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

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

data_ba_cs2_4
_database_code_depnum_ccdc_archive 'CCDC 1437764'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;

_audit_creation_method           olex2
_audit_block_code                ba_cs2
_audit_block_refno               1716
_audit_block_usercomment         'cs07, irregular, colourless'
_audit_creation_date             
;
'Mon Mar 04 15:40:02 2013'
;




_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H42 N2 P2 Si4'
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      110(1)
_chemical_formula_weight         532.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   7.1947(2)
_cell_length_b                   8.3354(2)
_cell_length_c                   13.4789(3)
_cell_angle_alpha                86.273(2)
_cell_angle_beta                 78.908(2)
_cell_angle_gamma                73.161(3)
_cell_volume                     759.19(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    110(1)
_cell_measurement_reflns_used    15413
_cell_measurement_theta_min      5.5080
_cell_measurement_theta_max      70.7340
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_F_000             286
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2107
_exptl_crystal_size_mid          0.0953
_exptl_crystal_size_min          0.0816
_exptl_absorpt_coefficient_mu    2.920
_shelx_estimated_absorpt_T_min   0.578
_shelx_estimated_absorpt_T_max   0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72195
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_reflns_number            22999
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.341
_diffrn_reflns_theta_max         70.888
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             2845
_reflns_number_gt                2583
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  
'encif (Wadepohl, 2012); encifer 1.4 (CCDC, 2011)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0462P)²+0.9522P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     iterative
_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         2845
_refine_ls_number_parameters     177
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1112
_refine_ls_wR_factor_gt          0.1089
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1A P 0.62265(14) 0.52117(9) 0.03188(6) 0.0276(3) Uani 0.781(3) 1 d . . P A 1
P1B P 0.4817(6) 0.5511(4) 0.0780(2) 0.0389(12) Uani 0.219(3) 1 d . . P A 2
Si1 Si 0.64512(9) 0.80977(7) 0.15864(4) 0.02663(18) Uani 1 1 d . . . . .
Si2 Si 0.73834(9) 0.44052(7) 0.24462(4) 0.02606(17) Uani 1 1 d . . . . .
N N 0.7212(3) 0.6530(2) 0.24582(13) 0.0269(4) Uani 1 1 d . . . . .
C1A C 0.4992(6) 0.7358(4) 0.0788(3) 0.0283(7) Uani 0.781(3) 1 d . . P A 1
H1AA H 0.3678 0.7393 0.1193 0.034 Uiso 0.781(3) 1 calc R U P A 1
H1AB H 0.4788 0.8132 0.0204 0.034 Uiso 0.781(3) 1 calc R U P A 1
C1B C 0.613(2) 0.7092(15) 0.0419(9) 0.036(3) Uani 0.219(3) 1 d . . P A 2
H1BA H 0.5376 0.7969 0.0000 0.043 Uiso 0.219(3) 1 calc R U P A 2
H1BB H 0.7438 0.6568 0.0009 0.043 Uiso 0.219(3) 1 calc R U P A 2
C2A C 0.5888(6) 0.4068(4) 0.1519(3) 0.0277(7) Uani 0.781(3) 1 d . . P A 1
H2AA H 0.6252 0.2856 0.1376 0.033 Uiso 0.781(3) 1 calc R U P A 1
H2AB H 0.4473 0.4420 0.1834 0.033 Uiso 0.781(3) 1 calc R U P A 1
C2B C 0.687(2) 0.3911(16) 0.1216(10) 0.033(3) Uani 0.219(3) 1 d . . P A 2
H2BA H 0.8082 0.3787 0.0696 0.039 Uiso 0.219(3) 1 calc R U P A 2
H2BB H 0.6565 0.2821 0.1280 0.039 Uiso 0.219(3) 1 calc R U P A 2
C3 C 0.8555(4) 0.8732(4) 0.0837(2) 0.0500(7) Uani 1 1 d . . . . .
H3A H 0.9182 0.9201 0.1286 0.075 Uiso 1 1 calc R U . . .
H3B H 0.8084 0.9581 0.0335 0.075 Uiso 1 1 calc R U . . .
H3C H 0.9517 0.7753 0.0492 0.075 Uiso 1 1 calc R U . . .
C4 C 0.4676(4) 0.9969(3) 0.2261(2) 0.0457(7) Uani 1 1 d . . . . .
H4A H 0.3590 0.9635 0.2696 0.069 Uiso 1 1 calc R U . . .
H4B H 0.4149 1.0807 0.1766 0.069 Uiso 1 1 calc R U . . .
H4C H 0.5357 1.0449 0.2676 0.069 Uiso 1 1 calc R U . . .
C5 C 0.9979(5) 0.3117(4) 0.2148(3) 0.0567(8) Uani 1 1 d . . . . .
H5A H 1.0612 0.3481 0.1497 0.085 Uiso 1 1 calc R U . . .
H5B H 1.0022 0.1936 0.2109 0.085 Uiso 1 1 calc R U . . .
H5C H 1.0679 0.3249 0.2679 0.085 Uiso 1 1 calc R U . . .
C6 C 0.6246(5) 0.3737(4) 0.3700(2) 0.0510(8) Uani 1 1 d . . . . .
H6A H 0.6790 0.4100 0.4230 0.076 Uiso 1 1 calc R U . . .
H6B H 0.6535 0.2513 0.3721 0.076 Uiso 1 1 calc R U . . .
H6C H 0.4814 0.4245 0.3809 0.076 Uiso 1 1 calc R U . . .
C7 C 0.8095(4) 0.7029(3) 0.32175(17) 0.0306(5) Uani 1 1 d . . . . .
C8 C 1.0107(4) 0.6877(4) 0.3041(2) 0.0455(7) Uani 1 1 d . . . . .
H8 H 1.0912 0.6442 0.2418 0.055 Uiso 1 1 calc R U . . .
C9 C 1.0934(6) 0.7362(4) 0.3777(3) 0.0685(11) Uani 1 1 d . . . . .
H9 H 1.2310 0.7255 0.3657 0.082 Uiso 1 1 calc R U . . .
C10 C 0.9781(7) 0.7997(4) 0.4680(3) 0.0772(13) Uani 1 1 d . . . . .
H10 H 1.0359 0.8329 0.5180 0.093 Uiso 1 1 calc R U . . .
C11 C 0.7792(7) 0.8150(4) 0.4859(2) 0.0653(10) Uani 1 1 d . . . . .
H11 H 0.6997 0.8588 0.5483 0.078 Uiso 1 1 calc R U . . .
C12 C 0.6938(5) 0.7666(3) 0.41313(19) 0.0425(6) Uani 1 1 d . . . . .
H12 H 0.5563 0.7771 0.4259 0.051 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1A C2A 1.835(4) . ?
P1A C1A 1.844(3) . ?
P1A P1A 2.2275(15) 2_665 ?
P1B C1B 1.822(14) . ?
P1B C2B 1.845(15) . ?
P1B P1B 2.259(6) 2_665 ?
Si1 N 1.7382(18) . ?
Si1 C3 1.843(3) . ?
Si1 C4 1.864(3) . ?
Si1 C1A 1.881(3) . ?
Si1 C1B 1.913(11) . ?
Si2 N 1.7405(18) . ?
Si2 C5 1.846(3) . ?
Si2 C6 1.856(3) . ?
Si2 C2B 1.862(13) . ?
Si2 C2A 1.881(3) . ?
N C7 1.443(3) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C2B H2BA 0.9900 . ?
C2B H2BB 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C12 1.388(4) . ?
C7 C8 1.391(4) . ?
C8 C9 1.386(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.375(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.374(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.388(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2A P1A C1A 98.56(17) . . ?
C2A P1A P1A 98.51(12) . 2_665 ?
C1A P1A P1A 98.59(12) . 2_665 ?
C1B P1B C2B 96.7(7) . . ?
C1B P1B P1B 97.6(4) . 2_665 ?
C2B P1B P1B 98.2(5) . 2_665 ?
N Si1 C3 111.54(12) . . ?
N Si1 C4 109.64(11) . . ?
C3 Si1 C4 108.60(14) . . ?
N Si1 C1A 108.56(11) . . ?
C3 Si1 C1A 113.19(16) . . ?
C4 Si1 C1A 105.07(16) . . ?
N Si1 C1B 108.9(4) . . ?
C3 Si1 C1B 90.4(5) . . ?
C4 Si1 C1B 126.0(5) . . ?
N Si2 C5 111.44(12) . . ?
N Si2 C6 110.05(11) . . ?
C5 Si2 C6 108.53(16) . . ?
N Si2 C2B 108.7(4) . . ?
C5 Si2 C2B 92.1(5) . . ?
C6 Si2 C2B 124.5(5) . . ?
N Si2 C2A 108.62(12) . . ?
C5 Si2 C2A 111.87(17) . . ?
C6 Si2 C2A 106.20(16) . . ?
C7 N Si1 114.23(14) . . ?
C7 N Si2 115.51(14) . . ?
Si1 N Si2 129.57(11) . . ?
P1A C1A Si1 112.58(18) . . ?
P1A C1A H1AA 109.1 . . ?
Si1 C1A H1AA 109.1 . . ?
P1A C1A H1AB 109.1 . . ?
Si1 C1A H1AB 109.1 . . ?
H1AA C1A H1AB 107.8 . . ?
P1B C1B Si1 111.0(6) . . ?
P1B C1B H1BA 109.4 . . ?
Si1 C1B H1BA 109.4 . . ?
P1B C1B H1BB 109.4 . . ?
Si1 C1B H1BB 109.4 . . ?
H1BA C1B H1BB 108.0 . . ?
P1A C2A Si2 114.01(18) . . ?
P1A C2A H2AA 108.7 . . ?
Si2 C2A H2AA 108.7 . . ?
P1A C2A H2AB 108.7 . . ?
Si2 C2A H2AB 108.7 . . ?
H2AA C2A H2AB 107.6 . . ?
P1B C2B Si2 113.8(7) . . ?
P1B C2B H2BA 108.8 . . ?
Si2 C2B H2BA 108.8 . . ?
P1B C2B H2BB 108.8 . . ?
Si2 C2B H2BB 108.8 . . ?
H2BA C2B H2BB 107.7 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C7 C8 119.4(2) . . ?
C12 C7 N 120.2(2) . . ?
C8 C7 N 120.4(2) . . ?
C9 C8 C7 119.8(3) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C10 C9 C8 120.6(3) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C11 C10 C9 119.9(3) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 120.3(3) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C7 C12 C11 120.0(3) . . ?
C7 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 Si1 N C7 63.4(2) . . . . ?
C4 Si1 N C7 -56.9(2) . . . . ?
C1A Si1 N C7 -171.2(2) . . . . ?
C1B Si1 N C7 161.6(5) . . . . ?
C3 Si1 N Si2 -106.54(18) . . . . ?
C4 Si1 N Si2 133.13(16) . . . . ?
C1A Si1 N Si2 18.9(2) . . . . ?
C1B Si1 N Si2 -8.3(6) . . . . ?
C5 Si2 N C7 -63.2(2) . . . . ?
C6 Si2 N C7 57.3(2) . . . . ?
C2B Si2 N C7 -163.2(5) . . . . ?
C2A Si2 N C7 173.2(2) . . . . ?
C5 Si2 N Si1 106.69(19) . . . . ?
C6 Si2 N Si1 -132.86(17) . . . . ?
C2B Si2 N Si1 6.7(5) . . . . ?
C2A Si2 N Si1 -17.0(2) . . . . ?
C2A P1A C1A Si1 70.8(2) . . . . ?
P1A P1A C1A Si1 170.83(16) 2_665 . . . ?
N Si1 C1A P1A -47.3(2) . . . . ?
C3 Si1 C1A P1A 77.2(2) . . . . ?
C4 Si1 C1A P1A -164.50(17) . . . . ?
C1B Si1 C1A P1A 47.8(8) . . . . ?
C2B P1B C1B Si1 -73.3(8) . . . . ?
P1B P1B C1B Si1 -172.6(6) 2_665 . . . ?
C1A P1A C2A Si2 -69.3(2) . . . . ?
P1A P1A C2A Si2 -169.40(18) 2_665 . . . ?
N Si2 C2A P1A 43.9(3) . . . . ?
C5 Si2 C2A P1A -79.5(2) . . . . ?
C6 Si2 C2A P1A 162.2(2) . . . . ?
C2B Si2 C2A P1A -50.1(11) . . . . ?
C1B P1B C2B Si2 73.2(9) . . . . ?
P1B P1B C2B Si2 171.9(7) 2_665 . . . ?
N Si2 C2B P1B -41.4(9) . . . . ?
C5 Si2 C2B P1B -154.9(7) . . . . ?
C6 Si2 C2B P1B 90.9(7) . . . . ?
C2A Si2 C2B P1B 52.3(9) . . . . ?
Si1 N C7 C12 92.3(2) . . . . ?
Si2 N C7 C12 -96.2(2) . . . . ?
Si1 N C7 C8 -87.6(2) . . . . ?
Si2 N C7 C8 83.8(2) . . . . ?
C12 C7 C8 C9 0.0(4) . . . . ?
N C7 C8 C9 180.0(2) . . . . ?
C7 C8 C9 C10 -0.1(5) . . . . ?
C8 C9 C10 C11 0.2(5) . . . . ?
C9 C10 C11 C12 0.0(5) . . . . ?
C8 C7 C12 C11 0.2(4) . . . . ?
N C7 C12 C11 -179.8(2) . . . . ?
C10 C11 C12 C7 -0.2(4) . . . . ?

_refine_diff_density_max         1.082
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.058

_shelxl_version_number           2013-2

_cell_oxdiff_length_a            7.1947(2)
_cell_oxdiff_length_b            8.3354(2)
_cell_oxdiff_length_c            13.4789(3)
_cell_oxdiff_angle_alpha         86.273(2)
_cell_oxdiff_angle_beta          78.908(2)
_cell_oxdiff_angle_gamma         73.161(2)
_cell_oxdiff_volume              759.19(3)
_cell_oxdiff_measurement_reflns_used 15413
_cell_oxdiff_twin_number         2
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -0.5801 0.1576 -0.3943 -1.1162 0.6078 0.2389 0.3732 1.4141 -0.4442
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2 5 2 0.0466 1.9978 4.9987 1.9952 -0.4615 -0.8251 -0.0862
1 -4 -2 0.0408 1.0005 -3.9982 -1.9963 0.2685 0.5635 0.6539
-1 4 2 0.0408 -1.0005 3.9982 1.9963 -0.2685 -0.5635 -0.6539
-4 -4 -1 0.0653 -3.9971 -3.9996 -0.9961 0.4831 0.7336 -0.4771
0 -1 8 0.0433 0.0015 -0.9979 7.9995 0.8457 -0.4247 -0.1147
3 0 -4 0.0889 2.9981 0.0001 -3.9996 -0.4377 0.1289 0.7678
2 -2 7 0.0695 2.0008 -1.9970 7.0004 0.8241 -0.3332 0.4486
0 1 -8 0.0433 -0.0015 0.9979 -7.9995 -0.8457 0.4247 0.1147
_diffrn_radiation_monochromator  mirror
_diffrn_orient_matrix_UB_11      -0.0247107000
_diffrn_orient_matrix_UB_12      -0.1187391000
_diffrn_orient_matrix_UB_13      0.0909153000
_diffrn_orient_matrix_UB_21      -0.0476067000
_diffrn_orient_matrix_UB_22      -0.1189281000
_diffrn_orient_matrix_UB_23      -0.0679146000
_diffrn_orient_matrix_UB_31      0.2210908000
_diffrn_orient_matrix_UB_32      -0.0951275000
_diffrn_orient_matrix_UB_33      -0.0262426000
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.7953 22595 409
2 0.2047 0 409
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -66.00   19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 85

#__ type_ start__ end____ width___ exp.time_
  2 omega  -67.00  -40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
  3 omega  -39.00   21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 60

#__ type_ start__ end____ width___ exp.time_
  4 omega  -22.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000   30.0000 82

#__ type_ start__ end____ width___ exp.time_
  5 omega   -6.00   19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   80.0000    6.9416 25

#__ type_ start__ end____ width___ exp.time_
  6 omega    8.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -21.9304 27

#__ type_ start__ end____ width___ exp.time_
  7 omega    7.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  -94.2727 25

#__ type_ start__ end____ width___ exp.time_
  8 omega    8.00   38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  164.4443 30

#__ type_ start__ end____ width___ exp.time_
  9 omega   14.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000   78.6284 27

#__ type_ start__ end____ width___ exp.time_
 10 omega   14.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -144.5204 25

#__ type_ start__ end____ width___ exp.time_
 11 omega   14.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   19.9077 26

#__ type_ start__ end____ width___ exp.time_
 12 omega   21.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   75.0000  -56.8140 36

#__ type_ start__ end____ width___ exp.time_
 13 omega   18.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  147.9313 25

#__ type_ start__ end____ width___ exp.time_
 14 omega   91.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   75.0000  -56.8140 27

#__ type_ start__ end____ width___ exp.time_
 15 omega   30.00   58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -180.0000 28

#__ type_ start__ end____ width___ exp.time_
 16 omega   28.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -124.8147 27

#__ type_ start__ end____ width___ exp.time_
 17 omega   99.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -124.8147 29

#__ type_ start__ end____ width___ exp.time_
 18 omega   32.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000  131.4379 33

#__ type_ start__ end____ width___ exp.time_
 19 omega  102.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000  131.4379 25

#__ type_ start__ end____ width___ exp.time_
 20 omega   30.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   28.2664 27

#__ type_ start__ end____ width___ exp.time_
 21 omega   38.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   69.0000  153.4029 52

#__ type_ start__ end____ width___ exp.time_
 22 omega   33.00   58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -17.0796 25

#__ type_ start__ end____ width___ exp.time_
 23 omega   86.00  125.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   96.4571 39

#__ type_ start__ end____ width___ exp.time_
 24 omega   96.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   69.0000  153.4029 34

#__ type_ start__ end____ width___ exp.time_
 25 omega   -8.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  124.2867 101

#__ type_ start__ end____ width___ exp.time_
 26 omega   46.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   42.0000  -17.8207 27

#__ type_ start__ end____ width___ exp.time_
 27 omega   91.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   61.0000 -149.3710 39

#__ type_ start__ end____ width___ exp.time_
 28 omega   34.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -124.3660 32

#__ type_ start__ end____ width___ exp.time_
 29 omega   33.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   96.4571 28

#__ type_ start__ end____ width___ exp.time_
 30 omega   42.00   76.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   61.0000 -149.3710 34

#__ type_ start__ end____ width___ exp.time_
 31 omega   44.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   61.0000  -76.5220 27

#__ type_ start__ end____ width___ exp.time_
 32 omega   53.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000   23.4079 27

#__ type_ start__ end____ width___ exp.time_
 33 omega   47.00   76.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   43.0000  -44.6197 29

#__ type_ start__ end____ width___ exp.time_
 34 omega   44.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000   45.4909 95

#__ type_ start__ end____ width___ exp.time_
 35 omega   28.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -80.0000  -74.8450 45

#__ type_ start__ end____ width___ exp.time_
 36 omega    5.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -78.0000 -130.3116 100

#__ type_ start__ end____ width___ exp.time_
 37 omega   44.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  138.7883 29

#__ type_ start__ end____ width___ exp.time_
 38 omega   57.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   58.0000 -111.8009 30

#__ type_ start__ end____ width___ exp.time_
 39 omega   55.00  126.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   66.0000  -31.8255 71

#__ type_ start__ end____ width___ exp.time_
 40 omega   15.00   97.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -79.0000   -3.7954 82

#__ type_ start__ end____ width___ exp.time_
 41 omega   55.00   90.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000  172.1519 35

#__ type_ start__ end____ width___ exp.time_
 42 omega  105.00  145.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   73.0000  -16.5479 40

#__ type_ start__ end____ width___ exp.time_
 43 omega   58.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   73.0000  -16.5479 41

#__ type_ start__ end____ width___ exp.time_
 44 omega   65.00   94.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   57.0000 -143.7746 29

#__ type_ start__ end____ width___ exp.time_
 45 omega   83.00  119.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0000   64.0000   89.8321 36

#__ type_ start__ end____ width___ exp.time_
 46 omega   79.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
 47 omega  138.00  165.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 48 omega   87.00  119.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 32

#__ type_ start__ end____ width___ exp.time_
 49 omega   79.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
 50 omega   79.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 51 omega   42.00   86.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   -2.0499 44

#__ type_ start__ end____ width___ exp.time_
 52 omega   78.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 53 omega   86.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 88

#__ type_ start__ end____ width___ exp.time_
 54 omega  139.00  173.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 34

#__ type_ start__ end____ width___ exp.time_
 55 omega   78.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 56 omega  131.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 43

#__ type_ start__ end____ width___ exp.time_
 57 omega   87.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 29

#__ type_ start__ end____ width___ exp.time_
 58 omega  121.00  168.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 47

#__ type_ start__ end____ width___ exp.time_
 59 omega   85.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 90

#__ type_ start__ end____ width___ exp.time_
 60 omega   37.00  139.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -34.6646 102

#__ type_ start__ end____ width___ exp.time_
 61 omega   77.00  105.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   42.1797 28

#__ type_ start__ end____ width___ exp.time_
 62 omega   83.00  119.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -150.0000 36

#__ type_ start__ end____ width___ exp.time_
 63 omega  108.00  139.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -122.2935 31

#__ type_ start__ end____ width___ exp.time_
 64 omega   40.00   65.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   42.1797 25

#__ type_ start__ end____ width___ exp.time_
 65 omega   82.00  163.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   90.0000 81

#__ type_ start__ end____ width___ exp.time_
 66 omega   50.00  100.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -122.2935 50

#__ type_ start__ end____ width___ exp.time_
 67 omega   93.00  143.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  -90.0000 50

#__ type_ start__ end____ width___ exp.time_
 68 omega  137.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 37

#__ type_ start__ end____ width___ exp.time_
 69 omega   85.00  121.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   30.0000 36

#__ type_ start__ end____ width___ exp.time_
 70 omega   85.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 89

#__ type_ start__ end____ width___ exp.time_
 71 omega   85.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 90

#__ type_ start__ end____ width___ exp.time_
 72 omega   85.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 89

#__ type_ start__ end____ width___ exp.time_
 73 omega   82.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 74 omega   38.00  138.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  119.7465 100

#__ type_ start__ end____ width___ exp.time_
 75 omega   85.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 89

#__ type_ start__ end____ width___ exp.time_
 76 omega   86.00  113.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
 77 omega   85.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 78 omega   85.00  134.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 49

#__ type_ start__ end____ width___ exp.time_
 79 omega   52.00   96.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
 80 omega   80.00  164.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 84

#__ type_ start__ end____ width___ exp.time_
 81 omega   78.00  105.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
 82 omega   83.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 83 omega  115.00  143.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 28

#__ type_ start__ end____ width___ exp.time_
 84 omega   79.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
 85 omega   83.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
 86 omega   57.00   92.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  150.0000 35

#__ type_ start__ end____ width___ exp.time_
 87 omega   79.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
 88 omega  -72.00   26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   60.0000 98

#__ type_ start__ end____ width___ exp.time_
 89 omega  -25.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000 -180.0000 90

#__ type_ start__ end____ width___ exp.time_
 90 omega   -2.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   67.0000   40.2977 92

#__ type_ start__ end____ width___ exp.time_
 91 omega   -6.00   46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   80.0000    6.9416 52

#__ type_ start__ end____ width___ exp.time_
 92 omega   -4.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000 -131.8738 100

#__ type_ start__ end____ width___ exp.time_
 93 omega    7.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  -94.2727 40

#__ type_ start__ end____ width___ exp.time_
 94 omega    6.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -21.9304 40

#__ type_ start__ end____ width___ exp.time_
 95 omega   10.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000   99.4925 36

#__ type_ start__ end____ width___ exp.time_
 96 omega   14.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -144.5204 32

#__ type_ start__ end____ width___ exp.time_
 97 omega  -19.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000    0.0000 146

#__ type_ start__ end____ width___ exp.time_
 98 omega  -19.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000  120.0000 146

#__ type_ start__ end____ width___ exp.time_
 99 omega  -19.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000    0.0000 146

#__ type_ start__ end____ width___ exp.time_
100 omega  -19.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000  120.0000 146

#__ type_ start__ end____ width___ exp.time_
101 omega  -19.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000  240.0000 146

#__ type_ start__ end____ width___ exp.time_
102 omega   29.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -139.8469 99

#__ type_ start__ end____ width___ exp.time_
103 omega   31.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000  131.4379 96

#__ type_ start__ end____ width___ exp.time_
104 omega  -12.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -78.0000 -177.7045 101

#__ type_ start__ end____ width___ exp.time_
105 omega   33.00  132.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -124.3660 99

#__ type_ start__ end____ width___ exp.time_
106 omega   -9.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  124.2867 103

#__ type_ start__ end____ width___ exp.time_
107 omega   37.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   69.0000  153.4029 93

#__ type_ start__ end____ width___ exp.time_
108 omega   32.00  132.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -17.0796 100

#__ type_ start__ end____ width___ exp.time_
109 omega   40.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   61.0000 -149.3710 90

#__ type_ start__ end____ width___ exp.time_
110 omega   44.00  134.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   61.0000  -76.5220 90

#__ type_ start__ end____ width___ exp.time_
111 omega   42.00  138.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   42.0000  178.8996 96

#__ type_ start__ end____ width___ exp.time_
112 omega   42.00  134.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000   23.4079 92

#__ type_ start__ end____ width___ exp.time_
113 omega   42.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000   45.4909 97

#__ type_ start__ end____ width___ exp.time_
114 omega   46.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   43.0000  -44.6197 96

#__ type_ start__ end____ width___ exp.time_
115 omega    4.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -78.0000 -130.3116 101

#__ type_ start__ end____ width___ exp.time_
116 omega   44.00  144.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  138.7883 100

#__ type_ start__ end____ width___ exp.time_
117 omega    3.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -80.0000  -74.8450 103

#__ type_ start__ end____ width___ exp.time_
118 omega   55.00  146.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   66.0000  -31.8255 91

#__ type_ start__ end____ width___ exp.time_
119 omega   57.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   58.0000 -111.8009 90

#__ type_ start__ end____ width___ exp.time_
120 omega   86.00  166.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   90.0000 80

#__ type_ start__ end____ width___ exp.time_
121 omega   38.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000   90.0000 66

;
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration .
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent EOS'
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_jb7_5
_database_code_depnum_ccdc_archive 'CCDC 1437765'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;

_audit_creation_method           olex2
_audit_block_code                ba_jb7
_audit_block_refno               1731
_audit_block_usercomment         'jb109, plate, colourless'
_audit_creation_date             
;
'Wed Mar 20 17:58:34 2013'
;




_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H63 Li3 N3 O6 P Si3'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      110(1)
_chemical_formula_weight         805.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.4277(2)
_cell_length_b                   13.1483(2)
_cell_length_c                   14.8044(3)
_cell_angle_alpha                106.9639(16)
_cell_angle_beta                 92.2955(16)
_cell_angle_gamma                98.2181(15)
_cell_volume                     2281.50(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(1)
_cell_measurement_reflns_used    23109
_cell_measurement_theta_min      3.5730
_cell_measurement_theta_max      70.4230
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.639
_shelx_estimated_absorpt_T_min   0.853
_shelx_estimated_absorpt_T_max   0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.56582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_reflns_number            67698
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.561
_diffrn_reflns_theta_max         71.142
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             9598
_reflns_number_gt                7720
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  
'encif (Wadepohl, 2012); encifer 1.4 (CCDC, 2011)'

_refine_special_details          
;
 Refined as a 2-component twin against singles and composites
 involving component 1 only.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0874P)²+1.4587P]
 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         9598
_refine_ls_number_parameters     503
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1576
_refine_ls_wR_factor_gt          0.1485
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P P 0.68668(5) 0.75941(6) 0.74779(5) 0.02181(18) Uani 1 1 d . . . . .
Si1 Si 0.64525(6) 0.97101(6) 0.70588(6) 0.02377(19) Uani 1 1 d . . . . .
Si2 Si 0.87855(6) 0.68203(6) 0.64145(6) 0.02291(19) Uani 1 1 d . . . . .
Si3 Si 0.57125(6) 0.65462(6) 0.89404(6) 0.02275(19) Uani 1 1 d . . . . .
O1 O 0.92617(17) 0.92839(17) 0.53182(15) 0.0286(5) Uani 1 1 d . . . . .
O2 O 0.91512(18) 0.94628(17) 0.93002(15) 0.0301(5) Uani 1 1 d . . . . .
O3 O 0.74221(15) 0.46152(16) 0.99886(15) 0.0267(5) Uani 1 1 d . . . . .
O4 O 0.92519(18) 0.36431(19) 1.02186(18) 0.0379(6) Uani 1 1 d . . . . .
N1 N 0.78430(18) 0.99376(18) 0.73324(16) 0.0197(5) Uani 1 1 d . . . . .
N2 N 0.94900(18) 0.80831(18) 0.70015(17) 0.0208(5) Uani 1 1 d . . . . .
N3 N 0.51168(18) 0.53224(19) 0.90336(18) 0.0229(5) Uani 1 1 d . . . . .
C1 C 0.5863(2) 0.8415(2) 0.7294(2) 0.0273(7) Uani 1 1 d . . . . .
H1A H 0.5459 0.8590 0.7852 0.033 Uiso 1 1 calc R U . . .
H1B H 0.5349 0.7990 0.6763 0.033 Uiso 1 1 calc R U . . .
C2 C 0.7331(2) 0.7040(2) 0.6284(2) 0.0240(6) Uani 1 1 d . . . . .
H2A H 0.7281 0.7539 0.5920 0.029 Uiso 1 1 calc R U . . .
H2B H 0.6869 0.6363 0.5950 0.029 Uiso 1 1 calc R U . . .
C3 C 0.6060(2) 0.6414(2) 0.7685(2) 0.0253(6) Uani 1 1 d . . . . .
H3A H 0.6456 0.5814 0.7482 0.030 Uiso 1 1 calc R U . . .
H3B H 0.5383 0.6230 0.7282 0.030 Uiso 1 1 calc R U . . .
C4 C 0.5757(3) 1.0785(3) 0.7819(3) 0.0427(9) Uani 1 1 d . . . . .
H4A H 0.6003 1.0921 0.8472 0.064 Uiso 1 1 calc R U . . .
H4B H 0.4982 1.0550 0.7729 0.064 Uiso 1 1 calc R U . . .
H4C H 0.5929 1.1434 0.7644 0.064 Uiso 1 1 calc R U . . .
C5 C 0.6024(3) 0.9545(3) 0.5788(3) 0.0387(8) Uani 1 1 d . . . . .
H5A H 0.6256 1.0208 0.5650 0.058 Uiso 1 1 calc R U . . .
H5B H 0.5244 0.9361 0.5681 0.058 Uiso 1 1 calc R U . . .
H5C H 0.6352 0.8981 0.5383 0.058 Uiso 1 1 calc R U . . .
C6 C 0.8477(2) 1.0919(2) 0.7384(2) 0.0208(6) Uani 1 1 d . . . . .
C7 C 0.8135(2) 1.1727(2) 0.7029(2) 0.0249(6) Uani 1 1 d . . . . .
H7 H 0.7422 1.1627 0.6764 0.030 Uiso 1 1 calc R U . . .
C8 C 0.8843(3) 1.2663(2) 0.7068(2) 0.0278(7) Uani 1 1 d . . . . .
H8 H 0.8591 1.3178 0.6835 0.033 Uiso 1 1 calc R U . . .
C9 C 0.9914(3) 1.2843(2) 0.7446(2) 0.0312(7) Uani 1 1 d . . . . .
H9 H 1.0385 1.3463 0.7456 0.037 Uiso 1 1 calc R U . . .
C10 C 1.0269(2) 1.2076(3) 0.7809(2) 0.0294(7) Uani 1 1 d . . . . .
H10 H 1.0986 1.2183 0.8067 0.035 Uiso 1 1 calc R U . . .
C11 C 0.9562(2) 1.1152(2) 0.7791(2) 0.0234(6) Uani 1 1 d . . . . .
H11 H 0.9816 1.0664 0.8059 0.028 Uiso 1 1 calc R U . . .
C12 C 0.9271(3) 0.6264(3) 0.5214(3) 0.0368(8) Uani 1 1 d . . . . .
H12A H 0.9132 0.6711 0.4827 0.055 Uiso 1 1 calc R U . . .
H12B H 0.8889 0.5545 0.4923 0.055 Uiso 1 1 calc R U . . .
H12C H 1.0040 0.6250 0.5279 0.055 Uiso 1 1 calc R U . . .
C13 C 0.8772(3) 0.5731(3) 0.7011(3) 0.0349(8) Uani 1 1 d . . . . .
H13A H 0.9432 0.5428 0.6911 0.052 Uiso 1 1 calc R U . . .
H13B H 0.8155 0.5176 0.6747 0.052 Uiso 1 1 calc R U . . .
H13C H 0.8721 0.6034 0.7679 0.052 Uiso 1 1 calc R U . . .
C14 C 1.0602(2) 0.8263(2) 0.7284(2) 0.0245(6) Uani 1 1 d . . . . .
C15 C 1.1258(2) 0.9250(2) 0.7329(2) 0.0265(6) Uani 1 1 d . . . . .
H15 H 1.0941 0.9759 0.7135 0.032 Uiso 1 1 calc R U . . .
C16 C 1.2354(2) 0.9491(3) 0.7651(3) 0.0357(8) Uani 1 1 d . . . . .
H16 H 1.2752 1.0154 0.7671 0.043 Uiso 1 1 calc R U . . .
C17 C 1.2863(3) 0.8757(3) 0.7944(3) 0.0464(10) Uani 1 1 d . . . . .
H17 H 1.3596 0.8917 0.8169 0.056 Uiso 1 1 calc R U . . .
C18 C 1.2242(3) 0.7775(3) 0.7889(3) 0.0508(11) Uani 1 1 d . . . . .
H18 H 1.2571 0.7264 0.8070 0.061 Uiso 1 1 calc R U . . .
C19 C 1.1147(3) 0.7532(3) 0.7572(3) 0.0399(9) Uani 1 1 d . . . . .
H19 H 1.0760 0.6864 0.7549 0.048 Uiso 1 1 calc R U . . .
C20 C 0.7033(3) 0.6998(3) 0.9705(3) 0.0348(8) Uani 1 1 d . . . . .
H20A H 0.6909 0.6973 1.0335 0.052 Uiso 1 1 calc R U . . .
H20B H 0.7322 0.7723 0.9726 0.052 Uiso 1 1 calc R U . . .
H20C H 0.7544 0.6531 0.9446 0.052 Uiso 1 1 calc R U . . .
C21 C 0.4882(3) 0.7650(3) 0.9386(3) 0.0342(7) Uani 1 1 d . . . . .
H21A H 0.4255 0.7539 0.8947 0.051 Uiso 1 1 calc R U . . .
H21B H 0.5319 0.8334 0.9443 0.051 Uiso 1 1 calc R U . . .
H21C H 0.4649 0.7641 0.9994 0.051 Uiso 1 1 calc R U . . .
C22 C 0.4396(2) 0.4599(2) 0.8314(2) 0.0236(6) Uani 1 1 d . . . . .
C23 C 0.4312(3) 0.3480(3) 0.8169(3) 0.0360(8) Uani 1 1 d . . . . .
H23 H 0.4759 0.3238 0.8554 0.043 Uiso 1 1 calc R U . . .
C24 C 0.3588(3) 0.2729(3) 0.7474(3) 0.0467(10) Uani 1 1 d . . . . .
H24 H 0.3561 0.1999 0.7402 0.056 Uiso 1 1 calc R U . . .
C25 C 0.2909(3) 0.3047(3) 0.6889(3) 0.0425(9) Uani 1 1 d . . . . .
H25 H 0.2427 0.2541 0.6421 0.051 Uiso 1 1 calc R U . . .
C26 C 0.2961(3) 0.4144(3) 0.7014(3) 0.0367(8) Uani 1 1 d . . . . .
H26 H 0.2504 0.4375 0.6629 0.044 Uiso 1 1 calc R U . . .
C27 C 0.3679(2) 0.4891(3) 0.7702(2) 0.0289(7) Uani 1 1 d . . . . .
H27 H 0.3693 0.5618 0.7768 0.035 Uiso 1 1 calc R U . . .
C28 C 1.0281(3) 0.9004(3) 0.4980(2) 0.0316(7) Uani 1 1 d . . . . .
H28A H 1.0173 0.8620 0.4307 0.038 Uiso 1 1 calc R U . . .
H28B H 1.0540 0.8532 0.5305 0.038 Uiso 1 1 calc R U . . .
C29 C 0.8882(3) 1.0000(3) 0.4852(2) 0.0313(7) Uani 1 1 d . . . . .
H29A H 0.8203 1.0200 0.5093 0.038 Uiso 1 1 calc R U . . .
H29B H 0.8744 0.9638 0.4177 0.038 Uiso 1 1 calc R U . . .
C30 C 0.9825(3) 0.8869(2) 0.9696(2) 0.0325(7) Uani 1 1 d . . . . .
H30A H 0.9889 0.8197 0.9222 0.039 Uiso 1 1 calc R U . . .
H30B H 0.9494 0.8699 1.0228 0.039 Uiso 1 1 calc R U . . .
C31 C 0.9068(3) 1.0471(3) 0.9980(2) 0.0330(7) Uani 1 1 d . . . . .
H31A H 0.8720 1.0341 1.0521 0.040 Uiso 1 1 calc R U . . .
H31B H 0.8618 1.0862 0.9699 0.040 Uiso 1 1 calc R U . . .
C32 C 0.8353(2) 0.5207(2) 1.0631(2) 0.0283(7) Uani 1 1 d . . . . .
H32A H 0.8117 0.5731 1.1163 0.034 Uiso 1 1 calc R U . . .
H32B H 0.8850 0.5592 1.0309 0.034 Uiso 1 1 calc R U . . .
C33 C 0.8927(3) 0.4448(3) 1.0983(3) 0.0351(7) Uani 1 1 d . . . . .
H33A H 0.9566 0.4851 1.1400 0.042 Uiso 1 1 calc R U . . .
H33B H 0.8444 0.4105 1.1346 0.042 Uiso 1 1 calc R U . . .
C34 C 0.8338(3) 0.3076(3) 0.9583(3) 0.0380(8) Uani 1 1 d . . . . .
H34A H 0.7832 0.2698 0.9904 0.046 Uiso 1 1 calc R U . . .
H34B H 0.8573 0.2545 0.9056 0.046 Uiso 1 1 calc R U . . .
C35 C 0.7768(3) 0.3821(3) 0.9213(2) 0.0348(7) Uani 1 1 d . . . . .
H35A H 0.8258 0.4174 0.8862 0.042 Uiso 1 1 calc R U . . .
H35B H 0.7139 0.3413 0.8785 0.042 Uiso 1 1 calc R U . . .
Li1 Li 0.8849(4) 0.9112(4) 0.6473(4) 0.0274(11) Uani 1 1 d . . . . .
Li2 Li 0.8530(4) 0.8947(4) 0.8031(4) 0.0241(10) Uani 1 1 d . . . . .
Li3 Li 0.5966(4) 0.4892(4) 0.9993(4) 0.0258(10) Uani 1 1 d . . . . .
O5 O 0.6289(5) 0.4276(3) 0.5144(4) 0.128(2) Uani 1 1 d D . . A 1
O6 O 0.6521(3) 0.2196(3) 0.5133(3) 0.0858(11) Uani 1 1 d D . . A 1
C36 C 0.5500(5) 0.3684(6) 0.5537(5) 0.115(3) Uani 1 1 d D . . A 1
H36A H 0.4902 0.3307 0.5063 0.139 Uiso 1 1 calc R U . A 1
H36B H 0.5211 0.4168 0.6064 0.139 Uiso 1 1 calc R U . A 1
C37 C 0.6013(4) 0.2925(5) 0.5859(4) 0.0831(17) Uani 1 1 d D . . A 1
H37A H 0.5468 0.2503 0.6112 0.100 Uiso 1 1 calc R U . A 1
H37B H 0.6563 0.3320 0.6372 0.100 Uiso 1 1 calc R U . A 1
C38 C 0.7260(4) 0.2803(4) 0.4752(4) 0.0691(13) Uani 1 1 d D . . A 1
H38A H 0.7565 0.2322 0.4234 0.083 Uiso 1 1 calc R U . A 1
H38B H 0.7853 0.3179 0.5232 0.083 Uiso 1 1 calc R U . A 1
C39 C 0.6794(4) 0.3603(4) 0.4396(4) 0.0715(14) Uani 1 1 d D . . A 1
H39A H 0.7367 0.4039 0.4183 0.086 Uiso 1 1 calc R U . A 1
H39B H 0.6259 0.3237 0.3863 0.086 Uiso 1 1 calc R U . A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P C1 1.824(3) . ?
P C3 1.834(3) . ?
P C2 1.854(3) . ?
P Li2 2.463(5) . ?
Si1 N1 1.722(2) . ?
Si1 C4 1.873(3) . ?
Si1 C5 1.876(4) . ?
Si1 C1 1.889(3) . ?
Si2 N2 1.720(2) . ?
Si2 C12 1.873(3) . ?
Si2 C2 1.883(3) . ?
Si2 C13 1.888(3) . ?
Si2 Li1 2.978(5) . ?
Si2 Li2 3.171(5) . ?
Si3 N3 1.719(2) . ?
Si3 C20 1.873(3) . ?
Si3 C21 1.879(3) . ?
Si3 C3 1.888(3) . ?
Si3 Li3 3.065(5) . ?
O1 C29 1.437(4) . ?
O1 C28 1.438(4) . ?
O1 Li1 1.871(5) . ?
O2 C31 1.432(4) . ?
O2 C30 1.438(4) . ?
O2 Li2 1.891(5) . ?
O3 C35 1.436(4) . ?
O3 C32 1.439(4) . ?
O3 Li3 1.896(5) . ?
O4 C34 1.412(4) . ?
O4 C33 1.423(4) . ?
N1 C6 1.392(3) . ?
N1 Li1 2.017(6) . ?
N1 Li2 2.129(5) . ?
N2 C14 1.394(4) . ?
N2 Li1 1.988(5) . ?
N2 Li2 2.136(5) . ?
N3 C22 1.390(4) . ?
N3 Li3 1.993(5) . ?
N3 Li3 2.062(5) 2_667 ?
C6 C11 1.409(4) . ?
C6 C7 1.422(4) . ?
C6 Li1 2.485(6) . ?
C7 C8 1.392(4) . ?
C8 C9 1.383(4) . ?
C9 C10 1.387(5) . ?
C10 C11 1.387(4) . ?
C14 C19 1.402(4) . ?
C14 C15 1.413(4) . ?
C15 C16 1.385(4) . ?
C16 C17 1.384(5) . ?
C17 C18 1.385(5) . ?
C18 C19 1.383(5) . ?
C22 C23 1.411(4) . ?
C22 C27 1.413(4) . ?
C22 Li3 2.475(6) 2_667 ?
C23 C24 1.387(5) . ?
C24 C25 1.374(5) . ?
C25 C26 1.392(5) . ?
C26 C27 1.375(5) . ?
C28 C29 1.502(4) 2_776 ?
C29 C28 1.502(4) 2_776 ?
C30 C31 1.497(5) 2_777 ?
C31 C30 1.497(5) 2_777 ?
C32 C33 1.502(4) . ?
C34 C35 1.496(5) . ?
Li1 Li2 2.422(7) . ?
Li3 N3 2.062(5) 2_667 ?
Li3 Li3 2.458(9) 2_667 ?
Li3 C22 2.475(6) 2_667 ?
O5 C36 1.412(8) . ?
O5 C39 1.430(7) . ?
O6 C38 1.376(6) . ?
O6 C37 1.449(6) . ?
C36 C37 1.436(9) . ?
C38 C39 1.482(6) . ?

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 P C3 104.63(13) . . ?
C1 P C2 104.17(14) . . ?
C3 P C2 103.26(13) . . ?
C1 P Li2 102.03(15) . . ?
C3 P Li2 143.82(15) . . ?
C2 P Li2 93.34(15) . . ?
N1 Si1 C4 112.94(15) . . ?
N1 Si1 C5 114.56(14) . . ?
C4 Si1 C5 107.84(18) . . ?
N1 Si1 C1 108.36(12) . . ?
C4 Si1 C1 106.10(15) . . ?
C5 Si1 C1 106.53(15) . . ?
N2 Si2 C12 111.77(14) . . ?
N2 Si2 C2 104.09(12) . . ?
C12 Si2 C2 109.70(15) . . ?
N2 Si2 C13 118.25(14) . . ?
C12 Si2 C13 106.18(16) . . ?
C2 Si2 C13 106.58(13) . . ?
N2 Si2 Li1 39.75(13) . . ?
C12 Si2 Li1 100.12(15) . . ?
C2 Si2 Li1 72.83(13) . . ?
C13 Si2 Li1 151.89(16) . . ?
N2 Si2 Li2 39.20(12) . . ?
C12 Si2 Li2 145.32(14) . . ?
C2 Si2 Li2 72.62(13) . . ?
C13 Si2 Li2 106.01(15) . . ?
Li1 Si2 Li2 46.26(13) . . ?
N3 Si3 C20 108.90(13) . . ?
N3 Si3 C21 113.52(14) . . ?
C20 Si3 C21 105.27(16) . . ?
N3 Si3 C3 110.54(13) . . ?
C20 Si3 C3 106.62(14) . . ?
C21 Si3 C3 111.59(14) . . ?
N3 Si3 Li3 37.35(12) . . ?
C20 Si3 Li3 71.68(13) . . ?
C21 Si3 Li3 121.71(15) . . ?
C3 Si3 Li3 125.29(14) . . ?
C29 O1 C28 109.9(2) . . ?
C29 O1 Li1 126.4(2) . . ?
C28 O1 Li1 120.3(2) . . ?
C31 O2 C30 110.8(2) . . ?
C31 O2 Li2 126.9(2) . . ?
C30 O2 Li2 122.3(2) . . ?
C35 O3 C32 109.7(2) . . ?
C35 O3 Li3 121.4(2) . . ?
C32 O3 Li3 128.4(2) . . ?
C34 O4 C33 110.2(2) . . ?
C6 N1 Si1 121.38(18) . . ?
C6 N1 Li1 91.7(2) . . ?
Si1 N1 Li1 122.0(2) . . ?
C6 N1 Li2 116.8(2) . . ?
Si1 N1 Li2 118.83(17) . . ?
Li1 N1 Li2 71.4(2) . . ?
C14 N2 Si2 122.36(19) . . ?
C14 N2 Li1 120.4(2) . . ?
Si2 N2 Li1 106.6(2) . . ?
C14 N2 Li2 114.5(2) . . ?
Si2 N2 Li2 110.19(17) . . ?
Li1 N2 Li2 71.8(2) . . ?
C22 N3 Si3 121.62(19) . . ?
C22 N3 Li3 123.7(2) . . ?
Si3 N3 Li3 111.11(19) . . ?
C22 N3 Li3 89.5(2) . 2_667 ?
Si3 N3 Li3 125.3(2) . 2_667 ?
Li3 N3 Li3 74.6(2) . 2_667 ?
P C1 Si1 114.79(15) . . ?
P C2 Si2 109.05(15) . . ?
P C3 Si3 116.93(16) . . ?
N1 C6 C11 119.5(2) . . ?
N1 C6 C7 125.4(3) . . ?
C11 C6 C7 115.1(2) . . ?
N1 C6 Li1 54.25(17) . . ?
C11 C6 Li1 88.0(2) . . ?
C7 C6 Li1 128.2(2) . . ?
C8 C7 C6 121.5(3) . . ?
C9 C8 C7 121.4(3) . . ?
C8 C9 C10 118.5(3) . . ?
C11 C10 C9 120.4(3) . . ?
C10 C11 C6 123.0(3) . . ?
N2 C14 C19 124.5(3) . . ?
N2 C14 C15 120.4(3) . . ?
C19 C14 C15 115.0(3) . . ?
C16 C15 C14 122.8(3) . . ?
C17 C16 C15 120.7(3) . . ?
C16 C17 C18 117.7(3) . . ?
C19 C18 C17 121.8(3) . . ?
C18 C19 C14 122.0(3) . . ?
N3 C22 C23 120.3(3) . . ?
N3 C22 C27 124.9(3) . . ?
C23 C22 C27 114.7(3) . . ?
N3 C22 Li3 56.39(18) . 2_667 ?
C23 C22 Li3 97.2(2) . 2_667 ?
C27 C22 Li3 116.0(2) . 2_667 ?
C24 C23 C22 122.4(3) . . ?
C25 C24 C23 121.0(3) . . ?
C24 C25 C26 118.4(3) . . ?
C27 C26 C25 120.7(3) . . ?
C26 C27 C22 122.8(3) . . ?
O1 C28 C29 110.5(3) . 2_776 ?
O1 C29 C28 110.3(3) . 2_776 ?
O2 C30 C31 109.4(3) . 2_777 ?
O2 C31 C30 110.4(3) . 2_777 ?
O3 C32 C33 109.9(2) . . ?
O4 C33 C32 111.3(3) . . ?
O4 C34 C35 111.4(3) . . ?
O3 C35 C34 109.7(3) . . ?
O1 Li1 N2 119.8(3) . . ?
O1 Li1 N1 126.8(3) . . ?
N2 Li1 N1 113.3(3) . . ?
O1 Li1 Li2 173.6(3) . . ?
N2 Li1 Li2 56.92(18) . . ?
N1 Li1 Li2 56.42(18) . . ?
O1 Li1 C6 104.0(2) . . ?
N2 Li1 C6 126.3(3) . . ?
N1 Li1 C6 34.05(12) . . ?
Li2 Li1 C6 76.1(2) . . ?
O1 Li1 Si2 109.4(2) . . ?
N2 Li1 Si2 33.61(11) . . ?
N1 Li1 Si2 116.3(2) . . ?
Li2 Li1 Si2 71.08(17) . . ?
C6 Li1 Si2 146.4(2) . . ?
O2 Li2 N1 123.0(3) . . ?
O2 Li2 N2 116.8(2) . . ?
N1 Li2 N2 103.3(2) . . ?
O2 Li2 Li1 141.1(3) . . ?
N1 Li2 Li1 52.15(17) . . ?
N2 Li2 Li1 51.24(17) . . ?
O2 Li2 P 124.3(2) . . ?
N1 Li2 P 88.66(18) . . ?
N2 Li2 P 94.14(19) . . ?
Li1 Li2 P 94.6(2) . . ?
O2 Li2 Si2 129.5(2) . . ?
N1 Li2 Si2 105.81(19) . . ?
N2 Li2 Si2 30.61(9) . . ?
Li1 Li2 Si2 62.66(17) . . ?
P Li2 Si2 63.93(11) . . ?
O3 Li3 N3 128.5(3) . . ?
O3 Li3 N3 125.9(3) . 2_667 ?
N3 Li3 N3 105.4(2) . 2_667 ?
O3 Li3 Li3 175.5(4) . 2_667 ?
N3 Li3 Li3 53.96(19) . 2_667 ?
N3 Li3 Li3 51.42(19) 2_667 2_667 ?
O3 Li3 C22 104.6(2) . 2_667 ?
N3 Li3 C22 122.1(2) . 2_667 ?
N3 Li3 C22 34.15(12) 2_667 2_667 ?
Li3 Li3 C22 74.8(2) 2_667 2_667 ?
O3 Li3 Si3 109.9(2) . . ?
N3 Li3 Si3 31.54(10) . . ?
N3 Li3 Si3 119.8(2) 2_667 . ?
Li3 Li3 Si3 74.1(2) 2_667 . ?
C22 Li3 Si3 116.8(2) 2_667 . ?
C36 O5 C39 112.9(4) . . ?
C38 O6 C37 108.2(4) . . ?
O5 C36 C37 108.4(5) . . ?
C36 C37 O6 114.4(5) . . ?
O6 C38 C39 114.2(4) . . ?
O5 C39 C38 108.9(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
C4 Si1 N1 C6 -51.7(3) . . . . ?
C5 Si1 N1 C6 72.3(3) . . . . ?
C1 Si1 N1 C6 -169.0(2) . . . . ?
C4 Si1 N1 Li1 -166.7(2) . . . . ?
C5 Si1 N1 Li1 -42.7(3) . . . . ?
C1 Si1 N1 Li1 76.0(2) . . . . ?
C4 Si1 N1 Li2 108.1(2) . . . . ?
C5 Si1 N1 Li2 -127.9(2) . . . . ?
C1 Si1 N1 Li2 -9.1(2) . . . . ?
C12 Si2 N2 C14 -65.2(3) . . . . ?
C2 Si2 N2 C14 176.5(2) . . . . ?
C13 Si2 N2 C14 58.5(3) . . . . ?
Li1 Si2 N2 C14 -144.6(3) . . . . ?
Li2 Si2 N2 C14 139.1(3) . . . . ?
C12 Si2 N2 Li1 79.4(2) . . . . ?
C2 Si2 N2 Li1 -38.9(2) . . . . ?
C13 Si2 N2 Li1 -156.9(2) . . . . ?
Li2 Si2 N2 Li1 -76.3(2) . . . . ?
C12 Si2 N2 Li2 155.69(19) . . . . ?
C2 Si2 N2 Li2 37.4(2) . . . . ?
C13 Si2 N2 Li2 -80.6(2) . . . . ?
Li1 Si2 N2 Li2 76.3(2) . . . . ?
C20 Si3 N3 C22 -154.4(2) . . . . ?
C21 Si3 N3 C22 88.7(3) . . . . ?
C3 Si3 N3 C22 -37.6(3) . . . . ?
Li3 Si3 N3 C22 -159.3(3) . . . . ?
C20 Si3 N3 Li3 4.9(2) . . . . ?
C21 Si3 N3 Li3 -112.0(2) . . . . ?
C3 Si3 N3 Li3 121.7(2) . . . . ?
C20 Si3 N3 Li3 90.6(2) . . . 2_667 ?
C21 Si3 N3 Li3 -26.3(3) . . . 2_667 ?
C3 Si3 N3 Li3 -152.6(2) . . . 2_667 ?
Li3 Si3 N3 Li3 85.7(3) . . . 2_667 ?
C3 P C1 Si1 -179.98(17) . . . . ?
C2 P C1 Si1 -71.9(2) . . . . ?
Li2 P C1 Si1 24.7(2) . . . . ?
N1 Si1 C1 P -13.0(2) . . . . ?
C4 Si1 C1 P -134.6(2) . . . . ?
C5 Si1 C1 P 110.7(2) . . . . ?
C1 P C2 Si2 150.23(14) . . . . ?
C3 P C2 Si2 -100.67(15) . . . . ?
Li2 P C2 Si2 46.93(17) . . . . ?
N2 Si2 C2 P -60.11(16) . . . . ?
C12 Si2 C2 P -179.84(15) . . . . ?
C13 Si2 C2 P 65.61(19) . . . . ?
Li1 Si2 C2 P -84.99(16) . . . . ?
Li2 Si2 C2 P -36.41(14) . . . . ?
C1 P C3 Si3 -85.55(19) . . . . ?
C2 P C3 Si3 165.70(16) . . . . ?
Li2 P C3 Si3 50.7(3) . . . . ?
N3 Si3 C3 P -172.07(14) . . . . ?
C20 Si3 C3 P -53.9(2) . . . . ?
C21 Si3 C3 P 60.6(2) . . . . ?
Li3 Si3 C3 P -132.87(16) . . . . ?
Si1 N1 C6 C11 167.3(2) . . . . ?
Li1 N1 C6 C11 -62.9(3) . . . . ?
Li2 N1 C6 C11 7.1(4) . . . . ?
Si1 N1 C6 C7 -14.8(4) . . . . ?
Li1 N1 C6 C7 115.0(3) . . . . ?
Li2 N1 C6 C7 -175.0(3) . . . . ?
Si1 N1 C6 Li1 -129.8(3) . . . . ?
Li2 N1 C6 Li1 70.0(2) . . . . ?
N1 C6 C7 C8 -176.6(3) . . . . ?
C11 C6 C7 C8 1.3(4) . . . . ?
Li1 C6 C7 C8 -107.3(3) . . . . ?
C6 C7 C8 C9 0.7(5) . . . . ?
C7 C8 C9 C10 -1.5(5) . . . . ?
C8 C9 C10 C11 0.1(5) . . . . ?
C9 C10 C11 C6 2.1(5) . . . . ?
N1 C6 C11 C10 175.3(3) . . . . ?
C7 C6 C11 C10 -2.8(4) . . . . ?
Li1 C6 C11 C10 129.1(3) . . . . ?
Si2 N2 C14 C19 -33.2(4) . . . . ?
Li1 N2 C14 C19 -173.1(3) . . . . ?
Li2 N2 C14 C19 104.3(4) . . . . ?
Si2 N2 C14 C15 149.1(2) . . . . ?
Li1 N2 C14 C15 9.2(4) . . . . ?
Li2 N2 C14 C15 -73.3(3) . . . . ?
N2 C14 C15 C16 176.6(3) . . . . ?
C19 C14 C15 C16 -1.2(5) . . . . ?
C14 C15 C16 C17 0.3(6) . . . . ?
C15 C16 C17 C18 0.9(6) . . . . ?
C16 C17 C18 C19 -1.2(7) . . . . ?
C17 C18 C19 C14 0.2(7) . . . . ?
N2 C14 C19 C18 -176.8(4) . . . . ?
C15 C14 C19 C18 1.0(6) . . . . ?
Si3 N3 C22 C23 150.1(2) . . . . ?
Li3 N3 C22 C23 -6.5(4) . . . . ?
Li3 N3 C22 C23 -77.6(3) 2_667 . . . ?
Si3 N3 C22 C27 -32.1(4) . . . . ?
Li3 N3 C22 C27 171.3(3) . . . . ?
Li3 N3 C22 C27 100.2(3) 2_667 . . . ?
Si3 N3 C22 Li3 -132.3(3) . . . 2_667 ?
Li3 N3 C22 Li3 71.0(3) . . . 2_667 ?
N3 C22 C23 C24 178.6(3) . . . . ?
C27 C22 C23 C24 0.6(5) . . . . ?
Li3 C22 C23 C24 123.5(4) 2_667 . . . ?
C22 C23 C24 C25 -0.1(6) . . . . ?
C23 C24 C25 C26 -0.4(6) . . . . ?
C24 C25 C26 C27 0.5(5) . . . . ?
C25 C26 C27 C22 0.0(5) . . . . ?
N3 C22 C27 C26 -178.4(3) . . . . ?
C23 C22 C27 C26 -0.5(4) . . . . ?
Li3 C22 C27 C26 -112.6(3) 2_667 . . . ?
C29 O1 C28 C29 58.1(4) . . . 2_776 ?
Li1 O1 C28 C29 -102.2(3) . . . 2_776 ?
C28 O1 C29 C28 -58.0(4) . . . 2_776 ?
Li1 O1 C29 C28 100.9(3) . . . 2_776 ?
C31 O2 C30 C31 -58.0(4) . . . 2_777 ?
Li2 O2 C30 C31 120.1(3) . . . 2_777 ?
C30 O2 C31 C30 58.6(4) . . . 2_777 ?
Li2 O2 C31 C30 -119.4(3) . . . 2_777 ?
C35 O3 C32 C33 -57.9(3) . . . . ?
Li3 O3 C32 C33 130.4(3) . . . . ?
C34 O4 C33 C32 -56.7(3) . . . . ?
O3 C32 C33 O4 57.3(3) . . . . ?
C33 O4 C34 C35 57.4(4) . . . . ?
C32 O3 C35 C34 58.4(3) . . . . ?
Li3 O3 C35 C34 -129.2(3) . . . . ?
O4 C34 C35 O3 -58.7(4) . . . . ?
C29 O1 Li1 N2 -179.3(3) . . . . ?
C28 O1 Li1 N2 -22.4(4) . . . . ?
C29 O1 Li1 N1 -3.0(5) . . . . ?
C28 O1 Li1 N1 153.9(3) . . . . ?
C29 O1 Li1 C6 -31.3(4) . . . . ?
C28 O1 Li1 C6 125.5(3) . . . . ?
C29 O1 Li1 Si2 145.4(2) . . . . ?
C28 O1 Li1 Si2 -57.7(3) . . . . ?
C31 O2 Li2 N1 12.1(4) . . . . ?
C30 O2 Li2 N1 -165.6(3) . . . . ?
C31 O2 Li2 N2 141.6(3) . . . . ?
C30 O2 Li2 N2 -36.1(4) . . . . ?
C31 O2 Li2 Li1 81.0(5) . . . . ?
C30 O2 Li2 Li1 -96.8(5) . . . . ?
C31 O2 Li2 P -102.1(3) . . . . ?
C30 O2 Li2 P 80.2(4) . . . . ?
C31 O2 Li2 Si2 175.2(2) . . . . ?
C30 O2 Li2 Si2 -2.6(4) . . . . ?
C35 O3 Li3 N3 -56.5(5) . . . . ?
C32 O3 Li3 N3 114.4(4) . . . . ?
C35 O3 Li3 N3 117.9(4) . . . 2_667 ?
C32 O3 Li3 N3 -71.2(4) . . . 2_667 ?
C35 O3 Li3 C22 147.9(2) . . . 2_667 ?
C32 O3 Li3 C22 -41.3(3) . . . 2_667 ?
C35 O3 Li3 Si3 -86.0(3) . . . . ?
C32 O3 Li3 Si3 84.9(3) . . . . ?
C39 O5 C36 C37 56.4(7) . . . . ?
O5 C36 C37 O6 -56.8(6) . . . . ?
C38 O6 C37 C36 56.0(6) . . . . ?
C37 O6 C38 C39 -54.3(6) . . . . ?
C36 O5 C39 C38 -55.1(6) . . . . ?
O6 C38 C39 O5 55.2(6) . . . . ?

_refine_diff_density_max         1.104
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.070

_shelxl_version_number           2013-2

_cell_oxdiff_length_a            12.4277(2)
_cell_oxdiff_length_b            13.1483(2)
_cell_oxdiff_length_c            14.8044(3)
_cell_oxdiff_angle_alpha         106.9639(16)
_cell_oxdiff_angle_beta          92.2955(16)
_cell_oxdiff_angle_gamma         98.2181(15)
_cell_oxdiff_volume              2281.50(7)
_cell_oxdiff_measurement_reflns_used 23109
_cell_oxdiff_twin_number         2
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -0.0470 -0.9504 -0.0014 -1.0481 0.0454 -0.0001 0.2626 -0.2600 -0.9993
_diffrn_radiation_monochromator  mirror
_diffrn_orient_matrix_UB_11      -0.1011888000
_diffrn_orient_matrix_UB_12      -0.0838219000
_diffrn_orient_matrix_UB_13      -0.0025361000
_diffrn_orient_matrix_UB_21      0.0714559000
_diffrn_orient_matrix_UB_22      -0.0893564000
_diffrn_orient_matrix_UB_23      -0.0192494000
_diffrn_orient_matrix_UB_31      0.0214449000
_diffrn_orient_matrix_UB_32      0.0199627000
_diffrn_orient_matrix_UB_33      0.1074634000
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.6104 60518 7180
2 0.3896 0 7180
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -26.00   25.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -60.0000 51

#__ type_ start__ end____ width___ exp.time_
  2 omega  -58.00  -21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 37

#__ type_ start__ end____ width___ exp.time_
  3 omega  -15.00   15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 30

#__ type_ start__ end____ width___ exp.time_
  4 omega  -21.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  150.0000 90

#__ type_ start__ end____ width___ exp.time_
  5 omega  -16.00   10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega   37.00   62.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
  7 omega   41.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -60.0000 25

#__ type_ start__ end____ width___ exp.time_
  8 omega  -72.00  -30.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000  -77.0000   30.0000 42

#__ type_ start__ end____ width___ exp.time_
  9 omega  -26.00   23.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000  -77.0000   30.0000 49

#__ type_ start__ end____ width___ exp.time_
 10 omega  -12.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   79.0000    0.9048 41

#__ type_ start__ end____ width___ exp.time_
 11 omega    7.00   43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  139.9541 36

#__ type_ start__ end____ width___ exp.time_
 12 omega    7.00   32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000   74.6890 25

#__ type_ start__ end____ width___ exp.time_
 13 omega   10.00   35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -43.5485 25

#__ type_ start__ end____ width___ exp.time_
 14 omega   10.00   41.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000 -126.2892 31

#__ type_ start__ end____ width___ exp.time_
 15 omega   15.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000  -90.8289 31

#__ type_ start__ end____ width___ exp.time_
 16 omega   14.00   39.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   32.0770 25

#__ type_ start__ end____ width___ exp.time_
 17 omega   17.00   48.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000 -178.4029 31

#__ type_ start__ end____ width___ exp.time_
 18 omega   15.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000   86.6376 25

#__ type_ start__ end____ width___ exp.time_
 19 omega   14.00   39.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -135.5268 25

#__ type_ start__ end____ width___ exp.time_
 20 omega   15.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -11.3574 29

#__ type_ start__ end____ width___ exp.time_
 21 omega   19.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -57.5532 25

#__ type_ start__ end____ width___ exp.time_
 22 omega   19.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  133.4643 25

#__ type_ start__ end____ width___ exp.time_
 23 omega   27.00   82.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000   30.0000 55

#__ type_ start__ end____ width___ exp.time_
 24 omega   93.00  120.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -119.5413 27

#__ type_ start__ end____ width___ exp.time_
 25 omega   30.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  108.5268 27

#__ type_ start__ end____ width___ exp.time_
 26 omega   30.00   55.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -171.8181 25

#__ type_ start__ end____ width___ exp.time_
 27 omega   84.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -18.8040 37

#__ type_ start__ end____ width___ exp.time_
 28 omega   30.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000   92.0111 26

#__ type_ start__ end____ width___ exp.time_
 29 omega   30.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  134.5465 27

#__ type_ start__ end____ width___ exp.time_
 30 omega   83.00  128.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  108.5268 45

#__ type_ start__ end____ width___ exp.time_
 31 omega   29.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -119.5413 27

#__ type_ start__ end____ width___ exp.time_
 32 omega   46.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -18.8040 25

#__ type_ start__ end____ width___ exp.time_
 33 omega   29.00   62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -33.1165 33

#__ type_ start__ end____ width___ exp.time_
 34 omega   34.00   62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000   53.8918 28

#__ type_ start__ end____ width___ exp.time_
 35 omega   55.00   82.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000 -129.2418 27

#__ type_ start__ end____ width___ exp.time_
 36 omega   32.00   59.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  162.2873 27

#__ type_ start__ end____ width___ exp.time_
 37 omega   39.00   87.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   65.0000  -96.7319 48

#__ type_ start__ end____ width___ exp.time_
 38 omega   42.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  139.3136 27

#__ type_ start__ end____ width___ exp.time_
 39 omega   -8.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  -23.5027 101

#__ type_ start__ end____ width___ exp.time_
 40 omega   34.00   61.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000  -76.3552 27

#__ type_ start__ end____ width___ exp.time_
 41 omega   37.00   63.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000   12.8870 26

#__ type_ start__ end____ width___ exp.time_
 42 omega   38.00   74.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  -67.9200 36

#__ type_ start__ end____ width___ exp.time_
 43 omega   91.00  118.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  -67.9200 27

#__ type_ start__ end____ width___ exp.time_
 44 omega   39.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000 -150.1490 32

#__ type_ start__ end____ width___ exp.time_
 45 omega   44.00   80.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000   41.0861 36

#__ type_ start__ end____ width___ exp.time_
 46 omega   88.00  133.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000   41.0861 45

#__ type_ start__ end____ width___ exp.time_
 47 omega   46.00   76.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   63.0000   96.2241 30

#__ type_ start__ end____ width___ exp.time_
 48 omega   45.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000  174.7436 26

#__ type_ start__ end____ width___ exp.time_
 49 omega   47.00  133.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   68.0000  -46.3085 86

#__ type_ start__ end____ width___ exp.time_
 50 omega   -1.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -79.0000 -155.8319 101

#__ type_ start__ end____ width___ exp.time_
 51 omega   53.00   81.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   58.0000  165.6294 28

#__ type_ start__ end____ width___ exp.time_
 52 omega   59.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   58.0000  141.0518 33

#__ type_ start__ end____ width___ exp.time_
 53 omega   47.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000  -92.0697 62

#__ type_ start__ end____ width___ exp.time_
 54 omega   55.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   58.0000   12.3433 39

#__ type_ start__ end____ width___ exp.time_
 55 omega   49.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   69.0000  -16.5278 28

#__ type_ start__ end____ width___ exp.time_
 56 omega   45.00   74.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000 -173.3292 29

#__ type_ start__ end____ width___ exp.time_
 57 omega   54.00  103.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000   22.1661 49

#__ type_ start__ end____ width___ exp.time_
 58 omega   58.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   54.0000  158.5506 25

#__ type_ start__ end____ width___ exp.time_
 59 omega   56.00   90.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   63.0000   97.3940 34

#__ type_ start__ end____ width___ exp.time_
 60 omega   51.00   79.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -78.0000   53.4230 28

#__ type_ start__ end____ width___ exp.time_
 61 omega   51.00  146.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000  177.3271 95

#__ type_ start__ end____ width___ exp.time_
 62 omega   57.00  145.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   55.0000   67.1198 88

#__ type_ start__ end____ width___ exp.time_
 63 omega   20.00   49.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -78.0000   53.4230 29

#__ type_ start__ end____ width___ exp.time_
 64 omega   58.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   60.0000 -133.7685 27

#__ type_ start__ end____ width___ exp.time_
 65 omega   49.00   76.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  103.1923 27

#__ type_ start__ end____ width___ exp.time_
 66 omega   55.00  145.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000  -50.6783 90

#__ type_ start__ end____ width___ exp.time_
 67 omega   54.00   81.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  178.4211 27

#__ type_ start__ end____ width___ exp.time_
 68 omega   62.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   44.0000  169.2628 27

#__ type_ start__ end____ width___ exp.time_
 69 omega   67.00  151.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   53.0000  -91.5182 84

#__ type_ start__ end____ width___ exp.time_
 70 omega   69.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   54.0000  133.7861 40

#__ type_ start__ end____ width___ exp.time_
 71 omega   16.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -80.0000   83.7515 65

#__ type_ start__ end____ width___ exp.time_
 72 omega   64.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   48.0000   62.6359 34

#__ type_ start__ end____ width___ exp.time_
 73 omega   65.00  100.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   56.0000 -139.3187 35

#__ type_ start__ end____ width___ exp.time_
 74 omega   70.00  136.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   69.0000 -133.0506 66

#__ type_ start__ end____ width___ exp.time_
 75 omega   73.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   56.0000  106.8157 30

#__ type_ start__ end____ width___ exp.time_
 76 omega   85.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
 77 omega   90.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
 78 omega   86.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 89

#__ type_ start__ end____ width___ exp.time_
 79 omega   64.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -131.8082 32

#__ type_ start__ end____ width___ exp.time_
 80 omega   80.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
 81 omega  119.00  156.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 37

#__ type_ start__ end____ width___ exp.time_
 82 omega   39.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -34.5427 100

#__ type_ start__ end____ width___ exp.time_
 83 omega   82.00  157.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -150.0000 75

#__ type_ start__ end____ width___ exp.time_
 84 omega   86.00  126.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 40

#__ type_ start__ end____ width___ exp.time_
 85 omega   85.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
 86 omega   86.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 87 omega   86.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
 88 omega   86.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
 89 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 90 omega   85.00  156.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 71

#__ type_ start__ end____ width___ exp.time_
 91 omega   86.00  173.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 87

#__ type_ start__ end____ width___ exp.time_
 92 omega  112.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 65

#__ type_ start__ end____ width___ exp.time_
 93 omega   78.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 29

#__ type_ start__ end____ width___ exp.time_
 94 omega   79.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
 95 omega  133.00  159.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 96 omega   78.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
 97 omega   78.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 27

#__ type_ start__ end____ width___ exp.time_
 98 omega   74.00  138.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   36.0281 64

#__ type_ start__ end____ width___ exp.time_
 99 omega  153.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 25

#__ type_ start__ end____ width___ exp.time_
100 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
101 omega   39.00   66.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   36.0281 27

#__ type_ start__ end____ width___ exp.time_
102 omega  152.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
103 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
104 omega   78.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 99

#__ type_ start__ end____ width___ exp.time_
105 omega  146.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 31

#__ type_ start__ end____ width___ exp.time_
106 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
107 omega  134.00  160.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
108 omega   79.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
109 omega  108.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 66

#__ type_ start__ end____ width___ exp.time_
110 omega   85.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
111 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
112 omega  153.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
113 omega   63.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -87.3038 43

#__ type_ start__ end____ width___ exp.time_
114 omega   79.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
115 omega   85.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 89

#__ type_ start__ end____ width___ exp.time_
116 omega  120.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 54

#__ type_ start__ end____ width___ exp.time_
117 omega   86.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 27

#__ type_ start__ end____ width___ exp.time_
118 omega   82.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 34

#__ type_ start__ end____ width___ exp.time_
119 omega   85.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
120 omega   83.00  110.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
121 omega   39.00  140.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  124.8496 101

#__ type_ start__ end____ width___ exp.time_
122 omega   84.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
123 omega  114.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   80.3130 25

#__ type_ start__ end____ width___ exp.time_
124 omega   72.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   80.3130 27

#__ type_ start__ end____ width___ exp.time_
125 omega   43.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   80.3130 27

#__ type_ start__ end____ width___ exp.time_
126 omega   82.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -30.0000 96

#__ type_ start__ end____ width___ exp.time_
127 omega   82.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   73.0000   39.1504 94

#__ type_ start__ end____ width___ exp.time_
128 omega   84.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
129 phi      0.00  120.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
   0.0000    0.0000  -20.0000     -     120

#__ type_ start__ end____ width___ exp.time_
130 omega  -72.00   26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   30.0000 98

#__ type_ start__ end____ width___ exp.time_
131 omega  -21.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 90

#__ type_ start__ end____ width___ exp.time_
132 omega   -8.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   77.0000  -87.2704 100

#__ type_ start__ end____ width___ exp.time_
133 omega   -3.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   76.0000  133.0261 99

#__ type_ start__ end____ width___ exp.time_
134 omega    5.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   55.0000   43.5068 90

#__ type_ start__ end____ width___ exp.time_
135 omega   10.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  151.2171 34

#__ type_ start__ end____ width___ exp.time_
136 omega   14.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -135.5268 32

#__ type_ start__ end____ width___ exp.time_
137 omega   19.00   47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -57.5532 28

#__ type_ start__ end____ width___ exp.time_
138 omega   -9.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  -23.5027 103

#__ type_ start__ end____ width___ exp.time_
139 omega   46.00  143.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000  -92.0697 97

#__ type_ start__ end____ width___ exp.time_
140 omega   57.00  147.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   54.0000  158.5506 90

#__ type_ start__ end____ width___ exp.time_
141 omega    7.00  110.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  178.4211 103

#__ type_ start__ end____ width___ exp.time_
142 omega    8.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -78.0000   53.4230 101

#__ type_ start__ end____ width___ exp.time_
143 omega   57.00  146.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   60.0000 -133.7685 89

#__ type_ start__ end____ width___ exp.time_
144 omega   57.00  147.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   55.0000   67.1198 90

#__ type_ start__ end____ width___ exp.time_
145 omega   54.00  146.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000   22.1661 92

#__ type_ start__ end____ width___ exp.time_
146 omega   49.00  148.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  103.1923 99

#__ type_ start__ end____ width___ exp.time_
147 omega   54.00  150.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   42.0000  -14.5033 96

#__ type_ start__ end____ width___ exp.time_
148 omega   51.00  147.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000  177.3271 96

;
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration .
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent EOS'
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_jb1
_database_code_depnum_ccdc_archive 'CCDC 1437766'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue Jun 12 14:54:34 2012'
;

_audit_block_code                ba_jb1
_audit_block_refno               1515
_audit_block_usercomment         'jbo 52_Ti, red, block'


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C27 H39 Cl N3 P Si3 Ti, 0.5(C7 H8)'
_chemical_formula_sum            'C30.50 H43 Cl N3 P Si3 Ti'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         650.27
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            red
_diffrn_ambient_temperature      110(1)
_chemical_oxdiff_formula         'C30 H42 Cl1 N3 P1 Si3 Ti1'
_chemical_oxdiff_usercomment     'jbo 52_Ti, red, block'
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'
Cl Cl 0.1484 0.1585 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2ybc'
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                   10.90658(10)
_cell_length_b                   18.00949(16)
_cell_length_c                   17.67069(16)
_cell_angle_alpha                90
_cell_angle_beta                 101.8442(9)
_cell_angle_gamma                90
_cell_volume                     3397.01(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20759
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      28.9533
_cell_measurement_theta_min      3.2597
_shelx_estimated_absorpt_T_max   0.951
_shelx_estimated_absorpt_T_min   0.951
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49411
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.017
_diffrn_reflns_theta_min         3.266
_diffrn_detector_area_resol_mean 15.9241
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -10.00   81.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3036   77.0000  150.0000 91

#__ type_ start__ end____ width___ exp.time_
  2 omega  -12.00   60.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3036  -99.0000 -150.0000 72

#__ type_ start__ end____ width___ exp.time_
  3 omega    6.00   87.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3036   57.0000   60.0000 81

#__ type_ start__ end____ width___ exp.time_
  4 omega   21.00   67.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3036   57.0000 -120.0000 46

#__ type_ start__ end____ width___ exp.time_
  5 omega  -50.00   40.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3036  -57.0000  -90.0000 90

#__ type_ start__ end____ width___ exp.time_
  6 omega  -50.00   25.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3036  -55.0000  142.0000 75

#__ type_ start__ end____ width___ exp.time_
  7 omega  -48.00   39.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3036  -57.0000    0.0000 87

#__ type_ start__ end____ width___ exp.time_
  8 omega   -3.00   84.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3036   77.0000  -60.0000 87

#__ type_ start__ end____ width___ exp.time_
  9 omega   -2.00   53.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.7723   38.0000   90.0000 55

#__ type_ start__ end____ width___ exp.time_
 10 omega  -72.00  -29.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.7723  118.0000   25.0000 43

;
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0453877000
_diffrn_orient_matrix_UB_12      -0.0214386000
_diffrn_orient_matrix_UB_13      -0.0252920000
_diffrn_orient_matrix_UB_21      0.0213429000
_diffrn_orient_matrix_UB_22      0.0147650000
_diffrn_orient_matrix_UB_23      -0.0322057000
_diffrn_orient_matrix_UB_31      0.0435834000
_diffrn_orient_matrix_UB_32      -0.0295579000
_diffrn_orient_matrix_UB_33      0.0022535000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7135
_reflns_number_total             8403
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         2.073
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         8403
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0380
_refine_ls_restrained_S_all      1.251
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0397P)²+3.6197P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0973
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C97-C94 \\sim C97-C96
 with sigma of 0.02
3. Restrained atomic chiral volume
 C95
 fixed at 0 with sigma of 0.1
4. Rigid body (RIGU) restrains
 C91, C92, C93, C94, C95
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C91(0.5) H91(0.5) C92(0.5) H92(0.5) C93(0.5) H93(0.5) C95(0.5)
 C94(0.5) H94(0.5) C96(0.5) H96(0.5) C97(0.5) H97A(0.5) H97B(0.5) H97C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C91(H91),
  C92(H92), C93(H93), C94(H94), C96(H96)
6.c Fitted hexagon refined as free rotating group:
 C91(C92,C93,C95,C94,C96)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C97(H97A,H97B,H97C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti Ti 0.84379(3) 0.73205(2) 0.33255(2) 0.01301(8) Uani 1 1 d . . . . .
Cl Cl 0.83168(4) 0.70819(3) 0.45985(2) 0.01998(10) Uani 1 1 d . . . . .
P P 0.83755(4) 0.75591(3) 0.19208(3) 0.01459(10) Uani 1 1 d . . . . .
Si1 Si 0.69095(5) 0.87937(3) 0.23393(3) 0.01838(11) Uani 1 1 d . . . . .
Si2 Si 0.73530(6) 0.60669(3) 0.19010(3) 0.02528(13) Uani 1 1 d . . . . .
Si3 Si 1.10742(5) 0.75900(3) 0.26633(3) 0.01642(11) Uani 1 1 d . . . . .
N1 N 0.72556(14) 0.81757(8) 0.31243(9) 0.0160(3) Uani 1 1 d . . . . .
N2 N 0.80428(14) 0.63378(8) 0.28487(9) 0.0177(3) Uani 1 1 d . . . . .
N3 N 1.02015(14) 0.75783(8) 0.33920(9) 0.0162(3) Uani 1 1 d . . . . .
C1 C 0.79872(17) 0.85116(10) 0.16843(11) 0.0182(4) Uani 1 1 d . . . . .
H1A H 0.7562 0.8560 0.1135 0.022 Uiso 1 1 calc R . . . .
H1B H 0.8751 0.8824 0.1778 0.022 Uiso 1 1 calc R . . . .
C2 C 0.72122(17) 0.69611(10) 0.13471(11) 0.0190(4) Uani 1 1 d . . . . .
H2A H 0.7389 0.6885 0.0825 0.023 Uiso 1 1 calc R . . . .
H2B H 0.6362 0.7174 0.1295 0.023 Uiso 1 1 calc R . . . .
C3 C 0.99151(17) 0.73446(11) 0.17465(11) 0.0196(4) Uani 1 1 d . . . . .
H3A H 1.0084 0.7639 0.1306 0.024 Uiso 1 1 calc R . . . .
H3B H 0.9976 0.6811 0.1626 0.024 Uiso 1 1 calc R . . . .
C4 C 0.65331(16) 0.83738(10) 0.36918(10) 0.0170(3) Uani 1 1 d . . . . .
C5 C 0.68856(19) 0.89640(11) 0.42003(11) 0.0235(4) Uani 1 1 d . . . . .
H5 H 0.7658 0.9212 0.4210 0.028 Uiso 1 1 calc R . . . .
C6 C 0.6114(2) 0.91924(12) 0.46937(12) 0.0296(5) Uani 1 1 d . . . . .
H6 H 0.6355 0.9603 0.5028 0.036 Uiso 1 1 calc R . . . .
C7 C 0.5004(2) 0.88283(14) 0.47018(12) 0.0311(5) Uani 1 1 d . . . . .
H7 H 0.4479 0.8989 0.5037 0.037 Uiso 1 1 calc R . . . .
C8 C 0.46656(19) 0.82294(14) 0.42189(12) 0.0310(5) Uani 1 1 d . . . . .
H8 H 0.3915 0.7967 0.4233 0.037 Uiso 1 1 calc R . . . .
C9 C 0.54145(18) 0.80043(12) 0.37098(11) 0.0240(4) Uani 1 1 d . . . . .
H9 H 0.5162 0.7597 0.3373 0.029 Uiso 1 1 calc R . . . .
C10 C 0.7255(2) 0.97846(12) 0.26116(13) 0.0327(5) Uani 1 1 d . . . . .
H10A H 0.6725 0.9946 0.2966 0.049 Uiso 1 1 calc GR . . . .
H10B H 0.7083 1.0094 0.2146 0.049 Uiso 1 1 calc GR . . . .
H10C H 0.8138 0.9834 0.2866 0.049 Uiso 1 1 calc GR . . . .
C11 C 0.52289(19) 0.87240(14) 0.18433(13) 0.0307(5) Uani 1 1 d . . . . .
H11A H 0.5042 0.8213 0.1666 0.046 Uiso 1 1 calc GR . . . .
H11B H 0.5066 0.9061 0.1399 0.046 Uiso 1 1 calc GR . . . .
H11C H 0.4696 0.8861 0.2205 0.046 Uiso 1 1 calc GR . . . .
C12 C 0.85295(17) 0.57186(10) 0.33353(10) 0.0172(3) Uani 1 1 d . . . . .
C13 C 0.77408(19) 0.52328(11) 0.36220(11) 0.0213(4) Uani 1 1 d . . . . .
H13 H 0.6865 0.5325 0.3525 0.026 Uiso 1 1 calc R . . . .
C14 C 0.8230(2) 0.46115(11) 0.40501(11) 0.0254(4) Uani 1 1 d . . . . .
H14 H 0.7680 0.4279 0.4234 0.031 Uiso 1 1 calc R . . . .
C15 C 0.9503(2) 0.44725(11) 0.42112(11) 0.0266(4) Uani 1 1 d . . . . .
H15 H 0.9831 0.4048 0.4503 0.032 Uiso 1 1 calc R . . . .
C16 C 1.0292(2) 0.49619(11) 0.39411(11) 0.0263(4) Uani 1 1 d . . . . .
H16 H 1.1170 0.4876 0.4056 0.032 Uiso 1 1 calc R . . . .
C17 C 0.98168(18) 0.55769(11) 0.35042(11) 0.0218(4) Uani 1 1 d . . . . .
H17 H 1.0371 0.5904 0.3318 0.026 Uiso 1 1 calc R . . . .
C18 C 0.5804(3) 0.56237(16) 0.18515(14) 0.0456(7) Uani 1 1 d . . . . .
H18A H 0.5916 0.5148 0.2126 0.068 Uiso 1 1 calc GR . . . .
H18B H 0.5402 0.5539 0.1309 0.068 Uiso 1 1 calc GR . . . .
H18C H 0.5275 0.5950 0.2093 0.068 Uiso 1 1 calc GR . . . .
C19 C 0.8421(3) 0.54181(13) 0.15079(14) 0.0403(6) Uani 1 1 d . . . . .
H19A H 0.8654 0.5642 0.1052 0.061 Uiso 1 1 calc GR . . . .
H19B H 0.7987 0.4947 0.1363 0.061 Uiso 1 1 calc GR . . . .
H19C H 0.9177 0.5328 0.1904 0.061 Uiso 1 1 calc GR . . . .
C20 C 1.08378(17) 0.78554(11) 0.41317(11) 0.0205(4) Uani 1 1 d . . . . .
C21 C 1.0733(2) 0.85985(13) 0.43234(13) 0.0318(5) Uani 1 1 d . . . . .
H21 H 1.0233 0.8925 0.3965 0.038 Uiso 1 1 calc R . . . .
C22 C 1.1360(3) 0.88669(16) 0.50407(15) 0.0483(7) Uani 1 1 d . . . . .
H22 H 1.1278 0.9374 0.5169 0.058 Uiso 1 1 calc R . . . .
C23 C 1.2094(3) 0.84033(19) 0.55620(14) 0.0522(8) Uani 1 1 d . . . . .
H23 H 1.2527 0.8591 0.6046 0.063 Uiso 1 1 calc R . . . .
C24 C 1.2202(2) 0.76638(18) 0.53811(13) 0.0443(7) Uani 1 1 d . . . . .
H24 H 1.2706 0.7342 0.5743 0.053 Uiso 1 1 calc R . . . .
C25 C 1.15758(19) 0.73868(14) 0.46715(12) 0.0296(5) Uani 1 1 d . . . . .
H25 H 1.1650 0.6876 0.4553 0.035 Uiso 1 1 calc R . . . .
C26 C 1.23694(18) 0.68933(11) 0.28299(12) 0.0246(4) Uani 1 1 d . . . . .
H26A H 1.2880 0.6958 0.3351 0.037 Uiso 1 1 calc GR . . . .
H26B H 1.2894 0.6964 0.2447 0.037 Uiso 1 1 calc GR . . . .
H26C H 1.2014 0.6392 0.2779 0.037 Uiso 1 1 calc GR . . . .
C27 C 1.17848(19) 0.85180(11) 0.25907(12) 0.0242(4) Uani 1 1 d . . . . .
H27A H 1.1120 0.8890 0.2454 0.036 Uiso 1 1 calc GR . . . .
H27B H 1.2288 0.8506 0.2191 0.036 Uiso 1 1 calc GR . . . .
H27C H 1.2321 0.8648 0.3089 0.036 Uiso 1 1 calc GR . . . .
C91 C 0.5007(4) 0.59171(12) 0.45985(19) 0.0371(12) Uani 0.5 1 d . U P A -1
H91 H 0.5034 0.6402 0.4391 0.045 Uiso 0.5 1 calc R . P A -1
C92 C 0.6113(3) 0.55612(17) 0.49420(18) 0.0352(11) Uani 0.5 1 d G U P A -1
H92 H 0.6895 0.5803 0.4969 0.042 Uiso 0.5 1 calc R . P A -1
C93 C 0.6074(2) 0.48516(17) 0.52455(18) 0.0276(12) Uani 0.5 1 d G U P A -1
H93 H 0.6829 0.4608 0.5480 0.033 Uiso 0.5 1 calc R . P A -1
C95 C 0.4929(3) 0.44979(12) 0.52055(19) 0.0237(8) Uani 0.5 1 d G U P A -1
C94 C 0.3824(2) 0.48537(17) 0.48620(18) 0.0197(10) Uani 0.5 1 d DG U P A -1
H94 H 0.3042 0.4612 0.4835 0.024 Uiso 0.5 1 calc R . P A -1
C96 C 0.3863(3) 0.55634(17) 0.45585(17) 0.0348(11) Uani 0.5 1 d DG . P A -1
H96 H 0.3108 0.5807 0.4324 0.042 Uiso 0.5 1 calc R . P A -1
C97 C 0.4920(5) 0.3734(3) 0.5529(3) 0.0384(12) Uani 0.5 1 d D . P A -1
H97A H 0.5562 0.3433 0.5360 0.058 Uiso 0.5 1 calc GR . P A -1
H97B H 0.4095 0.3509 0.5344 0.058 Uiso 0.5 1 calc GR . P A -1
H97C H 0.5096 0.3759 0.6095 0.058 Uiso 0.5 1 calc GR . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti Cl 2.3203(5) . ?
Ti P 2.5062(5) . ?
Ti N1 1.9933(15) . ?
Ti N2 1.9695(15) . ?
Ti N3 1.9587(15) . ?
P C1 1.7955(18) . ?
P C2 1.8081(18) . ?
P C3 1.8101(19) . ?
Si1 N1 1.7579(16) . ?
Si1 C1 1.8809(19) . ?
Si1 C10 1.867(2) . ?
Si1 C11 1.867(2) . ?
Si2 N2 1.7582(16) . ?
Si2 C2 1.8743(19) . ?
Si2 C18 1.854(2) . ?
Si2 C19 1.880(2) . ?
Si3 N3 1.7514(16) . ?
Si3 C3 1.8914(19) . ?
Si3 C26 1.867(2) . ?
Si3 C27 1.858(2) . ?
N1 C4 1.442(2) . ?
N2 C12 1.441(2) . ?
N3 C20 1.438(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.394(3) . ?
C4 C9 1.396(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.392(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.379(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.378(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.394(3) . ?
C9 H9 0.9500 . ?
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 C13 1.393(3) . ?
C12 C17 1.398(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.394(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.382(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.384(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.388(3) . ?
C17 H17 0.9500 . ?
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 C21 1.391(3) . ?
C20 C25 1.398(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.397(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.373(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.380(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.391(3) . ?
C25 H25 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C91 H91 0.9500 . ?
C91 C92 1.3900 . ?
C91 C96 1.3900 . ?
C92 H92 0.9500 . ?
C92 C93 1.3900 . ?
C93 H93 0.9500 . ?
C93 C95 1.3900 . ?
C95 C94 1.3900 . ?
C95 C97 1.490(6) . ?
C94 H94 0.9500 . ?
C94 C96 1.3900 . ?
C96 H96 0.9500 . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
C97 H97C 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
Cl Ti P 175.21(2) . . ?
N1 Ti Cl 98.78(5) . . ?
N1 Ti P 78.80(4) . . ?
N2 Ti Cl 101.38(5) . . ?
N2 Ti P 76.78(5) . . ?
N2 Ti N1 122.77(6) . . ?
N3 Ti Cl 103.67(5) . . ?
N3 Ti P 81.11(5) . . ?
N3 Ti N1 114.77(6) . . ?
N3 Ti N2 111.38(7) . . ?
C1 P Ti 110.58(6) . . ?
C1 P C2 109.49(9) . . ?
C1 P C3 110.30(9) . . ?
C2 P Ti 109.06(6) . . ?
C2 P C3 110.25(9) . . ?
C3 P Ti 107.12(6) . . ?
N1 Si1 C1 104.74(8) . . ?
N1 Si1 C10 113.74(9) . . ?
N1 Si1 C11 111.05(9) . . ?
C10 Si1 C1 107.35(9) . . ?
C10 Si1 C11 108.19(11) . . ?
C11 Si1 C1 111.74(9) . . ?
N2 Si2 C2 103.42(8) . . ?
N2 Si2 C18 111.84(10) . . ?
N2 Si2 C19 110.36(10) . . ?
C2 Si2 C19 109.37(10) . . ?
C18 Si2 C2 111.65(11) . . ?
C18 Si2 C19 110.02(13) . . ?
N3 Si3 C3 104.97(8) . . ?
N3 Si3 C26 112.57(8) . . ?
N3 Si3 C27 111.04(9) . . ?
C26 Si3 C3 109.22(9) . . ?
C27 Si3 C3 111.46(9) . . ?
C27 Si3 C26 107.61(9) . . ?
Si1 N1 Ti 131.01(8) . . ?
C4 N1 Ti 119.54(11) . . ?
C4 N1 Si1 109.44(11) . . ?
Si2 N2 Ti 132.08(9) . . ?
C12 N2 Ti 114.75(11) . . ?
C12 N2 Si2 112.75(12) . . ?
Si3 N3 Ti 129.34(8) . . ?
C20 N3 Ti 114.94(11) . . ?
C20 N3 Si3 115.50(12) . . ?
P C1 Si1 105.20(9) . . ?
P C1 H1A 110.7 . . ?
P C1 H1B 110.7 . . ?
Si1 C1 H1A 110.7 . . ?
Si1 C1 H1B 110.7 . . ?
H1A C1 H1B 108.8 . . ?
P C2 Si2 104.25(9) . . ?
P C2 H2A 110.9 . . ?
P C2 H2B 110.9 . . ?
Si2 C2 H2A 110.9 . . ?
Si2 C2 H2B 110.9 . . ?
H2A C2 H2B 108.9 . . ?
P C3 Si3 106.54(9) . . ?
P C3 H3A 110.4 . . ?
P C3 H3B 110.4 . . ?
Si3 C3 H3A 110.4 . . ?
Si3 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
C5 C4 N1 121.28(17) . . ?
C5 C4 C9 118.39(17) . . ?
C9 C4 N1 120.20(17) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.45(19) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 H6 119.6 . . ?
C7 C6 C5 120.7(2) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119.33(19) . . ?
C8 C7 H7 120.3 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.6(2) . . ?
C9 C8 H8 119.7 . . ?
C4 C9 H9 119.8 . . ?
C8 C9 C4 120.5(2) . . ?
C8 C9 H9 119.8 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 N2 121.57(17) . . ?
C13 C12 C17 118.41(17) . . ?
C17 C12 N2 119.97(17) . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C14 120.36(18) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 119.6 . . ?
C15 C14 C13 120.90(19) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 120.5 . . ?
C14 C15 C16 118.92(18) . . ?
C16 C15 H15 120.5 . . ?
C15 C16 H16 119.6 . . ?
C15 C16 C17 120.81(19) . . ?
C17 C16 H16 119.6 . . ?
C12 C17 H17 119.7 . . ?
C16 C17 C12 120.58(19) . . ?
C16 C17 H17 119.7 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 N3 120.46(18) . . ?
C21 C20 C25 118.6(2) . . ?
C25 C20 N3 120.91(19) . . ?
C20 C21 H21 119.8 . . ?
C20 C21 C22 120.3(2) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 119.7 . . ?
C23 C22 C21 120.5(3) . . ?
C23 C22 H22 119.7 . . ?
C22 C23 H23 120.1 . . ?
C22 C23 C24 119.8(2) . . ?
C24 C23 H23 120.1 . . ?
C23 C24 H24 119.8 . . ?
C23 C24 C25 120.4(2) . . ?
C25 C24 H24 119.8 . . ?
C20 C25 H25 119.8 . . ?
C24 C25 C20 120.4(2) . . ?
C24 C25 H25 119.8 . . ?
Si3 C26 H26A 109.5 . . ?
Si3 C26 H26B 109.5 . . ?
Si3 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si3 C27 H27A 109.5 . . ?
Si3 C27 H27B 109.5 . . ?
Si3 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C92 C91 H91 120.0 . . ?
C92 C91 C96 120.0 . . ?
C96 C91 H91 120.0 . . ?
C91 C92 H92 120.0 . . ?
C93 C92 C91 120.0 . . ?
C93 C92 H92 120.0 . . ?
C92 C93 H93 120.0 . . ?
C92 C93 C95 120.0 . . ?
C95 C93 H93 120.0 . . ?
C93 C95 C94 120.0 . . ?
C93 C95 C97 118.7(3) . . ?
C94 C95 C97 121.3(3) . . ?
C95 C94 H94 120.0 . . ?
C95 C94 C96 120.0 . . ?
C96 C94 H94 120.0 . . ?
C91 C96 H96 120.0 . . ?
C94 C96 C91 120.0 . . ?
C94 C96 H96 120.0 . . ?
C95 C97 H97A 109.5 . . ?
C95 C97 H97B 109.5 . . ?
C95 C97 H97C 109.5 . . ?
H97A C97 H97B 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 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
Ti P C1 Si1 -32.51(10) . . . . ?
Ti P C2 Si2 -37.43(10) . . . . ?
Ti P C3 Si3 -32.85(10) . . . . ?
Ti N1 C4 C5 100.49(18) . . . . ?
Ti N1 C4 C9 -83.58(19) . . . . ?
Ti N2 C12 C13 111.75(17) . . . . ?
Ti N2 C12 C17 -70.83(19) . . . . ?
Ti N3 C20 C21 -82.67(19) . . . . ?
Ti N3 C20 C25 97.54(18) . . . . ?
Si1 N1 C4 C5 -78.51(18) . . . . ?
Si1 N1 C4 C9 97.42(18) . . . . ?
Si2 N2 C12 C13 -74.82(19) . . . . ?
Si2 N2 C12 C17 102.60(17) . . . . ?
Si3 N3 C20 C21 92.45(19) . . . . ?
Si3 N3 C20 C25 -87.33(19) . . . . ?
N1 Si1 C1 P 23.27(11) . . . . ?
N1 C4 C5 C6 173.81(17) . . . . ?
N1 C4 C9 C8 -175.25(18) . . . . ?
N2 Si2 C2 P 22.61(11) . . . . ?
N2 C12 C13 C14 175.87(17) . . . . ?
N2 C12 C17 C16 -176.88(17) . . . . ?
N3 Si3 C3 P 21.89(12) . . . . ?
N3 C20 C21 C22 -179.54(19) . . . . ?
N3 C20 C25 C24 179.05(18) . . . . ?
C1 P C2 Si2 -158.55(9) . . . . ?
C1 P C3 Si3 87.56(11) . . . . ?
C1 Si1 N1 Ti -2.54(13) . . . . ?
C1 Si1 N1 C4 176.30(12) . . . . ?
C2 P C1 Si1 87.68(11) . . . . ?
C2 P C3 Si3 -151.40(9) . . . . ?
C2 Si2 N2 Ti 6.77(14) . . . . ?
C2 Si2 N2 C12 -165.18(13) . . . . ?
C3 P C1 Si1 -150.82(9) . . . . ?
C3 P C2 Si2 79.93(11) . . . . ?
C3 Si3 N3 Ti 3.07(13) . . . . ?
C3 Si3 N3 C20 -171.21(14) . . . . ?
C4 C5 C6 C7 1.6(3) . . . . ?
C5 C4 C9 C8 0.8(3) . . . . ?
C5 C6 C7 C8 0.5(3) . . . . ?
C6 C7 C8 C9 -1.9(3) . . . . ?
C7 C8 C9 C4 1.2(3) . . . . ?
C9 C4 C5 C6 -2.2(3) . . . . ?
C10 Si1 N1 Ti -119.46(12) . . . . ?
C10 Si1 N1 C4 59.39(15) . . . . ?
C10 Si1 C1 P 144.49(10) . . . . ?
C11 Si1 N1 Ti 118.23(12) . . . . ?
C11 Si1 N1 C4 -62.93(15) . . . . ?
C11 Si1 C1 P -97.04(11) . . . . ?
C12 C13 C14 C15 1.3(3) . . . . ?
C13 C12 C17 C16 0.6(3) . . . . ?
C13 C14 C15 C16 0.1(3) . . . . ?
C14 C15 C16 C17 -1.1(3) . . . . ?
C15 C16 C17 C12 0.7(3) . . . . ?
C17 C12 C13 C14 -1.6(3) . . . . ?
C18 Si2 N2 Ti -113.52(15) . . . . ?
C18 Si2 N2 C12 74.53(17) . . . . ?
C18 Si2 C2 P 143.02(12) . . . . ?
C19 Si2 N2 Ti 123.65(13) . . . . ?
C19 Si2 N2 C12 -48.29(16) . . . . ?
C19 Si2 C2 P -94.97(12) . . . . ?
C20 C21 C22 C23 0.5(4) . . . . ?
C21 C20 C25 C24 -0.7(3) . . . . ?
C21 C22 C23 C24 -0.9(4) . . . . ?
C22 C23 C24 C25 0.4(4) . . . . ?
C23 C24 C25 C20 0.4(3) . . . . ?
C25 C20 C21 C22 0.2(3) . . . . ?
C26 Si3 N3 Ti -115.62(12) . . . . ?
C26 Si3 N3 C20 70.09(16) . . . . ?
C26 Si3 C3 P 142.82(10) . . . . ?
C27 Si3 N3 Ti 123.65(11) . . . . ?
C27 Si3 N3 C20 -50.63(16) . . . . ?
C27 Si3 C3 P -98.40(11) . . . . ?
C91 C92 C93 C95 0.0 . . . . ?
C92 C91 C96 C94 0.0 . . . . ?
C92 C93 C95 C94 0.0 . . . . ?
C92 C93 C95 C97 179.4(4) . . . . ?
C93 C95 C94 C96 0.0 . . . . ?
C95 C94 C96 C91 0.0 . . . . ?
C96 C91 C92 C93 0.0 . . . . ?
C97 C95 C94 C96 -179.4(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            10.9066(2)
_cell_oxdiff_length_b            18.0088(4)
_cell_oxdiff_length_c            17.6705(4)
_cell_oxdiff_angle_alpha         90.0039(18)
_cell_oxdiff_angle_beta          101.8328(19)
_cell_oxdiff_angle_gamma         89.9979(17)
_cell_oxdiff_volume              3396.99(13)
_cell_oxdiff_measurement_reflns_used 20759
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent EOS'
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_jb3
_database_code_depnum_ccdc_archive 'CCDC 1437767'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon Sep 07 18:45:19 2015'
;

_audit_block_code                ba_jb3
_audit_block_refno               1536
_audit_block_usercomment         'jb053_Zr, irregular, colourless'


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C27 H39 Cl N3 P Si3 Zr'
_chemical_formula_sum            'C27 H39 Cl N3 P Si3 Zr'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         647.52
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      110(1)
_chemical_oxdiff_formula         'C27 H39 Cl1 N3 P1 Si3 Zr1'
_chemical_oxdiff_usercomment     'jb053_Zr, irregular, colourless'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2ybc'
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                   8.92072(7)
_cell_length_b                   17.53308(17)
_cell_length_c                   21.06985(16)
_cell_angle_alpha                90
_cell_angle_beta                 101.8664(7)
_cell_angle_gamma                90
_cell_volume                     3225.06(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    27497
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      72.0060
_cell_measurement_theta_min      4.2740
_shelx_estimated_absorpt_T_max   0.622
_shelx_estimated_absorpt_T_min   0.622
_exptl_absorpt_coefficient_mu    5.247
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.071
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73372
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.200
_diffrn_reflns_theta_min         4.288
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -65.00   21.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -60.0000 86

#__ type_ start__ end____ width___ exp.time_
  2 omega  -22.00   35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   80.0000  108.0000 57

#__ type_ start__ end____ width___ exp.time_
  3 omega  -46.00    3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.0000  -76.0000 -115.0000 49

#__ type_ start__ end____ width___ exp.time_
  4 omega   10.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000   77.0000 33

#__ type_ start__ end____ width___ exp.time_
  5 omega  -78.00  -12.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   90.0000 66

#__ type_ start__ end____ width___ exp.time_
  6 omega  -26.00   30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  -90.0000 56

#__ type_ start__ end____ width___ exp.time_
  7 omega  -95.00  -12.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -150.0000 83

#__ type_ start__ end____ width___ exp.time_
  8 omega  -63.00   26.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   57.0000   30.0000 89

#__ type_ start__ end____ width___ exp.time_
  9 omega   14.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   -1.0000 25

#__ type_ start__ end____ width___ exp.time_
 10 omega   14.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -51.0000 25

#__ type_ start__ end____ width___ exp.time_
 11 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -87.0000 25

#__ type_ start__ end____ width___ exp.time_
 12 omega   18.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   94.0000 25

#__ type_ start__ end____ width___ exp.time_
 13 omega   18.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -138.0000 25

#__ type_ start__ end____ width___ exp.time_
 14 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  172.0000 25

#__ type_ start__ end____ width___ exp.time_
 15 omega   24.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   32.0000 28

#__ type_ start__ end____ width___ exp.time_
 16 omega   60.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  137.0000 56

#__ type_ start__ end____ width___ exp.time_
 17 omega   26.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  137.0000 29

#__ type_ start__ end____ width___ exp.time_
 18 omega   23.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -172.0000 25

#__ type_ start__ end____ width___ exp.time_
 19 omega   81.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   32.0000 37

#__ type_ start__ end____ width___ exp.time_
 20 omega  -13.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296  -80.0000   99.0000 93

#__ type_ start__ end____ width___ exp.time_
 21 omega   28.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   -0.0000 36

#__ type_ start__ end____ width___ exp.time_
 22 omega   98.00  123.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -35.0000 25

#__ type_ start__ end____ width___ exp.time_
 23 omega   29.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -35.0000 26

#__ type_ start__ end____ width___ exp.time_
 24 omega   67.00  126.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   -0.0000 59

#__ type_ start__ end____ width___ exp.time_
 25 omega   29.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   99.0000 99

#__ type_ start__ end____ width___ exp.time_
 26 omega   29.00  123.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -155.0000 94

#__ type_ start__ end____ width___ exp.time_
 27 omega   28.00  123.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -118.0000 95

#__ type_ start__ end____ width___ exp.time_
 28 omega   29.00  125.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -59.0000 96

#__ type_ start__ end____ width___ exp.time_
 29 omega  103.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   50.0000 25

#__ type_ start__ end____ width___ exp.time_
 30 omega   30.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   50.0000 44

#__ type_ start__ end____ width___ exp.time_
 31 omega    7.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -80.0000   30.0000 73

#__ type_ start__ end____ width___ exp.time_
 32 omega    7.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  161.0000 74

#__ type_ start__ end____ width___ exp.time_
 33 omega   12.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -79.0000  -81.0000 85

#__ type_ start__ end____ width___ exp.time_
 34 omega   53.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -80.0000  141.0000 53

#__ type_ start__ end____ width___ exp.time_
 35 omega  149.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -30.0000 29

#__ type_ start__ end____ width___ exp.time_
 36 omega   40.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -80.0000  -12.0000 71

#__ type_ start__ end____ width___ exp.time_
 37 omega   75.00  142.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -80.0000  -99.0000 67

#__ type_ start__ end____ width___ exp.time_
 38 omega   85.00  110.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
 39 omega   88.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   64.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 40 omega   43.00   70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -80.0000  -99.0000 27

#__ type_ start__ end____ width___ exp.time_
 41 omega  116.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   90.0000 60

#__ type_ start__ end____ width___ exp.time_
 42 omega   81.00  110.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   90.0000 29

#__ type_ start__ end____ width___ exp.time_
 43 omega   85.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 44 omega   81.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -180.0000 95

#__ type_ start__ end____ width___ exp.time_
 45 omega   88.00  160.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   64.0000  -30.0000 72

#__ type_ start__ end____ width___ exp.time_
 46 omega  111.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -90.0000 67

#__ type_ start__ end____ width___ exp.time_
 47 omega   81.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 48 omega   88.00  118.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   64.0000 -120.0000 30

#__ type_ start__ end____ width___ exp.time_
 49 omega  136.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   30.0000 41

#__ type_ start__ end____ width___ exp.time_
 50 omega   81.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 51 omega  143.00  173.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -60.0000 30

#__ type_ start__ end____ width___ exp.time_
 52 omega   81.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -60.0000 58

#__ type_ start__ end____ width___ exp.time_
 53 omega  125.00  165.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  120.0000 40

#__ type_ start__ end____ width___ exp.time_
 54 omega   81.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
 55 omega  117.00  168.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -150.0000 51

#__ type_ start__ end____ width___ exp.time_
 56 omega   81.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 57 omega   85.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 58 omega   81.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
 59 omega   96.00  156.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000  150.0000 60

#__ type_ start__ end____ width___ exp.time_
 60 omega   85.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 61 omega   82.00  168.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   60.0000 86

#__ type_ start__ end____ width___ exp.time_
 62 omega   85.00  154.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000   60.0000 69

#__ type_ start__ end____ width___ exp.time_
 63 omega   92.00  119.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000  -60.0000 27

#__ type_ start__ end____ width___ exp.time_
 64 omega   90.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000   30.0000 25

#__ type_ start__ end____ width___ exp.time_
 65 omega  111.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000    0.0000 67

#__ type_ start__ end____ width___ exp.time_
 66 omega   81.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 67 omega   91.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000 -180.0000 47

#__ type_ start__ end____ width___ exp.time_
 68 omega   85.00  112.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000  -60.0000 27

#__ type_ start__ end____ width___ exp.time_
 69 omega   91.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 70 omega   85.00  118.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000 -180.0000 33

#__ type_ start__ end____ width___ exp.time_
 71 omega  138.00  165.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 72 omega   68.00  141.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -80.0000 -174.0000 73

#__ type_ start__ end____ width___ exp.time_
 73 omega   85.00  133.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000   90.0000 48

#__ type_ start__ end____ width___ exp.time_
 74 omega   85.00  118.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000  120.0000 33

#__ type_ start__ end____ width___ exp.time_
 75 omega   81.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 76 omega   81.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -120.0000 97

#__ type_ start__ end____ width___ exp.time_
 77 omega   48.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -80.0000   65.0000 59

#__ type_ start__ end____ width___ exp.time_
 78 omega  -69.00   21.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 90

#__ type_ start__ end____ width___ exp.time_
 79 omega  -26.00   72.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000    0.0000 98

#__ type_ start__ end____ width___ exp.time_
 80 omega   18.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  152.0000 28

#__ type_ start__ end____ width___ exp.time_
 81 omega   18.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -138.0000 28

#__ type_ start__ end____ width___ exp.time_
 82 omega   18.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -38.0000 28

#__ type_ start__ end____ width___ exp.time_
 83 omega   19.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -87.0000 28

#__ type_ start__ end____ width___ exp.time_
 84 omega   24.00  124.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   96.0000 100

#__ type_ start__ end____ width___ exp.time_
 85 omega   25.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  137.0000 39

#__ type_ start__ end____ width___ exp.time_
 86 omega   25.00  124.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000 -148.0000 99

#__ type_ start__ end____ width___ exp.time_
 87 omega   23.00   49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -172.0000 26

#__ type_ start__ end____ width___ exp.time_
 88 omega   11.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   19.0000  -30.0000 117

#__ type_ start__ end____ width___ exp.time_
 89 omega   30.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   38.0000 -150.0000 98

#__ type_ start__ end____ width___ exp.time_
 90 omega   29.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -59.0000 99

#__ type_ start__ end____ width___ exp.time_
 91 omega   29.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   50.0000 99

#__ type_ start__ end____ width___ exp.time_
 92 omega   28.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   -0.0000 100

#__ type_ start__ end____ width___ exp.time_
 93 omega   -5.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -135.0000 103

#__ type_ start__ end____ width___ exp.time_
 94 omega   -5.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -79.0000 -107.0000 102

#__ type_ start__ end____ width___ exp.time_
 95 omega    7.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000  -22.0000 102

#__ type_ start__ end____ width___ exp.time_
 96 omega    7.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  161.0000 103

#__ type_ start__ end____ width___ exp.time_
 97 omega   11.00  113.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -79.0000   75.0000 102

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.1714626000
_diffrn_orient_matrix_UB_12      -0.0195914000
_diffrn_orient_matrix_UB_13      -0.0092079000
_diffrn_orient_matrix_UB_21      -0.0259396000
_diffrn_orient_matrix_UB_22      0.0274794000
_diffrn_orient_matrix_UB_23      -0.0708548000
_diffrn_orient_matrix_UB_31      0.0326425000
_diffrn_orient_matrix_UB_32      -0.0811385000
_diffrn_orient_matrix_UB_33      -0.0217944000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5848
_reflns_number_total             6318
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         2.481
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0489
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0387P)²+10.4382P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1141
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr 0.35077(3) 0.22955(2) 0.70589(2) 0.01758(10) Uani 1 1 d . . . . .
Cl Cl 0.62503(10) 0.23269(6) 0.70902(5) 0.0304(2) Uani 1 1 d . . . . .
P1 P 0.04600(10) 0.22998(5) 0.70557(4) 0.01865(18) Uani 1 1 d . . . . .
Si1 Si 0.19073(11) 0.23206(6) 0.84555(4) 0.0192(2) Uani 1 1 d . . . . .
Si2 Si 0.09096(11) 0.37160(6) 0.63518(5) 0.0229(2) Uani 1 1 d . . . . .
Si3 Si 0.09081(11) 0.08646(6) 0.63646(5) 0.0226(2) Uani 1 1 d . . . . .
N1 N 0.3420(3) 0.23535(17) 0.80476(14) 0.0199(6) Uani 1 1 d . . . . .
N2 N 0.2680(3) 0.32592(17) 0.65075(14) 0.0207(6) Uani 1 1 d . . . . .
N3 N 0.2722(3) 0.12635(18) 0.66062(14) 0.0210(6) Uani 1 1 d . . . . .
C1 C 0.0153(4) 0.2604(2) 0.78422(17) 0.0220(7) Uani 1 1 d . . . . .
H1A H -0.0767 0.2353 0.7940 0.026 Uiso 1 1 calc R . . . .
H1B H 0.0005 0.3163 0.7848 0.026 Uiso 1 1 calc R . . . .
C2 C -0.0517(4) 0.2952(2) 0.64332(18) 0.0243(8) Uani 1 1 d . . . . .
H2A H -0.1427 0.3177 0.6563 0.029 Uiso 1 1 calc R . . . .
H2B H -0.0854 0.2680 0.6016 0.029 Uiso 1 1 calc R . . . .
C3 C -0.0294(4) 0.1342(2) 0.68858(17) 0.0222(7) Uani 1 1 d . . . . .
H3A H -0.1378 0.1363 0.6655 0.027 Uiso 1 1 calc R . . . .
H3B H -0.0234 0.1055 0.7295 0.027 Uiso 1 1 calc R . . . .
C4 C 0.2218(5) 0.2991(2) 0.91513(19) 0.0304(9) Uani 1 1 d . . . . .
H4A H 0.3155 0.2850 0.9461 0.046 Uiso 1 1 calc GR . . . .
H4B H 0.1344 0.2967 0.9366 0.046 Uiso 1 1 calc GR . . . .
H4C H 0.2321 0.3511 0.8995 0.046 Uiso 1 1 calc GR . . . .
C5 C 0.1675(4) 0.1340(2) 0.87668(18) 0.0260(8) Uani 1 1 d . . . . .
H5A H 0.1617 0.0971 0.8413 0.039 Uiso 1 1 calc GR . . . .
H5B H 0.0732 0.1316 0.8936 0.039 Uiso 1 1 calc GR . . . .
H5C H 0.2554 0.1218 0.9114 0.039 Uiso 1 1 calc GR . . . .
C6 C 0.4917(4) 0.2289(2) 0.84611(17) 0.0210(7) Uani 1 1 d . . . . .
C7 C 0.5613(4) 0.1577(2) 0.85994(19) 0.0272(8) Uani 1 1 d . . . . .
H7 H 0.5085 0.1129 0.8427 0.033 Uiso 1 1 calc R . . . .
C8 C 0.7071(5) 0.1519(3) 0.8987(2) 0.0363(10) Uani 1 1 d . . . . .
H8 H 0.7538 0.1033 0.9075 0.044 Uiso 1 1 calc R . . . .
C9 C 0.7846(5) 0.2171(3) 0.9247(2) 0.0367(10) Uani 1 1 d . . . . .
H9 H 0.8838 0.2130 0.9515 0.044 Uiso 1 1 calc R . . . .
C10 C 0.7172(5) 0.2879(3) 0.9115(2) 0.0348(10) Uani 1 1 d . . . . .
H10 H 0.7704 0.3325 0.9290 0.042 Uiso 1 1 calc R . . . .
C11 C 0.5709(4) 0.2937(2) 0.87250(19) 0.0275(8) Uani 1 1 d . . . . .
H11 H 0.5249 0.3425 0.8639 0.033 Uiso 1 1 calc R . . . .
C12 C 0.0839(5) 0.4502(2) 0.6942(2) 0.0346(9) Uani 1 1 d . . . . .
H12A H 0.1070 0.4297 0.7384 0.052 Uiso 1 1 calc GR . . . .
H12B H -0.0186 0.4729 0.6855 0.052 Uiso 1 1 calc GR . . . .
H12C H 0.1597 0.4892 0.6897 0.052 Uiso 1 1 calc GR . . . .
C13 C 0.0499(5) 0.4132(3) 0.5522(2) 0.0344(10) Uani 1 1 d . . . . .
H13A H 0.1206 0.4555 0.5502 0.052 Uiso 1 1 calc GR . . . .
H13B H -0.0557 0.4321 0.5420 0.052 Uiso 1 1 calc GR . . . .
H13C H 0.0632 0.3739 0.5207 0.052 Uiso 1 1 calc GR . . . .
C14 C 0.3870(4) 0.3652(2) 0.62703(19) 0.0251(8) Uani 1 1 d . . . . .
C15 C 0.4168(5) 0.3505(3) 0.5668(2) 0.0436(12) Uani 1 1 d . . . . .
H15 H 0.3589 0.3136 0.5391 0.052 Uiso 1 1 calc R . . . .
C16 C 0.5388(6) 0.3925(4) 0.5464(3) 0.0607(17) Uani 1 1 d . . . . .
H16 H 0.5610 0.3840 0.5048 0.073 Uiso 1 1 calc R . . . .
C17 C 0.6212(7) 0.4445(3) 0.5877(3) 0.0608(16) Uani 1 1 d . . . . .
H17 H 0.6988 0.4731 0.5736 0.073 Uiso 1 1 calc R . . . .
C18 C 0.5959(6) 0.4565(3) 0.6481(3) 0.0583(16) Uani 1 1 d . . . . .
H18 H 0.6588 0.4907 0.6769 0.070 Uiso 1 1 calc R . . . .
C19 C 0.4776(5) 0.4184(3) 0.6671(3) 0.0459(12) Uani 1 1 d . . . . .
H19 H 0.4568 0.4286 0.7088 0.055 Uiso 1 1 calc R . . . .
C20 C 0.0121(5) 0.1052(3) 0.54843(18) 0.0354(10) Uani 1 1 d . . . . .
H20A H 0.0118 0.1603 0.5403 0.053 Uiso 1 1 calc GR . . . .
H20B H -0.0928 0.0856 0.5366 0.053 Uiso 1 1 calc GR . . . .
H20C H 0.0762 0.0797 0.5223 0.053 Uiso 1 1 calc GR . . . .
C21 C 0.0962(5) -0.0183(2) 0.6492(2) 0.0339(9) Uani 1 1 d . . . . .
H21A H 0.1555 -0.0422 0.6203 0.051 Uiso 1 1 calc GR . . . .
H21B H -0.0085 -0.0385 0.6398 0.051 Uiso 1 1 calc GR . . . .
H21C H 0.1443 -0.0296 0.6944 0.051 Uiso 1 1 calc GR . . . .
C22 C 0.3920(4) 0.0902(2) 0.63542(17) 0.0218(7) Uani 1 1 d . . . . .
C23 C 0.4234(5) 0.1119(2) 0.57582(18) 0.0282(8) Uani 1 1 d . . . . .
H23 H 0.3622 0.1499 0.5507 0.034 Uiso 1 1 calc R . . . .
C24 C 0.5427(5) 0.0788(3) 0.5527(2) 0.0367(10) Uani 1 1 d . . . . .
H24 H 0.5629 0.0944 0.5121 0.044 Uiso 1 1 calc R . . . .
C25 C 0.6318(5) 0.0236(3) 0.5883(2) 0.0371(10) Uani 1 1 d . . . . .
H25 H 0.7136 0.0012 0.5723 0.045 Uiso 1 1 calc R . . . .
C26 C 0.6032(5) 0.0008(3) 0.6468(2) 0.0372(10) Uani 1 1 d . . . . .
H26 H 0.6647 -0.0376 0.6712 0.045 Uiso 1 1 calc R . . . .
C27 C 0.4836(5) 0.0340(2) 0.6706(2) 0.0327(9) Uani 1 1 d . . . . .
H27 H 0.4644 0.0180 0.7112 0.039 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr Cl 2.4346(9) . ?
Zr P1 2.7174(9) . ?
Zr N1 2.103(3) . ?
Zr N2 2.097(3) . ?
Zr N3 2.098(3) . ?
P1 C1 1.814(4) . ?
P1 C2 1.821(4) . ?
P1 C3 1.817(4) . ?
Si1 N1 1.743(3) . ?
Si1 C1 1.880(4) . ?
Si1 C4 1.855(4) . ?
Si1 C5 1.867(4) . ?
Si2 N2 1.740(3) . ?
Si2 C2 1.880(4) . ?
Si2 C12 1.866(4) . ?
Si2 C13 1.859(4) . ?
Si3 N3 1.740(3) . ?
Si3 C3 1.882(4) . ?
Si3 C20 1.872(4) . ?
Si3 C21 1.856(4) . ?
N1 C6 1.441(4) . ?
N2 C14 1.439(5) . ?
N3 C22 1.435(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.399(5) . ?
C6 C11 1.392(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.390(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.388(7) . ?
C9 H9 0.9500 . ?
C9 C10 1.382(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.396(5) . ?
C11 H11 0.9500 . ?
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 C15 1.374(6) . ?
C14 C19 1.398(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.450(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.366(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.354(9) . ?
C18 H18 0.9500 . ?
C18 C19 1.377(7) . ?
C19 H19 0.9500 . ?
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 1.395(5) . ?
C22 C27 1.392(5) . ?
C23 H23 0.9500 . ?
C23 C24 1.384(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.374(7) . ?
C25 H25 0.9500 . ?
C25 C26 1.368(7) . ?
C26 H26 0.9500 . ?
C26 C27 1.396(6) . ?
C27 H27 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl Zr P1 177.99(3) . . ?
N1 Zr Cl 102.36(8) . . ?
N1 Zr P1 76.18(8) . . ?
N2 Zr Cl 103.56(8) . . ?
N2 Zr P1 76.00(8) . . ?
N2 Zr N1 115.41(12) . . ?
N2 Zr N3 113.36(11) . . ?
N3 Zr Cl 105.78(9) . . ?
N3 Zr P1 76.15(8) . . ?
N3 Zr N1 114.52(12) . . ?
C1 P1 Zr 109.72(12) . . ?
C1 P1 C2 109.49(18) . . ?
C1 P1 C3 109.40(17) . . ?
C2 P1 Zr 109.51(12) . . ?
C3 P1 Zr 109.12(12) . . ?
C3 P1 C2 109.59(17) . . ?
N1 Si1 C1 105.76(15) . . ?
N1 Si1 C4 111.31(17) . . ?
N1 Si1 C5 110.90(16) . . ?
C4 Si1 C1 110.12(18) . . ?
C4 Si1 C5 108.40(19) . . ?
C5 Si1 C1 110.35(18) . . ?
N2 Si2 C2 105.05(16) . . ?
N2 Si2 C12 111.58(17) . . ?
N2 Si2 C13 110.70(18) . . ?
C12 Si2 C2 110.45(19) . . ?
C13 Si2 C2 111.04(18) . . ?
C13 Si2 C12 108.0(2) . . ?
N3 Si3 C3 104.93(16) . . ?
N3 Si3 C20 110.85(17) . . ?
N3 Si3 C21 111.15(18) . . ?
C20 Si3 C3 110.94(19) . . ?
C21 Si3 C3 110.90(18) . . ?
C21 Si3 C20 108.1(2) . . ?
Si1 N1 Zr 132.61(16) . . ?
C6 N1 Zr 112.1(2) . . ?
C6 N1 Si1 114.5(2) . . ?
Si2 N2 Zr 132.68(16) . . ?
C14 N2 Zr 112.2(2) . . ?
C14 N2 Si2 114.8(2) . . ?
Si3 N3 Zr 133.12(17) . . ?
C22 N3 Zr 110.1(2) . . ?
C22 N3 Si3 115.6(2) . . ?
P1 C1 Si1 106.84(18) . . ?
P1 C1 H1A 110.4 . . ?
P1 C1 H1B 110.4 . . ?
Si1 C1 H1A 110.4 . . ?
Si1 C1 H1B 110.4 . . ?
H1A C1 H1B 108.6 . . ?
P1 C2 Si2 106.28(18) . . ?
P1 C2 H2A 110.5 . . ?
P1 C2 H2B 110.5 . . ?
Si2 C2 H2A 110.5 . . ?
Si2 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
P1 C3 Si3 107.09(18) . . ?
P1 C3 H3A 110.3 . . ?
P1 C3 H3B 110.3 . . ?
Si3 C3 H3A 110.3 . . ?
Si3 C3 H3B 110.3 . . ?
H3A C3 H3B 108.6 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 120.8(3) . . ?
C11 C6 N1 120.6(3) . . ?
C11 C6 C7 118.5(3) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.6(4) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.1(4) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 119.9(4) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 120.0(4) . . ?
C11 C10 H10 120.0 . . ?
C6 C11 C10 120.8(4) . . ?
C6 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N2 121.9(4) . . ?
C15 C14 C19 119.1(4) . . ?
C19 C14 N2 119.1(4) . . ?
C14 C15 H15 120.7 . . ?
C14 C15 C16 118.5(5) . . ?
C16 C15 H15 120.7 . . ?
C15 C16 H16 120.4 . . ?
C17 C16 C15 119.3(5) . . ?
C17 C16 H16 120.4 . . ?
C16 C17 H17 119.0 . . ?
C18 C17 C16 122.0(5) . . ?
C18 C17 H17 119.0 . . ?
C17 C18 H18 120.5 . . ?
C17 C18 C19 119.0(6) . . ?
C19 C18 H18 120.5 . . ?
C14 C19 H19 119.0 . . ?
C18 C19 C14 122.0(5) . . ?
C18 C19 H19 119.0 . . ?
Si3 C20 H20A 109.5 . . ?
Si3 C20 H20B 109.5 . . ?
Si3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N3 121.0(3) . . ?
C27 C22 N3 121.1(3) . . ?
C27 C22 C23 117.9(4) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 C22 120.9(4) . . ?
C24 C23 H23 119.6 . . ?
C23 C24 H24 119.9 . . ?
C25 C24 C23 120.2(4) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.3(4) . . ?
C26 C25 H25 119.9 . . ?
C25 C26 H26 120.1 . . ?
C25 C26 C27 119.9(4) . . ?
C27 C26 H26 120.1 . . ?
C22 C27 C26 120.9(4) . . ?
C22 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?

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
Zr P1 C1 Si1 -28.6(2) . . . . ?
Zr P1 C2 Si2 -29.5(2) . . . . ?
Zr P1 C3 Si3 -29.51(19) . . . . ?
Zr N1 C6 C7 -80.2(4) . . . . ?
Zr N1 C6 C11 99.0(3) . . . . ?
Zr N2 C14 C15 93.5(4) . . . . ?
Zr N2 C14 C19 -84.7(4) . . . . ?
Zr N3 C22 C23 -81.9(4) . . . . ?
Zr N3 C22 C27 96.1(4) . . . . ?
Si1 N1 C6 C7 90.8(4) . . . . ?
Si1 N1 C6 C11 -90.0(4) . . . . ?
Si2 N2 C14 C15 -92.4(4) . . . . ?
Si2 N2 C14 C19 89.5(4) . . . . ?
Si3 N3 C22 C23 87.8(4) . . . . ?
Si3 N3 C22 C27 -94.2(4) . . . . ?
N1 Si1 C1 P1 30.1(2) . . . . ?
N1 C6 C7 C8 178.6(3) . . . . ?
N1 C6 C11 C10 -178.7(4) . . . . ?
N2 Si2 C2 P1 32.8(2) . . . . ?
N2 C14 C15 C16 -180.0(4) . . . . ?
N2 C14 C19 C18 178.2(4) . . . . ?
N3 Si3 C3 P1 31.3(2) . . . . ?
N3 C22 C23 C24 177.6(4) . . . . ?
N3 C22 C27 C26 -177.9(4) . . . . ?
C1 P1 C2 Si2 90.8(2) . . . . ?
C1 P1 C3 Si3 -149.55(17) . . . . ?
C1 Si1 N1 Zr -22.0(3) . . . . ?
C1 Si1 N1 C6 169.3(3) . . . . ?
C2 P1 C1 Si1 -148.79(18) . . . . ?
C2 P1 C3 Si3 90.4(2) . . . . ?
C2 Si2 N2 Zr -26.9(3) . . . . ?
C2 Si2 N2 C14 160.4(3) . . . . ?
C3 P1 C1 Si1 91.1(2) . . . . ?
C3 P1 C2 Si2 -149.20(18) . . . . ?
C3 Si3 N3 Zr -23.3(3) . . . . ?
C3 Si3 N3 C22 170.1(3) . . . . ?
C4 Si1 N1 Zr -141.6(2) . . . . ?
C4 Si1 N1 C6 49.7(3) . . . . ?
C4 Si1 C1 P1 150.49(19) . . . . ?
C5 Si1 N1 Zr 97.6(2) . . . . ?
C5 Si1 N1 C6 -71.1(3) . . . . ?
C5 Si1 C1 P1 -89.9(2) . . . . ?
C6 C7 C8 C9 0.6(6) . . . . ?
C7 C6 C11 C10 0.5(6) . . . . ?
C7 C8 C9 C10 -0.6(6) . . . . ?
C8 C9 C10 C11 0.5(6) . . . . ?
C9 C10 C11 C6 -0.5(6) . . . . ?
C11 C6 C7 C8 -0.6(6) . . . . ?
C12 Si2 N2 Zr 92.8(3) . . . . ?
C12 Si2 N2 C14 -79.9(3) . . . . ?
C12 Si2 C2 P1 -87.6(2) . . . . ?
C13 Si2 N2 Zr -146.9(2) . . . . ?
C13 Si2 N2 C14 40.5(3) . . . . ?
C13 Si2 C2 P1 152.6(2) . . . . ?
C14 C15 C16 C17 0.8(7) . . . . ?
C15 C14 C19 C18 0.0(7) . . . . ?
C15 C16 C17 C18 2.0(9) . . . . ?
C16 C17 C18 C19 -3.8(9) . . . . ?
C17 C18 C19 C14 2.8(8) . . . . ?
C19 C14 C15 C16 -1.8(7) . . . . ?
C20 Si3 N3 Zr 96.5(3) . . . . ?
C20 Si3 N3 C22 -70.1(3) . . . . ?
C20 Si3 C3 P1 -88.4(2) . . . . ?
C21 Si3 N3 Zr -143.2(2) . . . . ?
C21 Si3 N3 C22 50.2(3) . . . . ?
C21 Si3 C3 P1 151.41(19) . . . . ?
C22 C23 C24 C25 0.3(7) . . . . ?
C23 C22 C27 C26 0.2(6) . . . . ?
C23 C24 C25 C26 0.1(7) . . . . ?
C24 C25 C26 C27 -0.3(7) . . . . ?
C25 C26 C27 C22 0.2(7) . . . . ?
C27 C22 C23 C24 -0.4(6) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4 7 4 0.0305 3.9986 6.9995 4.0007 -0.8596 -0.1948 -0.5246
5 3 -9 0.0445 4.9994 2.9900 -9.0139 -0.8328 0.5912 0.1170
-4 5 10 0.0361 -3.9963 5.0102 9.9923 0.4950 -0.4667 -0.7547
1 10 5 0.0312 1.0052 10.0048 4.9724 -0.4141 -0.1035 -0.8873
0 4 -13 0.0455 -0.0033 3.9836 -13.0055 0.0423 1.0311 -0.0399
-1 -4 13 0.0388 -0.9993 -4.0033 12.9994 0.1301 -1.0052 0.0089
-2 9 9 0.0354 -2.0009 8.9941 9.0031 0.0840 -0.3389 -0.9913
-1 -2 13 0.0525 -0.9996 -2.0038 12.9999 0.0909 -0.9502 -0.1534
1 9 -8 0.0350 0.9987 9.0007 -7.9980 -0.2739 0.7881 -0.5234
-5 -1 -1 0.0444 -4.9992 -1.0024 -0.9988 0.8860 0.1729 -0.0601
-4 9 4 0.0372 -4.0006 8.9943 4.0037 0.4729 0.0673 -0.9476
4 -9 -4 0.0372 4.0006 -8.9943 -4.0037 -0.4729 -0.0673 0.9476
2 -9 -9 0.0354 2.0009 -8.9941 -9.0031 -0.0840 0.3389 0.9913

_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            8.92031(15)
_cell_oxdiff_length_b            17.5309(3)
_cell_oxdiff_length_c            21.0717(3)
_cell_oxdiff_angle_alpha         90.0170(13)
_cell_oxdiff_angle_beta          101.8433(13)
_cell_oxdiff_angle_gamma         89.9886(14)
_cell_oxdiff_volume              3225.06(9)
_cell_oxdiff_measurement_reflns_used 27497
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_ms11
_database_code_depnum_ccdc_archive 'CCDC 1437768'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon May 05 14:33:13 2014'
;

_audit_block_code                ba_ms11
_audit_block_refno               2031
_audit_block_usercomment         'pf34 plate yellow'


_shelxl_version_number           2014-3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C31 H46 N3 O P Si3 Zr'
_chemical_formula_sum            'C31 H46 N3 O P Si3 Zr'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         683.17
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      110(1)
_chemical_oxdiff_formula         'C31 H46 N3 O1 P1 Si3 Zr1'
_chemical_oxdiff_usercomment     'pf34 plate yellow'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   10.51494(10)
_cell_length_b                   15.79043(15)
_cell_length_c                   20.4802(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.1509(10)
_cell_angle_gamma                90
_cell_volume                     3297.26(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    45793
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.6650
_cell_measurement_theta_min      4.3210
_shelx_estimated_absorpt_T_max   0.664
_shelx_estimated_absorpt_T_min   0.664
_exptl_absorpt_coefficient_mu    4.456
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.1420
_exptl_crystal_size_mid          0.1075
_exptl_crystal_size_min          0.0484
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0933
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            146326
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.839
_diffrn_reflns_theta_min         3.576
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1457638000
_diffrn_orient_matrix_UB_12      0.0078494000
_diffrn_orient_matrix_UB_13      0.0372218000
_diffrn_orient_matrix_UB_21      0.0011823000
_diffrn_orient_matrix_UB_22      -0.0937266000
_diffrn_orient_matrix_UB_23      0.0208916000
_diffrn_orient_matrix_UB_31      0.0398773000
_diffrn_orient_matrix_UB_32      -0.0258310000
_diffrn_orient_matrix_UB_33      -0.0647854000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5815
_reflns_number_total             6306
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-14); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6306
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0323
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0304P)²+3.0918P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0723
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr 0.66836(2) 0.63492(2) 0.30448(2) 0.01283(7) Uani 1 1 d . . . . .
P P 0.90240(5) 0.66498(4) 0.27904(3) 0.01612(13) Uani 1 1 d . . . . .
Si1 Si 0.91301(6) 0.77627(4) 0.40000(3) 0.01842(14) Uani 1 1 d . . . . .
Si2 Si 0.91818(6) 0.48128(4) 0.31281(3) 0.01830(14) Uani 1 1 d . . . . .
Si3 Si 0.72165(6) 0.68689(4) 0.14558(3) 0.01745(14) Uani 1 1 d . . . . .
O O 0.50975(14) 0.53387(10) 0.28454(8) 0.0166(3) Uani 1 1 d . . . . .
N1 N 0.75502(17) 0.74340(12) 0.36454(10) 0.0162(4) Uani 1 1 d . . . . .
N2 N 0.79299(17) 0.52854(12) 0.34179(9) 0.0158(4) Uani 1 1 d . . . . .
N3 N 0.61890(17) 0.66262(12) 0.19841(10) 0.0164(4) Uani 1 1 d . . . . .
C1 C 1.0128(2) 0.71530(16) 0.35096(12) 0.0217(5) Uani 1 1 d . . . . .
H1A H 1.0730 0.7542 0.3353 0.026 Uiso 1 1 calc R . . . .
H1B H 1.0661 0.6717 0.3801 0.026 Uiso 1 1 calc R . . . .
C2 C 0.9835(2) 0.56717(15) 0.26508(13) 0.0207(5) Uani 1 1 d . . . . .
H2A H 1.0797 0.5726 0.2820 0.025 Uiso 1 1 calc R . . . .
H2B H 0.9635 0.5536 0.2164 0.025 Uiso 1 1 calc R . . . .
C3 C 0.8760(2) 0.72988(15) 0.20410(12) 0.0203(5) Uani 1 1 d . . . . .
H3A H 0.9512 0.7254 0.1832 0.024 Uiso 1 1 calc R . . . .
H3B H 0.8643 0.7900 0.2150 0.024 Uiso 1 1 calc R . . . .
C4 C 0.6402(2) 0.76963(14) 0.38358(11) 0.0166(5) Uani 1 1 d . . . . .
C5 C 0.5356(2) 0.71289(15) 0.35890(12) 0.0183(5) Uani 1 1 d . . . . .
C6 C 0.4152(2) 0.73431(16) 0.37176(13) 0.0227(5) Uani 1 1 d . . . . .
H6 H 0.3420 0.6982 0.3554 0.027 Uiso 1 1 calc R . . . .
C7 C 0.3985(2) 0.80674(16) 0.40771(13) 0.0237(5) Uani 1 1 d . . . . .
H7 H 0.3156 0.8188 0.4163 0.028 Uiso 1 1 calc R . . . .
C8 C 0.5031(2) 0.86089(16) 0.43081(13) 0.0241(5) Uani 1 1 d . . . . .
H8 H 0.4918 0.9105 0.4550 0.029 Uiso 1 1 calc R . . . .
C9 C 0.6256(2) 0.84284(16) 0.41871(12) 0.0223(5) Uani 1 1 d . . . . .
H9 H 0.6977 0.8800 0.4343 0.027 Uiso 1 1 calc R . . . .
C10 C 0.9663(3) 0.7442(2) 0.49008(13) 0.0335(7) Uani 1 1 d . . . . .
H10A H 0.9141 0.7746 0.5162 0.050 Uiso 1 1 calc GR . . . .
H10B H 1.0593 0.7579 0.5076 0.050 Uiso 1 1 calc GR . . . .
H10C H 0.9535 0.6830 0.4939 0.050 Uiso 1 1 calc GR . . . .
C11 C 0.9465(3) 0.89215(17) 0.39432(16) 0.0332(7) Uani 1 1 d . . . . .
H11A H 0.9120 0.9114 0.3479 0.050 Uiso 1 1 calc GR . . . .
H11B H 1.0413 0.9021 0.4078 0.050 Uiso 1 1 calc GR . . . .
H11C H 0.9037 0.9235 0.4243 0.050 Uiso 1 1 calc GR . . . .
C12 C 0.7471(2) 0.48930(15) 0.39400(11) 0.0169(5) Uani 1 1 d . . . . .
C13 C 0.7120(2) 0.54001(16) 0.44276(12) 0.0194(5) Uani 1 1 d . . . . .
H13 H 0.7240 0.5996 0.4419 0.023 Uiso 1 1 calc R . . . .
C14 C 0.6598(2) 0.50425(17) 0.49257(13) 0.0251(6) Uani 1 1 d . . . . .
H14 H 0.6341 0.5398 0.5245 0.030 Uiso 1 1 calc R . . . .
C15 C 0.6449(2) 0.41740(17) 0.49613(13) 0.0272(6) Uani 1 1 d . . . . .
H15 H 0.6097 0.3933 0.5304 0.033 Uiso 1 1 calc R . . . .
C16 C 0.6818(2) 0.36609(16) 0.44906(13) 0.0254(6) Uani 1 1 d . . . . .
H16 H 0.6734 0.3064 0.4516 0.031 Uiso 1 1 calc R . . . .
C17 C 0.7309(2) 0.40120(16) 0.39835(12) 0.0210(5) Uani 1 1 d . . . . .
H17 H 0.7542 0.3652 0.3659 0.025 Uiso 1 1 calc R . . . .
C18 C 1.0474(2) 0.4421(2) 0.38532(14) 0.0327(7) Uani 1 1 d . . . . .
H18A H 1.0830 0.4897 0.4149 0.049 Uiso 1 1 calc GR . . . .
H18B H 1.1179 0.4157 0.3688 0.049 Uiso 1 1 calc GR . . . .
H18C H 1.0096 0.4003 0.4105 0.049 Uiso 1 1 calc GR . . . .
C19 C 0.8637(3) 0.39397(17) 0.25020(14) 0.0280(6) Uani 1 1 d . . . . .
H19A H 0.8302 0.3466 0.2720 0.042 Uiso 1 1 calc GR . . . .
H19B H 0.9382 0.3748 0.2332 0.042 Uiso 1 1 calc GR . . . .
H19C H 0.7942 0.4149 0.2126 0.042 Uiso 1 1 calc GR . . . .
C20 C 0.4825(2) 0.65182(15) 0.16603(12) 0.0186(5) Uani 1 1 d . . . . .
C21 C 0.3861(2) 0.69124(16) 0.19146(13) 0.0235(5) Uani 1 1 d . . . . .
H21 H 0.4110 0.7292 0.2284 0.028 Uiso 1 1 calc R . . . .
C22 C 0.2535(2) 0.67549(17) 0.16327(15) 0.0317(7) Uani 1 1 d . . . . .
H22 H 0.1893 0.7012 0.1824 0.038 Uiso 1 1 calc R . . . .
C23 C 0.2142(3) 0.62322(17) 0.10815(15) 0.0347(7) Uani 1 1 d . . . . .
H23 H 0.1238 0.6123 0.0895 0.042 Uiso 1 1 calc R . . . .
C24 C 0.3084(3) 0.58688(18) 0.08040(15) 0.0337(7) Uani 1 1 d . . . . .
H24 H 0.2824 0.5527 0.0412 0.040 Uiso 1 1 calc R . . . .
C25 C 0.4409(2) 0.60000(17) 0.10940(13) 0.0269(6) Uani 1 1 d . . . . .
H25 H 0.5044 0.5733 0.0904 0.032 Uiso 1 1 calc R . . . .
C26 C 0.6503(2) 0.76909(16) 0.08188(13) 0.0233(5) Uani 1 1 d . . . . .
H26A H 0.5722 0.7463 0.0505 0.035 Uiso 1 1 calc GR . . . .
H26B H 0.7153 0.7853 0.0570 0.035 Uiso 1 1 calc GR . . . .
H26C H 0.6261 0.8189 0.1047 0.035 Uiso 1 1 calc GR . . . .
C27 C 0.7668(2) 0.59220(17) 0.10003(13) 0.0258(6) Uani 1 1 d . . . . .
H27A H 0.7717 0.5418 0.1285 0.039 Uiso 1 1 calc GR . . . .
H27B H 0.8521 0.6019 0.0900 0.039 Uiso 1 1 calc GR . . . .
H27C H 0.7000 0.5836 0.0579 0.039 Uiso 1 1 calc GR . . . .
C28 C 0.3945(2) 0.52977(17) 0.31195(14) 0.0270(6) Uani 1 1 d . . . . .
H28A H 0.3449 0.5836 0.3042 0.032 Uiso 1 1 calc R . . . .
H28B H 0.4198 0.5181 0.3609 0.032 Uiso 1 1 calc R . . . .
C29 C 0.3141(2) 0.45823(17) 0.27443(16) 0.0325(6) Uani 1 1 d . . . . .
H29A H 0.2562 0.4783 0.2316 0.039 Uiso 1 1 calc R . . . .
H29B H 0.2599 0.4314 0.3020 0.039 Uiso 1 1 calc R . . . .
C30 C 0.4164(3) 0.39755(17) 0.26174(14) 0.0294(6) Uani 1 1 d . . . . .
H30A H 0.4540 0.3629 0.3021 0.035 Uiso 1 1 calc R . . . .
H30B H 0.3794 0.3596 0.2233 0.035 Uiso 1 1 calc R . . . .
C31 C 0.5175(2) 0.45656(15) 0.24587(13) 0.0207(5) Uani 1 1 d . . . . .
H31A H 0.6062 0.4313 0.2597 0.025 Uiso 1 1 calc R . . . .
H31B H 0.4975 0.4690 0.1970 0.025 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr P 2.6796(6) . ?
Zr O 2.2718(15) . ?
Zr N1 2.1747(19) . ?
Zr N2 2.1525(18) . ?
Zr N3 2.1515(19) . ?
Zr C4 2.733(2) . ?
Zr C5 2.338(2) . ?
P C1 1.820(2) . ?
P C2 1.820(2) . ?
P C3 1.810(2) . ?
Si1 N1 1.7224(18) . ?
Si1 C1 1.885(3) . ?
Si1 C10 1.863(3) . ?
Si1 C11 1.872(3) . ?
Si2 N2 1.739(2) . ?
Si2 C2 1.896(3) . ?
Si2 C18 1.857(3) . ?
Si2 C19 1.875(3) . ?
Si3 N3 1.748(2) . ?
Si3 C3 1.892(2) . ?
Si3 C26 1.863(2) . ?
Si3 C27 1.884(3) . ?
O C28 1.457(3) . ?
O C31 1.468(3) . ?
N1 C4 1.418(3) . ?
N2 C12 1.419(3) . ?
N3 C20 1.436(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.413(3) . ?
C4 C9 1.390(3) . ?
C5 C6 1.396(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.394(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.382(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.400(4) . ?
C9 H9 0.9500 . ?
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 C13 1.398(3) . ?
C12 C17 1.407(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.391(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.384(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.386(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.384(4) . ?
C17 H17 0.9500 . ?
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 C21 1.394(4) . ?
C20 C25 1.399(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.394(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.378(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.381(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.390(4) . ?
C25 H25 0.9500 . ?
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 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.504(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.509(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.508(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P Zr C4 102.42(5) . . ?
O Zr P 139.31(4) . . ?
O Zr C4 118.16(6) . . ?
O Zr C5 87.59(7) . . ?
N1 Zr P 72.10(5) . . ?
N1 Zr O 147.42(7) . . ?
N1 Zr C4 31.02(7) . . ?
N1 Zr C5 62.11(7) . . ?
N2 Zr P 72.48(5) . . ?
N2 Zr O 82.66(6) . . ?
N2 Zr N1 106.22(7) . . ?
N2 Zr C4 122.80(7) . . ?
N2 Zr C5 128.64(8) . . ?
N3 Zr P 76.96(5) . . ?
N3 Zr O 88.60(6) . . ?
N3 Zr N1 112.05(7) . . ?
N3 Zr N2 119.54(7) . . ?
N3 Zr C4 113.94(7) . . ?
N3 Zr C5 110.43(8) . . ?
C5 Zr P 133.09(6) . . ?
C5 Zr C4 31.12(7) . . ?
C1 P Zr 110.77(8) . . ?
C1 P C2 105.48(11) . . ?
C2 P Zr 111.59(8) . . ?
C3 P Zr 107.90(8) . . ?
C3 P C1 111.99(11) . . ?
C3 P C2 109.15(12) . . ?
N1 Si1 C1 103.10(10) . . ?
N1 Si1 C10 111.17(11) . . ?
N1 Si1 C11 116.41(11) . . ?
C10 Si1 C1 108.47(12) . . ?
C10 Si1 C11 108.18(14) . . ?
C11 Si1 C1 109.17(12) . . ?
N2 Si2 C2 105.60(10) . . ?
N2 Si2 C18 109.69(11) . . ?
N2 Si2 C19 114.77(11) . . ?
C18 Si2 C2 111.35(12) . . ?
C18 Si2 C19 110.10(13) . . ?
C19 Si2 C2 105.19(12) . . ?
N3 Si3 C3 104.52(10) . . ?
N3 Si3 C26 112.48(10) . . ?
N3 Si3 C27 113.65(11) . . ?
C26 Si3 C3 109.25(11) . . ?
C26 Si3 C27 108.26(12) . . ?
C27 Si3 C3 108.52(11) . . ?
C28 O Zr 127.26(13) . . ?
C28 O C31 109.40(17) . . ?
C31 O Zr 123.08(13) . . ?
Si1 N1 Zr 134.70(11) . . ?
C4 N1 Zr 96.80(13) . . ?
C4 N1 Si1 126.45(16) . . ?
Si2 N2 Zr 131.27(11) . . ?
C12 N2 Zr 108.56(14) . . ?
C12 N2 Si2 119.70(15) . . ?
Si3 N3 Zr 129.50(10) . . ?
C20 N3 Zr 114.19(15) . . ?
C20 N3 Si3 116.04(15) . . ?
P C1 Si1 109.02(11) . . ?
P C1 H1A 109.9 . . ?
P C1 H1B 109.9 . . ?
Si1 C1 H1A 109.9 . . ?
Si1 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
P C2 Si2 106.46(12) . . ?
P C2 H2A 110.4 . . ?
P C2 H2B 110.4 . . ?
Si2 C2 H2A 110.4 . . ?
Si2 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
P C3 Si3 105.32(12) . . ?
P C3 H3A 110.7 . . ?
P C3 H3B 110.7 . . ?
Si3 C3 H3A 110.7 . . ?
Si3 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
N1 C4 Zr 52.19(11) . . ?
C5 C4 Zr 58.82(13) . . ?
C5 C4 N1 110.9(2) . . ?
C9 C4 Zr 174.73(18) . . ?
C9 C4 N1 126.5(2) . . ?
C9 C4 C5 122.5(2) . . ?
C4 C5 Zr 90.06(15) . . ?
C6 C5 Zr 153.12(18) . . ?
C6 C5 C4 116.2(2) . . ?
C5 C6 H6 118.8 . . ?
C7 C6 C5 122.4(2) . . ?
C7 C6 H6 118.8 . . ?
C6 C7 H7 120.1 . . ?
C8 C7 C6 119.7(2) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.2(2) . . ?
C9 C8 H8 119.9 . . ?
C4 C9 C8 118.9(2) . . ?
C4 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 N2 119.1(2) . . ?
C13 C12 C17 117.7(2) . . ?
C17 C12 N2 123.2(2) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 C12 120.8(2) . . ?
C14 C13 H13 119.6 . . ?
C13 C14 H14 119.6 . . ?
C15 C14 C13 120.7(3) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 120.4 . . ?
C14 C15 C16 119.2(2) . . ?
C16 C15 H15 120.4 . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.5(2) . . ?
C17 C16 H16 119.8 . . ?
C12 C17 H17 119.5 . . ?
C16 C17 C12 121.1(2) . . ?
C16 C17 H17 119.5 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 N3 120.7(2) . . ?
C21 C20 C25 117.5(2) . . ?
C25 C20 N3 121.8(2) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 C20 120.7(2) . . ?
C22 C21 H21 119.7 . . ?
C21 C22 H22 119.5 . . ?
C23 C22 C21 121.0(3) . . ?
C23 C22 H22 119.5 . . ?
C22 C23 H23 120.5 . . ?
C22 C23 C24 119.0(2) . . ?
C24 C23 H23 120.5 . . ?
C23 C24 H24 119.8 . . ?
C23 C24 C25 120.4(3) . . ?
C25 C24 H24 119.8 . . ?
C20 C25 H25 119.4 . . ?
C24 C25 C20 121.3(3) . . ?
C24 C25 H25 119.4 . . ?
Si3 C26 H26A 109.5 . . ?
Si3 C26 H26B 109.5 . . ?
Si3 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si3 C27 H27A 109.5 . . ?
Si3 C27 H27B 109.5 . . ?
Si3 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O C28 H28A 110.8 . . ?
O C28 H28B 110.8 . . ?
O C28 C29 104.6(2) . . ?
H28A C28 H28B 108.9 . . ?
C29 C28 H28A 110.8 . . ?
C29 C28 H28B 110.8 . . ?
C28 C29 H29A 111.1 . . ?
C28 C29 H29B 111.1 . . ?
C28 C29 C30 103.3(2) . . ?
H29A C29 H29B 109.1 . . ?
C30 C29 H29A 111.1 . . ?
C30 C29 H29B 111.1 . . ?
C29 C30 H30A 111.3 . . ?
C29 C30 H30B 111.3 . . ?
H30A C30 H30B 109.2 . . ?
C31 C30 C29 102.4(2) . . ?
C31 C30 H30A 111.3 . . ?
C31 C30 H30B 111.3 . . ?
O C31 C30 105.21(19) . . ?
O C31 H31A 110.7 . . ?
O C31 H31B 110.7 . . ?
C30 C31 H31A 110.7 . . ?
C30 C31 H31B 110.7 . . ?
H31A C31 H31B 108.8 . . ?

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
Zr P C1 Si1 -27.19(14) . . . . ?
Zr P C2 Si2 -26.67(13) . . . . ?
Zr P C3 Si3 -39.54(13) . . . . ?
Zr O C28 C29 171.79(15) . . . . ?
Zr O C31 C30 164.05(15) . . . . ?
Zr N1 C4 C5 3.3(2) . . . . ?
Zr N1 C4 C9 -173.6(2) . . . . ?
Zr N2 C12 C13 -44.4(2) . . . . ?
Zr N2 C12 C17 133.65(19) . . . . ?
Zr N3 C20 C21 52.6(3) . . . . ?
Zr N3 C20 C25 -125.6(2) . . . . ?
Zr C4 C5 C6 -174.0(2) . . . . ?
Zr C5 C6 C7 -167.6(3) . . . . ?
Si1 N1 C4 Zr -165.7(2) . . . . ?
Si1 N1 C4 C5 -162.38(17) . . . . ?
Si1 N1 C4 C9 20.7(3) . . . . ?
Si2 N2 C12 C13 142.53(17) . . . . ?
Si2 N2 C12 C17 -39.4(3) . . . . ?
Si3 N3 C20 C21 -132.8(2) . . . . ?
Si3 N3 C20 C25 49.0(3) . . . . ?
O C28 C29 C30 32.8(3) . . . . ?
N1 Si1 C1 P 10.47(15) . . . . ?
N1 C4 C5 Zr -3.02(18) . . . . ?
N1 C4 C5 C6 -177.1(2) . . . . ?
N1 C4 C9 C8 177.2(2) . . . . ?
N2 Si2 C2 P 7.10(14) . . . . ?
N2 C12 C13 C14 176.4(2) . . . . ?
N2 C12 C17 C16 -177.9(2) . . . . ?
N3 Si3 C3 P 39.03(14) . . . . ?
N3 C20 C21 C22 -174.9(2) . . . . ?
N3 C20 C25 C24 176.9(2) . . . . ?
C1 P C2 Si2 93.68(13) . . . . ?
C1 P C3 Si3 -161.69(11) . . . . ?
C1 Si1 N1 Zr 19.58(18) . . . . ?
C1 Si1 N1 C4 179.32(19) . . . . ?
C2 P C1 Si1 -148.08(12) . . . . ?
C2 P C3 Si3 81.89(13) . . . . ?
C2 Si2 N2 Zr 25.61(16) . . . . ?
C2 Si2 N2 C12 -163.14(16) . . . . ?
C3 P C1 Si1 93.31(14) . . . . ?
C3 P C2 Si2 -145.83(11) . . . . ?
C3 Si3 N3 Zr -23.63(16) . . . . ?
C3 Si3 N3 C20 162.71(17) . . . . ?
C4 C5 C6 C7 -0.9(4) . . . . ?
C5 C4 C9 C8 0.7(4) . . . . ?
C5 C6 C7 C8 1.2(4) . . . . ?
C6 C7 C8 C9 -0.5(4) . . . . ?
C7 C8 C9 C4 -0.4(4) . . . . ?
C9 C4 C5 Zr 174.0(2) . . . . ?
C9 C4 C5 C6 0.0(4) . . . . ?
C10 Si1 N1 Zr -96.46(18) . . . . ?
C10 Si1 N1 C4 63.3(2) . . . . ?
C10 Si1 C1 P 128.43(14) . . . . ?
C11 Si1 N1 Zr 139.06(16) . . . . ?
C11 Si1 N1 C4 -61.2(2) . . . . ?
C11 Si1 C1 P -113.90(14) . . . . ?
C12 C13 C14 C15 1.9(4) . . . . ?
C13 C12 C17 C16 0.2(3) . . . . ?
C13 C14 C15 C16 -0.4(4) . . . . ?
C14 C15 C16 C17 -1.1(4) . . . . ?
C15 C16 C17 C12 1.3(4) . . . . ?
C17 C12 C13 C14 -1.7(3) . . . . ?
C18 Si2 N2 Zr 145.70(14) . . . . ?
C18 Si2 N2 C12 -43.0(2) . . . . ?
C18 Si2 C2 P -111.90(14) . . . . ?
C19 Si2 N2 Zr -89.76(16) . . . . ?
C19 Si2 N2 C12 81.50(19) . . . . ?
C19 Si2 C2 P 128.86(13) . . . . ?
C20 C21 C22 C23 -2.5(4) . . . . ?
C21 C20 C25 C24 -1.3(4) . . . . ?
C21 C22 C23 C24 -0.6(4) . . . . ?
C22 C23 C24 C25 2.7(4) . . . . ?
C23 C24 C25 C20 -1.7(4) . . . . ?
C25 C20 C21 C22 3.4(4) . . . . ?
C26 Si3 N3 Zr -142.03(13) . . . . ?
C26 Si3 N3 C20 44.3(2) . . . . ?
C26 Si3 C3 P 159.61(12) . . . . ?
C27 Si3 N3 Zr 94.51(15) . . . . ?
C27 Si3 N3 C20 -79.16(18) . . . . ?
C27 Si3 C3 P -82.55(14) . . . . ?
C28 O C31 C30 -10.5(3) . . . . ?
C28 C29 C30 C31 -38.8(3) . . . . ?
C29 C30 C31 O 30.4(3) . . . . ?
C31 O C28 C29 -14.0(3) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 -10 3 0.0888 -0.9942 -10.0006 2.9931 -0.1120 0.9987 0.0248
3 -2 -13 0.0512 2.9957 -1.9969 -13.0040 -0.0630 -0.0810 1.0135
-5 -1 -7 0.0242 -5.0040 -1.0047 -6.9811 -0.9971 -0.0576 0.2787
5 1 7 0.0242 5.0040 1.0047 6.9811 0.9971 0.0576 -0.2787
5 -3 -10 0.0621 4.9980 -2.9950 -10.0129 0.3323 0.0774 0.9254
-5 3 10 0.0621 -4.9980 2.9950 10.0129 -0.3323 -0.0774 -0.9254
4 2 -12 0.0486 3.9945 2.0038 -12.0044 0.1512 -0.4339 0.8852
-4 -4 12 0.0499 -3.9936 -4.0038 12.0027 -0.1668 0.6213 -0.8334
-3 4 12 0.0446 -2.9971 3.9969 12.0063 0.0414 -0.1273 -1.0006
3 7 -9 0.0696 2.9933 7.0027 -8.9987 0.1563 -0.8408 0.5215
1 -10 -4 0.0794 1.0031 -9.9986 -4.0094 -0.0815 0.8546 0.5580
-2 9 7 0.0409 -2.0015 8.9977 7.0101 0.0398 -0.6992 -0.7664
_cell_oxdiff_length_a            10.51309(19)
_cell_oxdiff_length_b            15.7946(3)
_cell_oxdiff_length_c            20.4786(4)
_cell_oxdiff_angle_alpha         90.0557(17)
_cell_oxdiff_angle_beta          104.1530(17)
_cell_oxdiff_angle_gamma         89.9987(16)
_cell_oxdiff_volume              3297.26(11)
_cell_oxdiff_measurement_reflns_used 45793
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -23.00   28.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   45.0000  104.0000 51

#__ type_ start__ end____ width___ exp.time_
  2 omega  -69.00   23.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -45.0000  -46.0000 92

#__ type_ start__ end____ width___ exp.time_
  3 omega   54.00   79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   45.0000  104.0000 25

#__ type_ start__ end____ width___ exp.time_
  4 omega   30.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -45.0000  -46.0000 25

#__ type_ start__ end____ width___ exp.time_
  5 omega   37.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -46.0000 46

#__ type_ start__ end____ width___ exp.time_
  6 omega  107.00  132.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  104.0000 25

#__ type_ start__ end____ width___ exp.time_
  7 omega  -43.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000 -180.0000 92

#__ type_ start__ end____ width___ exp.time_
  8 omega  -71.00  -45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
  9 omega  -64.00    1.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 65

#__ type_ start__ end____ width___ exp.time_
 10 omega  -33.00   24.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   30.0000 57

#__ type_ start__ end____ width___ exp.time_
 11 omega    8.00   34.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   69.0000  128.0153 26

#__ type_ start__ end____ width___ exp.time_
 12 omega  -11.00   48.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   78.0000  -29.1734 59

#__ type_ start__ end____ width___ exp.time_
 13 omega   -7.00   19.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   79.0000 -121.0816 26

#__ type_ start__ end____ width___ exp.time_
 14 omega    3.00   30.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   78.0000  -87.9553 27

#__ type_ start__ end____ width___ exp.time_
 15 omega    4.00   37.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   80.0000 -164.4721 33

#__ type_ start__ end____ width___ exp.time_
 16 omega    3.00   34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   80.0000  102.8164 31

#__ type_ start__ end____ width___ exp.time_
 17 omega   13.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   77.0000  -28.3984 26

#__ type_ start__ end____ width___ exp.time_
 18 omega   17.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   76.0000  -55.8477 26

#__ type_ start__ end____ width___ exp.time_
 19 omega   14.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -21.6910 25

#__ type_ start__ end____ width___ exp.time_
 20 omega   14.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   90.7822 25

#__ type_ start__ end____ width___ exp.time_
 21 omega   17.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -152.5700 26

#__ type_ start__ end____ width___ exp.time_
 22 omega   18.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -62.8959 25

#__ type_ start__ end____ width___ exp.time_
 23 omega   19.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -130.5766 25

#__ type_ start__ end____ width___ exp.time_
 24 omega   21.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000  136.2841 27

#__ type_ start__ end____ width___ exp.time_
 25 omega   18.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000    2.0191 25

#__ type_ start__ end____ width___ exp.time_
 26 omega   18.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -146.9455 25

#__ type_ start__ end____ width___ exp.time_
 27 omega   19.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  174.1325 26

#__ type_ start__ end____ width___ exp.time_
 28 omega   19.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   36.3242 26

#__ type_ start__ end____ width___ exp.time_
 29 omega   24.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   99.1177 25

#__ type_ start__ end____ width___ exp.time_
 30 omega   25.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000 -105.3498 26

#__ type_ start__ end____ width___ exp.time_
 31 omega   26.00   52.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -70.4795 26

#__ type_ start__ end____ width___ exp.time_
 32 omega   25.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
 33 omega   31.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 34 omega   12.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000   60.0000 72

#__ type_ start__ end____ width___ exp.time_
 35 omega   25.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 36 omega   24.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 37 omega   24.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    9.6462 26

#__ type_ start__ end____ width___ exp.time_
 38 omega   79.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 30

#__ type_ start__ end____ width___ exp.time_
 39 omega   28.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -18.3284 27

#__ type_ start__ end____ width___ exp.time_
 40 omega   29.00   56.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  103.6400 27

#__ type_ start__ end____ width___ exp.time_
 41 omega   29.00   56.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   74.8268 27

#__ type_ start__ end____ width___ exp.time_
 42 omega  -13.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -79.0000    4.7805 101

#__ type_ start__ end____ width___ exp.time_
 43 omega   31.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000 -103.3673 26

#__ type_ start__ end____ width___ exp.time_
 44 omega   29.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -51.9153 26

#__ type_ start__ end____ width___ exp.time_
 45 omega   29.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -146.5075 34

#__ type_ start__ end____ width___ exp.time_
 46 omega   29.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000 -173.9755 58

#__ type_ start__ end____ width___ exp.time_
 47 omega   29.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   13.6737 26

#__ type_ start__ end____ width___ exp.time_
 48 omega   28.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   42.6015 29

#__ type_ start__ end____ width___ exp.time_
 49 omega  106.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000  123.1364 25

#__ type_ start__ end____ width___ exp.time_
 50 omega   -9.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -79.0000 -171.7088 102

#__ type_ start__ end____ width___ exp.time_
 51 omega   33.00   58.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  130.7482 25

#__ type_ start__ end____ width___ exp.time_
 52 omega   87.00  113.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -38.3724 26

#__ type_ start__ end____ width___ exp.time_
 53 omega   32.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -38.3724 37

#__ type_ start__ end____ width___ exp.time_
 54 omega   38.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  176.4097 30

#__ type_ start__ end____ width___ exp.time_
 55 omega   39.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000   25.7939 34

#__ type_ start__ end____ width___ exp.time_
 56 omega   39.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000 -105.7417 53

#__ type_ start__ end____ width___ exp.time_
 57 omega   38.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000  -58.5168 43

#__ type_ start__ end____ width___ exp.time_
 58 omega   40.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000   56.6276 26

#__ type_ start__ end____ width___ exp.time_
 59 omega   42.00  104.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000   67.5394 62

#__ type_ start__ end____ width___ exp.time_
 60 omega   42.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  103.3359 26

#__ type_ start__ end____ width___ exp.time_
 61 omega   42.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000   -7.8851 43

#__ type_ start__ end____ width___ exp.time_
 62 omega   48.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000 -132.5671 50

#__ type_ start__ end____ width___ exp.time_
 63 omega   45.00   70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000 -107.3383 25

#__ type_ start__ end____ width___ exp.time_
 64 omega   40.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000 -157.1243 26

#__ type_ start__ end____ width___ exp.time_
 65 omega   40.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000   45.1351 26

#__ type_ start__ end____ width___ exp.time_
 66 omega   69.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -79.0000  -60.3505 26

#__ type_ start__ end____ width___ exp.time_
 67 omega   54.00   80.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   55.0000 -142.8335 26

#__ type_ start__ end____ width___ exp.time_
 68 omega   46.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000 -102.1681 44

#__ type_ start__ end____ width___ exp.time_
 69 omega   45.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000  144.8589 32

#__ type_ start__ end____ width___ exp.time_
 70 omega   46.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000  -27.6863 27

#__ type_ start__ end____ width___ exp.time_
 71 omega   52.00  113.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   71.0000  110.4039 61

#__ type_ start__ end____ width___ exp.time_
 72 omega   59.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   60.0000  179.9027 33

#__ type_ start__ end____ width___ exp.time_
 73 omega   49.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000 -106.7858 26

#__ type_ start__ end____ width___ exp.time_
 74 omega   54.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   45.8960 49

#__ type_ start__ end____ width___ exp.time_
 75 omega   49.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   76.0000 -155.3264 26

#__ type_ start__ end____ width___ exp.time_
 76 omega   58.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   51.0000  108.2986 88

#__ type_ start__ end____ width___ exp.time_
 77 omega   60.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000 -124.5874 26

#__ type_ start__ end____ width___ exp.time_
 78 omega   61.00  104.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000  -82.5663 43

#__ type_ start__ end____ width___ exp.time_
 79 omega   49.00  123.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  -53.9518 74

#__ type_ start__ end____ width___ exp.time_
 80 omega   57.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   77.0000  -60.3435 26

#__ type_ start__ end____ width___ exp.time_
 81 omega   54.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000  111.0299 27

#__ type_ start__ end____ width___ exp.time_
 82 omega   55.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000 -151.1602 32

#__ type_ start__ end____ width___ exp.time_
 83 omega   54.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000    9.7748 31

#__ type_ start__ end____ width___ exp.time_
 84 omega   62.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   57.0000  151.5371 28

#__ type_ start__ end____ width___ exp.time_
 85 omega   54.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000  -23.6796 35

#__ type_ start__ end____ width___ exp.time_
 86 omega   61.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   63.0000  162.0219 26

#__ type_ start__ end____ width___ exp.time_
 87 omega   57.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   76.0000 -142.6389 33

#__ type_ start__ end____ width___ exp.time_
 88 omega   61.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   38.0000 -139.9877 26

#__ type_ start__ end____ width___ exp.time_
 89 omega   66.00  131.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   56.0000 -146.6562 65

#__ type_ start__ end____ width___ exp.time_
 90 omega   58.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   74.0000  -11.3622 26

#__ type_ start__ end____ width___ exp.time_
 91 omega   60.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   70.0000   87.2571 30

#__ type_ start__ end____ width___ exp.time_
 92 omega   70.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   61.0000   27.9832 33

#__ type_ start__ end____ width___ exp.time_
 93 omega   75.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   59.0000 -111.4885 26

#__ type_ start__ end____ width___ exp.time_
 94 omega   62.00  159.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   74.0000   46.0303 97

#__ type_ start__ end____ width___ exp.time_
 95 omega   67.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   65.0000  113.0799 30

#__ type_ start__ end____ width___ exp.time_
 96 omega   72.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   61.0000   13.0451 26

#__ type_ start__ end____ width___ exp.time_
 97 omega   68.00  138.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   66.0000 -102.1048 70

#__ type_ start__ end____ width___ exp.time_
 98 omega   74.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   54.0000  147.3546 25

#__ type_ start__ end____ width___ exp.time_
 99 omega   65.00  125.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   75.0000   27.7766 60

#__ type_ start__ end____ width___ exp.time_
100 omega   71.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   73.0000  -14.5369 26

#__ type_ start__ end____ width___ exp.time_
101 omega   66.00  133.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   74.0000  -61.1501 67

#__ type_ start__ end____ width___ exp.time_
102 omega   71.00  125.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   68.0000 -136.2851 54

#__ type_ start__ end____ width___ exp.time_
103 omega   76.00  102.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   64.0000  -13.7634 26

#__ type_ start__ end____ width___ exp.time_
104 omega   77.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   68.0000  143.7009 34

#__ type_ start__ end____ width___ exp.time_
105 omega   78.00  110.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   67.0000   47.0128 32

#__ type_ start__ end____ width___ exp.time_
106 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   72.0000  165.9104 26

#__ type_ start__ end____ width___ exp.time_
107 omega   72.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   77.0000  -95.4903 35

#__ type_ start__ end____ width___ exp.time_
108 omega   79.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0000   71.0000  174.9911 28

#__ type_ start__ end____ width___ exp.time_
109 omega   85.00  162.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 77

#__ type_ start__ end____ width___ exp.time_
110 omega  116.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 60

#__ type_ start__ end____ width___ exp.time_
111 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
112 omega  148.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
113 omega   87.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
114 omega   79.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 99

#__ type_ start__ end____ width___ exp.time_
115 omega   87.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 25

#__ type_ start__ end____ width___ exp.time_
116 omega   49.00  140.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -55.1860 91

#__ type_ start__ end____ width___ exp.time_
117 omega   85.00  142.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 57

#__ type_ start__ end____ width___ exp.time_
118 omega   85.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 90

#__ type_ start__ end____ width___ exp.time_
119 omega   74.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -126.0378 31

#__ type_ start__ end____ width___ exp.time_
120 omega   44.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -126.0378 26

#__ type_ start__ end____ width___ exp.time_
121 omega   85.00  140.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 55

#__ type_ start__ end____ width___ exp.time_
122 omega   88.00  120.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 32

#__ type_ start__ end____ width___ exp.time_
123 omega   85.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 89

#__ type_ start__ end____ width___ exp.time_
124 omega  112.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 66

#__ type_ start__ end____ width___ exp.time_
125 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
126 omega   79.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
127 omega   78.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 100

#__ type_ start__ end____ width___ exp.time_
128 omega   80.00  167.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 87

#__ type_ start__ end____ width___ exp.time_
129 omega   69.00  133.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   36.9520 64

#__ type_ start__ end____ width___ exp.time_
130 omega  131.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 46

#__ type_ start__ end____ width___ exp.time_
131 omega  117.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 57

#__ type_ start__ end____ width___ exp.time_
132 omega   37.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   89.1744 64

#__ type_ start__ end____ width___ exp.time_
133 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
134 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
135 omega   85.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
136 omega   79.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   -4.5384 26

#__ type_ start__ end____ width___ exp.time_
137 omega   87.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 90

#__ type_ start__ end____ width___ exp.time_
138 omega   81.00  173.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   72.0000   18.2055 92

#__ type_ start__ end____ width___ exp.time_
139 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
140 omega   69.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -175.7374 42

#__ type_ start__ end____ width___ exp.time_
141 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
142 omega   78.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 98

#__ type_ start__ end____ width___ exp.time_
143 omega   37.00  128.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  128.3665 91

#__ type_ start__ end____ width___ exp.time_
144 omega  -21.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 90

#__ type_ start__ end____ width___ exp.time_
145 omega  -21.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   30.0000 90

#__ type_ start__ end____ width___ exp.time_
146 omega  -44.00   73.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000 -120.0000 117

#__ type_ start__ end____ width___ exp.time_
147 omega  -72.00   26.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000 -180.0000 98

#__ type_ start__ end____ width___ exp.time_
148 omega  -70.00   30.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -60.0000 100

#__ type_ start__ end____ width___ exp.time_
149 omega   -7.00   86.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   69.0000  -32.5876 93

#__ type_ start__ end____ width___ exp.time_
150 omega   -8.00   87.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   70.0000   71.7442 95

#__ type_ start__ end____ width___ exp.time_
151 omega   -7.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   76.0000    2.0208 99

#__ type_ start__ end____ width___ exp.time_
152 omega   -3.00   96.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   76.0000   81.6941 99

#__ type_ start__ end____ width___ exp.time_
153 omega   -4.00   96.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000 -163.5961 100

#__ type_ start__ end____ width___ exp.time_
154 omega    7.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   78.0000 -146.5211 42

#__ type_ start__ end____ width___ exp.time_
155 omega    7.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  169.9867 40

#__ type_ start__ end____ width___ exp.time_
156 omega    6.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -74.3617 40

#__ type_ start__ end____ width___ exp.time_
157 omega   14.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -21.6910 32

#__ type_ start__ end____ width___ exp.time_
158 omega   14.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   90.7822 32

#__ type_ start__ end____ width___ exp.time_
159 omega   19.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  174.1325 28

#__ type_ start__ end____ width___ exp.time_
160 omega   18.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -146.9455 28

#__ type_ start__ end____ width___ exp.time_
161 omega   18.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000    2.0191 28

#__ type_ start__ end____ width___ exp.time_
162 omega   18.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -62.8959 28

#__ type_ start__ end____ width___ exp.time_
163 omega   18.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   36.3242 28

#__ type_ start__ end____ width___ exp.time_
164 omega  -15.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -90.0000 90

#__ type_ start__ end____ width___ exp.time_
165 omega   23.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -97.2918 26

#__ type_ start__ end____ width___ exp.time_
166 omega  -16.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  120.0000 100

#__ type_ start__ end____ width___ exp.time_
167 omega   23.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   99.1177 26

#__ type_ start__ end____ width___ exp.time_
168 omega   28.00  128.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -18.3284 100

#__ type_ start__ end____ width___ exp.time_
169 omega   28.00  128.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   42.6015 100

#__ type_ start__ end____ width___ exp.time_
170 omega  -13.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -79.0000    4.7805 102

#__ type_ start__ end____ width___ exp.time_
171 omega   34.00   59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  176.4097 25

#__ type_ start__ end____ width___ exp.time_
172 omega   34.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000  123.1364 97

#__ type_ start__ end____ width___ exp.time_
173 omega   43.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000  125.2574 91

#__ type_ start__ end____ width___ exp.time_
174 omega   38.00  135.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000  -58.5168 97

#__ type_ start__ end____ width___ exp.time_
175 omega   39.00  135.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000   25.7939 96

#__ type_ start__ end____ width___ exp.time_
176 omega   40.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000   45.1351 100

#__ type_ start__ end____ width___ exp.time_
177 omega   41.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000   67.5394 99

#__ type_ start__ end____ width___ exp.time_
178 omega   42.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000 -107.3383 97

#__ type_ start__ end____ width___ exp.time_
179 omega   -1.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -79.0000  -60.3505 102

#__ type_ start__ end____ width___ exp.time_
180 omega   41.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000   -7.8851 99

#__ type_ start__ end____ width___ exp.time_
181 omega   40.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000 -157.1243 100

#__ type_ start__ end____ width___ exp.time_
182 omega   47.00  143.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   71.0000  110.4039 96

#__ type_ start__ end____ width___ exp.time_
183 omega   45.00  144.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000  -27.6863 99

#__ type_ start__ end____ width___ exp.time_
184 omega   45.00  144.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000  144.8589 99

#__ type_ start__ end____ width___ exp.time_
185 omega   57.00  147.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   57.0000  155.0105 90

#__ type_ start__ end____ width___ exp.time_
186 omega   54.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000  -82.5663 92

#__ type_ start__ end____ width___ exp.time_
187 omega   51.00  147.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000   16.1732 96

#__ type_ start__ end____ width___ exp.time_
188 omega   56.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   62.0000 -141.5224 90

#__ type_ start__ end____ width___ exp.time_
189 omega   49.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   76.0000 -155.3264 99

#__ type_ start__ end____ width___ exp.time_
190 omega   52.00  147.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   45.8960 95

#__ type_ start__ end____ width___ exp.time_
191 omega   57.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   60.0000  179.9027 89

#__ type_ start__ end____ width___ exp.time_
192 omega   56.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   51.0000  108.2986 92

#__ type_ start__ end____ width___ exp.time_
193 omega   55.00  149.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   46.0000  153.7301 94

#__ type_ start__ end____ width___ exp.time_
194 omega   56.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   63.0000  -70.7009 90

#__ type_ start__ end____ width___ exp.time_
195 omega   49.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000 -106.7858 99

#__ type_ start__ end____ width___ exp.time_
196 omega   49.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  -53.9518 99

#__ type_ start__ end____ width___ exp.time_
197 omega    7.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000 -124.5874 102

;
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration .
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_jb17
_database_code_depnum_ccdc_archive 'CCDC 1437769'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;
_audit_creation_date             2015-06-30

_audit_block_code                ba_jb17
_audit_block_refno               2467
_audit_block_usercomment         jb256


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H47 N3 P2 Si3 Ti'
_chemical_formula_sum            'C30 H47 N3 P2 Si3 Ti'
_chemical_properties_physical    air-sensitive
_chemical_formula_weight         643.81
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            red
_diffrn_ambient_temperature      100(1)
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14

_chemical_absolute_configuration .

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

_cell_length_a                   11.600(5)
_cell_length_b                   17.549(7)
_cell_length_c                   17.579(7)
_cell_angle_alpha                90
_cell_angle_beta                 109.041(13)
_cell_angle_gamma                90
_cell_volume                     3383(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7483
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.51
_cell_measurement_theta_min      2.71
_shelx_estimated_absorpt_T_max   0.851
_shelx_estimated_absorpt_T_min   0.851
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.7098

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.350
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            86850
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.539
_diffrn_reflns_theta_min         1.688
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10028
_reflns_number_total             11765
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'

_computing_cell_refinement       
;
SAINT (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        
'SAINT V8.34A (Bruker AXS, 1997-2013),SADABS-2014_5 (Sheldrick and Bruker AXS, 1997-2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         11765
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0295
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0369P)²+1.8719P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0811
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group with stretchable bonds:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti Ti 0.22625(2) 0.24806(2) 0.35171(2) 0.00918(4) Uani 1 1 d . . . . .
P1 P 0.26546(2) 0.20713(2) 0.22763(2) 0.01266(5) Uani 1 1 d . . . . .
P2 P 0.14969(3) 0.10655(2) 0.40530(2) 0.01605(6) Uani 1 1 d . . . . .
Si1 Si 0.33350(3) 0.37687(2) 0.27259(2) 0.01157(6) Uani 1 1 d . . . . .
Si2 Si 0.00097(3) 0.19306(2) 0.17658(2) 0.01445(6) Uani 1 1 d . . . . .
Si3 Si 0.47236(3) 0.13768(2) 0.35169(2) 0.01369(6) Uani 1 1 d . . . . .
N1 N 0.26552(8) 0.35685(5) 0.34568(5) 0.01062(15) Uani 1 1 d . . . . .
N2 N 0.06121(8) 0.24686(5) 0.26422(5) 0.01187(15) Uani 1 1 d . . . . .
N3 N 0.39904(8) 0.20108(5) 0.39776(5) 0.01203(15) Uani 1 1 d . . . . .
C1 C 0.27331(10) 0.30324(6) 0.18965(6) 0.01506(19) Uani 1 1 d . . . . .
H1A H 0.1909(15) 0.3180(9) 0.1599(10) 0.018 Uiso 1 1 d R . . . .
H1B H 0.3202(15) 0.3039(9) 0.1553(10) 0.018 Uiso 1 1 d R . . . .
C2 C 0.14170(11) 0.15622(7) 0.15678(7) 0.0178(2) Uani 1 1 d . . . . .
H2A H 0.1509(15) 0.1041(10) 0.1696(10) 0.021 Uiso 1 1 d R . . . .
H2B H 0.1372(15) 0.1635(9) 0.1018(10) 0.021 Uiso 1 1 d R . . . .
C3 C 0.41095(11) 0.16176(7) 0.24145(7) 0.0187(2) Uani 1 1 d . . . . .
H3A H 0.4610(15) 0.1947(10) 0.2271(10) 0.022 Uiso 1 1 d R . . . .
H3B H 0.4021(15) 0.1189(10) 0.2078(10) 0.022 Uiso 1 1 d R . . . .
C4 C 0.50340(10) 0.36957(7) 0.31091(7) 0.0171(2) Uani 1 1 d . . . . .
H4A H 0.5360(4) 0.4126(5) 0.3419(6) 0.026 Uiso 1 1 calc GR . . . .
H4B H 0.5329(3) 0.3667(6) 0.2674(4) 0.026 Uiso 1 1 calc GR . . . .
H4C H 0.5264(3) 0.3258(5) 0.3426(6) 0.026 Uiso 1 1 calc GR . . . .
C5 C 0.28851(11) 0.47296(7) 0.22700(7) 0.0198(2) Uani 1 1 d . . . . .
H5A H 0.2055(9) 0.4791(3) 0.2143(6) 0.030 Uiso 1 1 calc GR . . . .
H5B H 0.3096(9) 0.4772(2) 0.1810(6) 0.030 Uiso 1 1 calc GR . . . .
H5C H 0.3282(9) 0.5100(4) 0.2632(5) 0.030 Uiso 1 1 calc GR . . . .
C6 C 0.25489(9) 0.41201(6) 0.40117(6) 0.01070(16) Uani 1 1 d . . . . .
C7 C 0.33881(10) 0.47209(6) 0.42772(6) 0.01424(18) Uani 1 1 d . . . . .
H7 H 0.4078(14) 0.4766(9) 0.4067(9) 0.017 Uiso 1 1 d R . . . .
C8 C 0.32699(11) 0.52501(6) 0.48360(7) 0.0179(2) Uani 1 1 d . . . . .
H8 H 0.3820(15) 0.5641(9) 0.4999(10) 0.021 Uiso 1 1 d R . . . .
C9 C 0.23258(12) 0.51956(7) 0.51549(7) 0.0194(2) Uani 1 1 d . . . . .
H9 H 0.2209(15) 0.5549(10) 0.5523(10) 0.023 Uiso 1 1 d R . . . .
C10 C 0.14952(11) 0.46022(6) 0.49070(7) 0.0168(2) Uani 1 1 d . . . . .
H10 H 0.0864(15) 0.4544(9) 0.5115(10) 0.020 Uiso 1 1 d R . . . .
C11 C 0.15968(10) 0.40736(6) 0.43422(6) 0.01361(18) Uani 1 1 d . . . . .
H11 H 0.1015(14) 0.3689(9) 0.4184(9) 0.016 Uiso 1 1 d R . . . .
C12 C -0.08875(12) 0.25181(8) 0.08842(7) 0.0246(2) Uani 1 1 d . . . . .
H12A H -0.1576(10) 0.2728(6) 0.0986(3) 0.037 Uiso 1 1 calc GR . . . .
H12B H -0.1150(9) 0.2207(4) 0.0419(5) 0.037 Uiso 1 1 calc GR . . . .
H12C H -0.0391(6) 0.2917(6) 0.0801(4) 0.037 Uiso 1 1 calc GR . . . .
C13 C -0.09662(11) 0.11305(7) 0.18898(8) 0.0222(2) Uani 1 1 d . . . . .
H13A H -0.0520(6) 0.0823(5) 0.2321(6) 0.033 Uiso 1 1 calc GR . . . .
H13B H -0.1218(9) 0.0840(5) 0.1417(6) 0.033 Uiso 1 1 calc GR . . . .
H13C H -0.1651(9) 0.1326(2) 0.1994(7) 0.033 Uiso 1 1 calc GR . . . .
C14 C -0.02088(9) 0.30326(6) 0.27521(6) 0.01183(17) Uani 1 1 d . . . . .
C15 C -0.02631(10) 0.37632(6) 0.24181(7) 0.01444(18) Uani 1 1 d . . . . .
H15 H 0.0296(14) 0.3882(9) 0.2118(9) 0.017 Uiso 1 1 d R . . . .
C16 C -0.10642(10) 0.43107(6) 0.25204(7) 0.01661(19) Uani 1 1 d . . . . .
H16 H -0.1076(14) 0.4816(9) 0.2296(10) 0.020 Uiso 1 1 d R . . . .
C17 C -0.18287(10) 0.41443(6) 0.29652(7) 0.0169(2) Uani 1 1 d . . . . .
H17 H -0.2364(14) 0.4547(9) 0.3043(10) 0.020 Uiso 1 1 d R . . . .
C18 C -0.17934(10) 0.34232(7) 0.32970(7) 0.01598(19) Uani 1 1 d . . . . .
H18 H -0.2286(15) 0.3302(9) 0.3587(10) 0.019 Uiso 1 1 d R . . . .
C19 C -0.09970(9) 0.28711(6) 0.31895(6) 0.01383(18) Uani 1 1 d . . . . .
H19 H -0.1004(14) 0.2375(9) 0.3411(9) 0.017 Uiso 1 1 d R . . . .
C20 C 0.43745(12) 0.03443(6) 0.36052(8) 0.0219(2) Uani 1 1 d . . . . .
H20A H 0.4754(9) 0.0180(2) 0.4148(6) 0.033 Uiso 1 1 calc GR . . . .
H20B H 0.4680(9) 0.0050(3) 0.3255(6) 0.033 Uiso 1 1 calc GR . . . .
H20C H 0.3512(9) 0.02764(14) 0.3458(7) 0.033 Uiso 1 1 calc GR . . . .
C21 C 0.64165(10) 0.15221(7) 0.38682(8) 0.0209(2) Uani 1 1 d . . . . .
H21A H 0.6586(2) 0.2035(5) 0.3887(6) 0.031 Uiso 1 1 calc GR . . . .
H21B H 0.6742(4) 0.1287(6) 0.3517(5) 0.031 Uiso 1 1 calc GR . . . .
H21C H 0.6753(4) 0.1315(6) 0.4373(6) 0.031 Uiso 1 1 calc GR . . . .
C22 C 0.46613(9) 0.21759(6) 0.47955(6) 0.01229(17) Uani 1 1 d . . . . .
C23 C 0.52647(10) 0.16013(6) 0.53375(7) 0.0176(2) Uani 1 1 d . . . . .
H23 H 0.5222(15) 0.1079(10) 0.5139(10) 0.021 Uiso 1 1 d R . . . .
C24 C 0.59650(11) 0.17664(7) 0.61279(7) 0.0196(2) Uani 1 1 d . . . . .
H24 H 0.6385(15) 0.1366(10) 0.6463(10) 0.023 Uiso 1 1 d R . . . .
C25 C 0.60701(11) 0.25098(7) 0.64101(7) 0.0183(2) Uani 1 1 d . . . . .
H25 H 0.6546(15) 0.2634(9) 0.6948(10) 0.022 Uiso 1 1 d R . . . .
C26 C 0.54644(11) 0.30833(7) 0.58889(7) 0.0184(2) Uani 1 1 d . . . . .
H26 H 0.5541(15) 0.3591(10) 0.6083(10) 0.022 Uiso 1 1 d R . . . .
C27 C 0.47761(10) 0.29225(6) 0.50952(7) 0.01516(19) Uani 1 1 d . . . . .
H27 H 0.4417(14) 0.3307(9) 0.4764(10) 0.018 Uiso 1 1 d R . . . .
C28 C 0.17093(10) 0.20222(6) 0.44651(6) 0.01418(18) Uani 1 1 d . . . . .
H28A H 0.2321(14) 0.2053(9) 0.4963(10) 0.017 Uiso 1 1 d R . . . .
H28B H 0.0974(14) 0.2239(9) 0.4505(9) 0.017 Uiso 1 1 d R . . . .
C29 C -0.00153(12) 0.07850(8) 0.40816(9) 0.0276(3) Uani 1 1 d . . . . .
H29A H -0.0067(4) 0.0890(6) 0.4612(6) 0.041 Uiso 1 1 calc GR . . . .
H29B H -0.0139(5) 0.0244(6) 0.3967(7) 0.041 Uiso 1 1 calc GR . . . .
H29C H -0.0640(7) 0.1073(6) 0.3680(7) 0.041 Uiso 1 1 calc GR . . . .
C30 C 0.24489(13) 0.04643(8) 0.48713(9) 0.0295(3) Uani 1 1 d . . . . .
H30A H 0.3281(10) 0.0638(5) 0.5028(5) 0.044 Uiso 1 1 calc GR . . . .
H30B H 0.2406(9) -0.0056(6) 0.4690(3) 0.044 Uiso 1 1 calc GR . . . .
H30C H 0.2159(8) 0.0495(6) 0.5325(6) 0.044 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti P1 2.4755(9) . ?
Ti P2 2.8963(9) . ?
Ti Si1 3.1179(8) . ?
Ti N1 1.9735(11) . ?
Ti N2 2.0274(11) . ?
Ti N3 2.0721(11) . ?
Ti C28 2.1292(12) . ?
P1 C1 1.8271(13) . ?
P1 C2 1.8010(13) . ?
P1 C3 1.8093(13) . ?
P2 C28 1.8133(13) . ?
P2 C29 1.8384(15) . ?
P2 C30 1.8345(14) . ?
Si1 N1 1.7485(10) . ?
Si1 C1 1.9023(12) . ?
Si1 C4 1.8676(14) . ?
Si1 C5 1.8669(13) . ?
Si2 N2 1.7466(11) . ?
Si2 C2 1.8907(14) . ?
Si2 C12 1.8696(14) . ?
Si2 C13 1.8606(14) . ?
Si3 N3 1.7512(10) . ?
Si3 C3 1.8816(14) . ?
Si3 C20 1.8742(14) . ?
Si3 C21 1.8739(14) . ?
N1 C6 1.4079(13) . ?
N2 C14 1.4296(14) . ?
N3 C22 1.4236(14) . ?
C1 H1A 0.963(16) . ?
C1 H1B 0.935(16) . ?
C2 H2A 0.939(17) . ?
C2 H2B 0.959(17) . ?
C3 H3A 0.912(17) . ?
C3 H3B 0.943(17) . ?
C4 H4A 0.936(9) . ?
C4 H4B 0.936(9) . ?
C4 H4C 0.936(9) . ?
C5 H5A 0.921(10) . ?
C5 H5B 0.921(10) . ?
C5 H5C 0.921(10) . ?
C6 C7 1.4074(15) . ?
C6 C11 1.4081(15) . ?
C7 H7 0.988(16) . ?
C7 C8 1.3908(16) . ?
C8 H8 0.916(16) . ?
C8 C9 1.3869(18) . ?
C9 H9 0.938(17) . ?
C9 C10 1.3889(18) . ?
C10 H10 0.924(16) . ?
C10 C11 1.3916(15) . ?
C11 H11 0.931(16) . ?
C12 H12A 0.948(11) . ?
C12 H12B 0.948(11) . ?
C12 H12C 0.948(11) . ?
C13 H13A 0.937(10) . ?
C13 H13B 0.937(10) . ?
C13 H13C 0.937(10) . ?
C14 C15 1.4028(15) . ?
C14 C19 1.4023(15) . ?
C15 H15 0.982(16) . ?
C15 C16 1.3886(16) . ?
C16 H16 0.969(16) . ?
C16 C17 1.3913(17) . ?
C17 H17 0.980(16) . ?
C17 C18 1.3885(17) . ?
C18 H18 0.907(16) . ?
C18 C19 1.3934(15) . ?
C19 H19 0.955(16) . ?
C20 H20A 0.956(10) . ?
C20 H20B 0.956(10) . ?
C20 H20C 0.956(10) . ?
C21 H21A 0.919(10) . ?
C21 H21B 0.919(10) . ?
C21 H21C 0.919(10) . ?
C22 C23 1.4067(15) . ?
C22 C27 1.4022(15) . ?
C23 H23 0.977(17) . ?
C23 C24 1.3921(17) . ?
C24 H24 0.944(17) . ?
C24 C25 1.3868(18) . ?
C25 H25 0.951(17) . ?
C25 C26 1.3879(17) . ?
C26 H26 0.948(17) . ?
C26 C27 1.3917(16) . ?
C27 H27 0.900(16) . ?
C28 H28A 0.931(16) . ?
C28 H28B 0.956(16) . ?
C29 H29A 0.972(11) . ?
C29 H29B 0.972(11) . ?
C29 H29C 0.972(11) . ?
C30 H30A 0.963(11) . ?
C30 H30B 0.963(11) . ?
C30 H30C 0.963(11) . ?

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
P1 Ti P2 101.64(2) . . ?
P1 Ti Si1 66.58(2) . . ?
P2 Ti Si1 167.427(11) . . ?
N1 Ti P1 96.97(3) . . ?
N1 Ti P2 161.36(3) . . ?
N1 Ti Si1 30.91(3) . . ?
N1 Ti N2 98.43(4) . . ?
N1 Ti N3 101.25(4) . . ?
N1 Ti C28 122.77(4) . . ?
N2 Ti P1 74.22(4) . . ?
N2 Ti P2 85.64(3) . . ?
N2 Ti Si1 94.85(4) . . ?
N2 Ti N3 147.77(4) . . ?
N2 Ti C28 97.97(5) . . ?
N3 Ti P1 78.25(3) . . ?
N3 Ti P2 83.80(3) . . ?
N3 Ti Si1 89.24(4) . . ?
N3 Ti C28 92.53(5) . . ?
C28 Ti P1 140.26(4) . . ?
C28 Ti P2 38.64(3) . . ?
C28 Ti Si1 152.75(3) . . ?
C1 P1 Ti 95.71(4) . . ?
C2 P1 Ti 114.78(5) . . ?
C2 P1 C1 109.19(6) . . ?
C2 P1 C3 111.88(6) . . ?
C3 P1 Ti 116.16(4) . . ?
C3 P1 C1 107.44(6) . . ?
C28 P2 Ti 47.15(4) . . ?
C28 P2 C29 104.09(6) . . ?
C28 P2 C30 104.51(7) . . ?
C29 P2 Ti 129.43(5) . . ?
C30 P2 Ti 125.32(5) . . ?
C30 P2 C29 99.21(7) . . ?
N1 Si1 Ti 35.44(3) . . ?
N1 Si1 C1 106.61(5) . . ?
N1 Si1 C4 113.40(5) . . ?
N1 Si1 C5 111.53(5) . . ?
C1 Si1 Ti 75.48(4) . . ?
C4 Si1 Ti 108.49(4) . . ?
C4 Si1 C1 108.06(5) . . ?
C5 Si1 Ti 138.59(4) . . ?
C5 Si1 C1 107.65(6) . . ?
C5 Si1 C4 109.34(6) . . ?
N2 Si2 C2 103.08(5) . . ?
N2 Si2 C12 112.79(6) . . ?
N2 Si2 C13 112.84(6) . . ?
C12 Si2 C2 108.45(6) . . ?
C13 Si2 C2 111.00(6) . . ?
C13 Si2 C12 108.53(7) . . ?
N3 Si3 C3 104.83(5) . . ?
N3 Si3 C20 115.17(6) . . ?
N3 Si3 C21 112.09(5) . . ?
C20 Si3 C3 106.44(6) . . ?
C21 Si3 C3 108.23(6) . . ?
C21 Si3 C20 109.62(6) . . ?
Si1 N1 Ti 113.66(4) . . ?
C6 N1 Ti 123.64(7) . . ?
C6 N1 Si1 122.23(7) . . ?
Si2 N2 Ti 132.98(5) . . ?
C14 N2 Ti 113.33(7) . . ?
C14 N2 Si2 113.64(7) . . ?
Si3 N3 Ti 128.75(5) . . ?
C22 N3 Ti 117.00(7) . . ?
C22 N3 Si3 114.11(7) . . ?
P1 C1 Si1 113.37(6) . . ?
P1 C1 H1A 106.7(10) . . ?
P1 C1 H1B 110.8(10) . . ?
Si1 C1 H1A 106.5(9) . . ?
Si1 C1 H1B 110.0(10) . . ?
H1A C1 H1B 109.2(13) . . ?
P1 C2 Si2 104.14(6) . . ?
P1 C2 H2A 108.4(10) . . ?
P1 C2 H2B 113.6(10) . . ?
Si2 C2 H2A 109.1(10) . . ?
Si2 C2 H2B 111.9(10) . . ?
H2A C2 H2B 109.6(14) . . ?
P1 C3 Si3 105.08(6) . . ?
P1 C3 H3A 109.5(10) . . ?
P1 C3 H3B 111.2(10) . . ?
Si3 C3 H3A 111.5(10) . . ?
Si3 C3 H3B 113.2(10) . . ?
H3A C3 H3B 106.3(14) . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 C11 120.25(9) . . ?
C7 C6 N1 122.51(9) . . ?
C7 C6 C11 117.22(9) . . ?
C6 C7 H7 119.6(9) . . ?
C8 C7 C6 121.17(10) . . ?
C8 C7 H7 119.2(9) . . ?
C7 C8 H8 120.0(10) . . ?
C9 C8 C7 120.81(11) . . ?
C9 C8 H8 119.2(10) . . ?
C8 C9 H9 123.0(10) . . ?
C8 C9 C10 118.91(10) . . ?
C10 C9 H9 118.1(10) . . ?
C9 C10 H10 121.1(10) . . ?
C9 C10 C11 120.81(11) . . ?
C11 C10 H10 118.1(10) . . ?
C6 C11 H11 120.6(10) . . ?
C10 C11 C6 121.07(10) . . ?
C10 C11 H11 118.3(10) . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N2 121.14(9) . . ?
C19 C14 N2 121.08(9) . . ?
C19 C14 C15 117.77(9) . . ?
C14 C15 H15 118.1(9) . . ?
C16 C15 C14 121.25(10) . . ?
C16 C15 H15 120.6(9) . . ?
C15 C16 H16 120.1(10) . . ?
C15 C16 C17 120.25(10) . . ?
C17 C16 H16 119.6(10) . . ?
C16 C17 H17 118.5(9) . . ?
C18 C17 C16 119.38(10) . . ?
C18 C17 H17 122.1(9) . . ?
C17 C18 H18 120.8(10) . . ?
C17 C18 C19 120.45(10) . . ?
C19 C18 H18 118.7(10) . . ?
C14 C19 H19 120.0(10) . . ?
C18 C19 C14 120.90(10) . . ?
C18 C19 H19 119.0(10) . . ?
Si3 C20 H20A 109.5 . . ?
Si3 C20 H20B 109.5 . . ?
Si3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N3 121.70(10) . . ?
C27 C22 N3 121.54(9) . . ?
C27 C22 C23 116.74(10) . . ?
C22 C23 H23 118.3(10) . . ?
C24 C23 C22 121.75(11) . . ?
C24 C23 H23 119.8(10) . . ?
C23 C24 H24 118.8(10) . . ?
C25 C24 C23 120.48(10) . . ?
C25 C24 H24 120.6(10) . . ?
C24 C25 H25 121.7(10) . . ?
C24 C25 C26 118.66(11) . . ?
C26 C25 H25 119.7(10) . . ?
C25 C26 H26 118.4(10) . . ?
C25 C26 C27 121.07(11) . . ?
C27 C26 H26 120.5(10) . . ?
C22 C27 H27 119.4(10) . . ?
C26 C27 C22 121.28(10) . . ?
C26 C27 H27 119.3(10) . . ?
Ti C28 H28A 112.4(10) . . ?
Ti C28 H28B 114.2(9) . . ?
P2 C28 Ti 94.21(5) . . ?
P2 C28 H28A 113.1(10) . . ?
P2 C28 H28B 112.9(10) . . ?
H28A C28 H28B 109.4(13) . . ?
P2 C29 H29A 109.5 . . ?
P2 C29 H29B 109.5 . . ?
P2 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
P2 C30 H30A 109.5 . . ?
P2 C30 H30B 109.5 . . ?
P2 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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
Ti P1 C1 Si1 30.77(6) . . . . ?
Ti P1 C2 Si2 27.39(7) . . . . ?
Ti P1 C3 Si3 14.15(7) . . . . ?
Ti Si1 N1 C6 172.36(11) . . . . ?
Ti N1 C6 C7 142.37(8) . . . . ?
Ti N1 C6 C11 -35.82(12) . . . . ?
Ti N2 C14 C15 90.40(11) . . . . ?
Ti N2 C14 C19 -90.35(10) . . . . ?
Ti N3 C22 C23 132.82(9) . . . . ?
Ti N3 C22 C27 -48.69(12) . . . . ?
Si1 N1 C6 C7 -29.23(13) . . . . ?
Si1 N1 C6 C11 152.59(8) . . . . ?
Si2 N2 C14 C15 -87.59(11) . . . . ?
Si2 N2 C14 C19 91.65(11) . . . . ?
Si3 N3 C22 C23 -43.20(12) . . . . ?
Si3 N3 C22 C27 135.28(9) . . . . ?
N1 C6 C7 C8 -178.93(10) . . . . ?
N1 C6 C11 C10 178.33(10) . . . . ?
N2 Si2 C2 P1 -9.10(7) . . . . ?
N2 C14 C15 C16 179.65(10) . . . . ?
N2 C14 C19 C18 179.83(10) . . . . ?
N3 Si3 C3 P1 -23.42(7) . . . . ?
N3 C22 C23 C24 177.14(11) . . . . ?
N3 C22 C27 C26 -177.99(10) . . . . ?
C1 P1 C2 Si2 -78.68(7) . . . . ?
C1 P1 C3 Si3 119.84(6) . . . . ?
C1 Si1 N1 Ti 29.49(6) . . . . ?
C1 Si1 N1 C6 -158.15(8) . . . . ?
C2 P1 C1 Si1 149.50(6) . . . . ?
C2 P1 C3 Si3 -120.32(7) . . . . ?
C2 Si2 N2 Ti -20.04(8) . . . . ?
C2 Si2 N2 C14 157.44(8) . . . . ?
C3 P1 C1 Si1 -88.96(7) . . . . ?
C3 P1 C2 Si2 162.52(6) . . . . ?
C3 Si3 N3 Ti 31.22(8) . . . . ?
C3 Si3 N3 C22 -153.33(8) . . . . ?
C4 Si1 N1 Ti -89.31(6) . . . . ?
C4 Si1 N1 C6 83.06(9) . . . . ?
C5 Si1 N1 Ti 146.74(5) . . . . ?
C5 Si1 N1 C6 -40.90(10) . . . . ?
C6 C7 C8 C9 0.69(17) . . . . ?
C7 C6 C11 C10 0.05(15) . . . . ?
C7 C8 C9 C10 -0.01(17) . . . . ?
C8 C9 C10 C11 -0.64(17) . . . . ?
C9 C10 C11 C6 0.62(16) . . . . ?
C11 C6 C7 C8 -0.69(15) . . . . ?
C12 Si2 N2 Ti -136.79(7) . . . . ?
C12 Si2 N2 C14 40.69(9) . . . . ?
C12 Si2 C2 P1 110.68(7) . . . . ?
C13 Si2 N2 Ti 99.77(8) . . . . ?
C13 Si2 N2 C14 -82.75(9) . . . . ?
C13 Si2 C2 P1 -130.17(6) . . . . ?
C14 C15 C16 C17 0.47(17) . . . . ?
C15 C14 C19 C18 -0.90(15) . . . . ?
C15 C16 C17 C18 -0.81(17) . . . . ?
C16 C17 C18 C19 0.29(17) . . . . ?
C17 C18 C19 C14 0.57(17) . . . . ?
C19 C14 C15 C16 0.38(16) . . . . ?
C20 Si3 N3 Ti -85.39(8) . . . . ?
C20 Si3 N3 C22 90.07(9) . . . . ?
C20 Si3 C3 P1 99.05(7) . . . . ?
C21 Si3 N3 Ti 148.39(6) . . . . ?
C21 Si3 N3 C22 -36.16(9) . . . . ?
C21 Si3 C3 P1 -143.20(6) . . . . ?
C22 C23 C24 C25 1.17(18) . . . . ?
C23 C22 C27 C26 0.57(16) . . . . ?
C23 C24 C25 C26 -0.03(18) . . . . ?
C24 C25 C26 C27 -0.82(18) . . . . ?
C25 C26 C27 C22 0.54(18) . . . . ?
C27 C22 C23 C24 -1.42(17) . . . . ?
C29 P2 C28 Ti -131.32(6) . . . . ?
C30 P2 C28 Ti 125.06(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            CCD-PXL-KAF2
####################################################################### 
# 
# 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_ba_jb18
_database_code_depnum_ccdc_archive 'CCDC 1442399'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;
_audit_creation_date             2015-12-14

_audit_block_code                ba_jb18
_audit_block_refno               2502
_audit_block_usercomment         jb270


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C31 H50 Hf N3 P Si4'
_chemical_formula_sum            'C31 H50 Hf N3 P Si4'
_chemical_properties_physical    moisture-sensitive
_chemical_formula_weight         786.56
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      100(1)
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'
Hf Hf -0.5830 6.1852 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2yn'
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                   13.187(6)
_cell_length_b                   17.538(7)
_cell_length_c                   15.841(6)
_cell_angle_alpha                90
_cell_angle_beta                 106.018(7)
_cell_angle_gamma                90
_cell_volume                     3521(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8130
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.35
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   0.584
_shelx_estimated_absorpt_T_min   0.493
_exptl_absorpt_coefficient_mu    3.169
_exptl_absorpt_correction_T_max  0.5655
_exptl_absorpt_correction_T_min  0.4844

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            89103
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.430
_diffrn_reflns_theta_min         2.129
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9442
_reflns_number_total             12131
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'

_computing_cell_refinement       
;
SAINT (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        
'SAINT V8.34A (Bruker AXS, 1997-2013),SADABS-2014_5 (Sheldrick and Bruker AXS, 1997-2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         1.766
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         12131
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0252
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0212P)²+7.1206P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0624
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf Hf 0.25072(2) 0.74886(2) 0.45580(2) 0.00853(3) Uani 1 1 d . . . . .
P P 0.40163(4) 0.73482(3) 0.60350(4) 0.01270(11) Uani 1 1 d . . . . .
Si1 Si 0.52500(5) 0.71212(4) 0.47743(4) 0.01277(11) Uani 1 1 d . . . . .
Si2 Si 0.22468(5) 0.65954(4) 0.65014(4) 0.01543(12) Uani 1 1 d . . . . .
Si3 Si 0.31215(5) 0.90134(4) 0.57773(4) 0.01415(12) Uani 1 1 d . . . . .
Si4 Si 0.16359(5) 0.58455(4) 0.31853(4) 0.01466(12) Uani 1 1 d . . . . .
N1 N 0.39479(15) 0.73340(11) 0.42273(12) 0.0131(3) Uani 1 1 d . . . . .
N2 N 0.17664(14) 0.70387(11) 0.54839(12) 0.0131(3) Uani 1 1 d . . . . .
N3 N 0.23745(14) 0.86739(11) 0.47511(12) 0.0130(3) Uani 1 1 d . . . . .
C1 C 0.52071(17) 0.68956(14) 0.59306(15) 0.0159(4) Uani 1 1 d . . . . .
H1A H 0.5180 0.6338 0.6018 0.019 Uiso 1 1 calc R . . . .
H1B H 0.5835 0.7104 0.6366 0.019 Uiso 1 1 calc R . . . .
C2 C 0.35988(17) 0.70265(15) 0.69768(15) 0.0162(4) Uani 1 1 d . . . . .
H2A H 0.3563 0.7460 0.7368 0.019 Uiso 1 1 calc R . . . .
H2B H 0.4096 0.6641 0.7317 0.019 Uiso 1 1 calc R . . . .
C3 C 0.42938(17) 0.83591(13) 0.61663(15) 0.0151(4) Uani 1 1 d . . . . .
H3A H 0.4815 0.8490 0.5844 0.018 Uiso 1 1 calc R . . . .
H3B H 0.4627 0.8462 0.6796 0.018 Uiso 1 1 calc R . . . .
C4 C 0.5816(2) 0.62796(15) 0.43377(17) 0.0212(5) Uani 1 1 d . . . . .
H4A H 0.5367 0.5833 0.4330 0.032 Uiso 1 1 calc GR . . . .
H4B H 0.6527 0.6176 0.4715 0.032 Uiso 1 1 calc GR . . . .
H4C H 0.5851 0.6389 0.3739 0.032 Uiso 1 1 calc GR . . . .
C5 C 0.61133(18) 0.79557(15) 0.47385(17) 0.0191(5) Uani 1 1 d . . . . .
H5A H 0.6078 0.8074 0.4126 0.029 Uiso 1 1 calc GR . . . .
H5B H 0.6843 0.7834 0.5061 0.029 Uiso 1 1 calc GR . . . .
H5C H 0.5873 0.8398 0.5010 0.029 Uiso 1 1 calc GR . . . .
C6 C 0.37970(16) 0.75562(13) 0.33309(14) 0.0125(4) Uani 1 1 d . . . . .
C7 C 0.35762(18) 0.83131(14) 0.30817(16) 0.0180(4) Uani 1 1 d . . . . .
H7 H 0.3579 0.8689 0.3514 0.022 Uiso 1 1 calc R . . . .
C8 C 0.3350(2) 0.85223(16) 0.21972(17) 0.0239(5) Uani 1 1 d . . . . .
H8 H 0.3172 0.9036 0.2030 0.029 Uiso 1 1 calc R . . . .
C9 C 0.3384(2) 0.79887(18) 0.15675(17) 0.0260(6) Uani 1 1 d . . . . .
H9 H 0.3236 0.8136 0.0969 0.031 Uiso 1 1 calc R . . . .
C10 C 0.3633(2) 0.72381(18) 0.18083(17) 0.0237(5) Uani 1 1 d . . . . .
H10 H 0.3669 0.6871 0.1376 0.028 Uiso 1 1 calc R . . . .
C11 C 0.38306(19) 0.70224(15) 0.26807(16) 0.0186(4) Uani 1 1 d . . . . .
H11 H 0.3991 0.6505 0.2840 0.022 Uiso 1 1 calc R . . . .
C12 C 0.1385(2) 0.67840(19) 0.72309(17) 0.0268(6) Uani 1 1 d . . . . .
H12A H 0.1292 0.7335 0.7278 0.040 Uiso 1 1 calc GR . . . .
H12B H 0.1714 0.6573 0.7815 0.040 Uiso 1 1 calc GR . . . .
H12C H 0.0696 0.6543 0.6984 0.040 Uiso 1 1 calc GR . . . .
C13 C 0.2427(3) 0.55410(16) 0.6450(2) 0.0301(6) Uani 1 1 d . . . . .
H13A H 0.1742 0.5299 0.6193 0.045 Uiso 1 1 calc GR . . . .
H13B H 0.2734 0.5342 0.7044 0.045 Uiso 1 1 calc GR . . . .
H13C H 0.2901 0.5429 0.6086 0.045 Uiso 1 1 calc GR . . . .
C14 C 0.06502(17) 0.70829(14) 0.51159(15) 0.0145(4) Uani 1 1 d . . . . .
C15 C 0.00149(19) 0.64289(15) 0.49571(17) 0.0201(5) Uani 1 1 d . . . . .
H15 H 0.0315 0.5946 0.5155 0.024 Uiso 1 1 calc R . . . .
C16 C -0.1052(2) 0.64807(17) 0.45124(18) 0.0248(5) Uani 1 1 d . . . . .
H16 H -0.1470 0.6031 0.4407 0.030 Uiso 1 1 calc R . . . .
C17 C -0.15109(19) 0.71740(18) 0.42215(17) 0.0239(5) Uani 1 1 d . . . . .
H17 H -0.2234 0.7202 0.3900 0.029 Uiso 1 1 calc R . . . .
C18 C -0.0902(2) 0.78299(17) 0.44047(17) 0.0218(5) Uani 1 1 d . . . . .
H18 H -0.1214 0.8312 0.4224 0.026 Uiso 1 1 calc R . . . .
C19 C 0.01665(18) 0.77837(15) 0.48526(16) 0.0176(4) Uani 1 1 d . . . . .
H19 H 0.0572 0.8238 0.4981 0.021 Uiso 1 1 calc R . . . .
C20 C 0.3679(2) 0.99788(15) 0.5689(2) 0.0266(6) Uani 1 1 d . . . . .
H20A H 0.4058 0.9971 0.5238 0.040 Uiso 1 1 calc GR . . . .
H20B H 0.4167 1.0120 0.6255 0.040 Uiso 1 1 calc GR . . . .
H20C H 0.3105 1.0352 0.5529 0.040 Uiso 1 1 calc GR . . . .
C21 C 0.2388(2) 0.90023(16) 0.66297(16) 0.0215(5) Uani 1 1 d . . . . .
H21A H 0.1859 0.9410 0.6508 0.032 Uiso 1 1 calc GR . . . .
H21B H 0.2883 0.9083 0.7210 0.032 Uiso 1 1 calc GR . . . .
H21C H 0.2036 0.8509 0.6618 0.032 Uiso 1 1 calc GR . . . .
C22 C 0.16321(17) 0.91669(12) 0.42025(14) 0.0122(4) Uani 1 1 d . . . . .
C23 C 0.12045(19) 0.97995(14) 0.45293(16) 0.0181(4) Uani 1 1 d . . . . .
H23 H 0.1402 0.9891 0.5144 0.022 Uiso 1 1 calc R . . . .
C24 C 0.0503(2) 1.02921(14) 0.39779(17) 0.0206(5) Uani 1 1 d . . . . .
H24 H 0.0236 1.0718 0.4220 0.025 Uiso 1 1 calc R . . . .
C25 C 0.01831(19) 1.01723(14) 0.30781(16) 0.0184(5) Uani 1 1 d . . . . .
H25 H -0.0293 1.0514 0.2700 0.022 Uiso 1 1 calc R . . . .
C26 C 0.05747(19) 0.95434(14) 0.27447(16) 0.0174(4) Uani 1 1 d . . . . .
H26 H 0.0352 0.9447 0.2131 0.021 Uiso 1 1 calc R . . . .
C27 C 0.12874(18) 0.90488(13) 0.32888(15) 0.0162(4) Uani 1 1 d . . . . .
H27 H 0.1546 0.8624 0.3040 0.019 Uiso 1 1 calc R . . . .
C28 C 0.14953(17) 0.68901(13) 0.33588(15) 0.0137(4) Uani 1 1 d . . . . .
H28A H 0.0751 0.6980 0.3349 0.016 Uiso 1 1 calc R . . . .
H28B H 0.1608 0.7154 0.2840 0.016 Uiso 1 1 calc R . . . .
C29 C 0.2819(2) 0.54423(15) 0.40175(18) 0.0247(5) Uani 1 1 d . . . . .
H29A H 0.3459 0.5694 0.3958 0.037 Uiso 1 1 calc GR . . . .
H29B H 0.2865 0.4893 0.3918 0.037 Uiso 1 1 calc GR . . . .
H29C H 0.2749 0.5529 0.4610 0.037 Uiso 1 1 calc GR . . . .
C30 C 0.0446(2) 0.53089(15) 0.33064(19) 0.0243(5) Uani 1 1 d . . . . .
H30A H 0.0498 0.5244 0.3931 0.036 Uiso 1 1 calc GR . . . .
H30B H 0.0417 0.4807 0.3028 0.036 Uiso 1 1 calc GR . . . .
H30C H -0.0194 0.5596 0.3023 0.036 Uiso 1 1 calc GR . . . .
C31 C 0.1791(2) 0.56199(15) 0.20649(16) 0.0194(5) Uani 1 1 d . . . . .
H31A H 0.1096 0.5519 0.1658 0.029 Uiso 1 1 calc GR . . . .
H31B H 0.2239 0.5168 0.2102 0.029 Uiso 1 1 calc GR . . . .
H31C H 0.2118 0.6054 0.1852 0.029 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf P 2.6316(9) . ?
Hf N1 2.123(2) . ?
Hf N2 2.126(2) . ?
Hf N3 2.115(2) . ?
Hf C28 2.257(2) . ?
P C1 1.807(2) . ?
P C2 1.817(2) . ?
P C3 1.811(3) . ?
Si1 N1 1.737(2) . ?
Si1 C1 1.890(2) . ?
Si1 C4 1.871(3) . ?
Si1 C5 1.864(3) . ?
Si2 N2 1.744(2) . ?
Si2 C2 1.891(2) . ?
Si2 C12 1.860(3) . ?
Si2 C13 1.869(3) . ?
Si3 N3 1.756(2) . ?
Si3 C3 1.887(2) . ?
Si3 C20 1.866(3) . ?
Si3 C21 1.866(3) . ?
Si4 C28 1.869(2) . ?
Si4 C29 1.881(3) . ?
Si4 C30 1.884(3) . ?
Si4 C31 1.884(3) . ?
N1 C6 1.432(3) . ?
N2 C14 1.428(3) . ?
N3 C22 1.411(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.393(3) . ?
C6 C11 1.402(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.399(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.377(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.385(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.386(3) . ?
C11 H11 0.9500 . ?
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 C15 1.402(3) . ?
C14 C19 1.394(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.391(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.380(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.387(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.394(3) . ?
C19 H19 0.9500 . ?
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 1.406(3) . ?
C22 C27 1.408(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.386(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.386(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.383(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.390(3) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 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
N1 Hf P 72.47(6) . . ?
N1 Hf N2 137.37(7) . . ?
N1 Hf C28 95.42(8) . . ?
N2 Hf P 74.37(6) . . ?
N2 Hf C28 97.50(8) . . ?
N3 Hf P 92.05(5) . . ?
N3 Hf N1 106.06(7) . . ?
N3 Hf N2 101.12(8) . . ?
N3 Hf C28 121.70(8) . . ?
C28 Hf P 146.24(6) . . ?
C1 P Hf 115.01(8) . . ?
C1 P C2 113.99(11) . . ?
C1 P C3 106.71(11) . . ?
C2 P Hf 115.66(8) . . ?
C3 P Hf 95.15(7) . . ?
C3 P C2 107.89(11) . . ?
N1 Si1 C1 103.80(10) . . ?
N1 Si1 C4 115.18(11) . . ?
N1 Si1 C5 110.12(11) . . ?
C4 Si1 C1 108.35(11) . . ?
C5 Si1 C1 112.06(11) . . ?
C5 Si1 C4 107.39(12) . . ?
N2 Si2 C2 104.60(10) . . ?
N2 Si2 C12 111.51(12) . . ?
N2 Si2 C13 114.76(12) . . ?
C12 Si2 C2 110.59(12) . . ?
C12 Si2 C13 108.06(14) . . ?
C13 Si2 C2 107.19(13) . . ?
N3 Si3 C3 107.21(10) . . ?
N3 Si3 C20 111.75(12) . . ?
N3 Si3 C21 113.32(11) . . ?
C20 Si3 C3 105.78(12) . . ?
C21 Si3 C3 107.40(11) . . ?
C21 Si3 C20 110.92(13) . . ?
C28 Si4 C29 111.23(11) . . ?
C28 Si4 C30 110.82(11) . . ?
C28 Si4 C31 112.66(11) . . ?
C29 Si4 C30 107.09(13) . . ?
C29 Si4 C31 107.27(12) . . ?
C31 Si4 C30 107.50(12) . . ?
Si1 N1 Hf 137.15(11) . . ?
C6 N1 Hf 108.72(13) . . ?
C6 N1 Si1 113.62(14) . . ?
Si2 N2 Hf 133.19(10) . . ?
C14 N2 Hf 108.45(14) . . ?
C14 N2 Si2 118.18(15) . . ?
Si3 N3 Hf 114.80(10) . . ?
C22 N3 Hf 125.73(14) . . ?
C22 N3 Si3 118.61(15) . . ?
P C1 Si1 104.82(11) . . ?
P C1 H1A 110.8 . . ?
P C1 H1B 110.8 . . ?
Si1 C1 H1A 110.8 . . ?
Si1 C1 H1B 110.8 . . ?
H1A C1 H1B 108.9 . . ?
P C2 Si2 105.26(11) . . ?
P C2 H2A 110.7 . . ?
P C2 H2B 110.7 . . ?
Si2 C2 H2A 110.7 . . ?
Si2 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
P C3 Si3 115.89(12) . . ?
P C3 H3A 108.3 . . ?
P C3 H3B 108.3 . . ?
Si3 C3 H3A 108.3 . . ?
Si3 C3 H3B 108.3 . . ?
H3A C3 H3B 107.4 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 120.1(2) . . ?
C7 C6 C11 118.4(2) . . ?
C11 C6 N1 121.5(2) . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.3(2) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.4(3) . . ?
C9 C8 H8 119.8 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 119.9(2) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 119.9(3) . . ?
C11 C10 H10 120.0 . . ?
C6 C11 H11 119.5 . . ?
C10 C11 C6 121.0(2) . . ?
C10 C11 H11 119.5 . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N2 121.8(2) . . ?
C19 C14 N2 120.3(2) . . ?
C19 C14 C15 117.8(2) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.5(2) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 119.5 . . ?
C17 C16 C15 121.1(2) . . ?
C17 C16 H16 119.5 . . ?
C16 C17 H17 120.5 . . ?
C16 C17 C18 119.0(2) . . ?
C18 C17 H17 120.5 . . ?
C17 C18 H18 119.9 . . ?
C17 C18 C19 120.3(3) . . ?
C19 C18 H18 119.9 . . ?
C14 C19 H19 119.4 . . ?
C18 C19 C14 121.2(2) . . ?
C18 C19 H19 119.4 . . ?
Si3 C20 H20A 109.5 . . ?
Si3 C20 H20B 109.5 . . ?
Si3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N3 122.5(2) . . ?
C23 C22 C27 116.5(2) . . ?
C27 C22 N3 121.0(2) . . ?
C22 C23 H23 119.1 . . ?
C24 C23 C22 121.7(2) . . ?
C24 C23 H23 119.1 . . ?
C23 C24 H24 119.5 . . ?
C23 C24 C25 120.9(2) . . ?
C25 C24 H24 119.5 . . ?
C24 C25 H25 120.9 . . ?
C26 C25 C24 118.3(2) . . ?
C26 C25 H25 120.9 . . ?
C25 C26 H26 119.3 . . ?
C25 C26 C27 121.4(2) . . ?
C27 C26 H26 119.3 . . ?
C22 C27 H27 119.4 . . ?
C26 C27 C22 121.1(2) . . ?
C26 C27 H27 119.4 . . ?
Hf C28 H28A 107.0 . . ?
Hf C28 H28B 107.0 . . ?
Si4 C28 Hf 121.34(11) . . ?
Si4 C28 H28A 107.0 . . ?
Si4 C28 H28B 107.0 . . ?
H28A C28 H28B 106.7 . . ?
Si4 C29 H29A 109.5 . . ?
Si4 C29 H29B 109.5 . . ?
Si4 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si4 C30 H30A 109.5 . . ?
Si4 C30 H30B 109.5 . . ?
Si4 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si4 C31 H31A 109.5 . . ?
Si4 C31 H31B 109.5 . . ?
Si4 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 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
Hf P C1 Si1 28.24(14) . . . . ?
Hf P C2 Si2 17.56(14) . . . . ?
Hf P C3 Si3 34.68(12) . . . . ?
Hf N1 C6 C7 65.2(2) . . . . ?
Hf N1 C6 C11 -112.6(2) . . . . ?
Hf N2 C14 C15 118.0(2) . . . . ?
Hf N2 C14 C19 -58.0(2) . . . . ?
Hf N3 C22 C23 146.71(19) . . . . ?
Hf N3 C22 C27 -33.8(3) . . . . ?
Si1 N1 C6 C7 -108.1(2) . . . . ?
Si1 N1 C6 C11 74.1(2) . . . . ?
Si2 N2 C14 C15 -57.7(3) . . . . ?
Si2 N2 C14 C19 126.3(2) . . . . ?
Si3 N3 C22 C23 -22.1(3) . . . . ?
Si3 N3 C22 C27 157.38(18) . . . . ?
N1 Si1 C1 P -21.42(14) . . . . ?
N1 C6 C7 C8 -175.2(2) . . . . ?
N1 C6 C11 C10 176.9(2) . . . . ?
N2 Si2 C2 P -24.61(14) . . . . ?
N2 C14 C15 C16 -173.0(2) . . . . ?
N2 C14 C19 C18 172.9(2) . . . . ?
N3 Si3 C3 P -44.64(15) . . . . ?
N3 C22 C23 C24 177.8(2) . . . . ?
N3 C22 C27 C26 -178.5(2) . . . . ?
C1 P C2 Si2 -119.08(13) . . . . ?
C1 P C3 Si3 152.73(12) . . . . ?
C1 Si1 N1 Hf 7.03(19) . . . . ?
C1 Si1 N1 C6 177.61(16) . . . . ?
C2 P C1 Si1 165.17(11) . . . . ?
C2 P C3 Si3 -84.40(14) . . . . ?
C2 Si2 N2 Hf 30.43(17) . . . . ?
C2 Si2 N2 C14 -155.18(17) . . . . ?
C3 P C1 Si1 -75.85(14) . . . . ?
C3 P C2 Si2 122.61(12) . . . . ?
C3 Si3 N3 Hf 27.74(13) . . . . ?
C3 Si3 N3 C22 -162.24(16) . . . . ?
C4 Si1 N1 Hf 125.31(16) . . . . ?
C4 Si1 N1 C6 -64.12(19) . . . . ?
C4 Si1 C1 P -144.31(12) . . . . ?
C5 Si1 N1 Hf -113.10(16) . . . . ?
C5 Si1 N1 C6 57.48(19) . . . . ?
C5 Si1 C1 P 97.38(14) . . . . ?
C6 C7 C8 C9 -2.6(4) . . . . ?
C7 C6 C11 C10 -1.0(3) . . . . ?
C7 C8 C9 C10 0.6(4) . . . . ?
C8 C9 C10 C11 1.1(4) . . . . ?
C9 C10 C11 C6 -0.9(4) . . . . ?
C11 C6 C7 C8 2.7(3) . . . . ?
C12 Si2 N2 Hf 149.99(15) . . . . ?
C12 Si2 N2 C14 -35.6(2) . . . . ?
C12 Si2 C2 P -144.79(13) . . . . ?
C13 Si2 N2 Hf -86.73(18) . . . . ?
C13 Si2 N2 C14 87.7(2) . . . . ?
C13 Si2 C2 P 97.64(15) . . . . ?
C14 C15 C16 C17 -0.3(4) . . . . ?
C15 C14 C19 C18 -3.3(3) . . . . ?
C15 C16 C17 C18 -2.2(4) . . . . ?
C16 C17 C18 C19 2.0(4) . . . . ?
C17 C18 C19 C14 0.8(4) . . . . ?
C19 C14 C15 C16 3.1(4) . . . . ?
C20 Si3 N3 Hf 143.21(12) . . . . ?
C20 Si3 N3 C22 -46.8(2) . . . . ?
C20 Si3 C3 P -164.02(14) . . . . ?
C21 Si3 N3 Hf -90.58(13) . . . . ?
C21 Si3 N3 C22 79.44(19) . . . . ?
C21 Si3 C3 P 77.46(15) . . . . ?
C22 C23 C24 C25 0.9(4) . . . . ?
C23 C22 C27 C26 1.0(3) . . . . ?
C23 C24 C25 C26 0.7(4) . . . . ?
C24 C25 C26 C27 -1.3(4) . . . . ?
C25 C26 C27 C22 0.5(4) . . . . ?
C27 C22 C23 C24 -1.7(4) . . . . ?
C29 Si4 C28 Hf -8.69(17) . . . . ?
C30 Si4 C28 Hf 110.33(15) . . . . ?
C31 Si4 C28 Hf -129.18(13) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            CCD-PXL-KAF2
####################################################################### 
# 
# 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_ba_jb4
_database_code_depnum_ccdc_archive 'CCDC 1442400'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;
_audit_creation_date             2015-12-14

_audit_block_code                ba_jb4
_audit_block_refno               1546
_audit_block_usercomment         jb053_Ta


_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H48 N4 P Si4 Ta'
_chemical_formula_sum            'C30 H48 N4 P Si4 Ta'
_chemical_properties_physical    moisture-sensitive
_chemical_formula_weight         789.00
_chemical_melting_point          ?
_exptl_crystal_description       blocl
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      100(1)
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_h-m   'P b c a'
_symmetry_int_tables_number      61

_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.2029(17)
_cell_length_b                   19.8978(19)
_cell_length_c                   20.392(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7386.0(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7450
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.05
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   0.785
_shelx_estimated_absorpt_T_min   0.529
_exptl_absorpt_coefficient_mu    3.174
_exptl_absorpt_correction_T_max  0.5655
_exptl_absorpt_correction_T_min  0.4365

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.080
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            180196
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.505
_diffrn_reflns_theta_min         1.816
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10407
_reflns_number_total             12952
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'

_computing_cell_refinement       
;
SAINT (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        
'SAINT V8.18C (Bruker AXS, 1997-2013),SADABS-2014_5 (Sheldrick and Bruker AXS, 1997-2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         1.959
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         12952
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0234
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0144P)²+11.5678P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0509
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta Ta 0.11905(2) 0.18977(2) 0.19728(2) 0.00842(2) Uani 1 1 d . . . . .
P P 0.12219(3) 0.32458(2) 0.17829(2) 0.01090(8) Uani 1 1 d . . . . .
Si1 Si 0.24946(3) 0.27068(3) 0.10429(3) 0.01207(9) Uani 1 1 d . . . . .
Si2 Si 0.12936(3) 0.30565(3) 0.32270(3) 0.01140(9) Uani 1 1 d . . . . .
Si3 Si -0.02182(3) 0.27811(3) 0.13216(3) 0.01402(10) Uani 1 1 d . . . . .
Si4 Si 0.11851(3) 0.01449(3) 0.22338(3) 0.01251(9) Uani 1 1 d . . . . .
N1 N 0.21606(8) 0.20050(8) 0.14755(8) 0.0114(3) Uani 1 1 d . . . . .
N2 N 0.11355(9) 0.22404(8) 0.29222(7) 0.0116(3) Uani 1 1 d . . . . .
N3 N 0.02559(9) 0.20190(8) 0.14289(8) 0.0117(3) Uani 1 1 d . . . . .
N4 N 0.11860(9) 0.10020(8) 0.20964(8) 0.0122(3) Uani 1 1 d . . . . .
C1 C 0.21168(11) 0.34744(10) 0.14662(10) 0.0154(4) Uani 1 1 d . . . . .
H1A H 0.2446 0.3614 0.1828 0.018 Uiso 1 1 calc R . . . .
H1B H 0.2073 0.3852 0.1152 0.018 Uiso 1 1 calc R . . . .
C2 C 0.10516(11) 0.36717(9) 0.25574(10) 0.0144(3) Uani 1 1 d . . . . .
H2A H 0.0529 0.3805 0.2591 0.017 Uiso 1 1 calc R . . . .
H2B H 0.1360 0.4080 0.2592 0.017 Uiso 1 1 calc R . . . .
C3 C 0.05025(10) 0.34550(10) 0.12021(10) 0.0148(3) Uani 1 1 d . . . . .
H3A H 0.0693 0.3449 0.0748 0.018 Uiso 1 1 calc R . . . .
H3B H 0.0297 0.3906 0.1295 0.018 Uiso 1 1 calc R . . . .
C4 C 0.35181(11) 0.27511(11) 0.10594(10) 0.0184(4) Uani 1 1 d . . . . .
H4A H 0.3682 0.3146 0.0813 0.028 Uiso 1 1 calc GR . . . .
H4B H 0.3723 0.2344 0.0860 0.028 Uiso 1 1 calc GR . . . .
H4C H 0.3687 0.2786 0.1515 0.028 Uiso 1 1 calc GR . . . .
C5 C 0.21855(13) 0.26733(12) 0.01762(10) 0.0239(4) Uani 1 1 d . . . . .
H5A H 0.1647 0.2680 0.0161 0.036 Uiso 1 1 calc GR . . . .
H5B H 0.2367 0.2260 -0.0028 0.036 Uiso 1 1 calc GR . . . .
H5C H 0.2379 0.3063 -0.0061 0.036 Uiso 1 1 calc GR . . . .
C6 C 0.25893(10) 0.14171(9) 0.13339(10) 0.0142(3) Uani 1 1 d . . . . .
C7 C 0.24116(13) 0.09928(11) 0.08149(11) 0.0232(4) Uani 1 1 d . . . . .
H7 H 0.1989 0.1082 0.0556 0.028 Uiso 1 1 calc R . . . .
C8 C 0.28518(15) 0.04362(12) 0.06722(13) 0.0315(5) Uani 1 1 d . . . . .
H8 H 0.2724 0.0149 0.0318 0.038 Uiso 1 1 calc R . . . .
C9 C 0.34709(14) 0.02992(12) 0.10412(13) 0.0310(6) Uani 1 1 d . . . . .
H9 H 0.3773 -0.0076 0.0940 0.037 Uiso 1 1 calc R . . . .
C10 C 0.36433(13) 0.07160(12) 0.15588(13) 0.0287(5) Uani 1 1 d . . . . .
H10 H 0.4067 0.0625 0.1816 0.034 Uiso 1 1 calc R . . . .
C11 C 0.32071(12) 0.12662(11) 0.17084(11) 0.0209(4) Uani 1 1 d . . . . .
H11 H 0.3331 0.1544 0.2071 0.025 Uiso 1 1 calc R . . . .
C12 C 0.07183(12) 0.32510(11) 0.39601(10) 0.0203(4) Uani 1 1 d . . . . .
H12A H 0.0200 0.3169 0.3857 0.030 Uiso 1 1 calc GR . . . .
H12B H 0.0785 0.3723 0.4082 0.030 Uiso 1 1 calc GR . . . .
H12C H 0.0868 0.2963 0.4326 0.030 Uiso 1 1 calc GR . . . .
C13 C 0.22831(11) 0.31494(11) 0.34429(11) 0.0203(4) Uani 1 1 d . . . . .
H13A H 0.2422 0.2798 0.3756 0.030 Uiso 1 1 calc GR . . . .
H13B H 0.2365 0.3592 0.3641 0.030 Uiso 1 1 calc GR . . . .
H13C H 0.2582 0.3107 0.3046 0.030 Uiso 1 1 calc GR . . . .
C14 C 0.10919(11) 0.17507(9) 0.34415(9) 0.0146(4) Uani 1 1 d . . . . .
C15 C 0.17094(13) 0.13836(11) 0.36350(10) 0.0205(4) Uani 1 1 d . . . . .
H15 H 0.2166 0.1456 0.3420 0.025 Uiso 1 1 calc R . . . .
C16 C 0.16640(16) 0.09135(12) 0.41378(11) 0.0296(5) Uani 1 1 d . . . . .
H16 H 0.2088 0.0665 0.4261 0.036 Uiso 1 1 calc R . . . .
C17 C 0.10071(18) 0.08052(12) 0.44594(11) 0.0339(6) Uani 1 1 d . . . . .
H17 H 0.0978 0.0484 0.4803 0.041 Uiso 1 1 calc R . . . .
C18 C 0.03890(16) 0.11682(12) 0.42764(11) 0.0303(5) Uani 1 1 d . . . . .
H18 H -0.0063 0.1097 0.4498 0.036 Uiso 1 1 calc R . . . .
C19 C 0.04274(13) 0.16362(11) 0.37691(11) 0.0217(4) Uani 1 1 d . . . . .
H19 H 0.0000 0.1879 0.3645 0.026 Uiso 1 1 calc R . . . .
C20 C -0.08271(13) 0.27638(12) 0.05904(12) 0.0262(5) Uani 1 1 d . . . . .
H20A H -0.0536 0.2657 0.0200 0.039 Uiso 1 1 calc GR . . . .
H20B H -0.1059 0.3205 0.0535 0.039 Uiso 1 1 calc GR . . . .
H20C H -0.1207 0.2421 0.0651 0.039 Uiso 1 1 calc GR . . . .
C21 C -0.07744(11) 0.29464(11) 0.20750(11) 0.0206(4) Uani 1 1 d . . . . .
H21A H -0.1152 0.2598 0.2120 0.031 Uiso 1 1 calc GR . . . .
H21B H -0.1010 0.3388 0.2039 0.031 Uiso 1 1 calc GR . . . .
H21C H -0.0453 0.2940 0.2460 0.031 Uiso 1 1 calc GR . . . .
C22 C -0.01806(10) 0.14471(10) 0.12484(9) 0.0138(3) Uani 1 1 d . . . . .
C23 C -0.06492(11) 0.11441(11) 0.17000(11) 0.0205(4) Uani 1 1 d . . . . .
H23 H -0.0664 0.1306 0.2138 0.025 Uiso 1 1 calc R . . . .
C24 C -0.10961(13) 0.06067(13) 0.15184(15) 0.0319(6) Uani 1 1 d . . . . .
H24 H -0.1413 0.0405 0.1832 0.038 Uiso 1 1 calc R . . . .
C25 C -0.10792(14) 0.03672(13) 0.08817(16) 0.0358(6) Uani 1 1 d . . . . .
H25 H -0.1387 0.0004 0.0755 0.043 Uiso 1 1 calc R . . . .
C26 C -0.06118(15) 0.06585(13) 0.04319(13) 0.0345(6) Uani 1 1 d . . . . .
H26 H -0.0595 0.0491 -0.0004 0.041 Uiso 1 1 calc R . . . .
C27 C -0.01630(13) 0.11956(12) 0.06106(11) 0.0245(5) Uani 1 1 d . . . . .
H27 H 0.0157 0.1391 0.0296 0.029 Uiso 1 1 calc R . . . .
C28 C 0.09672(14) -0.03150(11) 0.14582(11) 0.0251(5) Uani 1 1 d . . . . .
H28A H 0.0917 -0.0796 0.1552 0.038 Uiso 1 1 calc GR . . . .
H28B H 0.1365 -0.0246 0.1141 0.038 Uiso 1 1 calc GR . . . .
H28C H 0.0506 -0.0144 0.1275 0.038 Uiso 1 1 calc GR . . . .
C29 C 0.21008(11) -0.01284(11) 0.25499(11) 0.0203(4) Uani 1 1 d . . . . .
H29A H 0.2213 0.0115 0.2956 0.031 Uiso 1 1 calc GR . . . .
H29B H 0.2479 -0.0031 0.2221 0.031 Uiso 1 1 calc GR . . . .
H29C H 0.2091 -0.0612 0.2638 0.031 Uiso 1 1 calc GR . . . .
C30 C 0.04705(12) -0.00657(11) 0.28576(11) 0.0215(4) Uani 1 1 d . . . . .
H30A H 0.0529 -0.0534 0.2996 0.032 Uiso 1 1 calc GR . . . .
H30B H -0.0019 -0.0004 0.2666 0.032 Uiso 1 1 calc GR . . . .
H30C H 0.0526 0.0230 0.3238 0.032 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ta P 2.7109(5) . ?
Ta N1 2.0473(16) . ?
Ta N2 2.0551(15) . ?
Ta N3 2.0453(16) . ?
Ta N4 1.7999(16) . ?
P C1 1.810(2) . ?
P C2 1.819(2) . ?
P C3 1.8140(19) . ?
Si1 N1 1.7602(16) . ?
Si1 C1 1.884(2) . ?
Si1 C4 1.866(2) . ?
Si1 C5 1.856(2) . ?
Si2 N2 1.7624(16) . ?
Si2 C2 1.886(2) . ?
Si2 C12 1.866(2) . ?
Si2 C13 1.863(2) . ?
Si3 N3 1.7585(16) . ?
Si3 C3 1.892(2) . ?
Si3 C20 1.858(2) . ?
Si3 C21 1.869(2) . ?
Si4 N4 1.7284(17) . ?
Si4 C28 1.870(2) . ?
Si4 C29 1.868(2) . ?
Si4 C30 1.867(2) . ?
N1 C6 1.436(2) . ?
N2 C14 1.441(2) . ?
N3 C22 1.436(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.392(3) . ?
C6 C11 1.392(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.398(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.382(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.379(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.386(3) . ?
C11 H11 0.9500 . ?
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 C15 1.397(3) . ?
C14 C19 1.401(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.390(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.381(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.388(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.394(3) . ?
C19 H19 0.9500 . ?
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 1.392(3) . ?
C22 C27 1.394(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.394(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.383(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.379(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.394(3) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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
N1 Ta P 78.93(4) . . ?
N1 Ta N2 118.29(6) . . ?
N2 Ta P 78.88(4) . . ?
N3 Ta P 79.82(4) . . ?
N3 Ta N1 115.89(6) . . ?
N3 Ta N2 115.54(6) . . ?
N4 Ta P 179.04(5) . . ?
N4 Ta N1 100.17(7) . . ?
N4 Ta N2 101.33(7) . . ?
N4 Ta N3 100.90(7) . . ?
C1 P Ta 108.57(6) . . ?
C1 P C2 110.24(9) . . ?
C1 P C3 111.05(9) . . ?
C2 P Ta 109.47(6) . . ?
C3 P Ta 107.76(7) . . ?
C3 P C2 109.70(9) . . ?
N1 Si1 C1 106.70(8) . . ?
N1 Si1 C4 111.93(9) . . ?
N1 Si1 C5 110.12(10) . . ?
C4 Si1 C1 108.54(9) . . ?
C5 Si1 C1 110.78(10) . . ?
C5 Si1 C4 108.77(10) . . ?
N2 Si2 C2 107.73(8) . . ?
N2 Si2 C12 112.46(9) . . ?
N2 Si2 C13 109.43(9) . . ?
C12 Si2 C2 108.33(9) . . ?
C13 Si2 C2 109.42(9) . . ?
C13 Si2 C12 109.43(10) . . ?
N3 Si3 C3 106.67(8) . . ?
N3 Si3 C20 112.12(10) . . ?
N3 Si3 C21 108.37(9) . . ?
C20 Si3 C3 108.87(10) . . ?
C20 Si3 C21 109.86(11) . . ?
C21 Si3 C3 110.90(9) . . ?
N4 Si4 C28 110.24(9) . . ?
N4 Si4 C29 110.02(9) . . ?
N4 Si4 C30 109.42(9) . . ?
C29 Si4 C28 109.81(11) . . ?
C30 Si4 C28 108.58(11) . . ?
C30 Si4 C29 108.73(10) . . ?
Si1 N1 Ta 128.97(8) . . ?
C6 N1 Ta 118.92(12) . . ?
C6 N1 Si1 110.97(12) . . ?
Si2 N2 Ta 129.06(8) . . ?
C14 N2 Ta 118.07(12) . . ?
C14 N2 Si2 111.88(12) . . ?
Si3 N3 Ta 125.28(8) . . ?
C22 N3 Ta 120.38(12) . . ?
C22 N3 Si3 112.34(12) . . ?
Si4 N4 Ta 178.71(10) . . ?
P C1 Si1 106.75(10) . . ?
P C1 H1A 110.4 . . ?
P C1 H1B 110.4 . . ?
Si1 C1 H1A 110.4 . . ?
Si1 C1 H1B 110.4 . . ?
H1A C1 H1B 108.6 . . ?
P C2 Si2 106.65(9) . . ?
P C2 H2A 110.4 . . ?
P C2 H2B 110.4 . . ?
Si2 C2 H2A 110.4 . . ?
Si2 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
P C3 Si3 104.71(10) . . ?
P C3 H3A 110.8 . . ?
P C3 H3B 110.8 . . ?
Si3 C3 H3A 110.8 . . ?
Si3 C3 H3B 110.8 . . ?
H3A C3 H3B 108.9 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 121.39(18) . . ?
C11 C6 N1 120.30(18) . . ?
C11 C6 C7 118.30(19) . . ?
C6 C7 H7 119.8 . . ?
C6 C7 C8 120.4(2) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.7(2) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 120.5 . . ?
C10 C9 C8 118.9(2) . . ?
C10 C9 H9 120.5 . . ?
C9 C10 H10 119.6 . . ?
C9 C10 C11 120.9(2) . . ?
C11 C10 H10 119.6 . . ?
C6 C11 H11 119.6 . . ?
C10 C11 C6 120.8(2) . . ?
C10 C11 H11 119.6 . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N2 121.10(18) . . ?
C15 C14 C19 118.36(19) . . ?
C19 C14 N2 120.53(18) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.8(2) . . ?
C16 C15 H15 119.6 . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.4(2) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 120.2 . . ?
C16 C17 C18 119.5(2) . . ?
C18 C17 H17 120.2 . . ?
C17 C18 H18 119.8 . . ?
C17 C18 C19 120.4(2) . . ?
C19 C18 H18 119.8 . . ?
C14 C19 H19 119.8 . . ?
C18 C19 C14 120.4(2) . . ?
C18 C19 H19 119.8 . . ?
Si3 C20 H20A 109.5 . . ?
Si3 C20 H20B 109.5 . . ?
Si3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N3 120.84(18) . . ?
C23 C22 C27 118.40(19) . . ?
C27 C22 N3 120.73(18) . . ?
C22 C23 H23 119.5 . . ?
C22 C23 C24 120.9(2) . . ?
C24 C23 H23 119.5 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 120.0(2) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 120.2 . . ?
C26 C25 C24 119.6(2) . . ?
C26 C25 H25 120.2 . . ?
C25 C26 H26 119.7 . . ?
C25 C26 C27 120.7(2) . . ?
C27 C26 H26 119.7 . . ?
C22 C27 H27 119.8 . . ?
C26 C27 C22 120.4(2) . . ?
C26 C27 H27 119.8 . . ?
Si4 C28 H28A 109.5 . . ?
Si4 C28 H28B 109.5 . . ?
Si4 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si4 C29 H29A 109.5 . . ?
Si4 C29 H29B 109.5 . . ?
Si4 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si4 C30 H30A 109.5 . . ?
Si4 C30 H30B 109.5 . . ?
Si4 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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
Ta P C1 Si1 25.30(11) . . . . ?
Ta P C2 Si2 22.21(10) . . . . ?
Ta P C3 Si3 28.19(10) . . . . ?
Ta N1 C6 C7 79.3(2) . . . . ?
Ta N1 C6 C11 -102.12(19) . . . . ?
Ta N2 C14 C15 75.4(2) . . . . ?
Ta N2 C14 C19 -105.13(18) . . . . ?
Ta N3 C22 C23 77.6(2) . . . . ?
Ta N3 C22 C27 -104.54(19) . . . . ?
Si1 N1 C6 C7 -89.6(2) . . . . ?
Si1 N1 C6 C11 89.0(2) . . . . ?
Si2 N2 C14 C15 -94.20(19) . . . . ?
Si2 N2 C14 C19 85.2(2) . . . . ?
Si3 N3 C22 C23 -87.1(2) . . . . ?
Si3 N3 C22 C27 90.8(2) . . . . ?
N1 Si1 C1 P -32.71(12) . . . . ?
N1 C6 C7 C8 177.8(2) . . . . ?
N1 C6 C11 C10 -177.2(2) . . . . ?
N2 Si2 C2 P -29.42(12) . . . . ?
N2 C14 C15 C16 179.79(19) . . . . ?
N2 C14 C19 C18 -179.22(19) . . . . ?
N3 Si3 C3 P -40.34(11) . . . . ?
N3 C22 C23 C24 177.3(2) . . . . ?
N3 C22 C27 C26 -177.2(2) . . . . ?
C1 P C2 Si2 -97.16(11) . . . . ?
C1 P C3 Si3 146.98(9) . . . . ?
C1 Si1 N1 Ta 31.07(13) . . . . ?
C1 Si1 N1 C6 -161.50(13) . . . . ?
C2 P C1 Si1 145.21(10) . . . . ?
C2 P C3 Si3 -90.92(11) . . . . ?
C2 Si2 N2 Ta 28.96(13) . . . . ?
C2 Si2 N2 C14 -162.82(13) . . . . ?
C3 P C1 Si1 -93.00(11) . . . . ?
C3 P C2 Si2 140.26(10) . . . . ?
C3 Si3 N3 Ta 41.12(12) . . . . ?
C3 Si3 N3 C22 -155.06(13) . . . . ?
C4 Si1 N1 Ta 149.66(11) . . . . ?
C4 Si1 N1 C6 -42.91(16) . . . . ?
C4 Si1 C1 P -153.50(10) . . . . ?
C5 Si1 N1 Ta -89.22(13) . . . . ?
C5 Si1 N1 C6 78.21(15) . . . . ?
C5 Si1 C1 P 87.16(13) . . . . ?
C6 C7 C8 C9 -0.3(4) . . . . ?
C7 C6 C11 C10 1.4(3) . . . . ?
C7 C8 C9 C10 0.8(4) . . . . ?
C8 C9 C10 C11 -0.3(4) . . . . ?
C9 C10 C11 C6 -0.9(4) . . . . ?
C11 C6 C7 C8 -0.9(3) . . . . ?
C12 Si2 N2 Ta 148.26(11) . . . . ?
C12 Si2 N2 C14 -43.52(16) . . . . ?
C12 Si2 C2 P -151.32(10) . . . . ?
C13 Si2 N2 Ta -89.91(13) . . . . ?
C13 Si2 N2 C14 78.31(15) . . . . ?
C13 Si2 C2 P 89.46(12) . . . . ?
C14 C15 C16 C17 -0.5(3) . . . . ?
C15 C14 C19 C18 0.2(3) . . . . ?
C15 C16 C17 C18 0.2(4) . . . . ?
C16 C17 C18 C19 0.4(4) . . . . ?
C17 C18 C19 C14 -0.6(3) . . . . ?
C19 C14 C15 C16 0.4(3) . . . . ?
C20 Si3 N3 Ta 160.22(11) . . . . ?
C20 Si3 N3 C22 -35.97(16) . . . . ?
C20 Si3 C3 P -161.53(11) . . . . ?
C21 Si3 N3 Ta -78.35(12) . . . . ?
C21 Si3 N3 C22 85.46(15) . . . . ?
C21 Si3 C3 P 77.48(12) . . . . ?
C22 C23 C24 C25 -0.1(4) . . . . ?
C23 C22 C27 C26 0.7(3) . . . . ?
C23 C24 C25 C26 0.8(4) . . . . ?
C24 C25 C26 C27 -0.7(4) . . . . ?
C25 C26 C27 C22 0.0(4) . . . . ?
C27 C22 C23 C24 -0.7(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            CCD-PXL-KAF2



