
C63 C 0.90531(8) 0.32753(14) 0.57780(7) 0.0348(4) Uani 1 1 d . . . . .
H63 H 0.8877 0.2631 0.5733 0.042 Uiso 1 1 calc R . . . .
C53 C 0.85564(8) 1.03679(14) 0.62098(7) 0.0355(4) Uani 1 1 d . . . . .
H53 H 0.8839 1.0850 0.6293 0.043 Uiso 1 1 calc R . . . .
C65 C 0.98861(8) 0.42591(16) 0.59849(7) 0.0385(4) Uani 1 1 d . . . . .
H65 H 1.0268 0.4270 0.6080 0.046 Uiso 1 1 calc R . . . .
C37 C 0.85872(8) 0.72789(15) 0.36036(7) 0.0387(4) Uani 1 1 d . . . . .
H37 H 0.8418 0.6680 0.3721 0.046 Uiso 1 1 calc R . . . .
C78 C 0.73132(8) 0.54419(14) 0.65291(7) 0.0352(4) Uani 1 1 d . . . . .
H78 H 0.7494 0.5750 0.6260 0.042 Uiso 1 1 calc R . . . .
C42 C 0.69927(8) 1.01490(15) 0.24658(8) 0.0376(4) Uani 1 1 d . . . . .
H42 H 0.6853 1.0522 0.2739 0.045 Uiso 1 1 calc R . . . .
C11 C 0.82425(8) 1.03104(13) 0.06098(7) 0.0315(4) Uani 1 1 d . . . . .
H11 H 0.8041 0.9667 0.0679 0.038 Uiso 1 1 calc R . . . .
C54 C 0.86893(7) 0.93881(13) 0.60215(6) 0.0286(4) Uani 1 1 d . . . . .
C26 C 0.91888(7) 0.51127(14) 0.11248(8) 0.0343(4) Uani 1 1 d . . . . .
H26 H 0.9245 0.5868 0.1100 0.041 Uiso 1 1 calc R . . . .
C64 C 0.96166(8) 0.33158(15) 0.59262(7) 0.0405(5) Uani 1 1 d . . . . .
H64 H 0.9816 0.2700 0.5987 0.049 Uiso 1 1 calc R . . . .
C10 C 0.81344(9) 1.05651(15) 0.00205(8) 0.0437(5) Uani 1 1 d . . . . .
H10A H 0.8352 1.1162 -0.0062 0.066 Uiso 1 1 calc GR . . . .
H10B H 0.7746 1.0714 -0.0060 0.066 Uiso 1 1 calc GR . . . .
H10C H 0.8238 0.9978 -0.0184 0.066 Uiso 1 1 calc GR . . . .
C19 C 0.78131(8) 0.37723(13) 0.13206(7) 0.0329(4) Uani 1 1 d . . . . .
H19 H 0.7694 0.3130 0.1440 0.040 Uiso 1 1 calc R . . . .
C12 C 0.80061(9) 1.11843(15) 0.09318(8) 0.0451(5) Uani 1 1 d . . . . .
H12A H 0.8086 1.1042 0.1301 0.068 Uiso 1 1 calc GR . . . .
H12B H 0.7610 1.1225 0.0851 0.068 Uiso 1 1 calc GR . . . .
H12C H 0.8174 1.1835 0.0846 0.068 Uiso 1 1 calc GR . . . .
C80 C 0.94236(9) 0.41492(18) 0.71657(8) 0.0453(5) Uani 1 1 d . . . . .
H80 H 0.9611 0.4781 0.7147 0.054 Uiso 1 1 calc R . . . .
C6 C 1.00089(8) 0.97722(17) 0.08814(8) 0.0417(5) Uani 1 1 d . . . . .
H6 H 1.0393 0.9672 0.0922 0.050 Uiso 1 1 calc R . . . .
C38 C 0.84661(8) 0.76196(14) 0.30881(7) 0.0337(4) Uani 1 1 d . . . . .
H38 H 0.8213 0.7247 0.2865 0.040 Uiso 1 1 calc R . . . .
C30 C 0.91361(9) 1.20713(15) 0.23185(8) 0.0422(5) Uani 1 1 d . . . . .
H30 H 0.8979 1.2714 0.2390 0.051 Uiso 1 1 calc R . . . .
C7 C 0.97993(9) 1.07728(16) 0.08637(8) 0.0453(5) Uani 1 1 d . . . . .
H7 H 1.0042 1.1337 0.0901 0.054 Uiso 1 1 calc R . . . .
C31 C 0.97009(9) 1.19898(16) 0.22880(8) 0.0445(5) Uani 1 1 d . . . . .
H31 H 0.9928 1.2575 0.2337 0.053 Uiso 1 1 calc R . . . .
C90 C 0.88812(8) 0.54141(18) 0.82236(7) 0.0415(5) Uani 1 1 d . . . . .
H90 H 0.9049 0.4794 0.8132 0.050 Uiso 1 1 calc R . . . .
C32 C 0.99296(9) 1.10340(16) 0.21847(8) 0.0438(5) Uani 1 1 d . . . . .
H32 H 1.0313 1.0976 0.2165 0.053 Uiso 1 1 calc R . . . .
C14 C 0.99007(7) 0.78166(15) 0.08370(7) 0.0353(4) Uani 1 1 d . . . . .
H14 H 0.9589 0.7323 0.0828 0.042 Uiso 1 1 calc R . . . .
C77 C 0.67422(8) 0.52825(16) 0.64608(9) 0.0450(5) Uani 1 1 d . . . . .
H77 H 0.6545 0.5471 0.6145 0.054 Uiso 1 1 calc R . . . .
C56 C 0.92918(7) 0.91115(15) 0.59443(8) 0.0376(4) Uani 1 1 d . . . . .
H56 H 0.9303 0.8365 0.5863 0.045 Uiso 1 1 calc R . . . .
C44 C 0.68525(8) 0.92758(16) 0.16353(8) 0.0412(4) Uani 1 1 d . . . . .
H44 H 0.6616 0.9068 0.1347 0.049 Uiso 1 1 calc R . . . .
C24 C 0.68190(10) 0.58968(17) 0.02961(9) 0.0507(5) Uani 1 1 d . . . . .
H24A H 0.7066 0.5783 0.0025 0.076 Uiso 1 1 calc GR . . . .
H24B H 0.6544 0.6407 0.0179 0.076 Uiso 1 1 calc GR . . . .
H24C H 0.6637 0.5253 0.0371 0.076 Uiso 1 1 calc GR . . . .
C82 C 0.94532(15) 0.2292(2) 0.72698(9) 0.0723(9) Uani 1 1 d . . . . .
H82 H 0.9656 0.1676 0.7314 0.087 Uiso 1 1 calc R . . . .
C89 C 0.89797(9) 0.5792(2) 0.87332(9) 0.0629(7) Uani 1 1 d . . . . .
H89 H 0.9213 0.5430 0.8980 0.075 Uiso 1 1 calc R . . . .
C88 C 0.87322(13) 0.6704(2) 0.88714(10) 0.0762(10) Uani 1 1 d . . . . .
H88 H 0.8802 0.6967 0.9211 0.091 Uiso 1 1 calc R . . . .
C27 C 0.93927(9) 0.4621(2) 0.06300(10) 0.0633(7) Uani 1 1 d . . . . .
H27A H 0.9352 0.3877 0.0646 0.095 Uiso 1 1 calc GR . . . .
H27B H 0.9778 0.4793 0.0608 0.095 Uiso 1 1 calc GR . . . .
H27C H 0.9176 0.4884 0.0325 0.095 Uiso 1 1 calc GR . . . .
C86 C 0.82750(12) 0.68443(17) 0.79976(9) 0.0603(7) Uani 1 1 d . . . . .
H86 H 0.8029 0.7192 0.7756 0.072 Uiso 1 1 calc R . . . .
C72 C 0.80785(8) 0.39072(15) 0.48992(7) 0.0376(4) Uani 1 1 d . . . . .
H72A H 0.8225 0.4487 0.4716 0.056 Uiso 1 1 calc GR . . . .
H72B H 0.7693 0.3809 0.4781 0.056 Uiso 1 1 calc GR . . . .
H72C H 0.8284 0.3288 0.4829 0.056 Uiso 1 1 calc GR . . . .
C83 C 0.88807(14) 0.22636(17) 0.72396(9) 0.0651(8) Uani 1 1 d . . . . .
H83 H 0.8698 0.1630 0.7268 0.078 Uiso 1 1 calc R . . . .
C58 C 0.68772(10) 0.80163(18) 0.62780(13) 0.0741(9) Uani 1 1 d . . . . .
H58A H 0.7115 0.7751 0.6569 0.111 Uiso 1 1 calc GR . . . .
H58B H 0.6587 0.7520 0.6183 0.111 Uiso 1 1 calc GR . . . .
H58C H 0.6714 0.8663 0.6377 0.111 Uiso 1 1 calc GR . . . .
C81 C 0.97274(12) 0.3225(2) 0.72352(9) 0.0636(7) Uani 1 1 d . . . . .
H81 H 1.0115 0.3241 0.7258 0.076 Uiso 1 1 calc R . . . .
C75 C 0.67598(10) 0.45512(17) 0.73201(9) 0.0510(6) Uani 1 1 d . . . . .
H75 H 0.6575 0.4249 0.7588 0.061 Uiso 1 1 calc R . . . .
C74 C 0.73325(9) 0.47012(15) 0.73874(8) 0.0415(5) Uani 1 1 d . . . . .
H74 H 0.7527 0.4498 0.7702 0.050 Uiso 1 1 calc R . . . .
C13 C 1.02066(12) 0.7627(2) 0.03414(10) 0.0660(7) Uani 1 1 d . . . . .
H13A H 0.9954 0.7734 0.0034 0.099 Uiso 1 1 calc GR . . . .
H13B H 1.0344 0.6923 0.0343 0.099 Uiso 1 1 calc GR . . . .
H13C H 1.0514 0.8104 0.0336 0.099 Uiso 1 1 calc GR . . . .
C25 C 0.95244(9) 0.4739(2) 0.16207(10) 0.0565(6) Uani 1 1 d . . . . .
H25A H 0.9366 0.5017 0.1925 0.085 Uiso 1 1 calc GR . . . .
H25B H 0.9903 0.4973 0.1617 0.085 Uiso 1 1 calc GR . . . .
H25C H 0.9517 0.3990 0.1634 0.085 Uiso 1 1 calc GR . . . .
C70 C 0.78104(8) 0.33088(15) 0.57805(8) 0.0404(4) Uani 1 1 d . . . . .
H70A H 0.7930 0.2625 0.5686 0.061 Uiso 1 1 calc GR . . . .
H70B H 0.7419 0.3383 0.5681 0.061 Uiso 1 1 calc GR . . . .
H70C H 0.7879 0.3403 0.6154 0.061 Uiso 1 1 calc GR . . . .
C60 C 0.68624(10) 0.86100(19) 0.53230(12) 0.0710(8) Uani 1 1 d . . . . .
H60A H 0.6701 0.9268 0.5407 0.106 Uiso 1 1 calc GR . . . .
H60B H 0.6571 0.8119 0.5224 0.106 Uiso 1 1 calc GR . . . .
H60C H 0.7092 0.8700 0.5036 0.106 Uiso 1 1 calc GR . . . .
C43 C 0.66417(8) 0.98400(15) 0.20388(8) 0.0406(4) Uani 1 1 d . . . . .
H43 H 0.6265 1.0009 0.2021 0.049 Uiso 1 1 calc R . . . .
C87 C 0.83775(16) 0.7234(2) 0.85065(11) 0.0829(11) Uani 1 1 d . . . . .
H87 H 0.8208 0.7850 0.8602 0.099 Uiso 1 1 calc R . . . .
C76 C 0.64644(9) 0.48462(17) 0.68591(9) 0.0500(5) Uani 1 1 d . . . . .
H76 H 0.6080 0.4752 0.6816 0.060 Uiso 1 1 calc R . . . .
C55 C 0.96748(9) 0.9293(2) 0.64389(9) 0.0596(6) Uani 1 1 d . . . . .
H55A H 0.9681 1.0023 0.6523 0.089 Uiso 1 1 calc GR . . . .
H55B H 1.0045 0.9065 0.6381 0.089 Uiso 1 1 calc GR . . . .
H55C H 0.9541 0.8906 0.6726 0.089 Uiso 1 1 calc GR . . . .
C15 C 1.02777(9) 0.75876(19) 0.13322(9) 0.0542(6) Uani 1 1 d . . . . .
H15A H 1.0588 0.8062 0.1354 0.081 Uiso 1 1 calc GR . . . .
H15B H 1.0412 0.6884 0.1319 0.081 Uiso 1 1 calc GR . . . .
H15C H 1.0071 0.7673 0.1636 0.081 Uiso 1 1 calc GR . . . .
C67 C 1.02685(11) 0.6370(2) 0.64513(10) 0.0716(8) Uani 1 1 d . . . . .
H67A H 1.0039 0.6327 0.6741 0.107 Uiso 1 1 calc GR . . . .
H67B H 1.0447 0.7040 0.6453 0.107 Uiso 1 1 calc GR . . . .
H67C H 1.0547 0.5832 0.6485 0.107 Uiso 1 1 calc GR . . . .
C57 C 0.94964(9) 0.9694(2) 0.54772(9) 0.0536(6) Uani 1 1 d . . . . .
H57A H 0.9261 0.9530 0.5165 0.080 Uiso 1 1 calc GR . . . .
H57B H 0.9873 0.9489 0.5430 0.080 Uiso 1 1 calc GR . . . .
H57C H 0.9484 1.0432 0.5542 0.080 Uiso 1 1 calc GR . . . .
C69 C 1.02631(17) 0.6357(3) 0.54780(12) 0.1182(16) Uani 1 1 d . . . . .
H69A H 1.0544 0.5824 0.5492 0.177 Uiso 1 1 calc GR . . . .
H69B H 1.0438 0.7031 0.5494 0.177 Uiso 1 1 calc GR . . . .
H69C H 1.0030 0.6295 0.5155 0.177 Uiso 1 1 calc GR . . . .


_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 P1 2.2837(4) . ?
Ge1 C39 1.9761(16) . ?
Ge1 C40 1.9576(17) . ?
Ge1 C28 1.9647(17) . ?
Ge2 P2 2.2882(4) . ?
Ge2 C85 1.9725(17) . ?
Ge2 C73 1.9670(19) . ?
Ge2 C79 1.9610(18) . ?
P1 C1 1.7748(16) . ?
P2 C46 1.7800(16) . ?
N1 C1 1.3833(19) . ?
N1 C2 1.384(2) . ?
N1 C16 1.451(2) . ?
C48 N4 1.383(2) . ?
C48 C47 1.336(2) . ?
N4 C46 1.382(2) . ?
N4 C49 1.445(2) . ?
N2 C1 1.379(2) . ?
N2 C3 1.388(2) . ?
N2 C4 1.451(2) . ?
C3 C2 1.336(2) . ?
N3 C46 1.373(2) . ?
N3 C61 1.450(2) . ?
N3 C47 1.392(2) . ?
C21 C16 1.400(2) . ?
C21 C23 1.514(2) . ?
C21 C20 1.397(2) . ?
C61 C66 1.403(2) . ?
C61 C62 1.397(2) . ?
C39 C34 1.391(2) . ?
C39 C38 1.392(2) . ?
C17 C18 1.391(2) . ?
C17 C16 1.400(2) . ?
C17 C26 1.519(2) . ?
C45 C40 1.390(2) . ?
C45 C44 1.387(3) . ?
C40 C41 1.396(2) . ?
C5 C4 1.401(2) . ?
C5 C6 1.397(3) . ?
C5 C14 1.514(3) . ?
C18 C19 1.378(3) . ?
C50 C51 1.392(2) . ?
C50 C49 1.397(2) . ?
C50 C59 1.511(2) . ?
C28 C29 1.395(2) . ?
C28 C33 1.391(3) . ?
C71 C62 1.513(2) . ?
C71 C72 1.538(2) . ?
C71 C70 1.526(2) . ?
C51 C52 1.381(3) . ?
C84 C79 1.394(3) . ?
C84 C83 1.393(3) . ?
C29 C30 1.387(3) . ?
C85 C90 1.387(3) . ?
C85 C86 1.388(3) . ?
C49 C54 1.396(2) . ?
C73 C78 1.388(3) . ?
C73 C74 1.399(3) . ?
C23 C22 1.527(3) . ?
C23 C24 1.535(3) . ?
C35 C34 1.389(2) . ?
C35 C36 1.373(3) . ?
C52 C53 1.378(3) . ?
C20 C19 1.382(2) . ?
C66 C68 1.517(3) . ?
C66 C65 1.394(3) . ?
C4 C9 1.399(2) . ?
C33 C32 1.389(3) . ?
C68 C67 1.507(3) . ?
C68 C69 1.515(3) . ?
C79 C80 1.390(3) . ?
C62 C63 1.394(2) . ?
C59 C58 1.529(3) . ?
C59 C60 1.537(3) . ?
C41 C42 1.383(3) . ?
C36 C37 1.383(3) . ?
C9 C8 1.398(2) . ?
C9 C11 1.513(2) . ?
C8 C7 1.375(3) . ?
C63 C64 1.378(3) . ?
C53 C54 1.391(3) . ?
C65 C64 1.374(3) . ?
C37 C38 1.391(3) . ?
C78 C77 1.386(3) . ?
C42 C43 1.378(3) . ?
C11 C10 1.536(3) . ?
C11 C12 1.526(3) . ?
C54 C56 1.521(3) . ?
C26 C27 1.526(3) . ?
C26 C25 1.518(3) . ?
C80 C81 1.395(3) . ?
C6 C7 1.377(3) . ?
C30 C31 1.372(3) . ?
C31 C32 1.377(3) . ?
C90 C89 1.387(3) . ?
C14 C13 1.533(3) . ?
C14 C15 1.519(3) . ?
C77 C76 1.379(3) . ?
C56 C55 1.515(3) . ?
C56 C57 1.521(3) . ?
C44 C43 1.387(3) . ?
C82 C83 1.374(4) . ?
C82 C81 1.372(4) . ?
C89 C88 1.370(4) . ?
C88 C87 1.386(5) . ?
C86 C87 1.392(4) . ?
C75 C74 1.388(3) . ?
C75 C76 1.374(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C39 Ge1 P1 98.22(5) . . ?
C40 Ge1 P1 112.73(5) . . ?
C40 Ge1 C39 105.40(7) . . ?
C40 Ge1 C28 109.20(7) . . ?
C28 Ge1 P1 126.06(5) . . ?
C28 Ge1 C39 101.81(7) . . ?
C85 Ge2 P2 97.40(5) . . ?
C73 Ge2 P2 112.22(5) . . ?
C73 Ge2 C85 105.47(7) . . ?
C79 Ge2 P2 125.75(6) . . ?
C79 Ge2 C85 103.32(8) . . ?
C79 Ge2 C73 109.50(8) . . ?
C1 P1 Ge1 110.07(5) . . ?
C46 P2 Ge2 110.32(5) . . ?
C1 N1 C2 110.50(13) . . ?
C1 N1 C16 126.71(13) . . ?
C2 N1 C16 122.74(13) . . ?
C47 C48 N4 107.33(14) . . ?
C48 N4 C49 123.64(13) . . ?
C46 N4 C48 110.61(13) . . ?
C46 N4 C49 125.25(13) . . ?
C1 N2 C3 110.17(13) . . ?
C1 N2 C4 126.52(13) . . ?
C3 N2 C4 121.05(13) . . ?
N1 C1 P1 121.41(11) . . ?
N2 C1 P1 133.94(12) . . ?
N2 C1 N1 104.01(12) . . ?
C2 C3 N2 107.89(14) . . ?
C46 N3 C61 127.29(13) . . ?
C46 N3 C47 110.24(13) . . ?
C47 N3 C61 121.56(13) . . ?
C16 C21 C23 123.56(14) . . ?
C20 C21 C16 117.55(15) . . ?
C20 C21 C23 118.89(15) . . ?
N4 C46 P2 120.27(11) . . ?
N3 C46 P2 135.05(12) . . ?
N3 C46 N4 104.08(13) . . ?
C66 C61 N3 118.43(15) . . ?
C62 C61 N3 118.49(14) . . ?
C62 C61 C66 122.84(15) . . ?
C34 C39 Ge1 121.40(12) . . ?
C34 C39 C38 117.83(15) . . ?
C38 C39 Ge1 120.76(13) . . ?
C48 C47 N3 107.73(14) . . ?
C18 C17 C16 117.49(15) . . ?
C18 C17 C26 120.01(15) . . ?
C16 C17 C26 122.48(15) . . ?
C44 C45 C40 120.68(17) . . ?
C45 C40 Ge1 122.78(12) . . ?
C45 C40 C41 118.00(16) . . ?
C41 C40 Ge1 119.13(13) . . ?
C4 C5 C14 123.26(16) . . ?
C6 C5 C4 116.72(17) . . ?
C6 C5 C14 119.97(16) . . ?
C19 C18 C17 121.37(16) . . ?
C51 C50 C49 117.28(16) . . ?
C51 C50 C59 119.97(16) . . ?
C49 C50 C59 122.75(15) . . ?
C3 C2 N1 107.44(14) . . ?
C29 C28 Ge1 120.96(13) . . ?
C33 C28 Ge1 120.64(13) . . ?
C33 C28 C29 117.51(16) . . ?
C21 C16 N1 118.75(14) . . ?
C21 C16 C17 122.43(15) . . ?
C17 C16 N1 118.71(14) . . ?
C62 C71 C72 109.86(14) . . ?
C62 C71 C70 113.17(15) . . ?
C70 C71 C72 109.77(15) . . ?
C52 C51 C50 121.10(17) . . ?
C83 C84 C79 120.3(2) . . ?
C30 C29 C28 121.42(18) . . ?
C90 C85 Ge2 121.78(14) . . ?
C90 C85 C86 118.36(19) . . ?
C86 C85 Ge2 119.85(16) . . ?
C50 C49 N4 119.22(14) . . ?
C54 C49 N4 118.04(14) . . ?
C54 C49 C50 122.71(15) . . ?
C78 C73 Ge2 122.04(13) . . ?
C78 C73 C74 117.30(18) . . ?
C74 C73 Ge2 120.51(15) . . ?
C21 C23 C22 111.41(15) . . ?
C21 C23 C24 110.00(15) . . ?
C22 C23 C24 110.86(17) . . ?
C36 C35 C34 120.43(17) . . ?
C53 C52 C51 120.35(16) . . ?
C19 C20 C21 120.95(16) . . ?
C61 C66 C68 122.59(16) . . ?
C65 C66 C61 116.75(17) . . ?
C65 C66 C68 120.60(16) . . ?
C35 C34 C39 120.97(16) . . ?
C5 C4 N2 117.65(14) . . ?
C9 C4 N2 118.83(14) . . ?
C9 C4 C5 123.17(15) . . ?
C32 C33 C28 120.75(18) . . ?
C67 C68 C66 113.40(19) . . ?
C67 C68 C69 110.1(2) . . ?
C69 C68 C66 110.57(18) . . ?
C84 C79 Ge2 120.72(16) . . ?
C80 C79 Ge2 120.14(15) . . ?
C80 C79 C84 118.51(18) . . ?
C61 C62 C71 122.40(14) . . ?
C63 C62 C61 117.47(16) . . ?
C63 C62 C71 120.03(16) . . ?
C50 C59 C58 110.66(19) . . ?
C50 C59 C60 109.89(17) . . ?
C58 C59 C60 112.2(2) . . ?
C42 C41 C40 121.47(17) . . ?
C35 C36 C37 119.68(16) . . ?
C4 C9 C11 122.34(15) . . ?
C8 C9 C4 117.07(16) . . ?
C8 C9 C11 120.42(16) . . ?
C7 C8 C9 121.06(18) . . ?
C64 C63 C62 120.83(17) . . ?
C52 C53 C54 120.86(17) . . ?
C64 C65 C66 121.53(17) . . ?
C36 C37 C38 119.91(17) . . ?
C77 C78 C73 121.44(18) . . ?
C43 C42 C41 119.76(17) . . ?
C9 C11 C10 109.62(16) . . ?
C9 C11 C12 113.94(15) . . ?
C12 C11 C10 109.18(15) . . ?
C49 C54 C56 122.06(16) . . ?
C53 C54 C49 117.66(16) . . ?
C53 C54 C56 120.27(16) . . ?
C17 C26 C27 110.19(16) . . ?
C25 C26 C17 112.54(16) . . ?
C25 C26 C27 111.78(18) . . ?
C65 C64 C63 120.51(17) . . ?
C18 C19 C20 120.20(16) . . ?
C79 C80 C81 120.7(2) . . ?
C7 C6 C5 121.33(18) . . ?
C37 C38 C39 121.16(17) . . ?
C31 C30 C29 120.14(19) . . ?
C8 C7 C6 120.57(17) . . ?
C30 C31 C32 119.49(18) . . ?
C85 C90 C89 121.4(2) . . ?
C31 C32 C33 120.70(19) . . ?
C5 C14 C13 111.33(16) . . ?
C5 C14 C15 112.30(17) . . ?
C15 C14 C13 110.99(17) . . ?
C76 C77 C78 120.3(2) . . ?
C55 C56 C54 112.14(18) . . ?
C55 C56 C57 111.12(17) . . ?
C57 C56 C54 111.16(16) . . ?
C43 C44 C45 120.33(18) . . ?
C81 C82 C83 120.4(2) . . ?
C88 C89 C90 119.6(3) . . ?
C89 C88 C87 120.1(2) . . ?
C85 C86 C87 120.4(3) . . ?
C82 C83 C84 120.2(2) . . ?
C82 C81 C80 119.9(3) . . ?
C76 C75 C74 120.34(19) . . ?
C75 C74 C73 121.2(2) . . ?
C42 C43 C44 119.76(18) . . ?
C88 C87 C86 120.0(2) . . ?
C75 C76 C77 119.5(2) . . ?

_olex2_date_sample_data_collection 2015-08-08
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_2231
_database_code_depnum_ccdc_archive 'CCDC 1425916'
_audit_update_record             
;
2015-09-18 deposited with the CCDC.
2016-08-09 downloaded from the CCDC.
;





_audit_creation_date             2015-02-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014-3


_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C39 H39 N2 P Sn), C4 H10 O'
_chemical_formula_sum            'C160 H164 N8 O1.50 P4 Sn4'
_chemical_formula_weight         2821.62
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O P Sn'
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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.0114(3)
_cell_length_b                   17.0048(5)
_cell_length_c                   18.7117(5)
_cell_angle_alpha                111.389(3)
_cell_angle_beta                 94.838(2)
_cell_angle_gamma                110.638(3)
_cell_volume                     3498.22(18)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    14362
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.7850
_cell_measurement_theta_min      3.2620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.795
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25463
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.981
_diffrn_reflns_theta_min         2.808
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.795
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -59.00   36.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6647  -57.0000  -90.0000 95

#__ type_ start__ end____ width___ exp.time_
  2 omega  -20.00   51.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6647  -99.0000 -180.0000 71

#__ type_ start__ end____ width___ exp.time_
  3 omega  -14.00   78.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6647   57.0000   60.0000 92
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0179465000
_diffrn_orient_matrix_UB_12      -0.0209201000
_diffrn_orient_matrix_UB_13      -0.0419089000
_diffrn_orient_matrix_UB_21      -0.0340876000
_diffrn_orient_matrix_UB_22      -0.0425396000
_diffrn_orient_matrix_UB_23      0.0008034000
_diffrn_orient_matrix_UB_31      -0.0460941000
_diffrn_orient_matrix_UB_32      0.0131259000
_diffrn_orient_matrix_UB_33      0.0023557000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13745
_reflns_number_total             16210
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.228
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         16210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0326
_refine_ls_restrained_S_all      1.150
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0240P)²+1.6320P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0761
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(O2) = Uiso(C1A) = Uiso(C1B) = Uiso(C1C) = Uiso(C1D)
Uanis(C46) = Uanis(C47) = Uanis(C48) = Uanis(C43) = Uanis(C44) = Uanis(C45)
3. Others
 Fixed Sof: O2(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5) H1BA(0.5)
 H1BB(0.5) C1C(0.5) H1CA(0.5) H1CB(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) H1DC(0.5)
4.a Free rotating group:
 O2(C1A,C1B,C1C,C1D)
4.b Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C1C(H1CA,H1CB)
4.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C6(H6), C74(H74), C15(H15), C39(H39), C22(H22), C56(H56), C23(H23),
 C78(H78), C41(H41), C45(H45), C25(H25), C62(H62), C77(H77), C33(H33), C38(H38),
  C3(H3), C76(H76), C8(H8), C26(H26), C37(H37), C17(H17), C68(H68), C2(H2),
 C24(H24), C75(H75), C66(H66), C31(H31), C65(H65), C54(H54), C30(H30), C72(H72),
  C69(H69), C63(H63), C70(H70), C47(H47), C64(H64), C29(H29), C71(H71), C32(H32)
4.d Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C19(H19A,H19B,
 H19C), C58(H58A,H58B,H58C), C51(H51A,H51B,H51C), C49(H49A,H49B,H49C), C59(H59A,
 H59B,H59C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C50(H50A,H50B,H50C), C1A(H1AA,H1AB,H1AC), C1D(H1DA,H1DB,H1DC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.19825(2) 0.06705(2) 0.29124(2) 0.02477(4) Uani 1 1 d . . . . .
Sn2 Sn -0.15574(2) 0.42855(2) 0.18554(2) 0.02571(5) Uani 1 1 d . . . . .
P1 P 0.29466(5) -0.01738(4) 0.32941(4) 0.02779(13) Uani 1 1 d . . . . .
P2 P 0.03976(5) 0.44091(4) 0.19670(4) 0.02898(13) Uani 1 1 d . . . . .
N1 N 0.26113(15) -0.19556(13) 0.29176(12) 0.0275(4) Uani 1 1 d . . . . .
N3 N 0.17897(16) 0.41779(13) 0.29746(11) 0.0269(4) Uani 1 1 d . . . . .
C61 C -0.16370(19) 0.49289(16) 0.10622(15) 0.0299(5) Uani 1 1 d . . . . .
C73 C -0.30132(19) 0.29939(16) 0.12024(14) 0.0286(5) Uani 1 1 d . . . . .
C13 C 0.01613(18) -0.17764(15) 0.20998(14) 0.0267(5) Uani 1 1 d . . . . .
C1 C 0.21245(18) -0.13912(15) 0.28182(13) 0.0248(5) Uani 1 1 d . . . . .
N4 N 0.00650(16) 0.34371(13) 0.29961(11) 0.0271(4) Uani 1 1 d . . . . .
C40 C 0.06867(18) 0.39860(15) 0.26652(13) 0.0242(5) Uani 1 1 d . . . . .
C43 C -0.1142(2) 0.29070(19) 0.27947(17) 0.0391(2) Uani 1 1 d . . . . .
C9 C 0.40479(19) -0.14168(15) 0.41187(14) 0.0270(5) Uani 1 1 d . . . . .
C4 C 0.37720(18) -0.16340(15) 0.33168(14) 0.0254(5) Uani 1 1 d . . . . .
N2 N 0.10654(15) -0.19918(13) 0.23499(12) 0.0289(4) Uani 1 1 d . . . . .
C27 C 0.33124(19) 0.20589(16) 0.35201(14) 0.0279(5) Uani 1 1 d . . . . .
C5 C 0.4575(2) -0.15596(17) 0.28705(14) 0.0306(5) Uani 1 1 d . . . . .
C42 C 0.0780(2) 0.32950(18) 0.34903(14) 0.0340(5) Uani 1 1 d . . . . .
H42 H 0.0550 0.2936 0.3782 0.041 Uiso 1 1 calc R . . . .
C28 C 0.05370(19) 0.08110(15) 0.33360(14) 0.0267(5) Uani 1 1 d . . . . .
C67 C -0.1798(2) 0.51495(17) 0.29365(14) 0.0333(5) Uani 1 1 d . . . . .
C34 C 0.18098(19) 0.05049(15) 0.17103(13) 0.0270(5) Uani 1 1 d . . . . .
C7 C 0.59950(19) -0.10999(16) 0.40452(14) 0.0289(5) Uani 1 1 d . . . . .
C35 C 0.1251(2) 0.09206(18) 0.14104(16) 0.0356(6) Uani 1 1 d . . . . .
C6 C 0.56922(19) -0.12789(17) 0.32561(15) 0.0312(5) Uani 1 1 d . . . . .
H6 H 0.6262 -0.1209 0.2969 0.037 Uiso 1 1 calc R . . . .
C18 C -0.05354(19) -0.16098(16) 0.26111(14) 0.0289(5) Uani 1 1 d . . . . .
C74 C -0.2989(2) 0.24052(17) 0.04604(15) 0.0347(6) Uani 1 1 d . . . . .
H74 H -0.2310 0.2556 0.0285 0.042 Uiso 1 1 calc R . . . .
C14 C -0.00607(19) -0.18491(17) 0.13338(14) 0.0326(5) Uani 1 1 d . . . . .
C52 C 0.27683(18) 0.47619(16) 0.28195(14) 0.0272(5) Uani 1 1 d . . . . .
C36 C 0.1223(2) 0.08784(19) 0.06563(16) 0.0397(6) Uani 1 1 d . . . . .
C60 C 0.2583(2) 0.33496(17) 0.16322(16) 0.0413(6) Uani 1 1 d . . . . .
H60A H 0.2505 0.2981 0.1939 0.062 Uiso 1 1 calc GR . . . .
H60B H 0.3025 0.3187 0.1248 0.062 Uiso 1 1 calc GR . . . .
H60C H 0.1830 0.3219 0.1351 0.062 Uiso 1 1 calc GR . . . .
C15 C -0.1000(2) -0.17105(19) 0.10923(16) 0.0390(6) Uani 1 1 d . . . . .
H15 H -0.1155 -0.1736 0.0577 0.047 Uiso 1 1 calc R . . . .
C39 C 0.2373(2) 0.00567(17) 0.12314(14) 0.0333(5) Uani 1 1 d . . . . .
H39 H 0.2776 -0.0223 0.1424 0.040 Uiso 1 1 calc R . . . .
C22 C 0.3722(2) 0.25078(18) 0.43398(15) 0.0374(6) Uani 1 1 d . . . . .
H22 H 0.3416 0.2193 0.4652 0.045 Uiso 1 1 calc R . . . .
C12 C 0.7194(2) -0.08827(19) 0.44220(16) 0.0371(6) Uani 1 1 d . . . . .
H12A H 0.7280 -0.1463 0.4311 0.056 Uiso 1 1 calc GR . . . .
H12B H 0.7355 -0.0528 0.4996 0.056 Uiso 1 1 calc GR . . . .
H12C H 0.7724 -0.0517 0.4203 0.056 Uiso 1 1 calc GR . . . .
C56 C 0.4253(2) 0.62498(17) 0.31849(16) 0.0359(6) Uani 1 1 d . . . . .
H56 H 0.4616 0.6894 0.3521 0.043 Uiso 1 1 calc R . . . .
C44 C -0.1631(2) 0.21195(19) 0.20727(17) 0.0391(2) Uani 1 1 d . . . . .
C23 C 0.4566(2) 0.3402(2) 0.47123(16) 0.0446(7) Uani 1 1 d . . . . .
H23 H 0.4830 0.3691 0.5272 0.054 Uiso 1 1 calc R . . . .
C78 C -0.4028(2) 0.27494(18) 0.14340(16) 0.0366(6) Uani 1 1 d . . . . .
H78 H -0.4068 0.3133 0.1938 0.044 Uiso 1 1 calc R . . . .
C57 C 0.3287(2) 0.57005(17) 0.33304(15) 0.0308(5) Uani 1 1 d . . . . .
C10 C 0.3166(2) -0.14445(18) 0.45956(15) 0.0352(6) Uani 1 1 d . . . . .
H10A H 0.2903 -0.0963 0.4624 0.053 Uiso 1 1 calc GR . . . .
H10B H 0.3499 -0.1335 0.5131 0.053 Uiso 1 1 calc GR . . . .
H10C H 0.2525 -0.2054 0.4341 0.053 Uiso 1 1 calc GR . . . .
C41 C 0.1843(2) 0.37546(17) 0.34777(14) 0.0337(5) Uani 1 1 d . . . . .
H41 H 0.2510 0.3786 0.3759 0.040 Uiso 1 1 calc R . . . .
C48 C -0.1749(2) 0.31151(19) 0.33636(17) 0.0391(2) Uani 1 1 d . . . . .
C19 C -0.0294(2) -0.1575(2) 0.34234(15) 0.0412(6) Uani 1 1 d . . . . .
H19A H -0.0356 -0.2183 0.3379 0.062 Uiso 1 1 calc GR . . . .
H19B H -0.0842 -0.1411 0.3705 0.062 Uiso 1 1 calc GR . . . .
H19C H 0.0473 -0.1107 0.3716 0.062 Uiso 1 1 calc GR . . . .
C58 C 0.2810(2) 0.61045(19) 0.40063(16) 0.0419(7) Uani 1 1 d . . . . .
H58A H 0.2074 0.6076 0.3798 0.063 Uiso 1 1 calc GR . . . .
H58B H 0.3331 0.6752 0.4336 0.063 Uiso 1 1 calc GR . . . .
H58C H 0.2712 0.5749 0.4325 0.063 Uiso 1 1 calc GR . . . .
C45 C -0.2752(2) 0.15364(19) 0.19363(17) 0.0391(2) Uani 1 1 d . . . . .
H45 H -0.3100 0.1004 0.1445 0.047 Uiso 1 1 calc R . . . .
C25 C 0.4637(2) 0.34462(19) 0.34588(18) 0.0463(7) Uani 1 1 d . . . . .
H25 H 0.4949 0.3765 0.3151 0.056 Uiso 1 1 calc R . . . .
C62 C -0.1351(2) 0.4628(2) 0.03395(16) 0.0414(6) Uani 1 1 d . . . . .
H62 H -0.1058 0.4168 0.0216 0.050 Uiso 1 1 calc R . . . .
C77 C -0.4980(2) 0.1957(2) 0.09431(18) 0.0465(7) Uani 1 1 d . . . . .
H77 H -0.5667 0.1810 0.1109 0.056 Uiso 1 1 calc R . . . .
C33 C 0.0554(2) 0.1028(2) 0.41235(16) 0.0477(7) Uani 1 1 d . . . . .
H33 H 0.1179 0.1072 0.4462 0.057 Uiso 1 1 calc R . . . .
C38 C 0.2355(2) 0.00117(18) 0.04747(15) 0.0413(6) Uani 1 1 d . . . . .
H38 H 0.2743 -0.0299 0.0154 0.050 Uiso 1 1 calc R . . . .
C3 C 0.0914(2) -0.29060(17) 0.21589(17) 0.0399(6) Uani 1 1 d . . . . .
H3 H 0.0251 -0.3448 0.1838 0.048 Uiso 1 1 calc R . . . .
C76 C -0.4931(2) 0.1382(2) 0.02133(17) 0.0463(7) Uani 1 1 d . . . . .
H76 H -0.5581 0.0836 -0.0122 0.056 Uiso 1 1 calc R . . . .
C8 C 0.51701(19) -0.11543(16) 0.44729(14) 0.0288(5) Uani 1 1 d . . . . .
H8 H 0.5378 -0.1009 0.5020 0.035 Uiso 1 1 calc R . . . .
C51 C -0.0960(2) 0.18940(18) 0.14766(15) 0.0397(6) Uani 1 1 d . . . . .
H51A H -0.0941 0.2241 0.1155 0.060 Uiso 1 1 calc GR . . . .
H51B H -0.1313 0.1228 0.1133 0.060 Uiso 1 1 calc GR . . . .
H51C H -0.0185 0.2066 0.1751 0.060 Uiso 1 1 calc GR . . . .
C26 C 0.3796(2) 0.25529(18) 0.30913(16) 0.0381(6) Uani 1 1 d . . . . .
H26 H 0.3541 0.2268 0.2531 0.046 Uiso 1 1 calc R . . . .
C37 C 0.1776(2) 0.04154(18) 0.01873(15) 0.0415(6) Uani 1 1 d . . . . .
H37 H 0.1757 0.0376 -0.0334 0.050 Uiso 1 1 calc R . . . .
C17 C -0.1467(2) -0.14892(18) 0.23349(16) 0.0345(6) Uani 1 1 d . . . . .
H17 H -0.1951 -0.1370 0.2673 0.041 Uiso 1 1 calc R . . . .
C55 C 0.4699(2) 0.58822(18) 0.25640(18) 0.0395(6) Uani 1 1 d . . . . .
C68 C -0.0857(3) 0.5769(2) 0.35581(17) 0.0495(7) Uani 1 1 d . . . . .
H68 H -0.0134 0.5779 0.3504 0.059 Uiso 1 1 calc R . . . .
C2 C 0.1869(2) -0.28803(17) 0.25092(16) 0.0371(6) Uani 1 1 d . . . . .
H2 H 0.2013 -0.3399 0.2483 0.045 Uiso 1 1 calc R . . . .
C16 C -0.1714(2) -0.1537(2) 0.15778(17) 0.0389(6) Uani 1 1 d . . . . .
C24 C 0.5022(2) 0.38730(19) 0.42716(17) 0.0443(7) Uani 1 1 d . . . . .
H24 H 0.5597 0.4487 0.4526 0.053 Uiso 1 1 calc R . . . .
C75 C -0.3929(2) 0.16077(19) -0.00248(16) 0.0427(6) Uani 1 1 d . . . . .
H75 H -0.3889 0.1212 -0.0524 0.051 Uiso 1 1 calc R . . . .
C49 C -0.1209(3) 0.3950(2) 0.41430(17) 0.0567(8) Uani 1 1 d . . . . .
H49A H -0.0974 0.3767 0.4546 0.085 Uiso 1 1 calc GR . . . .
H49B H -0.1756 0.4216 0.4298 0.085 Uiso 1 1 calc GR . . . .
H49C H -0.0546 0.4413 0.4093 0.085 Uiso 1 1 calc GR . . . .
C59 C 0.5758(3) 0.6492(2) 0.2425(2) 0.0563(9) Uani 1 1 d . . . . .
H59A H 0.5595 0.6931 0.2262 0.084 Uiso 1 1 calc GR . . . .
H59B H 0.6003 0.6105 0.2008 0.084 Uiso 1 1 calc GR . . . .
H59C H 0.6359 0.6835 0.2915 0.084 Uiso 1 1 calc GR . . . .
C66 C -0.2049(2) 0.56114(19) 0.12293(19) 0.0420(6) Uani 1 1 d . . . . .
H66 H -0.2239 0.5835 0.1721 0.050 Uiso 1 1 calc R . . . .
C31 C -0.1233(2) 0.1118(2) 0.39621(19) 0.0484(7) Uani 1 1 d . . . . .
H31 H -0.1833 0.1224 0.4177 0.058 Uiso 1 1 calc R . . . .
C65 C -0.2185(3) 0.5971(2) 0.0689(2) 0.0612(10) Uani 1 1 d . . . . .
H65 H -0.2474 0.6433 0.0810 0.073 Uiso 1 1 calc R . . . .
C54 C 0.4149(2) 0.49421(18) 0.20637(17) 0.0386(6) Uani 1 1 d . . . . .
H54 H 0.4442 0.4687 0.1630 0.046 Uiso 1 1 calc R . . . .
C30 C -0.1279(2) 0.0900(2) 0.31796(19) 0.0443(7) Uani 1 1 d . . . . .
H30 H -0.1913 0.0852 0.2847 0.053 Uiso 1 1 calc R . . . .
C72 C -0.2842(2) 0.51633(19) 0.30355(17) 0.0432(7) Uani 1 1 d . . . . .
H72 H -0.3500 0.4756 0.2615 0.052 Uiso 1 1 calc R . . . .
C46 C -0.3384(2) 0.16942(19) 0.24812(17) 0.0391(2) Uani 1 1 d . . . . .
C53 C 0.3178(2) 0.43651(16) 0.21824(15) 0.0319(5) Uani 1 1 d . . . . .
C69 C -0.0949(3) 0.6377(2) 0.42599(18) 0.0643(10) Uani 1 1 d . . . . .
H69 H -0.0292 0.6802 0.4677 0.077 Uiso 1 1 calc R . . . .
C63 C -0.1486(3) 0.4985(2) -0.02012(19) 0.0562(8) Uani 1 1 d . . . . .
H63 H -0.1292 0.4768 -0.0693 0.067 Uiso 1 1 calc R . . . .
C11 C 0.4244(2) -0.1771(2) 0.20072(15) 0.0460(7) Uani 1 1 d . . . . .
H11A H 0.3762 -0.2434 0.1706 0.069 Uiso 1 1 calc GR . . . .
H11B H 0.4927 -0.1607 0.1810 0.069 Uiso 1 1 calc GR . . . .
H11C H 0.3827 -0.1411 0.1945 0.069 Uiso 1 1 calc GR . . . .
C70 C -0.1990(3) 0.6362(2) 0.43498(18) 0.0610(9) Uani 1 1 d . . . . .
H70 H -0.2057 0.6765 0.4834 0.073 Uiso 1 1 calc R . . . .
C47 C -0.2887(2) 0.24837(19) 0.31790(17) 0.0391(2) Uani 1 1 d . . . . .
H47 H -0.3327 0.2608 0.3551 0.047 Uiso 1 1 calc R . . . .
C20 C 0.0624(2) -0.2139(2) 0.07599(16) 0.0452(7) Uani 1 1 d . . . . .
H20A H 0.1415 -0.1890 0.1047 0.068 Uiso 1 1 calc GR . . . .
H20B H 0.0583 -0.1899 0.0360 0.068 Uiso 1 1 calc GR . . . .
H20C H 0.0319 -0.2818 0.0500 0.068 Uiso 1 1 calc GR . . . .
C64 C -0.1905(3) 0.5660(3) -0.0020(2) 0.0659(10) Uani 1 1 d . . . . .
H64 H -0.1998 0.5908 -0.0388 0.079 Uiso 1 1 calc R . . . .
C29 C -0.0398(2) 0.0749(2) 0.28697(16) 0.0382(6) Uani 1 1 d . . . . .
H29 H -0.0438 0.0599 0.2324 0.046 Uiso 1 1 calc R . . . .
C71 C -0.2934(3) 0.5764(2) 0.3742(2) 0.0558(8) Uani 1 1 d . . . . .
H71 H -0.3653 0.5761 0.3802 0.067 Uiso 1 1 calc R . . . .
C32 C -0.0328(3) 0.1183(3) 0.44305(18) 0.0633(10) Uani 1 1 d . . . . .
H32 H -0.0295 0.1336 0.4976 0.076 Uiso 1 1 calc R . . . .
C21 C -0.2742(3) -0.1407(3) 0.1299(2) 0.0624(9) Uani 1 1 d . . . . .
H21A H -0.2580 -0.0745 0.1531 0.094 Uiso 1 1 calc GR . . . .
H21B H -0.3386 -0.1741 0.1466 0.094 Uiso 1 1 calc GR . . . .
H21C H -0.2926 -0.1649 0.0721 0.094 Uiso 1 1 calc GR . . . .
C50 C -0.4596(3) 0.1014(3) 0.2325(3) 0.0815(13) Uani 1 1 d . . . . .
H50A H -0.5093 0.1340 0.2385 0.122 Uiso 1 1 calc GR . . . .
H50B H -0.4646 0.0736 0.2704 0.122 Uiso 1 1 calc GR . . . .
H50C H -0.4831 0.0525 0.1786 0.122 Uiso 1 1 calc GR . . . .
H35 H 0.087(2) 0.1229(19) 0.1716(17) 0.046(8) Uiso 1 1 d . . . . .
H36 H 0.084(2) 0.1141(19) 0.0447(16) 0.042(8) Uiso 1 1 d . . . . .
O2 O -0.5069(3) 0.5006(2) 0.02064(17) 0.0633(8) Uiso 0.5 1 d . . P A -1
C1A C -0.4899(5) 0.3649(3) 0.0198(3) 0.0633(8) Uiso 0.5 1 d G . P A -1
H1AA H -0.4736 0.3121 -0.0111 0.095 Uiso 0.5 1 calc GR . P A -1
H1AB H -0.5653 0.3421 0.0296 0.095 Uiso 0.5 1 calc GR . P A -1
H1AC H -0.4331 0.4028 0.0705 0.095 Uiso 0.5 1 calc GR . P A -1
C1B C -0.4862(5) 0.4232(3) -0.0258(2) 0.0633(8) Uiso 0.5 1 d G . P A -1
H1BA H -0.4111 0.4447 -0.0375 0.076 Uiso 0.5 1 calc R . P A -1
H1BB H -0.5444 0.3856 -0.0766 0.076 Uiso 0.5 1 calc R . P A -1
C1C C -0.5054(5) 0.5600(3) -0.0167(2) 0.0633(8) Uiso 0.5 1 d G . P A -1
H1CA H -0.5640 0.5252 -0.0674 0.076 Uiso 0.5 1 calc R . P A -1
H1CB H -0.4306 0.5842 -0.0283 0.076 Uiso 0.5 1 calc R . P A -1
C1D C -0.5284(5) 0.6398(3) 0.0381(3) 0.0633(8) Uiso 0.5 1 d G . P A -1
H1DA H -0.5355 0.6777 0.0107 0.095 Uiso 0.5 1 calc GR . P A -1
H1DB H -0.4657 0.6780 0.0855 0.095 Uiso 0.5 1 calc GR . P A -1
H1DC H -0.5990 0.6151 0.0533 0.095 Uiso 0.5 1 calc GR . P 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
Sn1 P1 2.4518(6) . ?
Sn1 C27 2.166(2) . ?
Sn1 C28 2.157(2) . ?
Sn1 C34 2.144(2) . ?
Sn2 P2 2.4617(6) . ?
Sn2 C61 2.156(2) . ?
Sn2 C73 2.150(2) . ?
Sn2 C67 2.147(2) . ?
P1 C1 1.777(2) . ?
P2 C40 1.777(2) . ?
N1 C1 1.377(3) . ?
N1 C4 1.438(3) . ?
N1 C2 1.385(3) . ?
N3 C40 1.376(3) . ?
N3 C52 1.440(3) . ?
N3 C41 1.388(3) . ?
C61 C62 1.394(4) . ?
C61 C66 1.390(3) . ?
C73 C74 1.395(3) . ?
C73 C78 1.395(3) . ?
C13 N2 1.440(3) . ?
C13 C18 1.395(3) . ?
C13 C14 1.389(3) . ?
C1 N2 1.364(3) . ?
N4 C40 1.372(3) . ?
N4 C43 1.441(3) . ?
N4 C42 1.398(3) . ?
C43 C44 1.399(4) . ?
C43 C48 1.395(4) . ?
C9 C4 1.389(3) . ?
C9 C10 1.510(3) . ?
C9 C8 1.390(3) . ?
C4 C5 1.391(3) . ?
N2 C3 1.396(3) . ?
C27 C22 1.393(3) . ?
C27 C26 1.396(3) . ?
C5 C6 1.395(3) . ?
C5 C11 1.508(3) . ?
C42 C41 1.335(3) . ?
C28 C33 1.378(3) . ?
C28 C29 1.384(3) . ?
C67 C68 1.385(4) . ?
C67 C72 1.394(4) . ?
C34 C35 1.388(3) . ?
C34 C39 1.388(3) . ?
C7 C6 1.385(3) . ?
C7 C12 1.512(3) . ?
C7 C8 1.389(3) . ?
C35 C36 1.383(4) . ?
C18 C19 1.501(3) . ?
C18 C17 1.387(3) . ?
C74 C75 1.381(4) . ?
C14 C15 1.393(4) . ?
C14 C20 1.509(3) . ?
C52 C57 1.391(3) . ?
C52 C53 1.391(3) . ?
C36 C37 1.382(4) . ?
C60 C53 1.506(3) . ?
C15 C16 1.384(4) . ?
C39 C38 1.387(4) . ?
C22 C23 1.388(4) . ?
C56 C57 1.394(3) . ?
C56 C55 1.384(4) . ?
C44 C45 1.381(4) . ?
C44 C51 1.498(4) . ?
C23 C24 1.379(4) . ?
C78 C77 1.386(4) . ?
C57 C58 1.503(3) . ?
C48 C49 1.500(4) . ?
C48 C47 1.409(4) . ?
C45 C46 1.373(4) . ?
C25 C26 1.385(4) . ?
C25 C24 1.379(4) . ?
C62 C63 1.384(4) . ?
C77 C76 1.382(4) . ?
C33 C32 1.389(4) . ?
C38 C37 1.376(4) . ?
C3 C2 1.334(4) . ?
C76 C75 1.384(4) . ?
C17 C16 1.392(4) . ?
C55 C59 1.513(4) . ?
C55 C54 1.390(4) . ?
C68 C69 1.389(4) . ?
C16 C21 1.512(4) . ?
C66 C65 1.387(4) . ?
C31 C30 1.363(4) . ?
C31 C32 1.354(5) . ?
C65 C64 1.371(5) . ?
C54 C53 1.393(3) . ?
C30 C29 1.389(3) . ?
C72 C71 1.390(4) . ?
C46 C47 1.376(4) . ?
C46 C50 1.517(4) . ?
C69 C70 1.371(5) . ?
C63 C64 1.385(5) . ?
C70 C71 1.370(5) . ?
O2 C1B 1.4196 . ?
O2 C1C 1.4193 . ?
C1A C1B 1.5181 . ?
C1C C1D 1.5179 . ?

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
C27 Sn1 P1 98.87(6) . . ?
C28 Sn1 P1 122.11(6) . . ?
C28 Sn1 C27 103.45(8) . . ?
C34 Sn1 P1 116.26(6) . . ?
C34 Sn1 C27 100.54(9) . . ?
C34 Sn1 C28 111.03(9) . . ?
C61 Sn2 P2 100.49(6) . . ?
C73 Sn2 P2 122.82(6) . . ?
C73 Sn2 C61 98.58(9) . . ?
C67 Sn2 P2 112.86(7) . . ?
C67 Sn2 C61 105.30(9) . . ?
C67 Sn2 C73 112.96(9) . . ?
C1 P1 Sn1 111.55(8) . . ?
C40 P2 Sn2 108.16(7) . . ?
C1 N1 C4 124.46(18) . . ?
C1 N1 C2 110.73(19) . . ?
C2 N1 C4 124.48(19) . . ?
C40 N3 C52 124.86(19) . . ?
C40 N3 C41 111.14(19) . . ?
C41 N3 C52 123.98(19) . . ?
C62 C61 Sn2 120.90(18) . . ?
C66 C61 Sn2 121.12(19) . . ?
C66 C61 C62 117.8(2) . . ?
C74 C73 Sn2 118.12(17) . . ?
C78 C73 Sn2 124.07(18) . . ?
C78 C73 C74 117.4(2) . . ?
C18 C13 N2 117.8(2) . . ?
C14 C13 N2 119.0(2) . . ?
C14 C13 C18 122.8(2) . . ?
N1 C1 P1 117.70(16) . . ?
N2 C1 P1 138.04(17) . . ?
N2 C1 N1 104.26(19) . . ?
C40 N4 C43 128.7(2) . . ?
C40 N4 C42 110.34(19) . . ?
C42 N4 C43 120.0(2) . . ?
N3 C40 P2 119.44(16) . . ?
N4 C40 P2 136.58(17) . . ?
N4 C40 N3 103.91(19) . . ?
C44 C43 N4 118.0(2) . . ?
C48 C43 N4 119.2(2) . . ?
C48 C43 C44 122.2(2) . . ?
C4 C9 C10 121.3(2) . . ?
C4 C9 C8 117.8(2) . . ?
C8 C9 C10 120.9(2) . . ?
C9 C4 N1 119.6(2) . . ?
C9 C4 C5 122.8(2) . . ?
C5 C4 N1 117.6(2) . . ?
C1 N2 C13 128.13(19) . . ?
C1 N2 C3 110.30(19) . . ?
C3 N2 C13 121.48(19) . . ?
C22 C27 Sn1 123.09(18) . . ?
C22 C27 C26 116.7(2) . . ?
C26 C27 Sn1 120.24(18) . . ?
C4 C5 C6 117.2(2) . . ?
C4 C5 C11 121.1(2) . . ?
C6 C5 C11 121.7(2) . . ?
C41 C42 N4 107.7(2) . . ?
C33 C28 Sn1 119.28(18) . . ?
C33 C28 C29 117.0(2) . . ?
C29 C28 Sn1 123.62(17) . . ?
C68 C67 Sn2 118.57(18) . . ?
C68 C67 C72 117.6(2) . . ?
C72 C67 Sn2 123.7(2) . . ?
C35 C34 Sn1 122.16(17) . . ?
C35 C34 C39 117.6(2) . . ?
C39 C34 Sn1 119.88(18) . . ?
C6 C7 C12 120.2(2) . . ?
C6 C7 C8 118.8(2) . . ?
C8 C7 C12 120.9(2) . . ?
C36 C35 C34 122.0(2) . . ?
C7 C6 C5 121.8(2) . . ?
C13 C18 C19 121.3(2) . . ?
C17 C18 C13 117.3(2) . . ?
C17 C18 C19 121.4(2) . . ?
C75 C74 C73 121.4(2) . . ?
C13 C14 C15 117.3(2) . . ?
C13 C14 C20 121.9(2) . . ?
C15 C14 C20 120.7(2) . . ?
C57 C52 N3 118.4(2) . . ?
C53 C52 N3 119.0(2) . . ?
C53 C52 C57 122.6(2) . . ?
C37 C36 C35 119.2(3) . . ?
C16 C15 C14 122.2(2) . . ?
C38 C39 C34 120.9(2) . . ?
C23 C22 C27 121.7(3) . . ?
C55 C56 C57 121.8(2) . . ?
C43 C44 C51 121.5(2) . . ?
C45 C44 C43 117.7(2) . . ?
C45 C44 C51 120.8(3) . . ?
C24 C23 C22 120.2(3) . . ?
C77 C78 C73 121.3(2) . . ?
C52 C57 C56 117.6(2) . . ?
C52 C57 C58 120.9(2) . . ?
C56 C57 C58 121.5(2) . . ?
C42 C41 N3 107.0(2) . . ?
C43 C48 C49 121.8(2) . . ?
C43 C48 C47 116.5(3) . . ?
C47 C48 C49 121.6(3) . . ?
C46 C45 C44 122.7(3) . . ?
C24 C25 C26 120.0(3) . . ?
C63 C62 C61 121.3(3) . . ?
C76 C77 C78 120.1(3) . . ?
C28 C33 C32 121.1(3) . . ?
C37 C38 C39 120.2(2) . . ?
C2 C3 N2 107.6(2) . . ?
C77 C76 C75 119.5(3) . . ?
C7 C8 C9 121.5(2) . . ?
C25 C26 C27 122.0(3) . . ?
C38 C37 C36 120.0(2) . . ?
C18 C17 C16 122.1(2) . . ?
C56 C55 C59 120.8(2) . . ?
C56 C55 C54 118.7(2) . . ?
C54 C55 C59 120.5(2) . . ?
C67 C68 C69 121.4(3) . . ?
C3 C2 N1 107.1(2) . . ?
C15 C16 C17 118.3(2) . . ?
C15 C16 C21 121.4(3) . . ?
C17 C16 C21 120.3(2) . . ?
C25 C24 C23 119.5(3) . . ?
C74 C75 C76 120.2(2) . . ?
C65 C66 C61 121.0(3) . . ?
C32 C31 C30 119.6(3) . . ?
C64 C65 C66 120.1(3) . . ?
C55 C54 C53 121.6(2) . . ?
C31 C30 C29 119.9(3) . . ?
C71 C72 C67 120.9(3) . . ?
C45 C46 C47 118.3(2) . . ?
C45 C46 C50 121.1(3) . . ?
C47 C46 C50 120.6(3) . . ?
C52 C53 C60 121.2(2) . . ?
C52 C53 C54 117.7(2) . . ?
C54 C53 C60 121.1(2) . . ?
C70 C69 C68 119.9(3) . . ?
C62 C63 C64 119.5(3) . . ?
C71 C70 C69 120.1(3) . . ?
C46 C47 C48 122.5(3) . . ?
C65 C64 C63 120.3(3) . . ?
C28 C29 C30 121.7(3) . . ?
C70 C71 C72 120.1(3) . . ?
C31 C32 C33 120.8(3) . . ?
C1C O2 C1B 113.5 . . ?
O2 C1B C1A 108.8 . . ?
O2 C1C C1D 108.8 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2015-08-28
_olex2_submission_special_instructions 'No special instructions were received'
