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

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

data_jr20_exo_exo_MesP4Mes
_database_code_depnum_ccdc_archive 'CCDC 1413820'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H58 P4'
_chemical_formula_sum            'C36 H58 P4'
_chemical_formula_weight         614.70

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_as_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                   16.7738(4)
_cell_length_b                   10.7853(2)
_cell_length_c                   20.6732(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.9430(10)
_cell_angle_gamma                90.00
_cell_volume                     3719.90(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9907
_cell_measurement_theta_min      5.015
_cell_measurement_theta_max      56.216

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8788
_exptl_absorpt_correction_T_max  0.9801
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            50752
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         29.00
_reflns_number_total             9868
_reflns_number_gt                7015
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker Apex V7.51A'
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine.
 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0647P)²+1.5680P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9868
_refine_ls_number_parameters     415
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1346
_refine_ls_wR_factor_gt          0.1181
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.92486(3) 0.96202(5) 0.32058(2) 0.02483(12) Uani 1 1 d . . .
P2 P 0.82611(3) 0.87367(5) 0.20755(2) 0.02406(12) Uani 1 1 d . . .
P3 P 0.95674(3) 0.84814(5) 0.23692(3) 0.02820(13) Uani 1 1 d . . .
P4 P 0.91008(3) 1.03349(5) 0.21949(3) 0.02777(13) Uani 1 1 d . . .
C1 C 1.02744(11) 1.02494(18) 0.34635(9) 0.0219(4) Uani 1 1 d . . .
C2 C 1.04530(11) 1.15224(18) 0.33667(9) 0.0230(4) Uani 1 1 d . . .
C3 C 1.12486(11) 1.18473(18) 0.33050(9) 0.0249(4) Uani 1 1 d . . .
H3 H 1.1365 1.2685 0.3208 0.030 Uiso 1 1 calc R . .
C4 C 1.18742(11) 1.10057(18) 0.33791(9) 0.0244(4) Uani 1 1 d . . .
C5 C 1.16923(11) 0.98211(19) 0.35829(10) 0.0261(4) Uani 1 1 d . . .
H5 H 1.2120 0.9253 0.3682 0.031 Uiso 1 1 calc R . .
C6 C 1.09144(12) 0.94226(17) 0.36496(9) 0.0231(4) Uani 1 1 d . . .
C7 C 0.98681(12) 1.26299(19) 0.34009(10) 0.0285(4) Uani 1 1 d . . .
C8 C 0.90365(13) 1.2289(2) 0.35920(13) 0.0391(5) Uani 1 1 d . . .
H8A H 0.8761 1.3041 0.3714 0.059 Uiso 1 1 calc R . .
H8B H 0.9094 1.1715 0.3961 0.059 Uiso 1 1 calc R . .
H8C H 0.8723 1.1892 0.3222 0.059 Uiso 1 1 calc R . .
C9 C 0.97764(15) 1.3375(2) 0.27684(12) 0.0395(5) Uani 1 1 d . . .
H9A H 0.9553 1.2842 0.2411 0.059 Uiso 1 1 calc R . .
H9B H 1.0302 1.3684 0.2676 0.059 Uiso 1 1 calc R . .
H9C H 0.9415 1.4077 0.2813 0.059 Uiso 1 1 calc R . .
C10 C 1.02396(16) 1.3486(2) 0.39531(13) 0.0432(6) Uani 1 1 d . . .
H10A H 0.9876 1.4179 0.4008 0.065 Uiso 1 1 calc R . .
H10B H 1.0754 1.3806 0.3841 0.065 Uiso 1 1 calc R . .
H10C H 1.0324 1.3013 0.4359 0.065 Uiso 1 1 calc R . .
C11 C 1.27477(12) 1.1373(2) 0.33145(11) 0.0300(4) Uani 1 1 d . . .
C12 C 1.28081(15) 1.2670(2) 0.30146(14) 0.0450(6) Uani 1 1 d . . .
H12A H 1.3369 1.2848 0.2955 0.067 Uiso 1 1 calc R . .
H12B H 1.2611 1.3290 0.3305 0.067 Uiso 1 1 calc R . .
H12C H 1.2484 1.2698 0.2593 0.067 Uiso 1 1 calc R . .
C13 C 1.32087(15) 1.1381(3) 0.39917(13) 0.0525(7) Uani 1 1 d . . .
H13A H 1.3208 1.0545 0.4178 0.079 Uiso 1 1 calc R . .
H13B H 1.2952 1.1957 0.4272 0.079 Uiso 1 1 calc R . .
H13C H 1.3762 1.1644 0.3960 0.079 Uiso 1 1 calc R . .
C14 C 1.31302(14) 1.0455(2) 0.28776(13) 0.0404(5) Uani 1 1 d . . .
H14A H 1.3689 1.0692 0.2846 0.061 Uiso 1 1 calc R . .
H14B H 1.2834 1.0462 0.2443 0.061 Uiso 1 1 calc R . .
H14C H 1.3113 0.9620 0.3063 0.061 Uiso 1 1 calc R . .
C15 C 1.08459(13) 0.8139(2) 0.39828(10) 0.0300(4) Uani 1 1 d . . .
C16 C 1.14413(16) 0.8145(2) 0.46063(12) 0.0443(6) Uani 1 1 d . . .
H16A H 1.1315 0.8837 0.4885 0.067 Uiso 1 1 calc R . .
H16B H 1.1989 0.8239 0.4488 0.067 Uiso 1 1 calc R . .
H16C H 1.1397 0.7362 0.4841 0.067 Uiso 1 1 calc R . .
C17 C 1.10885(17) 0.7085(2) 0.35471(13) 0.0465(6) Uani 1 1 d . . .
H17A H 1.1098 0.6301 0.3788 0.070 Uiso 1 1 calc R . .
H17B H 1.1622 0.7252 0.3415 0.070 Uiso 1 1 calc R . .
H17C H 1.0700 0.7026 0.3160 0.070 Uiso 1 1 calc R . .
C18 C 1.00300(15) 0.7845(3) 0.42043(14) 0.0511(7) Uani 1 1 d . . .
H18A H 0.9843 0.8555 0.4443 0.077 Uiso 1 1 calc R . .
H18B H 1.0074 0.7116 0.4489 0.077 Uiso 1 1 calc R . .
H18C H 0.9647 0.7674 0.3824 0.077 Uiso 1 1 calc R . .
C19 C 0.82492(10) 0.85385(17) 0.11733(9) 0.0197(4) Uani 1 1 d . . .
C20 C 0.80244(11) 0.95489(17) 0.07467(9) 0.0209(4) Uani 1 1 d . . .
C21 C 0.82990(11) 0.95341(18) 0.01304(9) 0.0233(4) Uani 1 1 d . . .
H21 H 0.8170 1.0219 -0.0150 0.028 Uiso 1 1 calc R . .
C22 C 0.87461(11) 0.85821(18) -0.00941(9) 0.0224(4) Uani 1 1 d . A .
C23 C 0.88449(11) 0.75398(17) 0.02965(9) 0.0229(4) Uani 1 1 d . . .
H23 H 0.9105 0.6839 0.0136 0.027 Uiso 1 1 calc R . .
C24 C 0.85818(10) 0.74636(16) 0.09151(9) 0.0200(4) Uani 1 1 d . . .
C25 C 0.74519(12) 1.06350(18) 0.08658(10) 0.0262(4) Uani 1 1 d . . .
C26 C 0.70568(13) 1.0621(2) 0.14986(11) 0.0347(5) Uani 1 1 d . . .
H26A H 0.7454 1.0842 0.1862 0.052 Uiso 1 1 calc R . .
H26B H 0.6847 0.9790 0.1570 0.052 Uiso 1 1 calc R . .
H26C H 0.6616 1.1222 0.1470 0.052 Uiso 1 1 calc R . .
C27 C 0.78715(15) 1.1890(2) 0.08222(13) 0.0418(6) Uani 1 1 d . . .
H27A H 0.7485 1.2560 0.0866 0.063 Uiso 1 1 calc R . .
H27B H 0.8087 1.1960 0.0401 0.063 Uiso 1 1 calc R . .
H27C H 0.8310 1.1955 0.1172 0.063 Uiso 1 1 calc R . .
C28 C 0.67484(14) 1.0564(2) 0.03157(12) 0.0425(6) Uani 1 1 d . . .
H28A H 0.6467 0.9773 0.0344 0.064 Uiso 1 1 calc R . .
H28B H 0.6959 1.0625 -0.0108 0.064 Uiso 1 1 calc R . .
H28C H 0.6375 1.1249 0.0364 0.064 Uiso 1 1 calc R . .
C29 C 0.90756(12) 0.8632(2) -0.07601(10) 0.0311(5) Uani 1 1 d D . .
C30A C 0.8966(6) 0.9796(7) -0.1113(4) 0.071(2) Uani 0.487(4) 1 d PD A 1
H30A H 0.9206 0.9732 -0.1525 0.106 Uiso 0.487(4) 1 calc PR A 1
H30B H 0.9226 1.0467 -0.0851 0.106 Uiso 0.487(4) 1 calc PR A 1
H30C H 0.8392 0.9972 -0.1203 0.106 Uiso 0.487(4) 1 calc PR A 1
C31A C 0.8692(4) 0.7519(7) -0.1189(3) 0.0589(19) Uani 0.487(4) 1 d PD A 1
H31A H 0.8800 0.6736 -0.0956 0.088 Uiso 0.487(4) 1 calc PR A 1
H31B H 0.8928 0.7492 -0.1603 0.088 Uiso 0.487(4) 1 calc PR A 1
H31C H 0.8112 0.7643 -0.1272 0.088 Uiso 0.487(4) 1 calc PR A 1
C32A C 0.9983(4) 0.8287(8) -0.0658(4) 0.0491(19) Uani 0.487(4) 1 d PD A 1
H32A H 1.0055 0.7543 -0.0387 0.074 Uiso 0.487(4) 1 calc PR A 1
H32B H 1.0286 0.8976 -0.0442 0.074 Uiso 0.487(4) 1 calc PR A 1
H32C H 1.0179 0.8127 -0.1081 0.074 Uiso 0.487(4) 1 calc PR A 1
C30B C 0.9364(8) 1.0034(8) -0.0886(6) 0.031(2) Uani 0.39(2) 1 d PD A 2
H37D H 0.9605 1.0069 -0.1298 0.047 Uiso 0.39(2) 1 calc PR A 2
H37E H 0.9761 1.0290 -0.0530 0.047 Uiso 0.39(2) 1 calc PR A 2
H37F H 0.8902 1.0593 -0.0907 0.047 Uiso 0.39(2) 1 calc PR A 2
C31B C 0.8363(9) 0.8438(15) -0.1282(9) 0.048(3) Uani 0.39(2) 1 d PD A 2
H31D H 0.8026 0.9182 -0.1312 0.072 Uiso 0.39(2) 1 calc PR A 2
H31E H 0.8046 0.7726 -0.1164 0.072 Uiso 0.39(2) 1 calc PR A 2
H31F H 0.8564 0.8282 -0.1704 0.072 Uiso 0.39(2) 1 calc PR A 2
C32B C 0.9750(8) 0.7814(13) -0.0825(11) 0.052(4) Uani 0.39(2) 1 d PD A 2
H32D H 0.9561 0.6954 -0.0862 0.078 Uiso 0.39(2) 1 calc PR A 2
H32E H 1.0141 0.7895 -0.0441 0.078 Uiso 0.39(2) 1 calc PR A 2
H32F H 1.0003 0.8039 -0.1215 0.078 Uiso 0.39(2) 1 calc PR A 2
C30C C 0.955(2) 0.985(2) -0.0776(18) 0.031(2) Uani 0.12(2) 1 d PD A 3
H30G H 0.9564 1.0122 -0.1228 0.047 Uiso 0.12(2) 1 calc PR A 3
H30H H 1.0104 0.9716 -0.0579 0.047 Uiso 0.12(2) 1 calc PR A 3
H30I H 0.9299 1.0492 -0.0531 0.047 Uiso 0.12(2) 1 calc PR A 3
C31C C 0.836(3) 0.871(5) -0.128(3) 0.048(3) Uani 0.12(2) 1 d PD A 3
H31G H 0.8001 0.9379 -0.1175 0.072 Uiso 0.12(2) 1 calc PR A 3
H31H H 0.8063 0.7919 -0.1297 0.072 Uiso 0.12(2) 1 calc PR A 3
H31I H 0.8547 0.8866 -0.1706 0.072 Uiso 0.12(2) 1 calc PR A 3
C32C C 0.961(3) 0.755(3) -0.089(4) 0.052(4) Uani 0.12(2) 1 d PD A 3
H32G H 1.0069 0.7529 -0.0556 0.078 Uiso 0.12(2) 1 calc PR A 3
H32H H 0.9798 0.7644 -0.1319 0.078 Uiso 0.12(2) 1 calc PR A 3
H32I H 0.9305 0.6777 -0.0874 0.078 Uiso 0.12(2) 1 calc PR A 3
C33 C 0.86364(12) 0.61428(18) 0.12196(10) 0.0267(4) Uani 1 1 d . . .
C34 C 0.82392(14) 0.5961(2) 0.18480(12) 0.0362(5) Uani 1 1 d . . .
H34A H 0.8181 0.5072 0.1931 0.054 Uiso 1 1 calc R . .
H34B H 0.7710 0.6354 0.1803 0.054 Uiso 1 1 calc R . .
H34C H 0.8573 0.6340 0.2212 0.054 Uiso 1 1 calc R . .
C35 C 0.95045(15) 0.5695(2) 0.13339(13) 0.0436(6) Uani 1 1 d . . .
H35A H 0.9806 0.6232 0.1654 0.065 Uiso 1 1 calc R . .
H35B H 0.9749 0.5723 0.0924 0.065 Uiso 1 1 calc R . .
H35C H 0.9515 0.4841 0.1497 0.065 Uiso 1 1 calc R . .
C36 C 0.8167(2) 0.5269(2) 0.07242(14) 0.0576(8) Uani 1 1 d . . .
H36A H 0.8200 0.4417 0.0890 0.086 Uiso 1 1 calc R . .
H36B H 0.8399 0.5308 0.0309 0.086 Uiso 1 1 calc R . .
H36C H 0.7604 0.5528 0.0660 0.086 Uiso 1 1 calc R . .


#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 1.8748(19) . ?
P1 P4 2.2171(7) . ?
P1 P3 2.2310(7) . ?
P2 C19 1.8754(19) . ?
P2 P4 2.2236(7) . ?
P2 P3 2.2294(7) . ?
P3 P4 2.1634(8) . ?
C1 C6 1.418(3) . ?
C1 C2 1.424(3) . ?
C2 C3 1.398(3) . ?
C2 C7 1.552(3) . ?
C3 C4 1.384(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(3) . ?
C4 C11 1.537(3) . ?
C5 C6 1.394(3) . ?
C5 H5 0.9500 . ?
C6 C15 1.556(3) . ?
C7 C9 1.529(3) . ?
C7 C8 1.533(3) . ?
C7 C10 1.548(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C14 1.526(3) . ?
C11 C13 1.528(3) . ?
C11 C12 1.537(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C18 1.521(3) . ?
C15 C17 1.532(3) . ?
C15 C16 1.547(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C24 1.415(3) . ?
C19 C20 1.428(3) . ?
C20 C21 1.399(3) . ?
C20 C25 1.550(3) . ?
C21 C22 1.380(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.384(3) . ?
C22 C29 1.537(3) . ?
C23 C24 1.398(3) . ?
C23 H23 0.9500 . ?
C24 C33 1.556(3) . ?
C25 C26 1.527(3) . ?
C25 C27 1.533(3) . ?
C25 C28 1.554(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C32B 1.451(7) . ?
C29 C30A 1.454(6) . ?
C29 C32C 1.509(14) . ?
C29 C31C 1.534(14) . ?
C29 C31B 1.540(7) . ?
C29 C30C 1.544(14) . ?
C29 C32A 1.560(7) . ?
C29 C31A 1.588(5) . ?
C29 C30B 1.618(7) . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C32A H32A 0.9800 . ?
C32A H32B 0.9800 . ?
C32A H32C 0.9800 . ?
C30B H37D 0.9800 . ?
C30B H37E 0.9800 . ?
C30B H37F 0.9800 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
C32B H32D 0.9800 . ?
C32B H32E 0.9800 . ?
C32B H32F 0.9800 . ?
C30C H30G 0.9800 . ?
C30C H30H 0.9800 . ?
C30C H30I 0.9800 . ?
C31C H31G 0.9800 . ?
C31C H31H 0.9800 . ?
C31C H31I 0.9800 . ?
C32C H32G 0.9800 . ?
C32C H32H 0.9800 . ?
C32C H32I 0.9800 . ?
C33 C35 1.529(3) . ?
C33 C34 1.533(3) . ?
C33 C36 1.546(3) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 P4 98.73(6) . . ?
C1 P1 P3 97.64(6) . . ?
P4 P1 P3 58.20(2) . . ?
C19 P2 P4 98.05(6) . . ?
C19 P2 P3 99.53(6) . . ?
P4 P2 P3 58.13(2) . . ?
P4 P3 P2 60.80(2) . . ?
P4 P3 P1 60.58(2) . . ?
P2 P3 P1 80.52(3) . . ?
P3 P4 P1 61.22(2) . . ?
P3 P4 P2 61.07(2) . . ?
P1 P4 P2 80.96(3) . . ?
C6 C1 C2 118.70(17) . . ?
C6 C1 P1 119.76(14) . . ?
C2 C1 P1 120.62(14) . . ?
C3 C2 C1 118.11(17) . . ?
C3 C2 C7 115.16(17) . . ?
C1 C2 C7 126.34(17) . . ?
C4 C3 C2 123.05(18) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C3 C4 C5 116.68(17) . . ?
C3 C4 C11 122.67(18) . . ?
C5 C4 C11 120.34(18) . . ?
C4 C5 C6 123.42(18) . . ?
C4 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
C5 C6 C1 118.00(17) . . ?
C5 C6 C15 115.53(17) . . ?
C1 C6 C15 126.24(17) . . ?
C9 C7 C8 109.44(18) . . ?
C9 C7 C10 108.33(19) . . ?
C8 C7 C10 105.10(19) . . ?
C9 C7 C2 111.94(17) . . ?
C8 C7 C2 115.04(17) . . ?
C10 C7 C2 106.52(17) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C11 C13 110.0(2) . . ?
C14 C11 C12 107.61(19) . . ?
C13 C11 C12 108.5(2) . . ?
C14 C11 C4 110.29(17) . . ?
C13 C11 C4 108.56(18) . . ?
C12 C11 C4 111.91(18) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18 C15 C17 108.9(2) . . ?
C18 C15 C16 105.87(19) . . ?
C17 C15 C16 107.77(19) . . ?
C18 C15 C6 115.40(18) . . ?
C17 C15 C6 111.34(17) . . ?
C16 C15 C6 107.12(17) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C24 C19 C20 118.78(16) . . ?
C24 C19 P2 120.31(13) . . ?
C20 C19 P2 120.15(14) . . ?
C21 C20 C19 117.58(17) . . ?
C21 C20 C25 114.89(16) . . ?
C19 C20 C25 127.36(17) . . ?
C22 C21 C20 123.81(17) . . ?
C22 C21 H21 118.1 . . ?
C20 C21 H21 118.1 . . ?
C21 C22 C23 116.40(17) . . ?
C21 C22 C29 122.26(17) . . ?
C23 C22 C29 121.24(18) . . ?
C22 C23 C24 123.46(17) . . ?
C22 C23 H23 118.3 . . ?
C24 C23 H23 118.3 . . ?
C23 C24 C19 118.12(16) . . ?
C23 C24 C33 114.39(16) . . ?
C19 C24 C33 127.33(16) . . ?
C26 C25 C27 107.56(18) . . ?
C26 C25 C20 117.36(16) . . ?
C27 C25 C20 111.24(17) . . ?
C26 C25 C28 105.22(18) . . ?
C27 C25 C28 108.62(18) . . ?
C20 C25 C28 106.41(16) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C32B C29 C30A 122.5(8) . . ?
C32B C29 C32C 15(2) . . ?
C30A C29 C32C 129(3) . . ?
C32B C29 C31C 122(4) . . ?
C30A C29 C31C 63.4(17) . . ?
C32C C29 C31C 110.7(13) . . ?
C32B C29 C22 114.7(8) . . ?
C30A C29 C22 116.2(3) . . ?
C32C C29 C22 114(3) . . ?
C31C C29 C22 108(3) . . ?
C32B C29 C31B 114.1(6) . . ?
C30A C29 C31B 73.5(7) . . ?
C32C C29 C31B 102(3) . . ?
C31C C29 C31B 11(2) . . ?
C22 C29 C31B 107.4(9) . . ?
C32B C29 C30C 96.0(16) . . ?
C30A C29 C30C 45.0(13) . . ?
C32C C29 C30C 109.6(12) . . ?
C31C C29 C30C 108.3(14) . . ?
C22 C29 C30C 106.6(15) . . ?
C31B C29 C30C 117.9(14) . . ?
C32B C29 C32A 27.0(7) . . ?
C30A C29 C32A 110.1(5) . . ?
C32C C29 C32A 42(2) . . ?
C31C C29 C32A 142(3) . . ?
C22 C29 C32A 107.9(4) . . ?
C31B C29 C32A 137.6(9) . . ?
C30C C29 C32A 72.7(16) . . ?
C32B C29 C31A 76.3(8) . . ?
C30A C29 C31A 110.4(5) . . ?
C32C C29 C31A 62(2) . . ?
C31C C29 C31A 53(2) . . ?
C22 C29 C31A 108.1(2) . . ?
C31B C29 C31A 42.8(7) . . ?
C30C C29 C31A 144.5(15) . . ?
C32A C29 C31A 103.2(4) . . ?
C32B C29 C30B 107.7(5) . . ?
C30A C29 C30B 30.3(6) . . ?
C32C C29 C30B 120(2) . . ?
C31C C29 C30B 93.7(16) . . ?
C22 C29 C30B 108.6(4) . . ?
C31B C29 C30B 103.7(5) . . ?
C30C C29 C30B 15.1(11) . . ?
C32A C29 C30B 86.6(6) . . ?
C31A C29 C30B 136.7(5) . . ?
C29 C30A H30A 109.5 . . ?
C29 C30A H30B 109.5 . . ?
H30A C30A H30B 109.5 . . ?
C29 C30A H30C 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C29 C31A H31A 109.5 . . ?
C29 C31A H31B 109.5 . . ?
H31A C31A H31B 109.5 . . ?
C29 C31A H31C 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C29 C32A H32A 109.5 . . ?
C29 C32A H32B 109.5 . . ?
H32A C32A H32B 109.5 . . ?
C29 C32A H32C 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 109.5 . . ?
C29 C30B H37D 109.5 . . ?
C29 C30B H37E 109.5 . . ?
H37D C30B H37E 109.5 . . ?
C29 C30B H37F 109.5 . . ?
H37D C30B H37F 109.5 . . ?
H37E C30B H37F 109.5 . . ?
C29 C31B H31D 109.5 . . ?
C29 C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C29 C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C29 C32B H32D 109.5 . . ?
C29 C32B H32E 109.5 . . ?
H32D C32B H32E 109.5 . . ?
C29 C32B H32F 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
C29 C30C H30G 109.5 . . ?
C29 C30C H30H 109.5 . . ?
H30G C30C H30H 109.5 . . ?
C29 C30C H30I 109.5 . . ?
H30G C30C H30I 109.5 . . ?
H30H C30C H30I 109.5 . . ?
C29 C31C H31G 109.5 . . ?
C29 C31C H31H 109.5 . . ?
H31G C31C H31H 109.5 . . ?
C29 C31C H31I 109.5 . . ?
H31G C31C H31I 109.5 . . ?
H31H C31C H31I 109.5 . . ?
C29 C32C H32G 109.5 . . ?
C29 C32C H32H 109.5 . . ?
H32G C32C H32H 109.5 . . ?
C29 C32C H32I 109.5 . . ?
H32G C32C H32I 109.5 . . ?
H32H C32C H32I 109.5 . . ?
C35 C33 C34 108.60(18) . . ?
C35 C33 C36 108.7(2) . . ?
C34 C33 C36 104.30(19) . . ?
C35 C33 C24 111.53(17) . . ?
C34 C33 C24 116.59(17) . . ?
C36 C33 C24 106.58(17) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C19 P2 P3 P4 93.61(6) . . . . ?
C19 P2 P3 P1 155.10(6) . . . . ?
P4 P2 P3 P1 61.49(2) . . . . ?
C1 P1 P3 P4 -95.57(6) . . . . ?
C1 P1 P3 P2 -157.29(6) . . . . ?
P4 P1 P3 P2 -61.72(2) . . . . ?
P2 P3 P4 P1 95.66(3) . . . . ?
P1 P3 P4 P2 -95.66(3) . . . . ?
C1 P1 P4 P3 93.62(7) . . . . ?
C1 P1 P4 P2 155.49(7) . . . . ?
P3 P1 P4 P2 61.87(2) . . . . ?
C19 P2 P4 P3 -96.26(6) . . . . ?
C19 P2 P4 P1 -158.29(6) . . . . ?
P3 P2 P4 P1 -62.03(2) . . . . ?
P4 P1 C1 C6 -118.29(14) . . . . ?
P3 P1 C1 C6 -59.44(15) . . . . ?
P4 P1 C1 C2 50.56(16) . . . . ?
P3 P1 C1 C2 109.41(15) . . . . ?
C6 C1 C2 C3 15.1(3) . . . . ?
P1 C1 C2 C3 -153.83(15) . . . . ?
C6 C1 C2 C7 -157.26(18) . . . . ?
P1 C1 C2 C7 33.8(3) . . . . ?
C1 C2 C3 C4 -4.7(3) . . . . ?
C7 C2 C3 C4 168.55(18) . . . . ?
C2 C3 C4 C5 -6.1(3) . . . . ?
C2 C3 C4 C11 -179.61(18) . . . . ?
C3 C4 C5 C6 6.6(3) . . . . ?
C11 C4 C5 C6 -179.70(19) . . . . ?
C4 C5 C6 C1 3.7(3) . . . . ?
C4 C5 C6 C15 -171.03(19) . . . . ?
C2 C1 C6 C5 -14.7(3) . . . . ?
P1 C1 C6 C5 154.41(15) . . . . ?
C2 C1 C6 C15 159.49(19) . . . . ?
P1 C1 C6 C15 -31.4(3) . . . . ?
C3 C2 C7 C9 64.9(2) . . . . ?
C1 C2 C7 C9 -122.5(2) . . . . ?
C3 C2 C7 C8 -169.35(19) . . . . ?
C1 C2 C7 C8 3.2(3) . . . . ?
C3 C2 C7 C10 -53.3(2) . . . . ?
C1 C2 C7 C10 119.2(2) . . . . ?
C3 C4 C11 C14 -132.5(2) . . . . ?
C5 C4 C11 C14 54.2(3) . . . . ?
C3 C4 C11 C13 106.9(2) . . . . ?
C5 C4 C11 C13 -66.4(3) . . . . ?
C3 C4 C11 C12 -12.7(3) . . . . ?
C5 C4 C11 C12 173.9(2) . . . . ?
C5 C6 C15 C18 165.7(2) . . . . ?
C1 C6 C15 C18 -8.6(3) . . . . ?
C5 C6 C15 C17 -69.5(2) . . . . ?
C1 C6 C15 C17 116.2(2) . . . . ?
C5 C6 C15 C16 48.1(2) . . . . ?
C1 C6 C15 C16 -126.2(2) . . . . ?
P4 P2 C19 C24 113.17(14) . . . . ?
P3 P2 C19 C24 54.29(14) . . . . ?
P4 P2 C19 C20 -56.73(14) . . . . ?
P3 P2 C19 C20 -115.60(14) . . . . ?
C24 C19 C20 C21 -13.4(3) . . . . ?
P2 C19 C20 C21 156.69(14) . . . . ?
C24 C19 C20 C25 161.76(17) . . . . ?
P2 C19 C20 C25 -28.2(2) . . . . ?
C19 C20 C21 C22 2.5(3) . . . . ?
C25 C20 C21 C22 -173.23(17) . . . . ?
C20 C21 C22 C23 7.1(3) . . . . ?
C20 C21 C22 C29 -176.61(18) . . . . ?
C21 C22 C23 C24 -6.0(3) . . . . ?
C29 C22 C23 C24 177.68(17) . . . . ?
C22 C23 C24 C19 -4.7(3) . . . . ?
C22 C23 C24 C33 170.91(17) . . . . ?
C20 C19 C24 C23 14.4(2) . . . . ?
P2 C19 C24 C23 -155.61(14) . . . . ?
C20 C19 C24 C33 -160.56(18) . . . . ?
P2 C19 C24 C33 29.4(2) . . . . ?
C21 C20 C25 C26 173.21(18) . . . . ?
C19 C20 C25 C26 -2.0(3) . . . . ?
C21 C20 C25 C27 -62.4(2) . . . . ?
C19 C20 C25 C27 122.4(2) . . . . ?
C21 C20 C25 C28 55.8(2) . . . . ?
C19 C20 C25 C28 -119.5(2) . . . . ?
C21 C22 C29 C32B 158.8(8) . . . . ?
C23 C22 C29 C32B -25.1(8) . . . . ?
C21 C22 C29 C30A 6.5(6) . . . . ?
C23 C22 C29 C30A -177.4(5) . . . . ?
C21 C22 C29 C32C 175(2) . . . . ?
C23 C22 C29 C32C -9(2) . . . . ?
C21 C22 C29 C31C -62(2) . . . . ?
C23 C22 C29 C31C 114(2) . . . . ?
C21 C22 C29 C31B -73.3(7) . . . . ?
C23 C22 C29 C31B 102.8(7) . . . . ?
C21 C22 C29 C30C 53.9(15) . . . . ?
C23 C22 C29 C30C -129.9(15) . . . . ?
C21 C22 C29 C32A 130.7(4) . . . . ?
C23 C22 C29 C32A -53.2(4) . . . . ?
C21 C22 C29 C31A -118.3(4) . . . . ?
C23 C22 C29 C31A 57.9(4) . . . . ?
C21 C22 C29 C30B 38.3(6) . . . . ?
C23 C22 C29 C30B -145.6(6) . . . . ?
C23 C24 C33 C35 63.5(2) . . . . ?
C19 C24 C33 C35 -121.3(2) . . . . ?
C23 C24 C33 C34 -170.94(18) . . . . ?
C19 C24 C33 C34 4.2(3) . . . . ?
C23 C24 C33 C36 -55.0(2) . . . . ?
C19 C24 C33 C36 120.1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.066
####################################################################### 
# 
# 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_ch_jr3_endo_exo_MesP4Mes
_database_code_depnum_ccdc_archive 'CCDC 1413821'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H58 P4'
_chemical_formula_sum            'C36 H58 P4'
_chemical_formula_weight         614.70

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   15.0599(7)
_cell_length_b                   18.3797(8)
_cell_length_c                   14.3330(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.316(3)
_cell_angle_gamma                90.00
_cell_volume                     3744.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5570
_cell_measurement_theta_min      5.279
_cell_measurement_theta_max      45.025

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9160
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52969
_diffrn_reflns_av_R_equivalents  0.0836
_diffrn_reflns_av_sigmaI/netI    0.0829
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         30.07
_reflns_number_total             10962
_reflns_number_gt                6386
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker Apex V7.51A'
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms were positioned geometrically and refined using a riding model, 
 with C---H = 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å 
 (methine groups) or 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times 
 Ueq(C) (methyl groups) or with Uiso(H) = 1.2 times 
 Ueq(C) (methylene  groups, aryl CH, methine groups). Torsion angles 
 of all methyl groups were allowed to refine.
 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0478P)²+1.0035P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10962
_refine_ls_number_parameters     423
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1342
_refine_ls_wR_factor_gt          0.1099
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.09795(4) 0.40325(3) 0.75178(4) 0.02476(12) Uani 1 1 d . . .
P2 P 0.08736(4) 0.39227(3) 0.90229(4) 0.03233(14) Uani 1 1 d . . .
P3 P 0.10766(4) 0.29497(3) 0.82508(4) 0.03222(14) Uani 1 1 d . . .
P4 P 0.22522(4) 0.33631(3) 0.95182(4) 0.03390(15) Uani 1 1 d . . .
C1 C -0.03187(13) 0.39835(10) 0.68211(14) 0.0233(4) Uani 1 1 d . . .
C2 C -0.06807(14) 0.33849(10) 0.61873(14) 0.0255(4) Uani 1 1 d . . .
C3 C -0.15839(14) 0.31421(11) 0.60922(15) 0.0296(5) Uani 1 1 d . . .
H3 H -0.1818 0.2724 0.5698 0.035 Uiso 1 1 calc R . .
C4 C -0.21568(14) 0.34791(11) 0.65433(15) 0.0276(4) Uani 1 1 d . A .
C5 C -0.18493(14) 0.41490(11) 0.69780(15) 0.0291(5) Uani 1 1 d . . .
H5 H -0.2267 0.4430 0.7205 0.035 Uiso 1 1 calc R . .
C6 C -0.09612(14) 0.44288(10) 0.70975(14) 0.0251(4) Uani 1 1 d . . .
C7 C -0.01894(15) 0.30082(12) 0.55210(15) 0.0317(5) Uani 1 1 d . . .
C8 C 0.07201(16) 0.33761(13) 0.55056(17) 0.0408(6) Uani 1 1 d . . .
H8A H 0.0903 0.3176 0.4961 0.061 Uiso 1 1 calc R . .
H8B H 0.1222 0.3286 0.6134 0.061 Uiso 1 1 calc R . .
H8C H 0.0616 0.3901 0.5411 0.061 Uiso 1 1 calc R . .
C9 C 0.00093(19) 0.22077(12) 0.58048(18) 0.0456(6) Uani 1 1 d . . .
H9A H -0.0582 0.1960 0.5751 0.068 Uiso 1 1 calc R . .
H9B H 0.0440 0.2174 0.6486 0.068 Uiso 1 1 calc R . .
H9C H 0.0297 0.1976 0.5358 0.068 Uiso 1 1 calc R . .
C10 C -0.08674(18) 0.30492(15) 0.44493(17) 0.0486(6) Uani 1 1 d . . .
H10A H -0.0570 0.2828 0.4005 0.073 Uiso 1 1 calc R . .
H10B H -0.1016 0.3559 0.4264 0.073 Uiso 1 1 calc R . .
H10C H -0.1448 0.2786 0.4397 0.073 Uiso 1 1 calc R . .
C11 C -0.30934(14) 0.31561(12) 0.65483(17) 0.0332(5) Uani 1 1 d . . .
C12A C -0.3303(3) 0.2425(2) 0.6030(4) 0.0831(15) Uani 0.873(3) 1 d PD A 1
H12A H -0.2797 0.2082 0.6357 0.125 Uiso 0.873(3) 1 calc PR A 1
H12B H -0.3344 0.2482 0.5337 0.125 Uiso 0.873(3) 1 calc PR A 1
H12C H -0.3902 0.2238 0.6061 0.125 Uiso 0.873(3) 1 calc PR A 1
C13A C -0.3904(2) 0.3661(2) 0.6027(3) 0.0730(12) Uani 0.873(3) 1 d PD A 1
H13A H -0.4493 0.3455 0.6061 0.109 Uiso 0.873(3) 1 calc PR A 1
H13B H -0.3947 0.3715 0.5333 0.109 Uiso 0.873(3) 1 calc PR A 1
H13C H -0.3796 0.4138 0.6350 0.109 Uiso 0.873(3) 1 calc PR A 1
C14A C -0.3055(2) 0.3062(2) 0.7612(2) 0.0710(12) Uani 0.873(3) 1 d PD A 1
H14A H -0.2546 0.2726 0.7951 0.106 Uiso 0.873(3) 1 calc PR A 1
H14B H -0.3656 0.2866 0.7625 0.106 Uiso 0.873(3) 1 calc PR A 1
H14C H -0.2939 0.3535 0.7947 0.106 Uiso 0.873(3) 1 calc PR A 1
C12B C -0.3636(16) 0.2942(14) 0.5455(15) 0.0831(15) Uani 0.127(3) 1 d PD A 2
H12D H -0.4267 0.2771 0.5400 0.125 Uiso 0.127(3) 1 calc PR A 2
H12E H -0.3294 0.2554 0.5249 0.125 Uiso 0.127(3) 1 calc PR A 2
H12F H -0.3686 0.3368 0.5028 0.125 Uiso 0.127(3) 1 calc PR A 2
C13B C -0.3675(15) 0.3685(11) 0.6857(19) 0.0730(12) Uani 0.127(3) 1 d PD A 2
H13D H -0.4279 0.3461 0.6810 0.109 Uiso 0.127(3) 1 calc PR A 2
H13E H -0.3785 0.4112 0.6426 0.109 Uiso 0.127(3) 1 calc PR A 2
H13F H -0.3348 0.3833 0.7542 0.109 Uiso 0.127(3) 1 calc PR A 2
C14B C -0.2870(14) 0.2482(12) 0.7144(16) 0.0710(12) Uani 0.127(3) 1 d PD A 2
H14D H -0.2471 0.2600 0.7820 0.106 Uiso 0.127(3) 1 calc PR A 2
H14E H -0.2536 0.2143 0.6848 0.106 Uiso 0.127(3) 1 calc PR A 2
H14F H -0.3455 0.2256 0.7159 0.106 Uiso 0.127(3) 1 calc PR A 2
C15 C -0.07867(15) 0.52295(11) 0.74413(16) 0.0312(5) Uani 1 1 d . . .
C16 C -0.08074(19) 0.53331(12) 0.84965(18) 0.0455(6) Uani 1 1 d . . .
H16A H -0.0253 0.5102 0.8967 0.068 Uiso 1 1 calc R . .
H16B H -0.1378 0.5109 0.8553 0.068 Uiso 1 1 calc R . .
H16C H -0.0805 0.5854 0.8644 0.068 Uiso 1 1 calc R . .
C17 C -0.15932(18) 0.56832(13) 0.6730(2) 0.0494(7) Uani 1 1 d . . .
H17A H -0.1490 0.6200 0.6901 0.074 Uiso 1 1 calc R . .
H17B H -0.2195 0.5529 0.6790 0.074 Uiso 1 1 calc R . .
H17C H -0.1605 0.5609 0.6049 0.074 Uiso 1 1 calc R . .
C18 C 0.01144(16) 0.55580(12) 0.73525(18) 0.0371(5) Uani 1 1 d . . .
H18A H 0.0661 0.5348 0.7860 0.056 Uiso 1 1 calc R . .
H18B H 0.0109 0.6086 0.7444 0.056 Uiso 1 1 calc R . .
H18C H 0.0151 0.5451 0.6696 0.056 Uiso 1 1 calc R . .
C19 C 0.30241(14) 0.38730(11) 0.89657(14) 0.0276(4) Uani 1 1 d . . .
C20 C 0.31504(14) 0.46324(11) 0.91027(15) 0.0288(4) Uani 1 1 d . . .
C21 C 0.33329(14) 0.50294(12) 0.83612(16) 0.0329(5) Uani 1 1 d . . .
H21 H 0.3378 0.5544 0.8424 0.039 Uiso 1 1 calc R . .
C22 C 0.34516(14) 0.47115(12) 0.75345(16) 0.0326(5) Uani 1 1 d . B .
C23 C 0.35276(14) 0.39616(12) 0.75442(16) 0.0335(5) Uani 1 1 d . . .
H23 H 0.3706 0.3734 0.7038 0.040 Uiso 1 1 calc R . .
C24 C 0.33548(14) 0.35231(11) 0.82614(15) 0.0289(4) Uani 1 1 d . . .
C25 C 0.31375(15) 0.50655(12) 1.00311(16) 0.0355(5) Uani 1 1 d . . .
C26 C 0.32037(18) 0.45895(14) 1.09285(17) 0.0474(6) Uani 1 1 d . . .
H26A H 0.3336 0.4897 1.1518 0.071 Uiso 1 1 calc R . .
H26B H 0.3711 0.4234 1.1027 0.071 Uiso 1 1 calc R . .
H26C H 0.2606 0.4334 1.0815 0.071 Uiso 1 1 calc R . .
C27 C 0.22642(16) 0.55530(13) 0.97989(18) 0.0426(6) Uani 1 1 d . . .
H27A H 0.1698 0.5249 0.9620 0.064 Uiso 1 1 calc R . .
H27B H 0.2236 0.5876 0.9246 0.064 Uiso 1 1 calc R . .
H27C H 0.2300 0.5845 1.0382 0.064 Uiso 1 1 calc R . .
C28 C 0.40167(17) 0.55586(14) 1.0366(2) 0.0498(7) Uani 1 1 d . . .
H28A H 0.4022 0.5834 1.0953 0.075 Uiso 1 1 calc R . .
H28B H 0.4001 0.5897 0.9832 0.075 Uiso 1 1 calc R . .
H28C H 0.4584 0.5257 1.0525 0.075 Uiso 1 1 calc R . .
C29 C 0.35223(17) 0.51636(13) 0.66679(17) 0.0418(6) Uani 1 1 d . . .
C30A C 0.4346(6) 0.5624(4) 0.6962(5) 0.084(3) Uani 0.491(5) 1 d PD B 1
H30A H 0.4358 0.5919 0.6397 0.127 Uiso 0.491(5) 1 calc PR B 1
H30B H 0.4912 0.5320 0.7186 0.127 Uiso 0.491(5) 1 calc PR B 1
H30C H 0.4325 0.5944 0.7501 0.127 Uiso 0.491(5) 1 calc PR B 1
C31A C 0.3642(5) 0.4623(3) 0.5805(4) 0.0573(19) Uani 0.491(5) 1 d PD B 1
H31A H 0.3656 0.4913 0.5237 0.086 Uiso 0.491(5) 1 calc PR B 1
H31B H 0.3111 0.4283 0.5596 0.086 Uiso 0.491(5) 1 calc PR B 1
H31C H 0.4231 0.4349 0.6067 0.086 Uiso 0.491(5) 1 calc PR B 1
C32A C 0.2599(5) 0.5518(4) 0.6178(5) 0.071(2) Uani 0.491(5) 1 d PD B 1
H32A H 0.2435 0.5824 0.6657 0.107 Uiso 0.491(5) 1 calc PR B 1
H32B H 0.2115 0.5144 0.5923 0.107 Uiso 0.491(5) 1 calc PR B 1
H32C H 0.2638 0.5820 0.5629 0.107 Uiso 0.491(5) 1 calc PR B 1
C30B C 0.3489(5) 0.6036(3) 0.6897(4) 0.0511(16) Uani 0.509(5) 1 d PD B 2
H30D H 0.4036 0.6167 0.7469 0.077 Uiso 0.509(5) 1 calc PR B 2
H30E H 0.2911 0.6147 0.7039 0.077 Uiso 0.509(5) 1 calc PR B 2
H30F H 0.3501 0.6316 0.6319 0.077 Uiso 0.509(5) 1 calc PR B 2
C31B C 0.4459(4) 0.5060(4) 0.6530(5) 0.069(2) Uani 0.509(5) 1 d PD B 2
H31D H 0.4518 0.5400 0.6027 0.103 Uiso 0.509(5) 1 calc PR B 2
H31E H 0.4509 0.4560 0.6316 0.103 Uiso 0.509(5) 1 calc PR B 2
H31F H 0.4962 0.5152 0.7157 0.103 Uiso 0.509(5) 1 calc PR B 2
C32B C 0.2705(4) 0.5031(3) 0.5792(4) 0.0592(19) Uani 0.509(5) 1 d PD B 2
H32D H 0.2727 0.5357 0.5259 0.089 Uiso 0.509(5) 1 calc PR B 2
H32E H 0.2129 0.5123 0.5949 0.089 Uiso 0.509(5) 1 calc PR B 2
H32F H 0.2711 0.4525 0.5581 0.089 Uiso 0.509(5) 1 calc PR B 2
C33 C 0.35925(15) 0.27030(12) 0.82332(17) 0.0363(5) Uani 1 1 d . . .
C34 C 0.29267(18) 0.23246(14) 0.7322(2) 0.0505(7) Uani 1 1 d . . .
H34A H 0.2285 0.2338 0.7348 0.076 Uiso 1 1 calc R . .
H34B H 0.3123 0.1818 0.7308 0.076 Uiso 1 1 calc R . .
H34C H 0.2944 0.2575 0.6725 0.076 Uiso 1 1 calc R . .
C35 C 0.3619(2) 0.22713(13) 0.9157(2) 0.0527(7) Uani 1 1 d . . .
H35A H 0.3978 0.2543 0.9750 0.079 Uiso 1 1 calc R . .
H35B H 0.3919 0.1799 0.9153 0.079 Uiso 1 1 calc R . .
H35C H 0.2975 0.2196 0.9160 0.079 Uiso 1 1 calc R . .
C36 C 0.45994(18) 0.26572(15) 0.8180(2) 0.0580(7) Uani 1 1 d . . .
H36A H 0.4615 0.2888 0.7570 0.087 Uiso 1 1 calc R . .
H36B H 0.4785 0.2146 0.8187 0.087 Uiso 1 1 calc R . .
H36C H 0.5037 0.2909 0.8751 0.087 Uiso 1 1 calc R . .


#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 1.880(2) . ?
P1 P2 2.2244(7) . ?
P1 P3 2.2326(8) . ?
P2 P3 2.1773(8) . ?
P2 P4 2.2131(8) . ?
P3 P4 2.2101(8) . ?
P4 C19 1.862(2) . ?
C1 C2 1.416(3) . ?
C1 C6 1.420(3) . ?
C2 C3 1.395(3) . ?
C2 C7 1.551(3) . ?
C3 C4 1.384(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(3) . ?
C4 C11 1.533(3) . ?
C5 C6 1.390(3) . ?
C5 H5 0.9500 . ?
C6 C15 1.547(3) . ?
C7 C9 1.529(3) . ?
C7 C8 1.534(3) . ?
C7 C10 1.540(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13B 1.471(19) . ?
C11 C14B 1.479(18) . ?
C11 C14A 1.517(4) . ?
C11 C12A 1.518(4) . ?
C11 C13A 1.519(4) . ?
C11 C12B 1.56(2) . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C14A H14A 0.9800 . ?
C14A H14B 0.9800 . ?
C14A H14C 0.9800 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C15 C18 1.528(3) . ?
C15 C16 1.535(3) . ?
C15 C17 1.546(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.414(3) . ?
C19 C24 1.419(3) . ?
C20 C21 1.389(3) . ?
C20 C25 1.556(3) . ?
C21 C22 1.385(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.383(3) . ?
C22 C29 1.527(3) . ?
C23 C24 1.397(3) . ?
C23 H23 0.9500 . ?
C24 C33 1.553(3) . ?
C25 C26 1.531(3) . ?
C25 C27 1.534(3) . ?
C25 C28 1.544(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30A 1.444(6) . ?
C29 C32B 1.458(6) . ?
C29 C32A 1.485(6) . ?
C29 C31B 1.500(6) . ?
C29 C30B 1.641(5) . ?
C29 C31A 1.643(6) . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C32A H32A 0.9800 . ?
C32A H32B 0.9800 . ?
C32A H32C 0.9800 . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 0.9800 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
C32B H32D 0.9800 . ?
C32B H32E 0.9800 . ?
C32B H32F 0.9800 . ?
C33 C34 1.526(3) . ?
C33 C35 1.533(3) . ?
C33 C36 1.545(3) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 P2 96.61(6) . . ?
C1 P1 P3 95.85(6) . . ?
P2 P1 P3 58.49(2) . . ?
P3 P2 P4 60.44(3) . . ?
P3 P2 P1 60.94(2) . . ?
P4 P2 P1 89.58(3) . . ?
P2 P3 P4 60.58(3) . . ?
P2 P3 P1 60.57(2) . . ?
P4 P3 P1 89.44(3) . . ?
C19 P4 P3 105.46(7) . . ?
C19 P4 P2 106.33(7) . . ?
P3 P4 P2 58.98(3) . . ?
C2 C1 C6 118.27(17) . . ?
C2 C1 P1 119.32(14) . . ?
C6 C1 P1 120.59(14) . . ?
C3 C2 C1 117.86(17) . . ?
C3 C2 C7 116.45(18) . . ?
C1 C2 C7 125.52(17) . . ?
C4 C3 C2 123.35(19) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
C3 C4 C5 116.08(18) . . ?
C3 C4 C11 123.08(18) . . ?
C5 C4 C11 120.82(18) . . ?
C4 C5 C6 123.23(18) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C5 C6 C1 117.98(18) . . ?
C5 C6 C15 116.52(17) . . ?
C1 C6 C15 125.29(17) . . ?
C9 C7 C8 109.32(19) . . ?
C9 C7 C10 108.62(19) . . ?
C8 C7 C10 105.35(18) . . ?
C9 C7 C2 110.90(17) . . ?
C8 C7 C2 114.96(17) . . ?
C10 C7 C2 107.36(17) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13B C11 C14B 115.1(12) . . ?
C13B C11 C14A 66.5(10) . . ?
C14B C11 C14A 53.0(10) . . ?
C13B C11 C12A 133.2(9) . . ?
C14B C11 C12A 60.7(10) . . ?
C14A C11 C12A 108.9(3) . . ?
C13B C11 C13A 44.2(9) . . ?
C14B C11 C13A 142.0(8) . . ?
C14A C11 C13A 108.7(3) . . ?
C12A C11 C13A 107.3(3) . . ?
C13B C11 C4 112.7(9) . . ?
C14B C11 C4 107.1(8) . . ?
C14A C11 C4 108.67(19) . . ?
C12A C11 C4 112.5(2) . . ?
C13A C11 C4 110.6(2) . . ?
C13B C11 C12B 107.6(11) . . ?
C14B C11 C12B 108.2(12) . . ?
C14A C11 C12B 144.6(9) . . ?
C12A C11 C12B 47.9(9) . . ?
C13A C11 C12B 65.9(10) . . ?
C4 C11 C12B 105.6(8) . . ?
C11 C12A H12A 109.5 . . ?
C11 C12A H12B 109.5 . . ?
C11 C12A H12C 109.5 . . ?
C11 C13A H13A 109.5 . . ?
C11 C13A H13B 109.5 . . ?
C11 C13A H13C 109.5 . . ?
C11 C14A H14A 109.5 . . ?
C11 C14A H14B 109.5 . . ?
C11 C14A H14C 109.5 . . ?
C11 C12B H12D 109.5 . . ?
C11 C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11 C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C11 C13B H13D 109.5 . . ?
C11 C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C11 C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C11 C14B H14D 109.5 . . ?
C11 C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
C11 C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C18 C15 C16 109.94(18) . . ?
C18 C15 C17 104.93(18) . . ?
C16 C15 C17 108.37(19) . . ?
C18 C15 C6 114.28(17) . . ?
C16 C15 C6 112.04(17) . . ?
C17 C15 C6 106.83(17) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C24 118.92(18) . . ?
C20 C19 P4 120.82(15) . . ?
C24 C19 P4 119.34(15) . . ?
C21 C20 C19 117.63(19) . . ?
C21 C20 C25 116.56(19) . . ?
C19 C20 C25 125.78(18) . . ?
C22 C21 C20 123.2(2) . . ?
C22 C21 H21 118.4 . . ?
C20 C21 H21 118.4 . . ?
C23 C22 C21 116.47(19) . . ?
C23 C22 C29 121.5(2) . . ?
C21 C22 C29 122.0(2) . . ?
C22 C23 C24 123.2(2) . . ?
C22 C23 H23 118.4 . . ?
C24 C23 H23 118.4 . . ?
C23 C24 C19 117.17(19) . . ?
C23 C24 C33 116.13(18) . . ?
C19 C24 C33 126.63(18) . . ?
C26 C25 C27 109.20(19) . . ?
C26 C25 C28 105.27(19) . . ?
C27 C25 C28 108.07(19) . . ?
C26 C25 C20 114.22(19) . . ?
C27 C25 C20 111.44(18) . . ?
C28 C25 C20 108.29(18) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30A C29 C32B 138.4(4) . . ?
C30A C29 C32A 117.4(5) . . ?
C32B C29 C32A 43.5(3) . . ?
C30A C29 C31B 50.1(4) . . ?
C32B C29 C31B 115.4(4) . . ?
C32A C29 C31B 140.1(4) . . ?
C30A C29 C22 111.5(3) . . ?
C32B C29 C22 110.1(3) . . ?
C32A C29 C22 108.5(3) . . ?
C31B C29 C22 111.1(3) . . ?
C30A C29 C30B 56.6(4) . . ?
C32B C29 C30B 105.2(4) . . ?
C32A C29 C30B 65.2(4) . . ?
C31B C29 C30B 104.0(4) . . ?
C22 C29 C30B 110.7(2) . . ?
C30A C29 C31A 106.1(4) . . ?
C32B C29 C31A 61.5(4) . . ?
C32A C29 C31A 103.2(4) . . ?
C31B C29 C31A 58.8(4) . . ?
C22 C29 C31A 109.7(2) . . ?
C30B C29 C31A 139.5(3) . . ?
C29 C30A H30A 109.5 . . ?
C29 C30A H30B 109.5 . . ?
C29 C30A H30C 109.5 . . ?
C29 C31A H31A 109.5 . . ?
C29 C31A H31B 109.5 . . ?
C29 C31A H31C 109.5 . . ?
C29 C32A H32A 109.5 . . ?
C29 C32A H32B 109.5 . . ?
C29 C32A H32C 109.5 . . ?
C29 C30B H30D 109.5 . . ?
C29 C30B H30E 109.5 . . ?
H30D C30B H30E 109.5 . . ?
C29 C30B H30F 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
C29 C31B H31D 109.5 . . ?
C29 C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C29 C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C29 C32B H32D 109.5 . . ?
C29 C32B H32E 109.5 . . ?
H32D C32B H32E 109.5 . . ?
C29 C32B H32F 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
C34 C33 C35 109.0(2) . . ?
C34 C33 C36 108.1(2) . . ?
C35 C33 C36 105.6(2) . . ?
C34 C33 C24 111.89(18) . . ?
C35 C33 C24 114.84(19) . . ?
C36 C33 C24 107.01(18) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 P1 P2 P3 92.83(6) . . . . ?
C1 P1 P2 P4 148.76(6) . . . . ?
P3 P1 P2 P4 55.93(3) . . . . ?
P1 P2 P3 P4 107.78(3) . . . . ?
P4 P2 P3 P1 -107.78(3) . . . . ?
C1 P1 P3 P2 -94.18(6) . . . . ?
C1 P1 P3 P4 -150.23(6) . . . . ?
P2 P1 P3 P4 -56.05(3) . . . . ?
P2 P3 P4 C19 -100.02(7) . . . . ?
P1 P3 P4 C19 -43.98(7) . . . . ?
P1 P3 P4 P2 56.04(3) . . . . ?
P3 P2 P4 C19 98.51(7) . . . . ?
P1 P2 P4 C19 42.16(7) . . . . ?
P1 P2 P4 P3 -56.35(3) . . . . ?
P2 P1 C1 C2 -114.52(14) . . . . ?
P3 P1 C1 C2 -55.65(15) . . . . ?
P2 P1 C1 C6 49.88(15) . . . . ?
P3 P1 C1 C6 108.75(15) . . . . ?
C6 C1 C2 C3 -17.6(3) . . . . ?
P1 C1 C2 C3 147.13(16) . . . . ?
C6 C1 C2 C7 157.35(18) . . . . ?
P1 C1 C2 C7 -37.9(3) . . . . ?
C1 C2 C3 C4 3.5(3) . . . . ?
C7 C2 C3 C4 -171.98(19) . . . . ?
C2 C3 C4 C5 10.0(3) . . . . ?
C2 C3 C4 C11 -171.80(19) . . . . ?
C3 C4 C5 C6 -9.4(3) . . . . ?
C11 C4 C5 C6 172.26(19) . . . . ?
C4 C5 C6 C1 -4.4(3) . . . . ?
C4 C5 C6 C15 170.59(19) . . . . ?
C2 C1 C6 C5 18.1(3) . . . . ?
P1 C1 C6 C5 -146.46(16) . . . . ?
C2 C1 C6 C15 -156.43(18) . . . . ?
P1 C1 C6 C15 39.0(3) . . . . ?
C3 C2 C7 C9 -65.9(2) . . . . ?
C1 C2 C7 C9 119.1(2) . . . . ?
C3 C2 C7 C8 169.50(19) . . . . ?
C1 C2 C7 C8 -5.5(3) . . . . ?
C3 C2 C7 C10 52.7(2) . . . . ?
C1 C2 C7 C10 -122.4(2) . . . . ?
C3 C4 C11 C13B -166.3(11) . . . . ?
C5 C4 C11 C13B 11.9(11) . . . . ?
C3 C4 C11 C14B 66.2(11) . . . . ?
C5 C4 C11 C14B -115.6(11) . . . . ?
C3 C4 C11 C14A 122.1(3) . . . . ?
C5 C4 C11 C14A -59.7(3) . . . . ?
C3 C4 C11 C12A 1.4(4) . . . . ?
C5 C4 C11 C12A 179.6(3) . . . . ?
C3 C4 C11 C13A -118.6(3) . . . . ?
C5 C4 C11 C13A 59.6(3) . . . . ?
C3 C4 C11 C12B -49.0(11) . . . . ?
C5 C4 C11 C12B 129.2(10) . . . . ?
C5 C6 C15 C18 -167.76(19) . . . . ?
C1 C6 C15 C18 6.8(3) . . . . ?
C5 C6 C15 C16 66.3(2) . . . . ?
C1 C6 C15 C16 -119.1(2) . . . . ?
C5 C6 C15 C17 -52.2(2) . . . . ?
C1 C6 C15 C17 122.4(2) . . . . ?
P3 P4 C19 C20 115.13(15) . . . . ?
P2 P4 C19 C20 53.56(17) . . . . ?
P3 P4 C19 C24 -53.74(17) . . . . ?
P2 P4 C19 C24 -115.30(15) . . . . ?
C24 C19 C20 C21 18.5(3) . . . . ?
P4 C19 C20 C21 -150.38(16) . . . . ?
C24 C19 C20 C25 -159.25(19) . . . . ?
P4 C19 C20 C25 31.8(3) . . . . ?
C19 C20 C21 C22 -4.0(3) . . . . ?
C25 C20 C21 C22 173.95(18) . . . . ?
C20 C21 C22 C23 -9.8(3) . . . . ?
C20 C21 C22 C29 171.78(19) . . . . ?
C21 C22 C23 C24 9.6(3) . . . . ?
C29 C22 C23 C24 -172.02(19) . . . . ?
C22 C23 C24 C19 4.4(3) . . . . ?
C22 C23 C24 C33 -172.74(19) . . . . ?
C20 C19 C24 C23 -18.7(3) . . . . ?
P4 C19 C24 C23 150.41(16) . . . . ?
C20 C19 C24 C33 158.15(19) . . . . ?
P4 C19 C24 C33 -32.8(3) . . . . ?
C21 C20 C25 C26 -164.13(19) . . . . ?
C19 C20 C25 C26 13.7(3) . . . . ?
C21 C20 C25 C27 71.5(2) . . . . ?
C19 C20 C25 C27 -110.7(2) . . . . ?
C21 C20 C25 C28 -47.2(3) . . . . ?
C19 C20 C25 C28 130.6(2) . . . . ?
C23 C22 C29 C30A -114.5(5) . . . . ?
C21 C22 C29 C30A 63.8(5) . . . . ?
C23 C22 C29 C32B 68.5(4) . . . . ?
C21 C22 C29 C32B -113.2(4) . . . . ?
C23 C22 C29 C32A 114.7(4) . . . . ?
C21 C22 C29 C32A -67.0(4) . . . . ?
C23 C22 C29 C31B -60.5(4) . . . . ?
C21 C22 C29 C31B 117.8(4) . . . . ?
C23 C22 C29 C30B -175.6(3) . . . . ?
C21 C22 C29 C30B 2.7(4) . . . . ?
C23 C22 C29 C31A 2.6(4) . . . . ?
C21 C22 C29 C31A -179.1(3) . . . . ?
C23 C24 C33 C34 -68.8(3) . . . . ?
C19 C24 C33 C34 114.4(2) . . . . ?
C23 C24 C33 C35 166.3(2) . . . . ?
C19 C24 C33 C35 -10.6(3) . . . . ?
C23 C24 C33 C36 49.5(3) . . . . ?
C19 C24 C33 C36 -127.4(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.07
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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_is_jr6b_endo_exo_MesP4Mes
_database_code_depnum_ccdc_archive 'CCDC 1413822'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H59 P4'
_chemical_formula_sum            'C36 H59 P4'
_chemical_formula_weight         615.71

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

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

_cell_length_a                   10.4770(5)
_cell_length_b                   13.2999(8)
_cell_length_c                   13.5005(7)
_cell_angle_alpha                102.674(4)
_cell_angle_beta                 93.615(4)
_cell_angle_gamma                90.136(4)
_cell_volume                     1831.46(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1412
_cell_measurement_theta_min      4.873
_cell_measurement_theta_max      44.279

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             670
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9622
_exptl_absorpt_correction_T_max  0.9932
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37485
_diffrn_reflns_av_R_equivalents  0.1593
_diffrn_reflns_av_sigmaI/netI    0.2061
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         26.50
_reflns_number_total             7574
_reflns_number_gt                3504
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker Apex V7.51A'
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms were positioned geometrically and refined using a riding model, 
 with C---H = 0.98 (methyl groups), 0.99Å (methylene groups), 
 1.00Å (methine groups) or 0.95 Å (aryl CH) and with Uiso(H) = 
 1.5 times Ueq(C) (methyl groups) or with Uiso(H) = 1.2 times 
 Ueq(C) (methylene  groups, aryl CH, methine groups). Torsion angles 
 of all methyl groups were allowed to refine.
 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0309P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7574
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1830
_refine_ls_R_factor_gt           0.0616
_refine_ls_wR_factor_ref         0.1226
_refine_ls_wR_factor_gt          0.0905
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      0.980
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.74367(8) 0.76304(8) 0.22089(7) 0.0217(3) Uani 1 1 d . . .
P2 P 0.93060(9) 0.69488(8) 0.17429(8) 0.0277(3) Uani 1 1 d . . .
P3 P 0.92889(8) 0.83038(8) 0.29853(8) 0.0266(3) Uani 1 1 d . . .
P4 P 0.97121(8) 0.67841(8) 0.33278(8) 0.0251(3) Uani 1 1 d . . .
C1 C 0.7121(3) 0.8512(3) 0.1320(3) 0.0175(9) Uani 1 1 d . . .
C2 C 0.7164(3) 0.8174(3) 0.0254(3) 0.0193(9) Uani 1 1 d . . .
C3 C 0.7416(3) 0.8917(3) -0.0311(3) 0.0210(9) Uani 1 1 d . . .
H3 H 0.7498 0.8688 -0.1022 0.025 Uiso 1 1 calc R . .
C4 C 0.7550(3) 0.9954(3) 0.0108(3) 0.0203(9) Uani 1 1 d . . .
C5 C 0.7260(3) 1.0265(3) 0.1116(3) 0.0222(9) Uani 1 1 d . . .
H5 H 0.7245 1.0983 0.1404 0.027 Uiso 1 1 calc R . .
C6 C 0.6988(3) 0.9589(3) 0.1732(3) 0.0192(9) Uani 1 1 d . . .
C7 C 0.6851(3) 0.7073(3) -0.0376(3) 0.0221(9) Uani 1 1 d . . .
C8 C 0.6156(3) 0.6389(3) 0.0209(3) 0.0318(10) Uani 1 1 d . . .
H8A H 0.6737 0.6242 0.0755 0.048 Uiso 1 1 calc R . .
H8B H 0.5881 0.5742 -0.0258 0.048 Uiso 1 1 calc R . .
H8C H 0.5407 0.6749 0.0503 0.048 Uiso 1 1 calc R . .
C9 C 0.8049(3) 0.6537(3) -0.0825(3) 0.0330(11) Uani 1 1 d . . .
H9A H 0.8454 0.6966 -0.1225 0.050 Uiso 1 1 calc R . .
H9B H 0.7805 0.5866 -0.1264 0.050 Uiso 1 1 calc R . .
H9C H 0.8653 0.6437 -0.0271 0.050 Uiso 1 1 calc R . .
C10 C 0.5898(3) 0.7154(3) -0.1278(3) 0.0285(10) Uani 1 1 d . . .
H10A H 0.5148 0.7540 -0.1019 0.043 Uiso 1 1 calc R . .
H10B H 0.5629 0.6461 -0.1651 0.043 Uiso 1 1 calc R . .
H10C H 0.6314 0.7513 -0.1735 0.043 Uiso 1 1 calc R . .
C11 C 0.7910(3) 1.0756(3) -0.0487(3) 0.0249(10) Uani 1 1 d . . .
C12 C 0.8232(4) 1.0269(3) -0.1570(3) 0.0382(11) Uani 1 1 d . . .
H12A H 0.8935 0.9786 -0.1553 0.057 Uiso 1 1 calc R . .
H12B H 0.8491 1.0809 -0.1911 0.057 Uiso 1 1 calc R . .
H12C H 0.7479 0.9897 -0.1944 0.057 Uiso 1 1 calc R . .
C13 C 0.6783(3) 1.1488(3) -0.0552(3) 0.0377(11) Uani 1 1 d . . .
H13A H 0.7013 1.1991 -0.0946 0.057 Uiso 1 1 calc R . .
H13B H 0.6593 1.1850 0.0136 0.057 Uiso 1 1 calc R . .
H13C H 0.6028 1.1088 -0.0886 0.057 Uiso 1 1 calc R . .
C14 C 0.9077(3) 1.1388(3) 0.0062(3) 0.0360(11) Uani 1 1 d . . .
H14A H 0.9814 1.0935 0.0063 0.054 Uiso 1 1 calc R . .
H14B H 0.8889 1.1697 0.0764 0.054 Uiso 1 1 calc R . .
H14C H 0.9273 1.1934 -0.0292 0.054 Uiso 1 1 calc R . .
C15 C 0.6483(3) 1.0087(3) 0.2777(3) 0.0215(9) Uani 1 1 d . . .
C16 C 0.5488(3) 1.0902(3) 0.2628(3) 0.0307(10) Uani 1 1 d . . .
H16A H 0.5906 1.1459 0.2394 0.046 Uiso 1 1 calc R . .
H16B H 0.5112 1.1183 0.3276 0.046 Uiso 1 1 calc R . .
H16C H 0.4814 1.0581 0.2120 0.046 Uiso 1 1 calc R . .
C17 C 0.7558(3) 1.0645(3) 0.3516(3) 0.0319(10) Uani 1 1 d . . .
H17A H 0.8223 1.0152 0.3614 0.048 Uiso 1 1 calc R . .
H17B H 0.7213 1.0947 0.4171 0.048 Uiso 1 1 calc R . .
H17C H 0.7928 1.1192 0.3236 0.048 Uiso 1 1 calc R . .
C18 C 0.5769(3) 0.9334(3) 0.3282(3) 0.0295(10) Uani 1 1 d . . .
H18A H 0.5106 0.8957 0.2797 0.044 Uiso 1 1 calc R . .
H18B H 0.5373 0.9723 0.3885 0.044 Uiso 1 1 calc R . .
H18C H 0.6377 0.8845 0.3484 0.044 Uiso 1 1 calc R . .
C19 C 0.8188(3) 0.6357(3) 0.3758(3) 0.0170(9) Uani 1 1 d . . .
C20 C 0.7582(3) 0.7020(3) 0.4548(3) 0.0189(9) Uani 1 1 d . . .
C21 C 0.6241(3) 0.6958(3) 0.4528(3) 0.0196(9) Uani 1 1 d . . .
H21 H 0.5814 0.7426 0.5030 0.024 Uiso 1 1 calc R . .
C22 C 0.5514(3) 0.6248(3) 0.3811(3) 0.0188(9) Uani 1 1 d . . .
C23 C 0.6173(3) 0.5477(3) 0.3198(3) 0.0221(9) Uani 1 1 d . . .
H23 H 0.5697 0.4915 0.2780 0.027 Uiso 1 1 calc R . .
C24 C 0.7501(3) 0.5484(3) 0.3163(3) 0.0189(9) Uani 1 1 d . . .
C25 C 0.8257(3) 0.7751(3) 0.5480(3) 0.0244(10) Uani 1 1 d . . .
C26 C 0.9708(3) 0.7642(3) 0.5592(3) 0.0380(12) Uani 1 1 d . . .
H26A H 1.0110 0.7967 0.5103 0.057 Uiso 1 1 calc R . .
H26B H 0.9921 0.6909 0.5462 0.057 Uiso 1 1 calc R . .
H26C H 1.0023 0.7979 0.6285 0.057 Uiso 1 1 calc R . .
C27 C 0.7947(3) 0.8890(3) 0.5508(3) 0.0344(11) Uani 1 1 d . . .
H27A H 0.8324 0.9324 0.6142 0.052 Uiso 1 1 calc R . .
H27B H 0.7017 0.8975 0.5474 0.052 Uiso 1 1 calc R . .
H27C H 0.8302 0.9096 0.4927 0.052 Uiso 1 1 calc R . .
C28 C 0.7748(3) 0.7470(3) 0.6436(3) 0.0283(10) Uani 1 1 d . . .
H28A H 0.7929 0.6747 0.6431 0.042 Uiso 1 1 calc R . .
H28B H 0.6823 0.7575 0.6437 0.042 Uiso 1 1 calc R . .
H28C H 0.8171 0.7911 0.7047 0.042 Uiso 1 1 calc R . .
C29 C 0.4050(3) 0.6273(3) 0.3701(3) 0.0240(10) Uani 1 1 d . . .
C30 C 0.3645(3) 0.6339(3) 0.2603(3) 0.0426(12) Uani 1 1 d . . .
H30A H 0.3990 0.6977 0.2467 0.064 Uiso 1 1 calc R . .
H30B H 0.2709 0.6336 0.2513 0.064 Uiso 1 1 calc R . .
H30C H 0.3976 0.5746 0.2129 0.064 Uiso 1 1 calc R . .
C31 C 0.3521(3) 0.7201(3) 0.4413(3) 0.0401(12) Uani 1 1 d . . .
H31A H 0.3704 0.7144 0.5119 0.060 Uiso 1 1 calc R . .
H31B H 0.2593 0.7225 0.4272 0.060 Uiso 1 1 calc R . .
H31C H 0.3923 0.7832 0.4307 0.060 Uiso 1 1 calc R . .
C32 C 0.3469(3) 0.5293(3) 0.3920(3) 0.0439(12) Uani 1 1 d . . .
H32A H 0.3776 0.4689 0.3446 0.066 Uiso 1 1 calc R . .
H32B H 0.2534 0.5315 0.3836 0.066 Uiso 1 1 calc R . .
H32C H 0.3725 0.5248 0.4620 0.066 Uiso 1 1 calc R . .
C33 C 0.8108(3) 0.4510(3) 0.2550(3) 0.0240(9) Uani 1 1 d . . .
C34 C 0.7544(3) 0.3569(3) 0.2883(3) 0.0345(11) Uani 1 1 d . . .
H34A H 0.7705 0.3652 0.3620 0.052 Uiso 1 1 calc R . .
H34B H 0.7949 0.2939 0.2531 0.052 Uiso 1 1 calc R . .
H34C H 0.6620 0.3521 0.2710 0.052 Uiso 1 1 calc R . .
C35 C 0.7793(4) 0.4367(3) 0.1397(3) 0.0389(11) Uani 1 1 d . . .
H35A H 0.6864 0.4381 0.1261 0.058 Uiso 1 1 calc R . .
H35B H 0.8117 0.3704 0.1042 0.058 Uiso 1 1 calc R . .
H35C H 0.8196 0.4926 0.1155 0.058 Uiso 1 1 calc R . .
C36 C 0.9565(3) 0.4443(3) 0.2745(3) 0.0383(11) Uani 1 1 d . . .
H36A H 0.9996 0.4934 0.2428 0.057 Uiso 1 1 calc R . .
H36B H 0.9841 0.3743 0.2454 0.057 Uiso 1 1 calc R . .
H36C H 0.9786 0.4610 0.3480 0.057 Uiso 1 1 calc R . .


#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 1.870(3) . ?
P1 P2 2.2286(14) . ?
P1 P3 2.2338(13) . ?
P2 P3 2.1768(15) . ?
P2 P4 2.2133(14) . ?
P3 P4 2.2101(14) . ?
P4 C19 1.863(3) . ?
C1 C2 1.413(4) . ?
C1 C6 1.429(5) . ?
C2 C3 1.408(4) . ?
C2 C7 1.546(5) . ?
C3 C4 1.375(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(4) . ?
C4 C11 1.529(5) . ?
C5 C6 1.393(4) . ?
C5 H5 0.9500 . ?
C6 C15 1.548(5) . ?
C7 C9 1.537(4) . ?
C7 C8 1.538(4) . ?
C7 C10 1.548(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.524(5) . ?
C11 C14 1.535(4) . ?
C11 C13 1.542(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.530(4) . ?
C15 C16 1.541(4) . ?
C15 C18 1.545(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.412(4) . ?
C19 C24 1.423(4) . ?
C20 C21 1.405(4) . ?
C20 C25 1.541(4) . ?
C21 C22 1.381(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.385(4) . ?
C22 C29 1.533(4) . ?
C23 C24 1.396(4) . ?
C23 H23 0.9500 . ?
C24 C33 1.539(5) . ?
C25 C26 1.529(4) . ?
C25 C27 1.544(5) . ?
C25 C28 1.545(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C31 1.518(5) . ?
C29 C32 1.531(5) . ?
C29 C30 1.537(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C36 1.538(4) . ?
C33 C35 1.540(5) . ?
C33 C34 1.548(5) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 P2 102.53(11) . . ?
C1 P1 P3 99.93(11) . . ?
P2 P1 P3 58.39(4) . . ?
P3 P2 P4 60.45(5) . . ?
P3 P2 P1 60.92(4) . . ?
P4 P2 P1 88.09(5) . . ?
P2 P3 P4 60.59(5) . . ?
P2 P3 P1 60.68(4) . . ?
P4 P3 P1 88.04(5) . . ?
C19 P4 P3 104.74(11) . . ?
C19 P4 P2 106.67(11) . . ?
P3 P4 P2 58.96(5) . . ?
C2 C1 C6 118.4(3) . . ?
C2 C1 P1 122.2(3) . . ?
C6 C1 P1 119.0(3) . . ?
C3 C2 C1 117.8(3) . . ?
C3 C2 C7 115.7(3) . . ?
C1 C2 C7 126.3(3) . . ?
C4 C3 C2 123.6(4) . . ?
C4 C3 H3 118.2 . . ?
C2 C3 H3 118.2 . . ?
C3 C4 C5 115.9(3) . . ?
C3 C4 C11 123.9(3) . . ?
C5 C4 C11 120.0(3) . . ?
C4 C5 C6 124.0(4) . . ?
C4 C5 H5 118.0 . . ?
C6 C5 H5 118.0 . . ?
C5 C6 C1 117.5(3) . . ?
C5 C6 C15 115.8(3) . . ?
C1 C6 C15 126.6(3) . . ?
C9 C7 C8 110.5(3) . . ?
C9 C7 C2 111.7(3) . . ?
C8 C7 C2 113.7(3) . . ?
C9 C7 C10 107.4(3) . . ?
C8 C7 C10 104.7(3) . . ?
C2 C7 C10 108.3(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C4 112.4(3) . . ?
C12 C11 C14 108.5(3) . . ?
C4 C11 C14 109.3(3) . . ?
C12 C11 C13 107.6(3) . . ?
C4 C11 C13 109.8(3) . . ?
C14 C11 C13 109.0(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C15 C16 107.2(3) . . ?
C17 C15 C18 109.6(3) . . ?
C16 C15 C18 104.9(3) . . ?
C17 C15 C6 111.3(3) . . ?
C16 C15 C6 108.8(3) . . ?
C18 C15 C6 114.5(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C24 119.2(3) . . ?
C20 C19 P4 119.3(3) . . ?
C24 C19 P4 120.1(3) . . ?
C21 C20 C19 117.3(3) . . ?
C21 C20 C25 116.4(3) . . ?
C19 C20 C25 126.1(3) . . ?
C22 C21 C20 123.1(3) . . ?
C22 C21 H21 118.4 . . ?
C20 C21 H21 118.4 . . ?
C21 C22 C23 116.6(3) . . ?
C21 C22 C29 123.0(3) . . ?
C23 C22 C29 120.4(3) . . ?
C22 C23 C24 123.2(3) . . ?
C22 C23 H23 118.4 . . ?
C24 C23 H23 118.4 . . ?
C23 C24 C19 117.3(3) . . ?
C23 C24 C33 117.1(3) . . ?
C19 C24 C33 125.3(3) . . ?
C26 C25 C20 115.2(3) . . ?
C26 C25 C27 108.9(3) . . ?
C20 C25 C27 111.9(3) . . ?
C26 C25 C28 105.3(3) . . ?
C20 C25 C28 107.1(3) . . ?
C27 C25 C28 108.1(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C31 C29 C32 108.7(3) . . ?
C31 C29 C22 112.0(3) . . ?
C32 C29 C22 110.5(3) . . ?
C31 C29 C30 108.0(3) . . ?
C32 C29 C30 109.2(3) . . ?
C22 C29 C30 108.4(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C36 C33 C24 115.0(3) . . ?
C36 C33 C35 108.8(3) . . ?
C24 C33 C35 112.1(3) . . ?
C36 C33 C34 105.1(3) . . ?
C24 C33 C34 107.7(3) . . ?
C35 C33 C34 107.7(3) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 P1 P2 P3 94.05(12) . . . . ?
C1 P1 P2 P4 150.95(12) . . . . ?
P3 P1 P2 P4 56.90(5) . . . . ?
P1 P2 P3 P4 105.75(5) . . . . ?
P4 P2 P3 P1 -105.75(5) . . . . ?
C1 P1 P3 P2 -98.68(12) . . . . ?
C1 P1 P3 P4 -155.70(12) . . . . ?
P2 P1 P3 P4 -57.03(5) . . . . ?
P2 P3 P4 C19 -100.83(12) . . . . ?
P1 P3 P4 C19 -43.72(12) . . . . ?
P1 P3 P4 P2 57.11(5) . . . . ?
P3 P2 P4 C19 97.46(13) . . . . ?
P1 P2 P4 C19 40.15(13) . . . . ?
P1 P2 P4 P3 -57.31(5) . . . . ?
P2 P1 C1 C2 52.1(3) . . . . ?
P3 P1 C1 C2 111.7(3) . . . . ?
P2 P1 C1 C6 -120.0(2) . . . . ?
P3 P1 C1 C6 -60.4(2) . . . . ?
C6 C1 C2 C3 16.6(4) . . . . ?
P1 C1 C2 C3 -155.5(2) . . . . ?
C6 C1 C2 C7 -158.0(3) . . . . ?
P1 C1 C2 C7 29.9(4) . . . . ?
C1 C2 C3 C4 -3.8(5) . . . . ?
C7 C2 C3 C4 171.4(3) . . . . ?
C2 C3 C4 C5 -8.1(5) . . . . ?
C2 C3 C4 C11 175.8(3) . . . . ?
C3 C4 C5 C6 7.3(5) . . . . ?
C11 C4 C5 C6 -176.5(3) . . . . ?
C4 C5 C6 C1 5.3(5) . . . . ?
C4 C5 C6 C15 -170.8(3) . . . . ?
C2 C1 C6 C5 -17.3(4) . . . . ?
P1 C1 C6 C5 155.1(2) . . . . ?
C2 C1 C6 C15 158.3(3) . . . . ?
P1 C1 C6 C15 -29.3(4) . . . . ?
C3 C2 C7 C9 73.4(4) . . . . ?
C1 C2 C7 C9 -111.9(4) . . . . ?
C3 C2 C7 C8 -160.6(3) . . . . ?
C1 C2 C7 C8 14.1(5) . . . . ?
C3 C2 C7 C10 -44.7(4) . . . . ?
C1 C2 C7 C10 130.0(3) . . . . ?
C3 C4 C11 C12 -5.6(5) . . . . ?
C5 C4 C11 C12 178.4(3) . . . . ?
C3 C4 C11 C14 -126.2(4) . . . . ?
C5 C4 C11 C14 57.8(4) . . . . ?
C3 C4 C11 C13 114.2(4) . . . . ?
C5 C4 C11 C13 -61.8(4) . . . . ?
C5 C6 C15 C17 -74.7(4) . . . . ?
C1 C6 C15 C17 109.6(4) . . . . ?
C5 C6 C15 C16 43.2(4) . . . . ?
C1 C6 C15 C16 -132.5(3) . . . . ?
C5 C6 C15 C18 160.2(3) . . . . ?
C1 C6 C15 C18 -15.4(5) . . . . ?
P3 P4 C19 C20 -52.8(3) . . . . ?
P2 P4 C19 C20 -114.3(2) . . . . ?
P3 P4 C19 C24 113.7(3) . . . . ?
P2 P4 C19 C24 52.2(3) . . . . ?
C24 C19 C20 C21 -17.5(5) . . . . ?
P4 C19 C20 C21 149.1(3) . . . . ?
C24 C19 C20 C25 157.5(3) . . . . ?
P4 C19 C20 C25 -35.9(4) . . . . ?
C19 C20 C21 C22 3.6(5) . . . . ?
C25 C20 C21 C22 -171.9(3) . . . . ?
C20 C21 C22 C23 10.1(5) . . . . ?
C20 C21 C22 C29 -171.6(3) . . . . ?
C21 C22 C23 C24 -10.5(5) . . . . ?
C29 C22 C23 C24 171.2(3) . . . . ?
C22 C23 C24 C19 -2.9(5) . . . . ?
C22 C23 C24 C33 172.4(3) . . . . ?
C20 C19 C24 C23 17.2(5) . . . . ?
P4 C19 C24 C23 -149.3(3) . . . . ?
C20 C19 C24 C33 -157.7(3) . . . . ?
P4 C19 C24 C33 35.8(5) . . . . ?
C21 C20 C25 C26 168.1(3) . . . . ?
C19 C20 C25 C26 -7.0(5) . . . . ?
C21 C20 C25 C27 -66.9(4) . . . . ?
C19 C20 C25 C27 118.1(4) . . . . ?
C21 C20 C25 C28 51.4(4) . . . . ?
C19 C20 C25 C28 -123.7(4) . . . . ?
C21 C22 C29 C31 4.0(5) . . . . ?
C23 C22 C29 C31 -177.7(3) . . . . ?
C21 C22 C29 C32 -117.3(4) . . . . ?
C23 C22 C29 C32 60.9(4) . . . . ?
C21 C22 C29 C30 123.1(4) . . . . ?
C23 C22 C29 C30 -58.7(4) . . . . ?
C23 C24 C33 C36 -165.5(3) . . . . ?
C19 C24 C33 C36 9.4(5) . . . . ?
C23 C24 C33 C35 69.5(4) . . . . ?
C19 C24 C33 C35 -115.5(4) . . . . ?
C23 C24 C33 C34 -48.8(4) . . . . ?
C19 C24 C33 C34 126.1(3) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.076
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_is_jb73_exo_exo_MesP4Mes_GaCl3_hexane
_database_code_depnum_ccdc_archive 'CCDC 1413823'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;

_vrf_CHEMW03_is_jb73_exo_exo_MesP4Mes_GaCl3_hexane 
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: PLATON/SQUEEZE was used to treat two heavily disordered 
n-hexane molecules in the unit cell. These were removed from the 
model, but included in the empirical formula. Additional PLATON/SQUEEZE 
details appear in _refine_special_details.
;
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H58 Cl3 Ga P4, 0.5(C6 H14)'
_chemical_formula_sum            'C39 H65 Cl3 Ga P4'
_chemical_formula_weight         833.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_Int_Tables_number      62

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

_cell_length_a                   26.7411(7)
_cell_length_b                   13.5063(4)
_cell_length_c                   12.5618(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4537.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9840
_cell_measurement_theta_min      4.449
_cell_measurement_theta_max      57.587

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1764
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7324
_exptl_absorpt_correction_T_max  0.8113
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and psi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            69297
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.69
_diffrn_reflns_theta_max         30.00
_reflns_number_total             6840
_reflns_number_gt                5540
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker Apex v2.0-2'
_computing_cell_refinement       'Bruker Apex v2.0-2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms were positioned geometrically and refined using a 
 riding model , with C---H = 0.98 (methyl groups), 0.99Å (methylene groups), 
 1.00Å (methine groups) or 0.95 Å (aryl CH) and with Uiso(H) = 
 1.5 times Ueq(C) (methyl groups) or with Uiso(H) = 1.2 times 
 Ueq(C) (methylene  groups, aryl CH, methine groups). Torsion angles 
 of all methyl groups (except the minor part of the disordered tBu group)were 
 allowed to refine.
 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.246 0.250 -0.134 136 27 ' '
2 0.754 0.750 0.134 136 28 ' '
3 0.254 0.750 0.366 136 29 ' '
4 0.746 0.250 0.634 136 27 ' '
_platon_squeeze_details          
;
The unit cell contains two n-hexane molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0640P)²+4.9244P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6840
_refine_ls_number_parameters     267
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1357
_refine_ls_wR_factor_gt          0.1301
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.404857(14) 0.2500 0.60464(3) 0.02585(10) Uani 1 2 d S . .
Cl1 Cl 0.48629(3) 0.2500 0.61140(7) 0.03207(17) Uani 1 2 d S . .
Cl2 Cl 0.37420(3) 0.11697(5) 0.67346(5) 0.04425(17) Uani 1 1 d . . .
P1 P 0.28307(3) 0.2500 0.48543(7) 0.0343(2) Uani 1 2 d S . .
P2 P 0.32220(2) 0.16857(5) 0.35558(5) 0.03356(15) Uani 1 1 d . . .
P3 P 0.38666(3) 0.2500 0.41588(6) 0.02343(16) Uani 1 2 d S . .
C1 C 0.22190(13) 0.2500 0.4151(3) 0.0375(8) Uani 1 2 d S . .
C2 C 0.20263(10) 0.1594(2) 0.3753(2) 0.0417(6) Uani 1 1 d . . .
C3 C 0.17570(11) 0.1614(2) 0.2802(3) 0.0458(7) Uani 1 1 d . . .
H3 H 0.1633 0.1009 0.2522 0.055 Uiso 1 1 calc R A 1
C5 C 0.20524(11) 0.0573(2) 0.4328(3) 0.0496(7) Uani 1 1 d . . .
C6 C 0.22975(15) 0.0606(3) 0.5439(3) 0.0656(10) Uani 1 1 d . . .
H6A H 0.2660 0.0692 0.5362 0.098 Uiso 1 1 calc R . .
H6B H 0.2230 -0.0015 0.5816 0.098 Uiso 1 1 calc R . .
H6C H 0.2159 0.1161 0.5846 0.098 Uiso 1 1 calc R . .
C7 C 0.23004(13) -0.0230(2) 0.3654(3) 0.0596(9) Uani 1 1 d . . .
H7A H 0.2150 -0.0236 0.2942 0.089 Uiso 1 1 calc R . .
H7B H 0.2250 -0.0877 0.3992 0.089 Uiso 1 1 calc R . .
H7C H 0.2659 -0.0094 0.3595 0.089 Uiso 1 1 calc R . .
C8 C 0.14946(13) 0.0275(3) 0.4522(3) 0.0678(10) Uani 1 1 d . . .
H8A H 0.1311 0.0303 0.3848 0.102 Uiso 1 1 calc R . .
H8B H 0.1343 0.0734 0.5033 0.102 Uiso 1 1 calc R . .
H8C H 0.1480 -0.0400 0.4808 0.102 Uiso 1 1 calc R . .
C4A C 0.1661(5) 0.2500 0.2239(13) 0.046(2) Uani 0.75(3) 2 d SPD . 1
C9A C 0.1423(5) 0.2500 0.1125(11) 0.055(3) Uani 0.75(3) 2 d SPD . 1
C10A C 0.1408(9) 0.1526(11) 0.0620(19) 0.072(4) Uani 0.374(16) 1 d PD . 1
H10A H 0.1746 0.1246 0.0597 0.109 Uiso 0.374(16) 1 calc PR . 1
H10B H 0.1278 0.1591 -0.0106 0.109 Uiso 0.374(16) 1 calc PR . 1
H10C H 0.1189 0.1087 0.1031 0.109 Uiso 0.374(16) 1 calc PR . 1
C11A C 0.1726(10) 0.3226(14) 0.0412(13) 0.106(8) Uani 0.374(16) 1 d PD . 1
H11A H 0.2082 0.3061 0.0452 0.159 Uiso 0.374(16) 1 calc PR . 1
H11B H 0.1674 0.3906 0.0663 0.159 Uiso 0.374(16) 1 calc PR . 1
H11C H 0.1611 0.3169 -0.0326 0.159 Uiso 0.374(16) 1 calc PR . 1
C12A C 0.0895(6) 0.2937(11) 0.1226(18) 0.088(7) Uani 0.374(16) 1 d PD . 1
H12A H 0.0913 0.3661 0.1178 0.133 Uiso 0.374(16) 1 calc PR . 1
H12B H 0.0751 0.2748 0.1913 0.133 Uiso 0.374(16) 1 calc PR . 1
H12C H 0.0684 0.2683 0.0649 0.133 Uiso 0.374(16) 1 calc PR . 1
C4B C 0.1623(15) 0.2500 0.236(4) 0.046(2) Uani 0.25(3) 2 d SPD . 2
C9B C 0.1278(13) 0.2500 0.138(3) 0.055(3) Uani 0.25(3) 2 d SPD . 2
C10B C 0.131(2) 0.160(2) 0.074(4) 0.072(4) Uani 0.126(16) 1 d PD . 2
H10D H 0.1175 0.1725 0.0033 0.109 Uiso 0.126(16) 1 calc PR . 2
H10E H 0.1125 0.1067 0.1088 0.109 Uiso 0.126(16) 1 calc PR . 2
H10F H 0.1665 0.1404 0.0678 0.109 Uiso 0.126(16) 1 calc PR . 2
C11B C 0.142(3) 0.341(3) 0.069(5) 0.106(8) Uani 0.126(16) 1 d PD . 2
H11D H 0.1271 0.3335 -0.0023 0.159 Uiso 0.126(16) 1 calc PR . 2
H11E H 0.1784 0.3451 0.0622 0.159 Uiso 0.126(16) 1 calc PR . 2
H11F H 0.1292 0.4015 0.1019 0.159 Uiso 0.126(16) 1 calc PR . 2
C12B C 0.0743(11) 0.267(4) 0.177(4) 0.088(7) Uani 0.126(16) 1 d PD . 2
H12D H 0.0511 0.2619 0.1171 0.133 Uiso 0.126(16) 1 calc PR . 2
H12E H 0.0716 0.3328 0.2094 0.133 Uiso 0.126(16) 1 calc PR . 2
H12F H 0.0657 0.2165 0.2307 0.133 Uiso 0.126(16) 1 calc PR . 2
C13 C 0.43203(11) 0.2500 0.3075(2) 0.0222(5) Uani 1 2 d S . .
C14 C 0.44429(9) 0.15872(15) 0.25771(17) 0.0247(4) Uani 1 1 d . . .
C15 C 0.46039(10) 0.16237(16) 0.15223(18) 0.0301(5) Uani 1 1 d . . .
H15 H 0.4675 0.1017 0.1170 0.036 Uiso 1 1 calc R . .
C16 C 0.46661(13) 0.2500 0.0960(3) 0.0296(6) Uani 1 2 d S . .
C17 C 0.44679(10) 0.05436(16) 0.30813(18) 0.0313(5) Uani 1 1 d . . .
C18 C 0.43711(11) 0.04849(18) 0.42782(19) 0.0364(6) Uani 1 1 d . . .
H18A H 0.4014 0.0583 0.4417 0.055 Uiso 1 1 calc R . .
H18B H 0.4564 0.1001 0.4642 0.055 Uiso 1 1 calc R . .
H18C H 0.4474 -0.0167 0.4543 0.055 Uiso 1 1 calc R . .
C19 C 0.50128(13) 0.0186(2) 0.2953(3) 0.0502(7) Uani 1 1 d . . .
H19A H 0.5100 0.0171 0.2196 0.075 Uiso 1 1 calc R . .
H19B H 0.5046 -0.0480 0.3253 0.075 Uiso 1 1 calc R . .
H19C H 0.5238 0.0640 0.3328 0.075 Uiso 1 1 calc R . .
C20 C 0.41134(14) -0.01773(19) 0.2515(2) 0.0498(8) Uani 1 1 d . . .
H20A H 0.4193 -0.0195 0.1754 0.075 Uiso 1 1 calc R . .
H20B H 0.3767 0.0043 0.2611 0.075 Uiso 1 1 calc R . .
H20C H 0.4153 -0.0841 0.2818 0.075 Uiso 1 1 calc R . .
C21 C 0.48396(17) 0.2500 -0.0195(3) 0.0423(9) Uani 1 2 d S . .
C22 C 0.4852(4) 0.3505(5) -0.0707(5) 0.065(2) Uani 0.50 1 d P . .
H22A H 0.4953 0.3438 -0.1453 0.098 Uiso 0.50 1 calc PR . .
H22B H 0.5092 0.3927 -0.0331 0.098 Uiso 0.50 1 calc PR . .
H22C H 0.4518 0.3805 -0.0670 0.098 Uiso 0.50 1 calc PR . .
C23 C 0.5368(3) 0.2025(7) -0.0238(6) 0.076(2) Uani 0.50 1 d P . .
H23A H 0.5478 0.1977 -0.0981 0.114 Uiso 0.50 1 calc PR . .
H23B H 0.5357 0.1362 0.0077 0.114 Uiso 0.50 1 calc PR . .
H23C H 0.5604 0.2438 0.0162 0.114 Uiso 0.50 1 calc PR . .
C24 C 0.4484(4) 0.1850(7) -0.0853(5) 0.069(2) Uani 0.50 1 d P . .
H24A H 0.4622 0.1758 -0.1569 0.104 Uiso 0.50 1 calc PR . .
H24B H 0.4157 0.2173 -0.0903 0.104 Uiso 0.50 1 calc PR . .
H24C H 0.4446 0.1204 -0.0506 0.104 Uiso 0.50 1 calc PR . .


#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Ga1 Cl2 2.1559(6) 7_565 ?
Ga1 Cl2 2.1559(6) . ?
Ga1 Cl1 2.1794(9) . ?
Ga1 P3 2.4206(8) . ?
P1 C1 1.859(4) . ?
P1 P2 2.2283(11) 7_565 ?
P1 P2 2.2283(11) . ?
P2 P3 2.1805(9) . ?
P2 P2 2.1997(13) 7_565 ?
P3 C13 1.824(3) . ?
P3 P2 2.1805(9) 7_565 ?
C1 C2 1.419(3) . ?
C1 C2 1.419(3) 7_565 ?
C2 C3 1.395(4) . ?
C2 C5 1.558(4) . ?
C3 C4B 1.364(16) . ?
C3 C4A 1.413(8) . ?
C3 H3 0.9500 . ?
C5 C7 1.527(5) . ?
C5 C6 1.543(5) . ?
C5 C8 1.564(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C4A C3 1.413(8) 7_565 ?
C4A C9A 1.537(7) . ?
C9A C10A 1.461(15) . ?
C9A C10A 1.461(15) 7_565 ?
C9A C12A 1.535(13) 7_565 ?
C9A C12A 1.535(13) . ?
C9A C11A 1.555(15) 7_565 ?
C9A C11A 1.555(15) . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C11A H11A 0.9800 . ?
C11A H11B 0.9800 . ?
C11A H11C 0.9800 . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C4B C3 1.364(16) 7_565 ?
C4B C9B 1.539(10) . ?
C9B C10B 1.462(17) . ?
C9B C10B 1.462(17) 7_565 ?
C9B C12B 1.530(15) 7_565 ?
C9B C12B 1.530(15) . ?
C9B C11B 1.556(17) 7_565 ?
C9B C11B 1.556(17) . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11B H11D 0.9800 . ?
C11B H11E 0.9800 . ?
C11B H11F 0.9800 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C13 C14 1.421(2) 7_565 ?
C13 C14 1.421(2) . ?
C14 C15 1.394(3) . ?
C14 C17 1.547(3) . ?
C15 C16 1.388(3) . ?
C15 H15 0.9500 . ?
C16 C15 1.388(3) 7_565 ?
C16 C21 1.523(5) . ?
C17 C18 1.528(3) . ?
C17 C20 1.534(4) . ?
C17 C19 1.544(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.502(7) 7_565 ?
C21 C22 1.502(7) . ?
C21 C24 1.536(8) . ?
C21 C24 1.536(8) 7_565 ?
C21 C23 1.554(9) 7_565 ?
C21 C23 1.554(9) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Ga1 Cl2 112.90(4) 7_565 . ?
Cl2 Ga1 Cl1 111.37(3) 7_565 . ?
Cl2 Ga1 Cl1 111.37(3) . . ?
Cl2 Ga1 P3 108.44(2) 7_565 . ?
Cl2 Ga1 P3 108.44(2) . . ?
Cl1 Ga1 P3 103.83(3) . . ?
C1 P1 P2 93.76(11) . 7_565 ?
C1 P1 P2 93.76(11) . . ?
P2 P1 P2 59.15(4) 7_565 . ?
P3 P2 P2 59.71(2) . 7_565 ?
P3 P2 P1 82.41(4) . . ?
P2 P2 P1 60.42(2) 7_565 . ?
C13 P3 P2 105.46(8) . . ?
C13 P3 P2 105.46(8) . 7_565 ?
P2 P3 P2 60.59(4) . 7_565 ?
C13 P3 Ga1 126.70(10) . . ?
P2 P3 Ga1 119.95(4) . . ?
P2 P3 Ga1 119.95(4) 7_565 . ?
C2 C1 C2 119.2(3) . 7_565 ?
C2 C1 P1 119.14(17) . . ?
C2 C1 P1 119.14(17) 7_565 . ?
C3 C2 C1 118.2(3) . . ?
C3 C2 C5 115.9(3) . . ?
C1 C2 C5 125.7(3) . . ?
C4B C3 C2 119.9(13) . . ?
C4B C3 C4A 7(3) . . ?
C2 C3 C4A 122.7(4) . . ?
C4B C3 H3 120.9 . . ?
C2 C3 H3 118.7 . . ?
C4A C3 H3 118.7 . . ?
C7 C5 C6 109.7(3) . . ?
C7 C5 C2 113.0(3) . . ?
C6 C5 C2 114.4(3) . . ?
C7 C5 C8 108.5(3) . . ?
C6 C5 C8 105.7(3) . . ?
C2 C5 C8 104.9(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C4A C3 115.6(9) 7_565 . ?
C3 C4A C9A 122.1(4) 7_565 . ?
C3 C4A C9A 122.1(4) . . ?
C10A C9A C10A 128.5(15) . 7_565 ?
C10A C9A C12A 70.3(12) . 7_565 ?
C10A C9A C12A 110.9(9) 7_565 7_565 ?
C10A C9A C12A 110.9(9) . . ?
C10A C9A C12A 70.3(12) 7_565 . ?
C12A C9A C12A 45.3(12) 7_565 . ?
C10A C9A C4A 114.0(8) . . ?
C10A C9A C4A 114.0(8) 7_565 . ?
C12A C9A C4A 107.7(7) 7_565 . ?
C12A C9A C4A 107.7(7) . . ?
C10A C9A C11A 36.6(12) . 7_565 ?
C10A C9A C11A 109.5(10) 7_565 7_565 ?
C12A C9A C11A 106.4(10) 7_565 7_565 ?
C12A C9A C11A 140.2(10) . 7_565 ?
C4A C9A C11A 108.0(8) . 7_565 ?
C10A C9A C11A 109.5(10) . . ?
C10A C9A C11A 36.6(12) 7_565 . ?
C12A C9A C11A 140.2(10) 7_565 . ?
C12A C9A C11A 106.4(10) . . ?
C4A C9A C11A 108.0(8) . . ?
C11A C9A C11A 78.2(18) 7_565 . ?
C3 C4B C3 123(2) 7_565 . ?
C3 C4B C9B 118.7(11) 7_565 . ?
C3 C4B C9B 118.7(11) . . ?
C10B C9B C10B 113(4) . 7_565 ?
C10B C9B C12B 97(4) . 7_565 ?
C10B C9B C12B 111.2(14) 7_565 7_565 ?
C10B C9B C12B 111.2(14) . . ?
C10B C9B C12B 97(4) 7_565 . ?
C12B C9B C12B 17(4) 7_565 . ?
C10B C9B C4B 113.7(13) . . ?
C10B C9B C4B 113.7(13) 7_565 . ?
C12B C9B C4B 107.7(12) 7_565 . ?
C12B C9B C4B 107.7(12) . . ?
C10B C9B C11B 11(4) . 7_565 ?
C10B C9B C11B 109.3(14) 7_565 7_565 ?
C12B C9B C11B 106.9(15) 7_565 7_565 ?
C12B C9B C11B 122(4) . 7_565 ?
C4B C9B C11B 107.8(13) . 7_565 ?
C10B C9B C11B 109.3(14) . . ?
C10B C9B C11B 11(4) 7_565 . ?
C12B C9B C11B 122(4) 7_565 . ?
C12B C9B C11B 106.9(15) . . ?
C4B C9B C11B 107.8(13) . . ?
C11B C9B C11B 104(5) 7_565 . ?
C9B C10B H10D 109.5 . . ?
C9B C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C9B C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C9B C11B H11D 109.5 . . ?
C9B C11B H11E 109.5 . . ?
H11D C11B H11E 109.5 . . ?
C9B C11B H11F 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
C9B C12B H12D 109.5 . . ?
C9B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C9B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C14 C13 C14 120.4(3) 7_565 . ?
C14 C13 P3 118.82(14) 7_565 . ?
C14 C13 P3 118.82(14) . . ?
C15 C14 C13 117.3(2) . . ?
C15 C14 C17 114.08(19) . . ?
C13 C14 C17 128.36(19) . . ?
C16 C15 C14 123.4(2) . . ?
C16 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
C15 C16 C15 117.0(3) 7_565 . ?
C15 C16 C21 121.39(14) 7_565 . ?
C15 C16 C21 121.39(14) . . ?
C18 C17 C20 108.6(2) . . ?
C18 C17 C19 104.3(2) . . ?
C20 C17 C19 109.6(2) . . ?
C18 C17 C14 116.29(18) . . ?
C20 C17 C14 111.2(2) . . ?
C19 C17 C14 106.5(2) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C22 129.2(6) 7_565 . ?
C22 C21 C16 114.5(3) 7_565 . ?
C22 C21 C16 114.5(3) . . ?
C22 C21 C24 42.8(5) 7_565 . ?
C22 C21 C24 107.4(6) . . ?
C16 C21 C24 108.9(4) . . ?
C22 C21 C24 107.4(6) 7_565 7_565 ?
C22 C21 C24 42.8(5) . 7_565 ?
C16 C21 C24 108.9(4) . 7_565 ?
C24 C21 C24 69.7(8) . 7_565 ?
C22 C21 C23 109.7(6) 7_565 7_565 ?
C22 C21 C23 66.0(6) . 7_565 ?
C16 C21 C23 108.1(4) . 7_565 ?
C24 C21 C23 141.3(5) . 7_565 ?
C24 C21 C23 108.0(5) 7_565 7_565 ?
C22 C21 C23 66.0(6) 7_565 . ?
C22 C21 C23 109.7(6) . . ?
C16 C21 C23 108.1(4) . . ?
C24 C21 C23 108.0(5) . . ?
C24 C21 C23 141.3(5) 7_565 . ?
C23 C21 C23 48.7(7) 7_565 . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 P1 P2 P3 151.50(6) . . . . ?
P2 P1 P2 P3 59.37(3) 7_565 . . . ?
C1 P1 P2 P2 92.14(6) . . . 7_565 ?
P2 P2 P3 C13 -99.30(6) 7_565 . . . ?
P1 P2 P3 C13 -159.37(6) . . . . ?
P1 P2 P3 P2 -60.08(3) . . . 7_565 ?
P2 P2 P3 Ga1 109.67(3) 7_565 . . . ?
P1 P2 P3 Ga1 49.59(4) . . . . ?
Cl2 Ga1 P3 C13 118.53(2) 7_565 . . . ?
Cl2 Ga1 P3 C13 -118.53(3) . . . . ?
Cl1 Ga1 P3 C13 0.0 . . . . ?
Cl2 Ga1 P3 P2 -97.07(3) 7_565 . . . ?
Cl2 Ga1 P3 P2 25.86(4) . . . . ?
Cl1 Ga1 P3 P2 144.40(3) . . . . ?
Cl2 Ga1 P3 P2 -25.86(4) 7_565 . . 7_565 ?
Cl2 Ga1 P3 P2 97.07(3) . . . 7_565 ?
Cl1 Ga1 P3 P2 -144.40(3) . . . 7_565 ?
P2 P1 C1 C2 110.6(3) 7_565 . . . ?
P2 P1 C1 C2 51.3(3) . . . . ?
P2 P1 C1 C2 -51.3(3) 7_565 . . 7_565 ?
P2 P1 C1 C2 -110.6(3) . . . 7_565 ?
C2 C1 C2 C3 16.8(5) 7_565 . . . ?
P1 C1 C2 C3 -145.1(3) . . . . ?
C2 C1 C2 C5 -158.2(2) 7_565 . . . ?
P1 C1 C2 C5 39.9(4) . . . . ?
C1 C2 C3 C4B -9(3) . . . . ?
C5 C2 C3 C4B 166(3) . . . . ?
C1 C2 C3 C4A -1.4(9) . . . . ?
C5 C2 C3 C4A 174.1(9) . . . . ?
C3 C2 C5 C7 60.5(4) . . . . ?
C1 C2 C5 C7 -124.4(3) . . . . ?
C3 C2 C5 C6 -172.9(3) . . . . ?
C1 C2 C5 C6 2.2(5) . . . . ?
C3 C2 C5 C8 -57.6(4) . . . . ?
C1 C2 C5 C8 117.5(3) . . . . ?
C4B C3 C4A C3 57(10) . . . 7_565 ?
C2 C3 C4A C3 -13.2(15) . . . 7_565 ?
C4B C3 C4A C9A -118(10) . . . . ?
C2 C3 C4A C9A 172.0(9) . . . . ?
C3 C4A C9A C10A 173.1(14) 7_565 . . . ?
C3 C4A C9A C10A -12.4(16) . . . . ?
C3 C4A C9A C10A 12.4(16) 7_565 . . 7_565 ?
C3 C4A C9A C10A -173.1(14) . . . 7_565 ?
C3 C4A C9A C12A -111.1(12) 7_565 . . 7_565 ?
C3 C4A C9A C12A 63.4(14) . . . 7_565 ?
C3 C4A C9A C12A -63.4(14) 7_565 . . . ?
C3 C4A C9A C12A 111.1(12) . . . . ?
C3 C4A C9A C11A 134.3(14) 7_565 . . 7_565 ?
C3 C4A C9A C11A -51.2(16) . . . 7_565 ?
C3 C4A C9A C11A 51.2(16) 7_565 . . . ?
C3 C4A C9A C11A -134.3(14) . . . . ?
C2 C3 C4B C3 2(6) . . . 7_565 ?
C4A C3 C4B C3 -112(12) . . . 7_565 ?
C2 C3 C4B C9B -173(2) . . . . ?
C4A C3 C4B C9B 73(10) . . . . ?
C3 C4B C9B C10B 157(4) 7_565 . . . ?
C3 C4B C9B C10B -27(5) . . . . ?
C3 C4B C9B C10B 27(5) 7_565 . . 7_565 ?
C3 C4B C9B C10B -157(4) . . . 7_565 ?
C3 C4B C9B C12B -97(4) 7_565 . . 7_565 ?
C3 C4B C9B C12B 79(4) . . . 7_565 ?
C3 C4B C9B C12B -79(4) 7_565 . . . ?
C3 C4B C9B C12B 97(4) . . . . ?
C3 C4B C9B C11B 148(4) 7_565 . . 7_565 ?
C3 C4B C9B C11B -36(5) . . . 7_565 ?
C3 C4B C9B C11B 36(5) 7_565 . . . ?
C3 C4B C9B C11B -148(4) . . . . ?
P2 P3 C13 C14 113.6(2) . . . 7_565 ?
P2 P3 C13 C14 50.5(2) 7_565 . . 7_565 ?
Ga1 P3 C13 C14 -97.9(2) . . . 7_565 ?
P2 P3 C13 C14 -50.5(2) . . . . ?
P2 P3 C13 C14 -113.6(2) 7_565 . . . ?
Ga1 P3 C13 C14 97.9(2) . . . . ?
C14 C13 C14 C15 -10.9(4) 7_565 . . . ?
P3 C13 C14 C15 153.0(2) . . . . ?
C14 C13 C14 C17 163.07(18) 7_565 . . . ?
P3 C13 C14 C17 -33.0(4) . . . . ?
C13 C14 C15 C16 2.4(4) . . . . ?
C17 C14 C15 C16 -172.4(3) . . . . ?
C14 C15 C16 C15 5.7(5) . . . 7_565 ?
C14 C15 C16 C21 -179.6(3) . . . . ?
C15 C14 C17 C18 171.2(2) . . . . ?
C13 C14 C17 C18 -2.9(4) . . . . ?
C15 C14 C17 C20 -63.9(3) . . . . ?
C13 C14 C17 C20 122.1(3) . . . . ?
C15 C14 C17 C19 55.5(3) . . . . ?
C13 C14 C17 C19 -118.6(3) . . . . ?
C15 C16 C21 C22 -175.8(6) 7_565 . . 7_565 ?
C15 C16 C21 C22 9.7(7) . . . 7_565 ?
C15 C16 C21 C22 -9.7(7) 7_565 . . . ?
C15 C16 C21 C22 175.8(6) . . . . ?
C15 C16 C21 C24 -129.9(5) 7_565 . . . ?
C15 C16 C21 C24 55.6(6) . . . . ?
C15 C16 C21 C24 -55.6(6) 7_565 . . 7_565 ?
C15 C16 C21 C24 129.9(5) . . . 7_565 ?
C15 C16 C21 C23 61.5(5) 7_565 . . 7_565 ?
C15 C16 C21 C23 -113.0(5) . . . 7_565 ?
C15 C16 C21 C23 113.0(5) 7_565 . . . ?
C15 C16 C21 C23 -61.5(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.088
####################################################################### 
# 
# 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_jb54_endo_exo_MesP4Mes_GaCl3_toluene
_database_code_depnum_ccdc_archive 'CCDC 1413824'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H58 Cl3 Ga P4, C7 H8'
_chemical_formula_sum            'C43 H66 Cl3 Ga P4'
_chemical_formula_weight         882.91

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/m'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_Int_Tables_number      11

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

_cell_length_a                   13.2689(4)
_cell_length_b                   12.9252(5)
_cell_length_c                   14.1556(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.676(2)
_cell_angle_gamma                90.00
_cell_volume                     2427.56(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9963
_cell_measurement_theta_min      5.277
_cell_measurement_theta_max      62.474

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             932
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6354
_exptl_absorpt_correction_T_max  0.8561
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48175
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         33.50
_reflns_number_total             9856
_reflns_number_gt                6949
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker Apex V7.51A'
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms were positioned geometrically and refined using a riding model, 
 with C---H = 0.98 (methyl groups), 0.99Å (methylene groups), 
 1.00Å (methine groups) or 0.95 Å (aryl CH) and with Uiso(H) = 
 1.5 times Ueq(C) (methyl groups) or with Uiso(H) = 1.2 times 
 Ueq(C) (methylene  groups, aryl CH, methine groups). Torsion angles 
 of all methyl groups (except C31b) were allowed to refine. The Uij of the atom 
 pairs in the disordered toluene molecule were restrained to be equal.
 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0374P)²+0.6528P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9856
_refine_ls_number_parameters     311
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.0945
_refine_ls_wR_factor_gt          0.0823
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.09357(3) 0.7500 0.30415(3) 0.01896(10) Uani 1 2 d S . .
P2 P 0.09967(3) 0.66461(3) 0.17108(2) 0.02405(8) Uani 1 1 d . . .
P3 P 0.24397(4) 0.7500 0.14838(3) 0.02136(10) Uani 1 2 d S . .
Ga1 Ga -0.080683(16) 0.7500 0.346794(15) 0.02321(6) Uani 1 2 d S . .
Cl1 Cl -0.10213(4) 0.7500 0.49746(4) 0.03331(12) Uani 1 2 d S . .
Cl2 Cl -0.14194(3) 0.61276(4) 0.28132(4) 0.05081(13) Uani 1 1 d . . .
C1 C 0.21423(13) 0.7500 0.36711(12) 0.0208(4) Uani 1 2 d S . .
C2 C 0.26631(10) 0.65496(12) 0.37585(9) 0.0260(3) Uani 1 1 d . . .
C3 C 0.37106(11) 0.65879(15) 0.36758(11) 0.0355(4) Uani 1 1 d . . .
H3 H 0.4078 0.5957 0.3702 0.043 Uiso 1 1 calc R . .
C4 C 0.42382(15) 0.7500 0.35576(15) 0.0362(6) Uani 1 2 d S . .
C5 C 0.21936(12) 0.54996(13) 0.40145(11) 0.0332(3) Uani 1 1 d . . .
C6 C 0.10667(12) 0.55336(14) 0.42346(13) 0.0372(4) Uani 1 1 d . . .
H6A H 0.0680 0.5621 0.3646 0.056 Uiso 1 1 calc R . .
H6B H 0.0931 0.6116 0.4658 0.056 Uiso 1 1 calc R . .
H6C H 0.0868 0.4886 0.4540 0.056 Uiso 1 1 calc R . .
C7 C 0.23683(16) 0.46855(15) 0.32495(15) 0.0502(5) Uani 1 1 d . . .
H7A H 0.2155 0.4006 0.3481 0.075 Uiso 1 1 calc R . .
H7B H 0.3086 0.4663 0.3096 0.075 Uiso 1 1 calc R . .
H7C H 0.1976 0.4865 0.2682 0.075 Uiso 1 1 calc R . .
C8 C 0.27234(16) 0.51431(19) 0.49382(14) 0.0571(6) Uani 1 1 d . . .
H8A H 0.2433 0.4485 0.5144 0.086 Uiso 1 1 calc R . .
H8B H 0.2628 0.5667 0.5430 0.086 Uiso 1 1 calc R . .
H8C H 0.3445 0.5052 0.4825 0.086 Uiso 1 1 calc R . .
C9 C 0.53654(17) 0.7500 0.33225(19) 0.0509(8) Uani 1 2 d S . .
C10 C 0.5541(3) 0.7001(5) 0.2443(4) 0.088(2) Uani 0.50 1 d P . .
H10A H 0.5139 0.7339 0.1946 0.133 Uiso 0.50 1 calc PR . .
H10B H 0.5346 0.6272 0.2488 0.133 Uiso 0.50 1 calc PR . .
H10C H 0.6257 0.7049 0.2290 0.133 Uiso 0.50 1 calc PR . .
C11 C 0.5967(3) 0.7295(11) 0.4157(4) 0.105(5) Uani 0.50 1 d P . .
H11A H 0.5879 0.6572 0.4347 0.157 Uiso 0.50 1 calc PR . .
H11B H 0.5752 0.7750 0.4670 0.157 Uiso 0.50 1 calc PR . .
H11C H 0.6678 0.7424 0.4021 0.157 Uiso 0.50 1 calc PR . .
C12 C 0.5726(3) 0.8747(4) 0.3114(4) 0.0563(12) Uani 0.50 1 d P . .
H12A H 0.6429 0.8757 0.2908 0.085 Uiso 0.50 1 calc PR . .
H12B H 0.5663 0.9153 0.3695 0.085 Uiso 0.50 1 calc PR . .
H12C H 0.5294 0.9046 0.2619 0.085 Uiso 0.50 1 calc PR . .
C13 C 0.23597(15) 0.7500 0.01685(13) 0.0229(4) Uani 1 2 d S . .
C14 C 0.22209(11) 0.65528(12) -0.03236(9) 0.0262(3) Uani 1 1 d . . .
C15 C 0.17064(12) 0.65867(13) -0.11921(10) 0.0296(3) Uani 1 1 d . . .
H15 H 0.1576 0.5955 -0.1514 0.036 Uiso 1 1 calc R . .
C16 C 0.13798(17) 0.7500 -0.16027(14) 0.0297(4) Uani 1 2 d S . .
C17 C 0.26505(12) 0.54796(13) -0.00355(10) 0.0315(3) Uani 1 1 d . . .
C18 C 0.33892(14) 0.55053(14) 0.08089(11) 0.0387(4) Uani 1 1 d . . .
H18A H 0.3019 0.5654 0.1388 0.058 Uiso 1 1 calc R . .
H18B H 0.3895 0.6046 0.0708 0.058 Uiso 1 1 calc R . .
H18C H 0.3725 0.4833 0.0869 0.058 Uiso 1 1 calc R . .
C19 C 0.32816(15) 0.50734(16) -0.08721(12) 0.0436(4) Uani 1 1 d . . .
H19A H 0.3580 0.4404 -0.0704 0.065 Uiso 1 1 calc R . .
H19B H 0.3819 0.5569 -0.1011 0.065 Uiso 1 1 calc R . .
H19C H 0.2845 0.4991 -0.1430 0.065 Uiso 1 1 calc R . .
C20 C 0.18103(15) 0.46921(14) 0.01440(13) 0.0426(4) Uani 1 1 d . . .
H20A H 0.2109 0.4015 0.0285 0.064 Uiso 1 1 calc R . .
H20B H 0.1377 0.4638 -0.0419 0.064 Uiso 1 1 calc R . .
H20C H 0.1408 0.4920 0.0681 0.064 Uiso 1 1 calc R . .
C21 C 0.07161(19) 0.7500 -0.24952(15) 0.0362(5) Uani 1 2 d S . .
C22 C 0.1312(4) 0.6988(4) -0.3305(2) 0.0614(12) Uani 0.50 1 d P . .
H22A H 0.1515 0.6288 -0.3117 0.092 Uiso 0.50 1 calc PR . .
H22B H 0.1914 0.7401 -0.3438 0.092 Uiso 0.50 1 calc PR . .
H22C H 0.0885 0.6952 -0.3874 0.092 Uiso 0.50 1 calc PR . .
C23 C -0.0206(4) 0.6817(5) -0.2310(4) 0.0776(18) Uani 0.50 1 d P . .
H23A H -0.0663 0.6840 -0.2858 0.116 Uiso 0.50 1 calc PR . .
H23B H -0.0558 0.7072 -0.1751 0.116 Uiso 0.50 1 calc PR . .
H23C H 0.0013 0.6102 -0.2201 0.116 Uiso 0.50 1 calc PR . .
C24 C 0.0409(5) 0.8535(4) -0.2810(3) 0.0703(16) Uani 0.50 1 d P . .
H24A H -0.0040 0.8475 -0.3362 0.106 Uiso 0.50 1 calc PR . .
H24B H 0.1007 0.8936 -0.2980 0.106 Uiso 0.50 1 calc PR . .
H24C H 0.0054 0.8887 -0.2299 0.106 Uiso 0.50 1 calc PR . .
C25A C 0.5029(12) 0.2500 0.2520(12) 0.083(2) Uani 0.82(6) 2 d SPD A 1
C26A C 0.4022(12) 0.2500 0.2603(13) 0.065(2) Uani 0.82(6) 2 d SPD A 1
H26A H 0.3735 0.2500 0.3215 0.078 Uiso 0.82(6) 2 calc SPR A 1
C27A C 0.3417(10) 0.2500 0.1843(15) 0.069(3) Uani 0.82(6) 2 d SPD A 1
H27A H 0.2705 0.2500 0.1906 0.082 Uiso 0.82(6) 2 calc SPR A 1
C28A C 0.3862(10) 0.2500 0.0943(13) 0.078(2) Uani 0.82(6) 2 d SPD A 1
H28A H 0.3449 0.2500 0.0390 0.094 Uiso 0.82(6) 2 calc SPR A 1
C29A C 0.4884(10) 0.2500 0.0867(11) 0.081(2) Uani 0.82(6) 2 d SPD A 1
H29A H 0.5190 0.2500 0.0263 0.097 Uiso 0.82(6) 2 calc SPR A 1
C30A C 0.5469(11) 0.2500 0.1676(11) 0.098(3) Uani 0.82(6) 2 d SPD A 1
H30A H 0.6183 0.2500 0.1635 0.117 Uiso 0.82(6) 2 calc SPR A 1
C31A C 0.5709(16) 0.2500 0.3410(12) 0.190(5) Uani 0.82(6) 2 d SPD A 1
H31A H 0.6341 0.2141 0.3274 0.285 Uiso 0.41(3) 1 calc PR A 1
H31B H 0.5363 0.2144 0.3925 0.285 Uiso 0.41(3) 1 calc PR A 1
H31C H 0.5854 0.3215 0.3598 0.285 Uiso 0.41(3) 1 calc PR A 1
C25B C 0.480(4) 0.2500 0.235(4) 0.083(2) Uani 0.18(6) 2 d SPD A 2
C26B C 0.379(4) 0.2500 0.237(4) 0.065(2) Uani 0.18(6) 2 d SPD A 2
H26B H 0.3466 0.2500 0.2961 0.078 Uiso 0.18(6) 2 calc SPR A 2
C27B C 0.324(3) 0.2500 0.157(5) 0.069(3) Uani 0.18(6) 2 d SPD A 2
H27B H 0.2526 0.2500 0.1592 0.082 Uiso 0.18(6) 2 calc SPR A 2
C28B C 0.375(4) 0.2500 0.070(4) 0.078(2) Uani 0.18(6) 2 d SPD A 2
H28B H 0.3372 0.2500 0.0124 0.094 Uiso 0.18(6) 2 calc SPR A 2
C29B C 0.477(4) 0.2500 0.069(4) 0.081(2) Uani 0.18(6) 2 d SPD A 2
H29B H 0.5118 0.2500 0.0104 0.097 Uiso 0.18(6) 2 calc SPR A 2
C30B C 0.530(3) 0.2500 0.153(4) 0.098(3) Uani 0.18(6) 2 d SPD A 2
H30B H 0.6016 0.2500 0.1531 0.117 Uiso 0.18(6) 2 calc SPR A 2
C31B C 0.543(6) 0.2500 0.327(4) 0.190(5) Uani 0.18(6) 2 d SPD A 2
H31D H 0.6151 0.2500 0.3118 0.285 Uiso 0.18(6) 2 calc SPR A 2
H31E H 0.5272 0.1881 0.3638 0.285 Uiso 0.09(3) 1 calc PR A 2
H31F H 0.5272 0.3119 0.3638 0.285 Uiso 0.09(3) 1 calc PR A 2


#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 1.8232(18) . ?
P1 P2 2.1854(5) . ?
P1 P2 2.1854(5) 4_575 ?
P1 Ga1 2.3966(5) . ?
P2 P2 2.2074(8) 4_575 ?
P2 P3 2.2365(6) . ?
P3 C13 1.8637(18) . ?
P3 P2 2.2365(6) 4_575 ?
Ga1 Cl1 2.1550(5) . ?
Ga1 Cl2 2.1560(5) . ?
Ga1 Cl2 2.1560(5) 4_575 ?
C1 C2 1.4142(17) 4_575 ?
C1 C2 1.4141(17) . ?
C2 C3 1.397(2) . ?
C2 C5 1.538(2) . ?
C3 C4 1.382(2) . ?
C3 H3 0.9500 . ?
C4 C3 1.382(2) 4_575 ?
C4 C9 1.536(3) . ?
C5 C7 1.529(3) . ?
C5 C6 1.532(2) . ?
C5 C8 1.547(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.424(5) . ?
C9 C10 1.424(5) 4_575 ?
C9 C11 1.442(5) 4_575 ?
C9 C11 1.442(5) . ?
C9 C12 1.708(5) . ?
C9 C12 1.708(5) 4_575 ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.4196(17) . ?
C13 C14 1.4196(17) 4_575 ?
C14 C15 1.3998(19) . ?
C14 C17 1.552(2) . ?
C15 C16 1.3831(19) . ?
C15 H15 0.9500 . ?
C16 C15 1.3831(19) 4_575 ?
C16 C21 1.532(3) . ?
C17 C20 1.533(3) . ?
C17 C18 1.537(2) . ?
C17 C19 1.550(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C24 1.467(5) 4_575 ?
C21 C24 1.467(5) . ?
C21 C23 1.534(5) . ?
C21 C23 1.534(5) 4_575 ?
C21 C22 1.549(5) . ?
C21 C22 1.549(5) 4_575 ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25A C30A 1.336(7) . ?
C25A C26A 1.342(6) . ?
C25A C31A 1.541(8) . ?
C26A C27A 1.336(6) . ?
C26A H26A 0.9500 . ?
C27A C28A 1.411(7) . ?
C27A H27A 0.9500 . ?
C28A C29A 1.362(7) . ?
C28A H28A 0.9500 . ?
C29A C30A 1.376(7) . ?
C29A H29A 0.9500 . ?
C30A H30A 0.9500 . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C25B C30B 1.337(10) . ?
C25B C26B 1.339(10) . ?
C25B C31B 1.543(11) . ?
C26B C27B 1.339(10) . ?
C26B H26B 0.9500 . ?
C27B C28B 1.410(10) . ?
C27B H27B 0.9500 . ?
C28B C29B 1.361(10) . ?
C28B H28B 0.9500 . ?
C29B C30B 1.376(11) . ?
C29B H29B 0.9500 . ?
C30B H30B 0.9500 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 P2 112.34(5) . . ?
C1 P1 P2 112.34(5) . 4_575 ?
P2 P1 P2 60.67(2) . 4_575 ?
C1 P1 Ga1 136.15(6) . . ?
P2 P1 Ga1 105.23(2) . . ?
P2 P1 Ga1 105.23(2) 4_575 . ?
P1 P2 P2 59.667(12) . 4_575 ?
P1 P2 P3 85.13(2) . . ?
P2 P2 P3 60.429(12) 4_575 . ?
C13 P3 P2 96.02(6) . . ?
C13 P3 P2 96.02(6) . 4_575 ?
P2 P3 P2 59.14(2) . 4_575 ?
Cl1 Ga1 Cl2 111.835(17) . . ?
Cl1 Ga1 Cl2 111.835(17) . 4_575 ?
Cl2 Ga1 Cl2 110.72(3) . 4_575 ?
Cl1 Ga1 P1 112.85(2) . . ?
Cl2 Ga1 P1 104.575(15) . . ?
Cl2 Ga1 P1 104.574(15) 4_575 . ?
C2 C1 C2 120.61(17) 4_575 . ?
C2 C1 P1 117.91(9) 4_575 . ?
C2 C1 P1 117.91(9) . . ?
C3 C2 C1 116.58(15) . . ?
C3 C2 C5 117.20(14) . . ?
C1 C2 C5 126.02(13) . . ?
C4 C3 C2 123.10(16) . . ?
C4 C3 H3 118.4 . . ?
C2 C3 H3 118.4 . . ?
C3 C4 C3 117.05(19) 4_575 . ?
C3 C4 C9 121.47(10) 4_575 . ?
C3 C4 C9 121.47(10) . . ?
C7 C5 C6 108.68(16) . . ?
C7 C5 C2 112.02(13) . . ?
C6 C5 C2 114.94(13) . . ?
C7 C5 C8 108.80(16) . . ?
C6 C5 C8 105.76(14) . . ?
C2 C5 C8 106.29(15) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C10 53.9(6) . 4_575 ?
C10 C9 C11 134.8(4) . 4_575 ?
C10 C9 C11 122.6(5) 4_575 4_575 ?
C10 C9 C11 122.6(5) . . ?
C10 C9 C11 134.8(4) 4_575 . ?
C11 C9 C11 21.2(12) 4_575 . ?
C10 C9 C4 111.0(2) . . ?
C10 C9 C4 111.0(2) 4_575 . ?
C11 C9 C4 110.7(3) 4_575 . ?
C11 C9 C4 110.7(3) . . ?
C10 C9 C12 103.1(4) . . ?
C10 C9 C12 51.1(3) 4_575 . ?
C11 C9 C12 79.3(6) 4_575 . ?
C11 C9 C12 99.3(6) . . ?
C4 C9 C12 108.25(15) . . ?
C10 C9 C12 51.1(3) . 4_575 ?
C10 C9 C12 103.1(4) 4_575 4_575 ?
C11 C9 C12 99.3(6) 4_575 4_575 ?
C11 C9 C12 79.3(6) . 4_575 ?
C4 C9 C12 108.25(15) . 4_575 ?
C12 C9 C12 141.3(3) . 4_575 ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C14 119.19(17) . 4_575 ?
C14 C13 P3 119.72(9) . . ?
C14 C13 P3 119.72(8) 4_575 . ?
C15 C14 C13 117.58(14) . . ?
C15 C14 C17 115.63(13) . . ?
C13 C14 C17 126.63(13) . . ?
C16 C15 C14 122.88(15) . . ?
C16 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
C15 C16 C15 117.18(19) 4_575 . ?
C15 C16 C21 121.39(9) 4_575 . ?
C15 C16 C21 121.39(9) . . ?
C20 C17 C18 110.11(14) . . ?
C20 C17 C19 107.59(14) . . ?
C18 C17 C19 104.84(14) . . ?
C20 C17 C14 111.80(13) . . ?
C18 C17 C14 114.44(13) . . ?
C19 C17 C14 107.57(13) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C24 C21 C24 131.7(4) 4_575 . ?
C24 C21 C16 113.93(17) 4_575 . ?
C24 C21 C16 113.93(17) . . ?
C24 C21 C23 46.2(3) 4_575 . ?
C24 C21 C23 111.0(4) . . ?
C16 C21 C23 108.1(2) . . ?
C24 C21 C23 111.0(4) 4_575 4_575 ?
C24 C21 C23 46.2(3) . 4_575 ?
C16 C21 C23 108.1(2) . 4_575 ?
C23 C21 C23 70.3(5) . 4_575 ?
C24 C21 C22 61.8(3) 4_575 . ?
C24 C21 C22 107.9(3) . . ?
C16 C21 C22 108.5(2) . . ?
C23 C21 C22 107.2(3) . . ?
C23 C21 C22 142.0(3) 4_575 . ?
C24 C21 C22 107.9(3) 4_575 4_575 ?
C24 C21 C22 61.8(3) . 4_575 ?
C16 C21 C22 108.5(2) . 4_575 ?
C23 C21 C22 142.0(3) . 4_575 ?
C23 C21 C22 107.2(3) 4_575 4_575 ?
C22 C21 C22 50.6(4) . 4_575 ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30A C25A C26A 121.6(5) . . ?
C30A C25A C31A 118.2(5) . . ?
C26A C25A C31A 120.1(5) . . ?
C27A C26A C25A 121.3(5) . . ?
C27A C26A H26A 119.4 . . ?
C25A C26A H26A 119.4 . . ?
C26A C27A C28A 118.3(4) . . ?
C26A C27A H27A 120.9 . . ?
C28A C27A H27A 120.9 . . ?
C29A C28A C27A 119.9(5) . . ?
C29A C28A H28A 120.0 . . ?
C27A C28A H28A 120.0 . . ?
C28A C29A C30A 119.1(5) . . ?
C28A C29A H29A 120.4 . . ?
C30A C29A H29A 120.4 . . ?
C25A C30A C29A 119.8(5) . . ?
C25A C30A H30A 120.1 . . ?
C29A C30A H30A 120.1 . . ?
C30B C25B C26B 121.6(12) . . ?
C30B C25B C31B 117.7(13) . . ?
C26B C25B C31B 120.7(13) . . ?
C25B C26B C27B 121.2(12) . . ?
C25B C26B H26B 119.4 . . ?
C27B C26B H26B 119.4 . . ?
C26B C27B C28B 118.4(12) . . ?
C26B C27B H27B 120.8 . . ?
C28B C27B H27B 120.8 . . ?
C29B C28B C27B 119.8(12) . . ?
C29B C28B H28B 120.1 . . ?
C27B C28B H28B 120.1 . . ?
C28B C29B C30B 119.2(12) . . ?
C28B C29B H29B 120.4 . . ?
C30B C29B H29B 120.4 . . ?
C25B C30B C29B 119.8(12) . . ?
C25B C30B H30B 120.1 . . ?
C29B C30B H30B 120.1 . . ?
C25B C31B H31D 109.5 . . ?
C25B C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C25B C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 P1 P2 P2 -103.91(4) . . . 4_575 ?
Ga1 P1 P2 P2 99.169(14) . . . 4_575 ?
C1 P1 P2 P3 -45.51(4) . . . . ?
P2 P1 P2 P3 58.400(17) 4_575 . . . ?
Ga1 P1 P2 P3 157.569(14) . . . . ?
P1 P2 P3 C13 -151.12(3) . . . . ?
P2 P2 P3 C13 -93.43(3) 4_575 . . . ?
P1 P2 P3 P2 -57.696(16) . . . 4_575 ?
C1 P1 Ga1 Cl1 0.0 . . . . ?
P2 P1 Ga1 Cl1 148.438(13) . . . . ?
P2 P1 Ga1 Cl1 -148.438(13) 4_575 . . . ?
C1 P1 Ga1 Cl2 -121.778(18) . . . . ?
P2 P1 Ga1 Cl2 26.66(2) . . . . ?
P2 P1 Ga1 Cl2 89.78(2) 4_575 . . . ?
C1 P1 Ga1 Cl2 121.778(18) . . . 4_575 ?
P2 P1 Ga1 Cl2 -89.78(2) . . . 4_575 ?
P2 P1 Ga1 Cl2 -26.66(2) 4_575 . . 4_575 ?
P2 P1 C1 C2 112.53(12) . . . 4_575 ?
P2 P1 C1 C2 46.34(14) 4_575 . . 4_575 ?
Ga1 P1 C1 C2 -100.57(13) . . . 4_575 ?
P2 P1 C1 C2 -46.34(14) . . . . ?
P2 P1 C1 C2 -112.53(12) 4_575 . . . ?
Ga1 P1 C1 C2 100.57(13) . . . . ?
C2 C1 C2 C3 -16.8(3) 4_575 . . . ?
P1 C1 C2 C3 141.49(12) . . . . ?
C2 C1 C2 C5 157.93(12) 4_575 . . . ?
P1 C1 C2 C5 -43.8(2) . . . . ?
C1 C2 C3 C4 2.9(2) . . . . ?
C5 C2 C3 C4 -172.32(16) . . . . ?
C2 C3 C4 C3 10.3(3) . . . 4_575 ?
C2 C3 C4 C9 -170.78(18) . . . . ?
C3 C2 C5 C7 -63.69(19) . . . . ?
C1 C2 C5 C7 121.62(18) . . . . ?
C3 C2 C5 C6 171.63(14) . . . . ?
C1 C2 C5 C6 -3.1(2) . . . . ?
C3 C2 C5 C8 55.02(19) . . . . ?
C1 C2 C5 C8 -119.67(17) . . . . ?
C3 C4 C9 C10 -119.6(4) 4_575 . . . ?
C3 C4 C9 C10 61.5(4) . . . . ?
C3 C4 C9 C10 -61.5(4) 4_575 . . 4_575 ?
C3 C4 C9 C10 119.6(4) . . . 4_575 ?
C3 C4 C9 C11 78.1(7) 4_575 . . 4_575 ?
C3 C4 C9 C11 -100.8(6) . . . 4_575 ?
C3 C4 C9 C11 100.8(6) 4_575 . . . ?
C3 C4 C9 C11 -78.1(7) . . . . ?
C3 C4 C9 C12 -7.1(3) 4_575 . . . ?
C3 C4 C9 C12 174.0(2) . . . . ?
C3 C4 C9 C12 -174.0(2) 4_575 . . 4_575 ?
C3 C4 C9 C12 7.1(3) . . . 4_575 ?
P2 P3 C13 C14 -53.52(15) . . . . ?
P2 P3 C13 C14 -113.03(14) 4_575 . . . ?
P2 P3 C13 C14 113.03(14) . . . 4_575 ?
P2 P3 C13 C14 53.52(15) 4_575 . . 4_575 ?
C14 C13 C14 C15 -16.2(3) 4_575 . . . ?
P3 C13 C14 C15 150.39(13) . . . . ?
C14 C13 C14 C17 158.92(12) 4_575 . . . ?
P3 C13 C14 C17 -34.5(2) . . . . ?
C13 C14 C15 C16 3.3(3) . . . . ?
C17 C14 C15 C16 -172.35(17) . . . . ?
C14 C15 C16 C15 9.2(3) . . . 4_575 ?
C14 C15 C16 C21 -172.94(18) . . . . ?
C15 C14 C17 C20 -65.86(18) . . . . ?
C13 C14 C17 C20 118.90(18) . . . . ?
C15 C14 C17 C18 168.09(14) . . . . ?
C13 C14 C17 C18 -7.1(2) . . . . ?
C15 C14 C17 C19 52.05(18) . . . . ?
C13 C14 C17 C19 -123.18(18) . . . . ?
C15 C16 C21 C24 -177.7(4) 4_575 . . 4_575 ?
C15 C16 C21 C24 4.6(4) . . . 4_575 ?
C15 C16 C21 C24 -4.6(4) 4_575 . . . ?
C15 C16 C21 C24 177.7(4) . . . . ?
C15 C16 C21 C23 -128.4(3) 4_575 . . . ?
C15 C16 C21 C23 53.9(4) . . . . ?
C15 C16 C21 C23 -53.9(4) 4_575 . . 4_575 ?
C15 C16 C21 C23 128.4(3) . . . 4_575 ?
C15 C16 C21 C22 115.6(3) 4_575 . . . ?
C15 C16 C21 C22 -62.1(3) . . . . ?
C15 C16 C21 C22 62.1(3) 4_575 . . 4_575 ?
C15 C16 C21 C22 -115.6(3) . . . 4_575 ?
C30A C25A C26A C27A 0.0 . . . . ?
C31A C25A C26A C27A 180.000(1) . . . . ?
C25A C26A C27A C28A 0.000(1) . . . . ?
C26A C27A C28A C29A 0.000(1) . . . . ?
C27A C28A C29A C30A 0.0 . . . . ?
C26A C25A C30A C29A 0.000(1) . . . . ?
C31A C25A C30A C29A 180.000(2) . . . . ?
C28A C29A C30A C25A 0.0 . . . . ?
C30B C25B C26B C27B 0.000(3) . . . . ?
C31B C25B C26B C27B 180.000(3) . . . . ?
C25B C26B C27B C28B 0.000(4) . . . . ?
C26B C27B C28B C29B 0.000(4) . . . . ?
C27B C28B C29B C30B 0.0 . . . . ?
C26B C25B C30B C29B 0.000(3) . . . . ?
C31B C25B C30B C29B 180.000(5) . . . . ?
C28B C29B C30B C25B 0.000(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        33.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.065
####################################################################### 
# 
# 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_jb73_2_endo_exo_MesP4Mes_GaCl3_CH2Cl2
_database_code_depnum_ccdc_archive 'CCDC 1413825'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;

_vrf_CHEMW03_jb73_2_endo_exo_MesP4Mes_GaCl3_CH2Cl2 
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: PLATON/SQUEEZE was used to treat three heavily disordered 
dichloromethane molecules in the unit cell. These were removed from the 
model, but included in the empirical formula. Additional PLATON/SQUEEZE 
details appear in _refine_special_details.
;
_vrf_PLAT051_jb73_2_endo_exo_MesP4Mes_GaCl3_CH2Cl2 
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      16.05 %    
RESPONSE: PLATON/SQUEEZE was used to treat three heavily disordered 
dichloromethane molecules in the unit cell. These were removed from the 
model, but included in the empirical formula. Additional PLATON/SQUEEZE 
details appear in _refine_special_details.
;
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H58 Cl3 Ga P4, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C37.50 H61 Cl6 Ga P4'
_chemical_formula_weight         918.16

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/m'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_Int_Tables_number      11

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

_cell_length_a                   13.3333(4)
_cell_length_b                   12.9538(4)
_cell_length_c                   14.1349(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.834(2)
_cell_angle_gamma                90.00
_cell_volume                     2440.09(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9971
_cell_measurement_theta_min      5.194
_cell_measurement_theta_max      64.808

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             958
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6225
_exptl_absorpt_correction_T_max  0.7510
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43086
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         32.00
_reflns_number_total             8787
_reflns_number_gt                7521
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker Apex v2.0-2'
_computing_cell_refinement       'Bruker Apex v2.0-2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms  were positioned geometrically and refined using a 
 riding model , with C---H = 0.98 (methyl groups), 0.99Å (methylene groups), 
 1.00Å (methine groups) or 0.95 Å (aryl CH) and with Uiso(H) = 
 1.5 times Ueq(C) (methyl groups) or with Uiso(H) = 1.2 times 
 Ueq(C) (methylene  groups, aryl CH, methine groups). Torsion angles 
 of all methyl groups were allowed to refine.
 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.578 0.250 0.696 263 57 ' '
2 0.422 0.750 0.304 263 57 ' '
_platon_squeeze_details          
;
The unit cell contains three dichloromethane molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0394P)²+0.0339P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8787
_refine_ls_number_parameters     256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0726
_refine_ls_wR_factor_gt          0.0710
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.24910(2) 0.2500 0.36174(2) 0.02374(7) Uani 1 2 d S . .
P2 P 0.104957(17) 0.335274(17) 0.335524(16) 0.02524(5) Uani 1 1 d . . .
P3 P 0.09508(2) 0.2500 0.20195(2) 0.01988(6) Uani 1 2 d S . .
Ga1 Ga -0.079568(9) 0.2500 0.155267(9) 0.02386(4) Uani 1 2 d S . .
Cl1 Cl -0.10272(3) 0.2500 0.00349(2) 0.03360(7) Uani 1 2 d S . .
Cl2 Cl -0.13959(2) 0.38710(2) 0.21978(2) 0.04639(7) Uani 1 1 d . . .
C1 C 0.24029(9) 0.2500 0.49335(8) 0.0253(2) Uani 1 2 d S . .
C2 C 0.22500(7) 0.34441(7) 0.54178(6) 0.02790(17) Uani 1 1 d . . .
C3 C 0.17039(8) 0.34158(7) 0.62465(7) 0.03106(19) Uani 1 1 d . . .
H3 H 0.1564 0.4047 0.6558 0.037 Uiso 1 1 calc R . .
C4 C 0.13573(11) 0.2500 0.66329(9) 0.0304(3) Uani 1 2 d S . .
C5 C 0.27147(8) 0.45028(8) 0.51668(7) 0.0357(2) Uani 1 1 d . . .
C6 C 0.34479(9) 0.44665(9) 0.43514(8) 0.0439(3) Uani 1 1 d . . .
H6A H 0.3072 0.4360 0.3752 0.066 Uiso 1 1 calc R . .
H6B H 0.3922 0.3897 0.4456 0.066 Uiso 1 1 calc R . .
H6C H 0.3817 0.5120 0.4326 0.066 Uiso 1 1 calc R . .
C7 C 0.19132(11) 0.53248(8) 0.49664(9) 0.0474(3) Uani 1 1 d . . .
H7A H 0.2238 0.5988 0.4844 0.071 Uiso 1 1 calc R . .
H7B H 0.1487 0.5391 0.5516 0.071 Uiso 1 1 calc R . .
H7C H 0.1501 0.5122 0.4411 0.071 Uiso 1 1 calc R . .
C8 C 0.33561(11) 0.48459(11) 0.60448(8) 0.0510(3) Uani 1 1 d . . .
H8A H 0.3861 0.4317 0.6198 0.077 Uiso 1 1 calc R . .
H8B H 0.2921 0.4939 0.6584 0.077 Uiso 1 1 calc R . .
H8C H 0.3692 0.5500 0.5908 0.077 Uiso 1 1 calc R . .
C9 C 0.06598(13) 0.2500 0.74725(11) 0.0396(3) Uani 1 2 d S . .
C10 C 0.1196(3) 0.3056(3) 0.83293(19) 0.0752(10) Uani 0.50 1 d P . .
H10A H 0.1777 0.2648 0.8549 0.113 Uiso 0.50 1 calc PR . .
H10B H 0.0727 0.3129 0.8845 0.113 Uiso 0.50 1 calc PR . .
H10C H 0.1421 0.3741 0.8132 0.113 Uiso 0.50 1 calc PR . .
C11 C -0.0241(3) 0.3185(4) 0.7217(3) 0.0929(14) Uani 0.50 1 d P . .
H11A H -0.0651 0.2855 0.6715 0.139 Uiso 0.50 1 calc PR . .
H11B H -0.0005 0.3857 0.6995 0.139 Uiso 0.50 1 calc PR . .
H11C H -0.0645 0.3284 0.7777 0.139 Uiso 0.50 1 calc PR . .
C12 C 0.0381(3) 0.1469(2) 0.7805(2) 0.0651(9) Uani 0.50 1 d P . .
H12A H 0.0989 0.1077 0.7975 0.098 Uiso 0.50 1 calc PR . .
H12B H 0.0002 0.1106 0.7301 0.098 Uiso 0.50 1 calc PR . .
H12C H -0.0035 0.1535 0.8362 0.098 Uiso 0.50 1 calc PR . .
C13 C 0.21298(8) 0.2500 0.13950(8) 0.0195(2) Uani 1 2 d S . .
C14 C 0.26468(6) 0.34486(6) 0.13028(6) 0.02291(15) Uani 1 1 d . . .
C15 C 0.36924(6) 0.34140(7) 0.13589(7) 0.02831(18) Uani 1 1 d . . .
H15 H 0.4054 0.4045 0.1327 0.034 Uiso 1 1 calc R . .
C16 C 0.42294(9) 0.2500 0.14588(9) 0.0293(3) Uani 1 2 d S . .
C17 C 0.21671(7) 0.45069(7) 0.10612(7) 0.02843(17) Uani 1 1 d . . .
C18 C 0.10345(7) 0.44765(8) 0.08479(8) 0.0348(2) Uani 1 1 d . . .
H18A H 0.0878 0.3911 0.0407 0.052 Uiso 1 1 calc R . .
H18B H 0.0819 0.5133 0.0563 0.052 Uiso 1 1 calc R . .
H18C H 0.0682 0.4366 0.1437 0.052 Uiso 1 1 calc R . .
C19 C 0.23892(9) 0.53018(8) 0.18442(9) 0.0424(2) Uani 1 1 d . . .
H19A H 0.2040 0.5103 0.2416 0.064 Uiso 1 1 calc R . .
H19B H 0.2156 0.5984 0.1633 0.064 Uiso 1 1 calc R . .
H19C H 0.3114 0.5327 0.1984 0.064 Uiso 1 1 calc R . .
C20 C 0.26456(9) 0.48843(10) 0.01435(9) 0.0466(3) Uani 1 1 d . . .
H20A H 0.3368 0.4981 0.0257 0.070 Uiso 1 1 calc R . .
H20B H 0.2340 0.5541 -0.0053 0.070 Uiso 1 1 calc R . .
H20C H 0.2532 0.4370 -0.0357 0.070 Uiso 1 1 calc R . .
C21 C 0.53699(12) 0.241(3) 0.16545(13) 0.035(3) Uani 0.50 1 d P . .
C22 C 0.5574(2) 0.2880(3) 0.2626(2) 0.0734(11) Uani 0.50 1 d P . .
H22A H 0.5357 0.3603 0.2624 0.110 Uiso 0.50 1 calc PR . .
H22B H 0.6295 0.2845 0.2783 0.110 Uiso 0.50 1 calc PR . .
H22C H 0.5204 0.2495 0.3098 0.110 Uiso 1 2 calc SR . .
C23 C 0.58954(18) 0.3006(3) 0.0891(3) 0.0875(14) Uani 0.50 1 d P . .
H23A H 0.5691 0.3732 0.0908 0.131 Uiso 0.50 1 calc PR . .
H23B H 0.5713 0.2711 0.0271 0.131 Uiso 0.50 1 calc PR . .
H23C H 0.6623 0.2957 0.1001 0.131 Uiso 0.50 1 calc PR . .
C24 C 0.57812(17) 0.1303(2) 0.1693(3) 0.0623(8) Uani 0.50 1 d P . .
H24A H 0.5482 0.0931 0.2218 0.093 Uiso 0.50 1 calc PR . .
H24B H 0.6512 0.1321 0.1791 0.093 Uiso 0.50 1 calc PR . .
H24C H 0.5612 0.0950 0.1096 0.093 Uiso 0.50 1 calc PR . .


#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 1.8678(12) . ?
P1 P2 2.2373(4) 4_565 ?
P1 P2 2.2373(4) . ?
P2 P3 2.1878(3) . ?
P2 P2 2.2092(5) 4_565 ?
P3 C13 1.8273(11) . ?
P3 P2 2.1878(3) 4_565 ?
P3 Ga1 2.3999(3) . ?
Ga1 Cl1 2.1576(4) . ?
Ga1 Cl2 2.1617(3) 4_565 ?
Ga1 Cl2 2.1617(3) . ?
C1 C2 1.4195(11) . ?
C1 C2 1.4195(11) 4_565 ?
C2 C3 1.3994(13) . ?
C2 C5 1.5507(13) . ?
C3 C4 1.3912(12) . ?
C3 H3 0.9500 . ?
C4 C3 1.3912(12) 4_565 ?
C4 C9 1.531(2) . ?
C5 C7 1.5286(17) . ?
C5 C6 1.5357(15) . ?
C5 C8 1.5496(15) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C12 1.468(3) 4_565 ?
C9 C12 1.468(3) . ?
C9 C11 1.528(4) 4_565 ?
C9 C11 1.528(4) . ?
C9 C10 1.562(3) . ?
C9 C10 1.562(3) 4_565 ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.4170(10) 4_565 ?
C13 C14 1.4170(10) . ?
C14 C15 1.3946(12) . ?
C14 C17 1.5463(12) . ?
C15 C16 1.3886(11) . ?
C15 H15 0.9500 . ?
C16 C15 1.3886(11) 4_565 ?
C16 C21 1.541(3) 4_565 ?
C16 C21 1.541(3) . ?
C17 C18 1.5310(13) . ?
C17 C19 1.5336(14) . ?
C17 C20 1.5433(14) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C21 0.22(7) 4_565 ?
C21 C23 1.413(15) 4_565 ?
C21 C22 1.443(10) 4_565 ?
C21 C23 1.513(19) . ?
C21 C22 1.517(15) . ?
C21 C24 1.54(3) . ?
C21 C24 1.75(4) 4_565 ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 P2 94.81(4) . 4_565 ?
C1 P1 P2 94.81(4) . . ?
P2 P1 P2 59.170(14) 4_565 . ?
P3 P2 P2 59.675(7) . 4_565 ?
P3 P2 P1 85.487(12) . . ?
P2 P2 P1 60.415(7) 4_565 . ?
C13 P3 P2 112.83(3) . . ?
C13 P3 P2 112.83(3) . 4_565 ?
P2 P3 P2 60.649(14) . 4_565 ?
C13 P3 Ga1 135.18(4) . . ?
P2 P3 Ga1 105.567(12) . . ?
P2 P3 Ga1 105.567(12) 4_565 . ?
Cl1 Ga1 Cl2 112.107(10) . 4_565 ?
Cl1 Ga1 Cl2 112.107(10) . . ?
Cl2 Ga1 Cl2 110.487(19) 4_565 . ?
Cl1 Ga1 P3 112.336(13) . . ?
Cl2 Ga1 P3 104.659(9) 4_565 . ?
Cl2 Ga1 P3 104.659(9) . . ?
C2 C1 C2 119.00(11) . 4_565 ?
C2 C1 P1 119.66(5) . . ?
C2 C1 P1 119.66(5) 4_565 . ?
C3 C2 C1 117.89(8) . . ?
C3 C2 C5 115.92(8) . . ?
C1 C2 C5 125.95(9) . . ?
C4 C3 C2 122.63(9) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C3 C4 C3 117.02(12) 4_565 . ?
C3 C4 C9 121.47(6) 4_565 . ?
C3 C4 C9 121.47(6) . . ?
C7 C5 C6 109.90(9) . . ?
C7 C5 C8 108.26(10) . . ?
C6 C5 C8 105.17(9) . . ?
C7 C5 C2 112.10(9) . . ?
C6 C5 C2 114.41(8) . . ?
C8 C5 C2 106.54(8) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C12 C9 C12 131.0(2) 4_565 . ?
C12 C9 C11 113.5(3) 4_565 4_565 ?
C12 C9 C11 48.8(2) . 4_565 ?
C12 C9 C11 48.8(2) 4_565 . ?
C12 C9 C11 113.5(3) . . ?
C11 C9 C11 71.1(4) 4_565 . ?
C12 C9 C4 114.52(12) 4_565 . ?
C12 C9 C4 114.52(12) . . ?
C11 C9 C4 108.02(16) 4_565 . ?
C11 C9 C4 108.02(16) . . ?
C12 C9 C10 56.4(2) 4_565 . ?
C12 C9 C10 106.6(2) . . ?
C11 C9 C10 142.0(2) 4_565 . ?
C11 C9 C10 104.6(3) . . ?
C4 C9 C10 109.07(16) . . ?
C12 C9 C10 106.6(2) 4_565 4_565 ?
C12 C9 C10 56.4(2) . 4_565 ?
C11 C9 C10 104.6(3) 4_565 4_565 ?
C11 C9 C10 142.0(2) . 4_565 ?
C4 C9 C10 109.07(16) . 4_565 ?
C10 C9 C10 54.9(3) . 4_565 ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C14 120.27(10) 4_565 . ?
C14 C13 P3 118.23(5) 4_565 . ?
C14 C13 P3 118.23(5) . . ?
C15 C14 C13 117.09(8) . . ?
C15 C14 C17 116.53(7) . . ?
C13 C14 C17 126.17(7) . . ?
C16 C15 C14 122.99(8) . . ?
C16 C15 H15 118.5 . . ?
C14 C15 H15 118.5 . . ?
C15 C16 C15 117.01(11) 4_565 . ?
C15 C16 C21 125.6(14) 4_565 4_565 ?
C15 C16 C21 117.3(14) . 4_565 ?
C15 C16 C21 117.3(14) 4_565 . ?
C15 C16 C21 125.6(14) . . ?
C21 C16 C21 8(3) 4_565 . ?
C18 C17 C19 109.02(9) . . ?
C18 C17 C20 105.92(8) . . ?
C19 C17 C20 108.57(9) . . ?
C18 C17 C14 114.78(7) . . ?
C19 C17 C14 111.53(8) . . ?
C20 C17 C14 106.70(8) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C21 C21 C23 112.6(14) 4_565 4_565 ?
C21 C21 C22 105.3(14) 4_565 4_565 ?
C23 C21 C22 122.8(18) 4_565 4_565 ?
C21 C21 C23 59.6(12) 4_565 . ?
C23 C21 C23 53.0(4) 4_565 . ?
C22 C21 C23 137.3(9) 4_565 . ?
C21 C21 C22 66.5(13) 4_565 . ?
C23 C21 C22 139.9(2) 4_565 . ?
C22 C21 C22 38.8(3) 4_565 . ?
C23 C21 C22 111.7(19) . . ?
C21 C21 C24 159.1(5) 4_565 . ?
C23 C21 C24 58.9(12) 4_565 . ?
C22 C21 C24 70.3(13) 4_565 . ?
C23 C21 C24 109.0(9) . . ?
C22 C21 C24 106.6(10) . . ?
C21 C21 C16 85.8(14) 4_565 . ?
C23 C21 C16 113.7(7) 4_565 . ?
C22 C21 C16 110.2(4) 4_565 . ?
C23 C21 C16 108.2(11) . . ?
C22 C21 C16 106.3(9) . . ?
C24 C21 C16 115.0(19) . . ?
C21 C21 C24 18.3(4) 4_565 4_565 ?
C23 C21 C24 103.1(12) 4_565 4_565 ?
C22 C21 C24 99.9(13) 4_565 4_565 ?
C23 C21 C24 52.4(10) . 4_565 ?
C22 C21 C24 63.0(12) . 4_565 ?
C24 C21 C24 140.8(2) . 4_565 ?
C16 C21 C24 104.1(18) . 4_565 ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 P1 P2 P3 -150.22(2) . . . . ?
P2 P1 P2 P3 -57.480(10) 4_565 . . . ?
C1 P1 P2 P2 -92.74(2) . . . 4_565 ?
P2 P2 P3 C13 -104.25(2) 4_565 . . . ?
P1 P2 P3 C13 -46.09(2) . . . . ?
P1 P2 P3 P2 58.157(11) . . . 4_565 ?
P2 P2 P3 Ga1 99.378(9) 4_565 . . . ?
P1 P2 P3 Ga1 157.535(9) . . . . ?
C13 P3 Ga1 Cl1 0.0 . . . . ?
P2 P3 Ga1 Cl1 148.391(8) . . . . ?
P2 P3 Ga1 Cl1 -148.391(8) 4_565 . . . ?
C13 P3 Ga1 Cl2 121.872(10) . . . 4_565 ?
P2 P3 Ga1 Cl2 -89.737(13) . . . 4_565 ?
P2 P3 Ga1 Cl2 -26.519(14) 4_565 . . 4_565 ?
C13 P3 Ga1 Cl2 -121.872(10) . . . . ?
P2 P3 Ga1 Cl2 26.519(14) . . . . ?
P2 P3 Ga1 Cl2 89.737(13) 4_565 . . . ?
P2 P1 C1 C2 -112.25(9) 4_565 . . . ?
P2 P1 C1 C2 -52.85(9) . . . . ?
P2 P1 C1 C2 52.85(9) 4_565 . . 4_565 ?
P2 P1 C1 C2 112.25(9) . . . 4_565 ?
C2 C1 C2 C3 -16.92(17) 4_565 . . . ?
P1 C1 C2 C3 148.28(8) . . . . ?
C2 C1 C2 C5 157.12(8) 4_565 . . . ?
P1 C1 C2 C5 -37.68(14) . . . . ?
C1 C2 C3 C4 3.46(16) . . . . ?
C5 C2 C3 C4 -171.17(10) . . . . ?
C2 C3 C4 C3 9.7(2) . . . 4_565 ?
C2 C3 C4 C9 -172.79(12) . . . . ?
C3 C2 C5 C7 -63.60(11) . . . . ?
C1 C2 C5 C7 122.26(11) . . . . ?
C3 C2 C5 C6 170.40(9) . . . . ?
C1 C2 C5 C6 -3.74(15) . . . . ?
C3 C2 C5 C8 54.65(12) . . . . ?
C1 C2 C5 C8 -119.49(11) . . . . ?
C3 C4 C9 C12 178.8(2) 4_565 . . 4_565 ?
C3 C4 C9 C12 1.4(3) . . . 4_565 ?
C3 C4 C9 C12 -1.4(3) 4_565 . . . ?
C3 C4 C9 C12 -178.8(2) . . . . ?
C3 C4 C9 C11 -53.6(3) 4_565 . . 4_565 ?
C3 C4 C9 C11 128.9(2) . . . 4_565 ?
C3 C4 C9 C11 -128.9(2) 4_565 . . . ?
C3 C4 C9 C11 53.6(3) . . . . ?
C3 C4 C9 C10 117.92(19) 4_565 . . . ?
C3 C4 C9 C10 -59.5(2) . . . . ?
C3 C4 C9 C10 59.5(2) 4_565 . . 4_565 ?
C3 C4 C9 C10 -117.92(19) . . . 4_565 ?
P2 P3 C13 C14 113.03(7) . . . 4_565 ?
P2 P3 C13 C14 46.60(8) 4_565 . . 4_565 ?
Ga1 P3 C13 C14 -100.19(7) . . . 4_565 ?
P2 P3 C13 C14 -46.60(8) . . . . ?
P2 P3 C13 C14 -113.03(7) 4_565 . . . ?
Ga1 P3 C13 C14 100.19(7) . . . . ?
C14 C13 C14 C15 -15.64(15) 4_565 . . . ?
P3 C13 C14 C15 143.56(7) . . . . ?
C14 C13 C14 C17 158.80(7) 4_565 . . . ?
P3 C13 C14 C17 -42.01(12) . . . . ?
C13 C14 C15 C16 2.77(14) . . . . ?
C17 C14 C15 C16 -172.21(9) . . . . ?
C14 C15 C16 C15 9.50(18) . . . 4_565 ?
C14 C15 C16 C21 -171.47(11) . . . 4_565 ?
C14 C15 C16 C21 -171.56(12) . . . . ?
C15 C14 C17 C18 170.49(8) . . . . ?
C13 C14 C17 C18 -3.97(13) . . . . ?
C15 C14 C17 C19 -64.91(11) . . . . ?
C13 C14 C17 C19 120.63(10) . . . . ?
C15 C14 C17 C20 53.50(11) . . . . ?
C13 C14 C17 C20 -120.96(10) . . . . ?
C15 C16 C21 C21 179.49(10) 4_565 . . 4_565 ?
C15 C16 C21 C21 0.55(11) . . . 4_565 ?
C15 C16 C21 C23 67(2) 4_565 . . 4_565 ?
C15 C16 C21 C23 -112(2) . . . 4_565 ?
C21 C16 C21 C23 -113(2) 4_565 . . 4_565 ?
C15 C16 C21 C22 -76(2) 4_565 . . 4_565 ?
C15 C16 C21 C22 105(2) . . . 4_565 ?
C21 C16 C21 C22 105(2) 4_565 . . 4_565 ?
C15 C16 C21 C23 123.4(16) 4_565 . . . ?
C15 C16 C21 C23 -55.5(16) . . . . ?
C21 C16 C21 C23 -56.1(16) 4_565 . . . ?
C15 C16 C21 C22 -116.5(17) 4_565 . . . ?
C15 C16 C21 C22 64.6(17) . . . . ?
C21 C16 C21 C22 64.1(17) 4_565 . . . ?
C15 C16 C21 C24 1.3(3) 4_565 . . . ?
C15 C16 C21 C24 -177.6(2) . . . . ?
C21 C16 C21 C24 -178.2(2) 4_565 . . . ?
C15 C16 C21 C24 178.00(17) 4_565 . . 4_565 ?
C15 C16 C21 C24 -0.9(2) . . . 4_565 ?
C21 C16 C21 C24 -1.49(17) 4_565 . . 4_565 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        32.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.044
####################################################################### 
# 
# 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_is_jb10_3_MesPPNiPr2
_database_code_depnum_ccdc_archive 'CCDC 1413826'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H43 N P2'
_chemical_formula_weight         407.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   10.0058(5)
_cell_length_b                   26.4841(11)
_cell_length_c                   9.9173(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.035(2)
_cell_angle_gamma                90.00
_cell_volume                     2579.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9904
_cell_measurement_theta_min      5.164
_cell_measurement_theta_max      63.015

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8640
_exptl_absorpt_correction_T_max  0.9825
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            45447
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         30.00
_reflns_number_total             7502
_reflns_number_gt                5859
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker Apex V7.51A'
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine.
 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0737P)²+0.9911P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7502
_refine_ls_number_parameters     288
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1407
_refine_ls_wR_factor_gt          0.1263
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.78097(4) 0.085784(14) 0.06037(4) 0.03021(11) Uani 1 1 d . . .
P2 P 0.77526(4) 0.097430(14) 0.26232(4) 0.02947(11) Uani 1 1 d . . .
N1 N 0.70648(14) 0.04661(5) 0.32163(14) 0.0308(3) Uani 1 1 d . . .
C1 C 0.87736(14) 0.14536(5) 0.04917(14) 0.0217(3) Uani 1 1 d . . .
C2 C 0.80719(13) 0.19172(5) 0.01368(14) 0.0217(3) Uani 1 1 d . . .
C3 C 0.88103(13) 0.23646(5) 0.03987(14) 0.0226(3) Uani 1 1 d . . .
H3 H 0.8339 0.2676 0.0205 0.027 Uiso 1 1 calc R . .
C4 C 1.01998(13) 0.23791(5) 0.09288(14) 0.0205(2) Uani 1 1 d . A .
C5 C 1.08770(14) 0.19212(5) 0.11037(15) 0.0247(3) Uani 1 1 d . . .
H5 H 1.1837 0.1924 0.1403 0.030 Uiso 1 1 calc R . .
C6 C 1.02183(14) 0.14559(5) 0.08626(15) 0.0245(3) Uani 1 1 d . . .
C7 C 0.65647(14) 0.19584(6) -0.06211(16) 0.0285(3) Uani 1 1 d . . .
C8 C 0.6344(2) 0.16241(10) -0.1901(2) 0.0528(5) Uani 1 1 d . . .
H8A H 0.6547 0.1272 -0.1629 0.079 Uiso 1 1 calc R . .
H8B H 0.6949 0.1734 -0.2512 0.079 Uiso 1 1 calc R . .
H8C H 0.5395 0.1651 -0.2380 0.079 Uiso 1 1 calc R . .
C9 C 0.55196(17) 0.18204(9) 0.0259(2) 0.0488(5) Uani 1 1 d . . .
H9A H 0.5738 0.1999 0.1140 0.073 Uiso 1 1 calc R . .
H9B H 0.5543 0.1455 0.0423 0.073 Uiso 1 1 calc R . .
H9C H 0.4608 0.1919 -0.0222 0.073 Uiso 1 1 calc R . .
C10 C 0.6213(2) 0.24981(9) -0.1124(3) 0.0705(8) Uani 1 1 d . . .
H10A H 0.5272 0.2509 -0.1633 0.106 Uiso 1 1 calc R . .
H10B H 0.6831 0.2604 -0.1727 0.106 Uiso 1 1 calc R . .
H10C H 0.6311 0.2726 -0.0333 0.106 Uiso 1 1 calc R . .
C11 C 1.09279(15) 0.28859(5) 0.12146(15) 0.0268(3) Uani 1 1 d . . .
C12A C 1.0211(3) 0.31943(9) 0.2192(3) 0.0437(6) Uani 0.810(4) 1 d P A 1
H12A H 1.0242 0.3006 0.3049 0.066 Uiso 0.810(4) 1 calc PR A 1
H12B H 0.9260 0.3253 0.1754 0.066 Uiso 0.810(4) 1 calc PR A 1
H12C H 1.0676 0.3519 0.2395 0.066 Uiso 0.810(4) 1 calc PR A 1
C13A C 1.0814(3) 0.31796(8) -0.0125(2) 0.0430(6) Uani 0.810(4) 1 d P A 1
H13A H 1.1256 0.3509 0.0062 0.065 Uiso 0.810(4) 1 calc PR A 1
H13B H 0.9851 0.3229 -0.0535 0.065 Uiso 0.810(4) 1 calc PR A 1
H13C H 1.1260 0.2990 -0.0762 0.065 Uiso 0.810(4) 1 calc PR A 1
C14A C 1.2407(2) 0.28300(10) 0.1875(4) 0.0546(9) Uani 0.810(4) 1 d P A 1
H14A H 1.2889 0.2651 0.1247 0.082 Uiso 0.810(4) 1 calc PR A 1
H14B H 1.2482 0.2638 0.2730 0.082 Uiso 0.810(4) 1 calc PR A 1
H14C H 1.2812 0.3165 0.2077 0.082 Uiso 0.810(4) 1 calc PR A 1
C13B C 1.2025(14) 0.2929(4) 0.0175(13) 0.058(4) Uani 0.190(4) 1 d P A 2
H13D H 1.1533 0.2935 -0.0780 0.086 Uiso 0.190(4) 1 calc PR A 2
H13E H 1.2639 0.2637 0.0312 0.086 Uiso 0.190(4) 1 calc PR A 2
H13F H 1.2557 0.3240 0.0373 0.086 Uiso 0.190(4) 1 calc PR A 2
C12B C 1.0106(13) 0.3336(4) 0.109(2) 0.074(6) Uani 0.190(4) 1 d P A 2
H12D H 1.0687 0.3629 0.1380 0.111 Uiso 0.190(4) 1 calc PR A 2
H12E H 0.9419 0.3306 0.1665 0.111 Uiso 0.190(4) 1 calc PR A 2
H12F H 0.9654 0.3380 0.0126 0.111 Uiso 0.190(4) 1 calc PR A 2
C14B C 1.1926(16) 0.2876(5) 0.2659(13) 0.055(3) Uani 0.190(4) 1 d P A 2
H14D H 1.2535 0.3169 0.2736 0.083 Uiso 0.190(4) 1 calc PR A 2
H14E H 1.2466 0.2565 0.2743 0.083 Uiso 0.190(4) 1 calc PR A 2
H14F H 1.1394 0.2888 0.3392 0.083 Uiso 0.190(4) 1 calc PR A 2
C15 C 1.11268(18) 0.09766(6) 0.0922(2) 0.0409(4) Uani 1 1 d . . .
C16 C 1.0633(3) 0.06324(7) -0.0324(3) 0.0597(6) Uani 1 1 d . . .
H16A H 1.1273 0.0352 -0.0316 0.090 Uiso 1 1 calc R . .
H16B H 1.0581 0.0827 -0.1172 0.090 Uiso 1 1 calc R . .
H16C H 0.9730 0.0499 -0.0277 0.090 Uiso 1 1 calc R . .
C17 C 1.1216(3) 0.06762(9) 0.2256(3) 0.0636(7) Uani 1 1 d . . .
H17A H 1.0313 0.0545 0.2315 0.095 Uiso 1 1 calc R . .
H17B H 1.1541 0.0897 0.3043 0.095 Uiso 1 1 calc R . .
H17C H 1.1851 0.0394 0.2264 0.095 Uiso 1 1 calc R . .
C18 C 1.2582(2) 0.11235(8) 0.0778(3) 0.0639(7) Uani 1 1 d . . .
H18A H 1.3054 0.1278 0.1635 0.096 Uiso 1 1 calc R . .
H18B H 1.2540 0.1365 0.0022 0.096 Uiso 1 1 calc R . .
H18C H 1.3077 0.0821 0.0586 0.096 Uiso 1 1 calc R . .
C19 C 0.67100(18) -0.00059(6) 0.24485(18) 0.0326(3) Uani 1 1 d . . .
H19 H 0.7078 0.0021 0.1582 0.039 Uiso 1 1 calc R . .
C20 C 0.7377(2) -0.04641(7) 0.3224(2) 0.0510(5) Uani 1 1 d . . .
H20A H 0.8364 -0.0413 0.3456 0.077 Uiso 1 1 calc R . .
H20B H 0.7177 -0.0765 0.2647 0.077 Uiso 1 1 calc R . .
H20C H 0.7019 -0.0509 0.4069 0.077 Uiso 1 1 calc R . .
C21 C 0.5180(2) -0.00731(8) 0.2031(2) 0.0513(5) Uani 1 1 d . . .
H21A H 0.4776 -0.0090 0.2856 0.077 Uiso 1 1 calc R . .
H21B H 0.4983 -0.0387 0.1506 0.077 Uiso 1 1 calc R . .
H21C H 0.4792 0.0214 0.1463 0.077 Uiso 1 1 calc R . .
C22 C 0.6722(2) 0.05028(7) 0.46063(18) 0.0400(4) Uani 1 1 d . . .
H22 H 0.6280 0.0177 0.4781 0.048 Uiso 1 1 calc R . .
C23 C 0.7987(3) 0.05574(10) 0.5714(2) 0.0660(7) Uani 1 1 d . . .
H23A H 0.8616 0.0280 0.5640 0.099 Uiso 1 1 calc R . .
H23B H 0.7731 0.0548 0.6620 0.099 Uiso 1 1 calc R . .
H23C H 0.8431 0.0880 0.5599 0.099 Uiso 1 1 calc R . .
C24 C 0.5688(3) 0.09216(9) 0.4675(2) 0.0594(6) Uani 1 1 d . . .
H24A H 0.6099 0.1250 0.4544 0.089 Uiso 1 1 calc R . .
H24B H 0.5419 0.0914 0.5575 0.089 Uiso 1 1 calc R . .
H24C H 0.4884 0.0870 0.3952 0.089 Uiso 1 1 calc R . .


#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 1.8636(13) . ?
P1 P2 2.0380(6) . ?
P2 N1 1.6690(12) . ?
N1 C19 1.472(2) . ?
N1 C22 1.486(2) . ?
C1 C6 1.4217(19) . ?
C1 C2 1.4248(19) . ?
C2 C3 1.3942(18) . ?
C2 C7 1.5547(18) . ?
C3 C4 1.3896(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.3837(18) . ?
C4 C11 1.5275(18) . ?
C5 C6 1.3965(19) . ?
C5 H5 0.9500 . ?
C6 C15 1.556(2) . ?
C7 C8 1.528(3) . ?
C7 C9 1.529(2) . ?
C7 C10 1.532(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12B 1.440(12) . ?
C11 C14A 1.507(3) . ?
C11 C13A 1.525(3) . ?
C11 C12A 1.545(3) . ?
C11 C14B 1.582(11) . ?
C11 C13B 1.648(11) . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C14A H14A 0.9800 . ?
C14A H14B 0.9800 . ?
C14A H14C 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C15 C17 1.531(3) . ?
C15 C16 1.539(3) . ?
C15 C18 1.540(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C21 1.518(3) . ?
C19 C20 1.521(2) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.516(3) . ?
C22 C24 1.527(3) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 P2 92.44(5) . . ?
N1 P2 P1 108.38(5) . . ?
C19 N1 C22 117.38(12) . . ?
C19 N1 P2 125.29(11) . . ?
C22 N1 P2 117.26(10) . . ?
C6 C1 C2 119.26(11) . . ?
C6 C1 P1 120.03(10) . . ?
C2 C1 P1 120.54(10) . . ?
C3 C2 C1 117.89(12) . . ?
C3 C2 C7 117.45(12) . . ?
C1 C2 C7 124.50(12) . . ?
C4 C3 C2 123.38(12) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
C5 C4 C3 116.98(12) . . ?
C5 C4 C11 122.82(12) . . ?
C3 C4 C11 120.11(12) . . ?
C4 C5 C6 123.25(12) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C5 C6 C1 118.11(12) . . ?
C5 C6 C15 117.41(13) . . ?
C1 C6 C15 124.34(13) . . ?
C8 C7 C9 109.25(15) . . ?
C8 C7 C10 106.41(18) . . ?
C9 C7 C10 105.62(17) . . ?
C8 C7 C2 109.47(13) . . ?
C9 C7 C2 114.41(13) . . ?
C10 C7 C2 111.33(12) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12B C11 C14A 128.1(5) . . ?
C12B C11 C13A 63.5(8) . . ?
C14A C11 C13A 109.41(19) . . ?
C12B C11 C4 117.9(4) . . ?
C14A C11 C4 112.85(15) . . ?
C13A C11 C4 109.45(13) . . ?
C12B C11 C12A 45.0(8) . . ?
C14A C11 C12A 108.3(2) . . ?
C13A C11 C12A 108.10(17) . . ?
C4 C11 C12A 108.59(13) . . ?
C12B C11 C14B 110.2(9) . . ?
C14A C11 C14B 37.6(6) . . ?
C13A C11 C14B 136.6(5) . . ?
C4 C11 C14B 110.5(4) . . ?
C12A C11 C14B 74.3(7) . . ?
C12B C11 C13B 108.9(9) . . ?
C14A C11 C13B 64.0(5) . . ?
C13A C11 C13B 50.8(5) . . ?
C4 C11 C13B 107.2(4) . . ?
C12A C11 C13B 143.2(4) . . ?
C14B C11 C13B 100.8(8) . . ?
C11 C12A H12A 109.5 . . ?
C11 C12A H12B 109.5 . . ?
C11 C12A H12C 109.5 . . ?
C11 C13A H13A 109.5 . . ?
C11 C13A H13B 109.5 . . ?
C11 C13A H13C 109.5 . . ?
C11 C14A H14A 109.5 . . ?
C11 C14A H14B 109.5 . . ?
C11 C14A H14C 109.5 . . ?
C11 C13B H13D 109.5 . . ?
C11 C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C11 C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C11 C12B H12D 109.5 . . ?
C11 C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11 C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C11 C14B H14D 109.5 . . ?
C11 C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
C11 C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C17 C15 C16 110.04(18) . . ?
C17 C15 C18 108.15(18) . . ?
C16 C15 C18 103.83(18) . . ?
C17 C15 C6 113.19(16) . . ?
C16 C15 C6 110.92(16) . . ?
C18 C15 C6 110.26(13) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 C21 111.80(14) . . ?
N1 C19 C20 112.16(15) . . ?
C21 C19 C20 111.50(15) . . ?
N1 C19 H19 107.0 . . ?
C21 C19 H19 107.0 . . ?
C20 C19 H19 107.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N1 C22 C23 111.72(17) . . ?
N1 C22 C24 111.57(15) . . ?
C23 C22 C24 112.15(19) . . ?
N1 C22 H22 107.0 . . ?
C23 C22 H22 107.0 . . ?
C24 C22 H22 107.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 P1 P2 N1 -174.18(7) . . . . ?
P1 P2 N1 C19 6.39(15) . . . . ?
P1 P2 N1 C22 -170.49(12) . . . . ?
P2 P1 C1 C6 86.16(11) . . . . ?
P2 P1 C1 C2 -89.03(11) . . . . ?
C6 C1 C2 C3 -11.0(2) . . . . ?
P1 C1 C2 C3 164.22(11) . . . . ?
C6 C1 C2 C7 164.27(13) . . . . ?
P1 C1 C2 C7 -20.50(19) . . . . ?
C1 C2 C3 C4 2.9(2) . . . . ?
C7 C2 C3 C4 -172.68(13) . . . . ?
C2 C3 C4 C5 4.7(2) . . . . ?
C2 C3 C4 C11 -178.71(13) . . . . ?
C3 C4 C5 C6 -4.4(2) . . . . ?
C11 C4 C5 C6 179.12(14) . . . . ?
C4 C5 C6 C1 -3.5(2) . . . . ?
C4 C5 C6 C15 172.41(15) . . . . ?
C2 C1 C6 C5 11.3(2) . . . . ?
P1 C1 C6 C5 -163.94(11) . . . . ?
C2 C1 C6 C15 -164.32(14) . . . . ?
P1 C1 C6 C15 20.4(2) . . . . ?
C3 C2 C7 C8 125.06(16) . . . . ?
C1 C2 C7 C8 -50.2(2) . . . . ?
C3 C2 C7 C9 -111.96(17) . . . . ?
C1 C2 C7 C9 72.7(2) . . . . ?
C3 C2 C7 C10 7.7(2) . . . . ?
C1 C2 C7 C10 -167.61(18) . . . . ?
C5 C4 C11 C12B -175.8(10) . . . . ?
C3 C4 C11 C12B 7.8(10) . . . . ?
C5 C4 C11 C14A -7.5(3) . . . . ?
C3 C4 C11 C14A 176.1(2) . . . . ?
C5 C4 C11 C13A 114.54(18) . . . . ?
C3 C4 C11 C13A -61.8(2) . . . . ?
C5 C4 C11 C12A -127.66(18) . . . . ?
C3 C4 C11 C12A 56.0(2) . . . . ?
C5 C4 C11 C14B -48.0(7) . . . . ?
C3 C4 C11 C14B 135.6(7) . . . . ?
C5 C4 C11 C13B 60.9(6) . . . . ?
C3 C4 C11 C13B -115.4(6) . . . . ?
C5 C6 C15 C17 102.87(19) . . . . ?
C1 C6 C15 C17 -81.5(2) . . . . ?
C5 C6 C15 C16 -132.88(16) . . . . ?
C1 C6 C15 C16 42.8(2) . . . . ?
C5 C6 C15 C18 -18.4(2) . . . . ?
C1 C6 C15 C18 157.24(18) . . . . ?
C22 N1 C19 C21 67.9(2) . . . . ?
P2 N1 C19 C21 -108.97(16) . . . . ?
C22 N1 C19 C20 -58.2(2) . . . . ?
P2 N1 C19 C20 124.95(15) . . . . ?
C19 N1 C22 C23 116.74(18) . . . . ?
P2 N1 C22 C23 -66.13(19) . . . . ?
C19 N1 C22 C24 -116.84(18) . . . . ?
P2 N1 C22 C24 60.30(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.059
####################################################################### 
# 
# 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_ah_jb49_MesPTMS2
_database_code_depnum_ccdc_archive 'CCDC 1413827'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H47 P Si2'
_chemical_formula_sum            'C24 H47 P Si2'
_chemical_formula_weight         422.77

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'
Si Si 0.0817 0.0704 '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'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   9.3749(6)
_cell_length_b                   16.9528(11)
_cell_length_c                   17.6869(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.224(3)
_cell_angle_gamma                90.00
_cell_volume                     2757.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4439
_cell_measurement_theta_min      5.040
_cell_measurement_theta_max      45.885

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9532
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33224
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.90
_diffrn_reflns_theta_max         28.38
_reflns_number_total             6891
_reflns_number_gt                4340
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker Apex V7.51A'
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms were positioned geometrically and refined using a riding model, 
 with C---H = 0.98 (methyl groups), 0.99Å (methylene groups), 
 1.00Å (methine groups) or 0.95 Å (aryl CH) and with Uiso(H) = 
 1.5 times Ueq(C) (methyl groups) or with Uiso(H) = 1.2 times 
 Ueq(C) (methylene  groups, aryl CH, methine groups). Torsion angles 
 of all methyl groups were allowed to refine.

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0508P)²+0.4774P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6891
_refine_ls_number_parameters     269
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1154
_refine_ls_wR_factor_gt          0.0979
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.40678(5) 0.97616(3) 0.17800(3) 0.02225(13) Uani 1 1 d . . .
Si1 Si 0.62370(6) 0.99997(3) 0.25529(3) 0.03171(15) Uani 1 1 d . . .
Si2 Si 0.41561(7) 0.86531(3) 0.11052(3) 0.03429(16) Uani 1 1 d . . .
C1 C 0.26965(17) 1.00323(10) 0.23725(9) 0.0179(4) Uani 1 1 d . . .
C2 C 0.21305(18) 1.08057(10) 0.22228(9) 0.0185(4) Uani 1 1 d . . .
C3 C 0.16944(18) 1.12196(10) 0.28223(9) 0.0207(4) Uani 1 1 d . . .
H3 H 0.1382 1.1750 0.2733 0.025 Uiso 1 1 calc R . .
C4 C 0.16944(18) 1.08948(11) 0.35404(9) 0.0202(4) Uani 1 1 d . A .
C5 C 0.19859(18) 1.00929(10) 0.36168(9) 0.0222(4) Uani 1 1 d . . .
H5 H 0.1858 0.9838 0.4077 0.027 Uiso 1 1 calc R . .
C6 C 0.24546(18) 0.96433(10) 0.30550(9) 0.0192(4) Uani 1 1 d . . .
C7 C 0.19146(19) 1.12404(10) 0.14310(9) 0.0218(4) Uani 1 1 d . . .
C8 C 0.1352(2) 1.06774(12) 0.07575(10) 0.0327(5) Uani 1 1 d . . .
H8A H 0.1123 1.0979 0.0276 0.049 Uiso 1 1 calc R . .
H8B H 0.0474 1.0410 0.0848 0.049 Uiso 1 1 calc R . .
H8C H 0.2101 1.0284 0.0719 0.049 Uiso 1 1 calc R . .
C9 C 0.3300(2) 1.16607(12) 0.13180(11) 0.0307(5) Uani 1 1 d . . .
H9A H 0.3079 1.2002 0.0863 0.046 Uiso 1 1 calc R . .
H9B H 0.4029 1.1269 0.1245 0.046 Uiso 1 1 calc R . .
H9C H 0.3680 1.1981 0.1774 0.046 Uiso 1 1 calc R . .
C10 C 0.0726(2) 1.18781(11) 0.13808(11) 0.0317(5) Uani 1 1 d . . .
H10A H 0.1085 1.2311 0.1734 0.047 Uiso 1 1 calc R . .
H10B H -0.0143 1.1648 0.1524 0.047 Uiso 1 1 calc R . .
H10C H 0.0480 1.2081 0.0852 0.047 Uiso 1 1 calc R . .
C11 C 0.1328(2) 1.13756(11) 0.42104(10) 0.0274(4) Uani 1 1 d . . .
C12A C 0.1302(3) 1.22587(13) 0.40548(13) 0.0482(7) Uani 0.958(3) 1 d PD A 1
H12A H 0.1121 1.2542 0.4510 0.072 Uiso 0.958(3) 1 calc PR A 1
H12B H 0.0527 1.2379 0.3612 0.072 Uiso 0.958(3) 1 calc PR A 1
H12C H 0.2240 1.2423 0.3942 0.072 Uiso 0.958(3) 1 calc PR A 1
C13A C -0.0169(4) 1.1143(2) 0.4331(2) 0.0896(14) Uani 0.958(3) 1 d PD A 1
H13A H -0.0185 1.0577 0.4440 0.134 Uiso 0.958(3) 1 calc PR A 1
H13B H -0.0888 1.1262 0.3864 0.134 Uiso 0.958(3) 1 calc PR A 1
H13C H -0.0404 1.1440 0.4766 0.134 Uiso 0.958(3) 1 calc PR A 1
C14A C 0.2459(4) 1.12269(19) 0.49301(14) 0.0882(14) Uani 0.958(3) 1 d PD A 1
H14A H 0.3424 1.1359 0.4832 0.132 Uiso 0.958(3) 1 calc PR A 1
H14B H 0.2438 1.0669 0.5074 0.132 Uiso 0.958(3) 1 calc PR A 1
H14C H 0.2249 1.1555 0.5351 0.132 Uiso 0.958(3) 1 calc PR A 1
C12B C 0.095(7) 1.077(3) 0.486(3) 0.0482(7) Uani 0.042(3) 1 d PD A 2
H12D H 0.1607 1.0312 0.4895 0.072 Uiso 0.042(3) 1 calc PR A 2
H12E H -0.0055 1.0590 0.4705 0.072 Uiso 0.042(3) 1 calc PR A 2
H12F H 0.1086 1.1036 0.5355 0.072 Uiso 0.042(3) 1 calc PR A 2
C13B C 0.254(6) 1.179(4) 0.449(4) 0.0896(14) Uani 0.042(3) 1 d PD A 2
H13D H 0.3344 1.1419 0.4678 0.134 Uiso 0.042(3) 1 calc PR A 2
H13E H 0.2379 1.2119 0.4920 0.134 Uiso 0.042(3) 1 calc PR A 2
H13F H 0.2797 1.2119 0.4085 0.134 Uiso 0.042(3) 1 calc PR A 2
C14B C -0.010(8) 1.180(4) 0.394(3) 0.0882(14) Uani 0.042(3) 1 d PD A 2
H14D H -0.0787 1.1442 0.3613 0.132 Uiso 0.042(3) 1 calc PR A 2
H14E H 0.0060 1.2263 0.3634 0.132 Uiso 0.042(3) 1 calc PR A 2
H14F H -0.0506 1.1964 0.4382 0.132 Uiso 0.042(3) 1 calc PR A 2
C15 C 0.25895(19) 0.87433(10) 0.31858(10) 0.0232(4) Uani 1 1 d . . .
C16 C 0.1956(2) 0.84723(12) 0.38844(11) 0.0346(5) Uani 1 1 d . . .
H16A H 0.1964 0.7895 0.3909 0.052 Uiso 1 1 calc R . .
H16B H 0.0955 0.8664 0.3830 0.052 Uiso 1 1 calc R . .
H16C H 0.2547 0.8686 0.4358 0.052 Uiso 1 1 calc R . .
C17 C 0.4159(2) 0.84537(11) 0.33367(11) 0.0305(5) Uani 1 1 d . . .
H17A H 0.4608 0.8591 0.2898 0.046 Uiso 1 1 calc R . .
H17B H 0.4176 0.7880 0.3405 0.046 Uiso 1 1 calc R . .
H17C H 0.4702 0.8704 0.3805 0.046 Uiso 1 1 calc R . .
C18 C 0.1679(2) 0.83331(11) 0.24808(11) 0.0306(5) Uani 1 1 d . . .
H18A H 0.2027 0.8493 0.2016 0.046 Uiso 1 1 calc R . .
H18B H 0.0656 0.8484 0.2432 0.046 Uiso 1 1 calc R . .
H18C H 0.1773 0.7760 0.2544 0.046 Uiso 1 1 calc R . .
C19 C 0.7198(3) 1.07285(16) 0.20350(15) 0.0601(7) Uani 1 1 d . . .
H19A H 0.6651 1.1224 0.1970 0.090 Uiso 1 1 calc R . .
H19B H 0.7272 1.0518 0.1528 0.090 Uiso 1 1 calc R . .
H19C H 0.8176 1.0825 0.2336 0.090 Uiso 1 1 calc R . .
C20 C 0.5886(2) 1.04540(13) 0.34601(12) 0.0414(5) Uani 1 1 d . . .
H20A H 0.5514 1.0051 0.3769 0.062 Uiso 1 1 calc R . .
H20B H 0.5166 1.0877 0.3333 0.062 Uiso 1 1 calc R . .
H20C H 0.6794 1.0673 0.3755 0.062 Uiso 1 1 calc R . .
C21 C 0.7497(2) 0.91395(15) 0.27815(13) 0.0494(6) Uani 1 1 d . . .
H21A H 0.8451 0.9325 0.3052 0.074 Uiso 1 1 calc R . .
H21B H 0.7601 0.8876 0.2302 0.074 Uiso 1 1 calc R . .
H21C H 0.7100 0.8767 0.3111 0.074 Uiso 1 1 calc R . .
C22 C 0.5645(3) 0.89121(15) 0.05827(13) 0.0580(7) Uani 1 1 d . . .
H22A H 0.6543 0.9013 0.0957 0.087 Uiso 1 1 calc R . .
H22B H 0.5372 0.9386 0.0270 0.087 Uiso 1 1 calc R . .
H22C H 0.5799 0.8473 0.0247 0.087 Uiso 1 1 calc R . .
C23 C 0.2409(3) 0.85385(15) 0.03925(13) 0.0606(7) Uani 1 1 d . . .
H23A H 0.2455 0.8063 0.0083 0.091 Uiso 1 1 calc R . .
H23B H 0.2257 0.9001 0.0054 0.091 Uiso 1 1 calc R . .
H23C H 0.1601 0.8492 0.0668 0.091 Uiso 1 1 calc R . .
C24 C 0.4635(3) 0.76754(12) 0.15726(13) 0.0482(6) Uani 1 1 d . . .
H24A H 0.3862 0.7508 0.1839 0.072 Uiso 1 1 calc R . .
H24B H 0.5553 0.7720 0.1946 0.072 Uiso 1 1 calc R . .
H24C H 0.4742 0.7285 0.1179 0.072 Uiso 1 1 calc R . .


#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 1.8671(16) . ?
P1 Si2 2.2364(7) . ?
P1 Si1 2.2550(7) . ?
Si1 C20 1.866(2) . ?
Si1 C19 1.871(2) . ?
Si1 C21 1.871(2) . ?
Si2 C24 1.867(2) . ?
Si2 C22 1.870(2) . ?
Si2 C23 1.872(2) . ?
C1 C2 1.420(2) . ?
C1 C6 1.432(2) . ?
C2 C3 1.397(2) . ?
C2 C7 1.560(2) . ?
C3 C4 1.384(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(2) . ?
C4 C11 1.532(2) . ?
C5 C6 1.390(2) . ?
C5 H5 0.9500 . ?
C6 C15 1.545(2) . ?
C7 C9 1.528(3) . ?
C7 C8 1.537(2) . ?
C7 C10 1.543(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13B 1.35(5) . ?
C11 C14A 1.511(3) . ?
C11 C13A 1.512(3) . ?
C11 C14B 1.51(5) . ?
C11 C12A 1.522(3) . ?
C11 C12B 1.62(4) . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C14A H14A 0.9800 . ?
C14A H14B 0.9800 . ?
C14A H14C 0.9800 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C15 C17 1.525(2) . ?
C15 C18 1.534(2) . ?
C15 C16 1.541(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 Si2 127.39(6) . . ?
C1 P1 Si1 104.71(6) . . ?
Si2 P1 Si1 110.56(3) . . ?
C20 Si1 C19 109.31(12) . . ?
C20 Si1 C21 110.21(11) . . ?
C19 Si1 C21 106.06(12) . . ?
C20 Si1 P1 107.82(7) . . ?
C19 Si1 P1 106.55(8) . . ?
C21 Si1 P1 116.66(8) . . ?
C24 Si2 C22 106.79(11) . . ?
C24 Si2 C23 108.03(12) . . ?
C22 Si2 C23 109.32(12) . . ?
C24 Si2 P1 122.70(7) . . ?
C22 Si2 P1 100.09(9) . . ?
C23 Si2 P1 109.15(8) . . ?
C2 C1 C6 117.89(14) . . ?
C2 C1 P1 113.29(12) . . ?
C6 C1 P1 126.82(13) . . ?
C3 C2 C1 118.43(15) . . ?
C3 C2 C7 115.97(15) . . ?
C1 C2 C7 125.59(14) . . ?
C4 C3 C2 123.28(16) . . ?
C4 C3 H3 118.4 . . ?
C2 C3 H3 118.4 . . ?
C3 C4 C5 116.34(15) . . ?
C3 C4 C11 122.58(16) . . ?
C5 C4 C11 121.03(15) . . ?
C4 C5 C6 123.45(15) . . ?
C4 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
C5 C6 C1 118.31(16) . . ?
C5 C6 C15 117.56(15) . . ?
C1 C6 C15 124.02(15) . . ?
C9 C7 C8 111.11(15) . . ?
C9 C7 C10 106.77(15) . . ?
C8 C7 C10 104.80(15) . . ?
C9 C7 C2 111.87(14) . . ?
C8 C7 C2 111.54(14) . . ?
C10 C7 C2 110.40(13) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13B C11 C14A 51(3) . . ?
C13B C11 C13A 146(2) . . ?
C14A C11 C13A 110.9(2) . . ?
C13B C11 C14B 121(3) . . ?
C14A C11 C14B 141(2) . . ?
C13A C11 C14B 52(3) . . ?
C13B C11 C12A 63(3) . . ?
C14A C11 C12A 107.5(2) . . ?
C13A C11 C12A 107.4(2) . . ?
C14B C11 C12A 60(3) . . ?
C13B C11 C4 105(2) . . ?
C14A C11 C4 109.66(17) . . ?
C13A C11 C4 108.92(17) . . ?
C14B C11 C4 109(2) . . ?
C12A C11 C4 112.44(15) . . ?
C13B C11 C12B 110(3) . . ?
C14A C11 C12B 61(2) . . ?
C13A C11 C12B 53(2) . . ?
C14B C11 C12B 103(3) . . ?
C12A C11 C12B 138.8(17) . . ?
C4 C11 C12B 108.5(17) . . ?
C11 C12A H12A 109.5 . . ?
C11 C12A H12B 109.5 . . ?
C11 C12A H12C 109.5 . . ?
C11 C13A H13A 109.5 . . ?
C11 C13A H13B 109.5 . . ?
C11 C13A H13C 109.5 . . ?
C11 C14A H14A 109.5 . . ?
C11 C14A H14B 109.5 . . ?
C11 C14A H14C 109.5 . . ?
C11 C12B H12D 109.5 . . ?
C11 C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11 C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C11 C13B H13D 109.5 . . ?
C11 C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C11 C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C11 C14B H14D 109.5 . . ?
C11 C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
C11 C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C17 C15 C18 111.20(15) . . ?
C17 C15 C16 105.84(15) . . ?
C18 C15 C16 106.05(15) . . ?
C17 C15 C6 113.10(14) . . ?
C18 C15 C6 108.03(14) . . ?
C16 C15 C6 112.42(14) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 C19 H19A 109.5 . . ?
Si1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si1 C20 H20A 109.5 . . ?
Si1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si1 C21 H21A 109.5 . . ?
Si1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si2 C22 H22A 109.5 . . ?
Si2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si2 C23 H23A 109.5 . . ?
Si2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 P1 Si1 C20 -4.65(10) . . . . ?
Si2 P1 Si1 C20 -144.91(8) . . . . ?
C1 P1 Si1 C19 -121.90(11) . . . . ?
Si2 P1 Si1 C19 97.83(10) . . . . ?
C1 P1 Si1 C21 119.93(10) . . . . ?
Si2 P1 Si1 C21 -20.34(9) . . . . ?
C1 P1 Si2 C24 -70.27(12) . . . . ?
Si1 P1 Si2 C24 58.64(10) . . . . ?
C1 P1 Si2 C22 172.16(10) . . . . ?
Si1 P1 Si2 C22 -58.93(9) . . . . ?
C1 P1 Si2 C23 57.48(12) . . . . ?
Si1 P1 Si2 C23 -173.61(10) . . . . ?
Si2 P1 C1 C2 -131.92(11) . . . . ?
Si1 P1 C1 C2 96.96(12) . . . . ?
Si2 P1 C1 C6 64.62(17) . . . . ?
Si1 P1 C1 C6 -66.51(16) . . . . ?
C6 C1 C2 C3 15.5(2) . . . . ?
P1 C1 C2 C3 -149.54(13) . . . . ?
C6 C1 C2 C7 -163.11(16) . . . . ?
P1 C1 C2 C7 31.8(2) . . . . ?
C1 C2 C3 C4 -4.5(3) . . . . ?
C7 C2 C3 C4 174.27(16) . . . . ?
C2 C3 C4 C5 -7.6(3) . . . . ?
C2 C3 C4 C11 175.06(16) . . . . ?
C3 C4 C5 C6 8.8(3) . . . . ?
C11 C4 C5 C6 -173.84(16) . . . . ?
C4 C5 C6 C1 2.2(3) . . . . ?
C4 C5 C6 C15 -174.10(16) . . . . ?
C2 C1 C6 C5 -14.4(2) . . . . ?
P1 C1 C6 C5 148.36(14) . . . . ?
C2 C1 C6 C15 161.58(15) . . . . ?
P1 C1 C6 C15 -35.6(2) . . . . ?
C3 C2 C7 C9 95.75(18) . . . . ?
C1 C2 C7 C9 -85.6(2) . . . . ?
C3 C2 C7 C8 -139.09(16) . . . . ?
C1 C2 C7 C8 39.6(2) . . . . ?
C3 C2 C7 C10 -23.0(2) . . . . ?
C1 C2 C7 C10 155.66(17) . . . . ?
C3 C4 C11 C13B -79(4) . . . . ?
C5 C4 C11 C13B 104(4) . . . . ?
C3 C4 C11 C14A -132.2(2) . . . . ?
C5 C4 C11 C14A 50.7(3) . . . . ?
C3 C4 C11 C13A 106.3(3) . . . . ?
C5 C4 C11 C13A -70.9(3) . . . . ?
C3 C4 C11 C14B 51(3) . . . . ?
C5 C4 C11 C14B -126(3) . . . . ?
C3 C4 C11 C12A -12.6(3) . . . . ?
C5 C4 C11 C12A 170.20(19) . . . . ?
C3 C4 C11 C12B 163(2) . . . . ?
C5 C4 C11 C12B -14(2) . . . . ?
C5 C6 C15 C17 -111.48(17) . . . . ?
C1 C6 C15 C17 72.5(2) . . . . ?
C5 C6 C15 C18 125.00(16) . . . . ?
C1 C6 C15 C18 -51.0(2) . . . . ?
C5 C6 C15 C16 8.3(2) . . . . ?
C1 C6 C15 C16 -167.72(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.38
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.053
