# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2161777'
loop_
_audit_author_name
_audit_author_address
'Jiayu Zhang'
;College of Chemistry, Beijing Normal University,
China
;
_audit_update_record             
;
2022-03-24 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H61 O2 P2 Si2 Ti'
_chemical_formula_weight         619.80

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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 '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      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

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

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

_cell_length_a                   16.1891(2)
_cell_length_b                   13.1418(2)
_cell_length_c                   16.9923(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3615.18(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12072
_cell_measurement_theta_min      4.3230
_cell_measurement_theta_max      76.2450

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_F_000             1348
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    3.645
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  Rigaku
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13919
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.363
_diffrn_reflns_theta_max         76.510
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.776
_diffrn_reflns_point_group_measured_fraction_full 0.834
_reflns_number_total             5894
_reflns_number_gt                5744
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.566
_reflns_Friedel_fraction_max     0.582
_reflns_Friedel_fraction_full    0.656

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0531P)²+0.7806P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00059(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1995 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5894
_refine_ls_number_parameters     335
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0703
_refine_ls_wR_factor_gt          0.0698
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_restrained_S_all      0.875
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

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
C1 C 0.14339(13) 0.32023(18) 0.46564(14) 0.0163(4) Uani 1 1 d . . . . .
C2 C 0.14370(14) 0.41745(19) 0.49921(14) 0.0195(5) Uani 1 1 d . . . . .
C3 C 0.18933(16) 0.4455(2) 0.56514(15) 0.0253(5) Uani 1 1 d . . . . .
H3 H 0.1858 0.5110 0.5856 0.030 Uiso 1 1 calc R U . . .
C4 C 0.24018(17) 0.3732(2) 0.59943(16) 0.0273(6) Uani 1 1 d . . . . .
H4 H 0.2709 0.3901 0.6438 0.033 Uiso 1 1 calc R U . . .
C5 C 0.24570(16) 0.2760(2) 0.56845(15) 0.0237(5) Uani 1 1 d . . . . .
H5 H 0.2802 0.2275 0.5911 0.028 Uiso 1 1 calc R U . . .
C6 C 0.19839(15) 0.25278(19) 0.50271(14) 0.0191(5) Uani 1 1 d . . . . .
C7 C 0.25499(14) 0.15390(18) 0.31811(15) 0.0192(5) Uani 1 1 d . . . . .
C8 C 0.25671(16) 0.26920(18) 0.30110(16) 0.0224(5) Uani 1 1 d . . . . .
H8A H 0.2659 0.3057 0.3493 0.034 Uiso 1 1 calc R U . . .
H8B H 0.3005 0.2840 0.2647 0.034 Uiso 1 1 calc R U . . .
H8C H 0.2049 0.2897 0.2787 0.034 Uiso 1 1 calc R U . . .
C9 C 0.33859(15) 0.1238(2) 0.35408(17) 0.0249(5) Uani 1 1 d . . . . .
H9A H 0.3462 0.1591 0.4030 0.037 Uiso 1 1 calc R U . . .
H9B H 0.3396 0.0517 0.3632 0.037 Uiso 1 1 calc R U . . .
H9C H 0.3822 0.1418 0.3184 0.037 Uiso 1 1 calc R U . . .
C10 C 0.24018(15) 0.0992(2) 0.23958(15) 0.0234(5) Uani 1 1 d . . . . .
H10A H 0.1877 0.1194 0.2185 0.035 Uiso 1 1 calc R U . . .
H10B H 0.2831 0.1171 0.2031 0.035 Uiso 1 1 calc R U . . .
H10C H 0.2405 0.0270 0.2480 0.035 Uiso 1 1 calc R U . . .
C11 C 0.14482(15) -0.00777(17) 0.39590(17) 0.0266(5) Uani 1 1 d . . . . .
C12 C 0.1007(2) -0.0207(2) 0.4750(2) 0.0407(8) Uani 1 1 d . . . . .
H12A H 0.1376 -0.0021 0.5169 0.061 Uiso 1 1 calc R U . . .
H12B H 0.0528 0.0223 0.4764 0.061 Uiso 1 1 calc R U . . .
H12C H 0.0842 -0.0904 0.4812 0.061 Uiso 1 1 calc R U . . .
C13 C 0.22051(16) -0.07856(18) 0.3960(2) 0.0326(6) Uani 1 1 d . . . . .
H13A H 0.2570 -0.0595 0.4380 0.049 Uiso 1 1 calc R U . . .
H13B H 0.2028 -0.1476 0.4033 0.049 Uiso 1 1 calc R U . . .
H13C H 0.2490 -0.0727 0.3466 0.049 Uiso 1 1 calc R U . . .
C14 C 0.08608(18) -0.0374(2) 0.3290(2) 0.0337(7) Uani 1 1 d . . . . .
H14A H 0.1137 -0.0293 0.2795 0.051 Uiso 1 1 calc R U . . .
H14B H 0.0695 -0.1071 0.3353 0.051 Uiso 1 1 calc R U . . .
H14C H 0.0382 0.0056 0.3305 0.051 Uiso 1 1 calc R U . . .
C15 C 0.06195(16) 0.55305(19) 0.31866(16) 0.0245(5) Uani 1 1 d . . . . .
C16 C 0.0854(2) 0.6608(2) 0.3463(2) 0.0380(7) Uani 1 1 d . . . . .
H16A H 0.1272 0.6564 0.3862 0.057 Uiso 1 1 calc R U . . .
H16B H 0.1062 0.6992 0.3025 0.057 Uiso 1 1 calc R U . . .
H16C H 0.0375 0.6941 0.3674 0.057 Uiso 1 1 calc R U . . .
C17 C 0.14074(17) 0.5044(2) 0.28467(17) 0.0272(6) Uani 1 1 d . . . . .
H17A H 0.1824 0.5013 0.3248 0.041 Uiso 1 1 calc R U . . .
H17B H 0.1285 0.4369 0.2665 0.041 Uiso 1 1 calc R U . . .
H17C H 0.1604 0.5448 0.2415 0.041 Uiso 1 1 calc R U . . .
C18 C -0.00492(18) 0.5582(2) 0.25467(17) 0.0313(6) Uani 1 1 d . . . . .
H18A H -0.0189 0.4906 0.2381 0.047 Uiso 1 1 calc R U . . .
H18B H -0.0532 0.5911 0.2754 0.047 Uiso 1 1 calc R U . . .
H18C H 0.0155 0.5962 0.2105 0.047 Uiso 1 1 calc R U . . .
C19 C -0.06853(16) 0.5124(2) 0.44796(16) 0.0255(6) Uani 1 1 d . . . . .
C20 C -0.07774(18) 0.6280(2) 0.45219(18) 0.0317(6) Uani 1 1 d . . . . .
H20A H -0.0308 0.6566 0.4788 0.048 Uiso 1 1 calc R U . . .
H20B H -0.0810 0.6553 0.3999 0.048 Uiso 1 1 calc R U . . .
H20C H -0.1272 0.6448 0.4806 0.048 Uiso 1 1 calc R U . . .
C21 C -0.06437(18) 0.4696(2) 0.53226(17) 0.0322(6) Uani 1 1 d . . . . .
H21A H -0.0174 0.4979 0.5590 0.048 Uiso 1 1 calc R U . . .
H21B H -0.1139 0.4875 0.5601 0.048 Uiso 1 1 calc R U . . .
H21C H -0.0592 0.3969 0.5302 0.048 Uiso 1 1 calc R U . . .
C22 C -0.14331(15) 0.4673(2) 0.40558(19) 0.0327(6) Uani 1 1 d . . . . .
H22A H -0.1377 0.3946 0.4028 0.049 Uiso 1 1 calc R U . . .
H22B H -0.1927 0.4842 0.4340 0.049 Uiso 1 1 calc R U . . .
H22C H -0.1465 0.4947 0.3533 0.049 Uiso 1 1 calc R U . . .
C23 C 0.02355(15) 0.25709(19) 0.25823(15) 0.0201(5) Uani 1 1 d . . . . .
H23A H 0.0396 0.3233 0.2382 0.024 Uiso 1 1 calc R U . . .
H23B H 0.0641 0.2093 0.2382 0.024 Uiso 1 1 calc R U . . .
C24 C -0.06928(18) 0.2622(2) 0.10071(17) 0.0295(6) Uani 1 1 d . . . . .
H24A H -0.1205 0.2450 0.0755 0.044 Uiso 1 1 calc R U . . .
H24B H -0.0601 0.3342 0.0965 0.044 Uiso 1 1 calc R U . . .
H24C H -0.0248 0.2264 0.0756 0.044 Uiso 1 1 calc R U . . .
C25 C -0.0936(2) 0.0853(2) 0.20914(19) 0.0388(7) Uani 1 1 d . . . . .
H25A H -0.1444 0.0707 0.1824 0.058 Uiso 1 1 calc R U . . .
H25B H -0.0490 0.0505 0.1834 0.058 Uiso 1 1 calc R U . . .
H25C H -0.0973 0.0627 0.2627 0.058 Uiso 1 1 calc R U . . .
C26 C -0.16809(18) 0.2911(3) 0.2471(2) 0.0454(9) Uani 1 1 d . . . . .
H26A H -0.2158 0.2706 0.2176 0.068 Uiso 1 1 calc R U . . .
H26B H -0.1754 0.2729 0.3014 0.068 Uiso 1 1 calc R U . . .
H26C H -0.1611 0.3635 0.2429 0.068 Uiso 1 1 calc R U . . .
C27 C -0.05459(15) 0.1854(2) 0.44005(15) 0.0227(5) Uani 1 1 d . . . . .
H27A H -0.1036 0.2207 0.4219 0.027 Uiso 1 1 calc R U . . .
H27B H -0.0555 0.1197 0.4141 0.027 Uiso 1 1 calc R U . . .
C28 C -0.1018(2) 0.0170(2) 0.56309(18) 0.0370(7) Uani 1 1 d . . . . .
H28A H -0.1126 0.0062 0.6180 0.056 Uiso 1 1 calc R U . . .
H28B H -0.1497 -0.0014 0.5330 0.056 Uiso 1 1 calc R U . . .
H28C H -0.0558 -0.0242 0.5471 0.056 Uiso 1 1 calc R U . . .
C29 C -0.1709(2) 0.2275(3) 0.5798(2) 0.0502(9) Uani 1 1 d . . . . .
H29A H -0.1817 0.2117 0.6340 0.075 Uiso 1 1 calc R U . . .
H29B H -0.1614 0.2993 0.5744 0.075 Uiso 1 1 calc R U . . .
H29C H -0.2176 0.2082 0.5484 0.075 Uiso 1 1 calc R U . . .
C30 C 0.01143(19) 0.1885(2) 0.61300(17) 0.0333(6) Uani 1 1 d . . . . .
H30A H -0.0032 0.1719 0.6662 0.050 Uiso 1 1 calc R U . . .
H30B H 0.0595 0.1505 0.5978 0.050 Uiso 1 1 calc R U . . .
H30C H 0.0230 0.2600 0.6093 0.050 Uiso 1 1 calc R U . . .
O1 O 0.20957(11) 0.15426(14) 0.47287(11) 0.0242(4) Uani 1 1 d . . . . .
O2 O 0.09678(11) 0.49616(13) 0.46650(11) 0.0247(4) Uani 1 1 d . . . . .
Ti1 Ti 0.04466(2) 0.26406(3) 0.38577(2) 0.01447(10) Uani 1 1 d . . . . .
P1 P 0.02784(3) 0.46543(4) 0.39961(4) 0.01839(13) Uani 1 1 d . . . . .
P2 P 0.16639(3) 0.13175(4) 0.38711(4) 0.01725(13) Uani 1 1 d . . . . .
Si1 Si -0.07407(4) 0.22528(5) 0.20712(4) 0.02174(15) Uani 1 1 d . . . . .
Si2 Si -0.07681(4) 0.15569(6) 0.54578(5) 0.02775(17) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.399(3) . ?
C1 C6 1.405(3) . ?
C1 Ti1 2.223(2) . ?
C2 O2 1.399(3) . ?
C2 C3 1.392(3) . ?
C3 C4 1.387(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.388(4) . ?
C5 H5 0.9300 . ?
C6 O1 1.402(3) . ?
C7 C10 1.535(3) . ?
C7 C9 1.537(3) . ?
C7 C8 1.543(3) . ?
C7 P2 1.875(2) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C14 1.532(4) . ?
C11 C12 1.531(4) . ?
C11 C13 1.539(3) . ?
C11 P2 1.872(2) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C18 1.536(4) . ?
C15 C16 1.540(4) . ?
C15 C17 1.539(4) . ?
C15 P1 1.877(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C22 1.528(4) . ?
C19 C20 1.529(4) . ?
C19 C21 1.540(4) . ?
C19 P1 1.868(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 Si1 1.851(3) . ?
C23 Ti1 2.196(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 Si1 1.874(3) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 Si1 1.867(3) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 Si1 1.878(3) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 Si2 1.873(3) . ?
C27 Ti1 2.122(2) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 Si2 1.890(3) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 Si2 1.883(3) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 Si2 1.879(3) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
O1 P2 1.6431(19) . ?
O2 P1 1.6434(18) . ?
Ti1 P2 2.6281(6) . ?
Ti1 P1 2.6707(7) . ?

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
C2 C1 C6 113.0(2) . . ?
C2 C1 Ti1 123.69(16) . . ?
C6 C1 Ti1 121.31(17) . . ?
O2 C2 C3 114.3(2) . . ?
O2 C2 C1 120.8(2) . . ?
C3 C2 C1 124.9(2) . . ?
C4 C3 C2 118.1(2) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C3 C4 C5 120.8(2) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 118.2(2) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C5 C6 O1 115.0(2) . . ?
C5 C6 C1 124.9(2) . . ?
O1 C6 C1 120.1(2) . . ?
C10 C7 C9 111.3(2) . . ?
C10 C7 C8 107.4(2) . . ?
C9 C7 C8 108.1(2) . . ?
C10 C7 P2 110.58(16) . . ?
C9 C7 P2 112.65(17) . . ?
C8 C7 P2 106.47(16) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C11 C12 109.5(2) . . ?
C14 C11 C13 110.0(2) . . ?
C12 C11 C13 107.7(2) . . ?
C14 C11 P2 107.78(18) . . ?
C12 C11 P2 105.40(18) . . ?
C13 C11 P2 116.34(17) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18 C15 C16 110.4(2) . . ?
C18 C15 C17 109.7(2) . . ?
C16 C15 C17 107.0(2) . . ?
C18 C15 P1 109.80(18) . . ?
C16 C15 P1 114.4(2) . . ?
C17 C15 P1 105.32(17) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C19 C20 109.3(2) . . ?
C22 C19 C21 109.4(2) . . ?
C20 C19 C21 108.8(2) . . ?
C22 C19 P1 109.04(18) . . ?
C20 C19 P1 115.5(2) . . ?
C21 C19 P1 104.60(17) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 Ti1 127.25(13) . . ?
Si1 C23 H23A 105.5 . . ?
Ti1 C23 H23A 105.5 . . ?
Si1 C23 H23B 105.5 . . ?
Ti1 C23 H23B 105.5 . . ?
H23A C23 H23B 106.1 . . ?
Si1 C24 H24A 109.5 . . ?
Si1 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si1 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si1 C25 H25A 109.5 . . ?
Si1 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si1 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si1 C26 H26A 109.5 . . ?
Si1 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si1 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si2 C27 Ti1 131.59(14) . . ?
Si2 C27 H27A 104.4 . . ?
Ti1 C27 H27A 104.4 . . ?
Si2 C27 H27B 104.4 . . ?
Ti1 C27 H27B 104.4 . . ?
H27A C27 H27B 105.6 . . ?
Si2 C28 H28A 109.5 . . ?
Si2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si2 C29 H29A 109.5 . . ?
Si2 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si2 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si2 C30 H30A 109.5 . . ?
Si2 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si2 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C6 O1 P2 115.59(15) . . ?
C2 O2 P1 117.52(16) . . ?
C27 Ti1 C23 106.91(10) . . ?
C27 Ti1 C1 116.17(9) . . ?
C23 Ti1 C1 136.74(9) . . ?
C27 Ti1 P2 103.99(7) . . ?
C23 Ti1 P2 95.60(7) . . ?
C1 Ti1 P2 71.05(6) . . ?
C27 Ti1 P1 111.55(7) . . ?
C23 Ti1 P1 96.45(7) . . ?
C1 Ti1 P1 71.97(6) . . ?
P2 Ti1 P1 136.99(2) . . ?
O2 P1 C19 100.48(11) . . ?
O2 P1 C15 98.99(11) . . ?
C19 P1 C15 111.43(12) . . ?
O2 P1 Ti1 103.60(7) . . ?
C19 P1 Ti1 116.82(9) . . ?
C15 P1 Ti1 120.89(8) . . ?
O1 P2 C11 100.65(11) . . ?
O1 P2 C7 101.61(11) . . ?
C11 P2 C7 110.15(11) . . ?
O1 P2 Ti1 101.98(7) . . ?
C11 P2 Ti1 120.58(8) . . ?
C7 P2 Ti1 117.74(8) . . ?
C23 Si1 C25 110.99(13) . . ?
C23 Si1 C24 111.03(12) . . ?
C25 Si1 C24 106.26(14) . . ?
C23 Si1 C26 114.70(13) . . ?
C25 Si1 C26 108.08(17) . . ?
C24 Si1 C26 105.29(15) . . ?
C27 Si2 C29 110.22(16) . . ?
C27 Si2 C30 112.90(12) . . ?
C29 Si2 C30 108.24(16) . . ?
C27 Si2 C28 113.04(13) . . ?
C29 Si2 C28 105.20(16) . . ?
C30 Si2 C28 106.83(14) . . ?

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
C6 C1 C2 O2 175.7(2) . . . . ?
Ti1 C1 C2 O2 -20.2(3) . . . . ?
C6 C1 C2 C3 -3.5(3) . . . . ?
Ti1 C1 C2 C3 160.63(19) . . . . ?
O2 C2 C3 C4 -177.5(2) . . . . ?
C1 C2 C3 C4 1.8(4) . . . . ?
C2 C3 C4 C5 0.5(4) . . . . ?
C3 C4 C5 C6 -0.6(4) . . . . ?
C4 C5 C6 O1 177.7(2) . . . . ?
C4 C5 C6 C1 -1.4(4) . . . . ?
C2 C1 C6 C5 3.3(3) . . . . ?
Ti1 C1 C6 C5 -161.2(2) . . . . ?
C2 C1 C6 O1 -175.8(2) . . . . ?
Ti1 C1 C6 O1 19.7(3) . . . . ?
C5 C6 O1 P2 -170.13(18) . . . . ?
C1 C6 O1 P2 9.0(3) . . . . ?
C3 C2 O2 P1 -168.55(17) . . . . ?
C1 C2 O2 P1 12.2(3) . . . . ?
C2 O2 P1 C19 120.23(19) . . . . ?
C2 O2 P1 C15 -125.85(18) . . . . ?
C2 O2 P1 Ti1 -0.89(18) . . . . ?
C22 C19 P1 O2 -165.49(19) . . . . ?
C20 C19 P1 O2 71.0(2) . . . . ?
C21 C19 P1 O2 -48.6(2) . . . . ?
C22 C19 P1 C15 90.4(2) . . . . ?
C20 C19 P1 C15 -33.1(2) . . . . ?
C21 C19 P1 C15 -152.68(19) . . . . ?
C22 C19 P1 Ti1 -54.3(2) . . . . ?
C20 C19 P1 Ti1 -177.80(17) . . . . ?
C21 C19 P1 Ti1 62.6(2) . . . . ?
C18 C15 P1 O2 -166.73(18) . . . . ?
C16 C15 P1 O2 -41.9(2) . . . . ?
C17 C15 P1 O2 75.24(18) . . . . ?
C18 C15 P1 C19 -61.7(2) . . . . ?
C16 C15 P1 C19 63.1(2) . . . . ?
C17 C15 P1 C19 -179.69(17) . . . . ?
C18 C15 P1 Ti1 81.43(19) . . . . ?
C16 C15 P1 Ti1 -153.77(18) . . . . ?
C17 C15 P1 Ti1 -36.6(2) . . . . ?
C6 O1 P2 C11 -150.50(17) . . . . ?
C6 O1 P2 C7 96.14(18) . . . . ?
C6 O1 P2 Ti1 -25.82(17) . . . . ?
C14 C11 P2 O1 166.82(18) . . . . ?
C12 C11 P2 O1 50.0(2) . . . . ?
C13 C11 P2 O1 -69.2(2) . . . . ?
C14 C11 P2 C7 -86.50(19) . . . . ?
C12 C11 P2 C7 156.66(19) . . . . ?
C13 C11 P2 C7 37.5(3) . . . . ?
C14 C11 P2 Ti1 55.9(2) . . . . ?
C12 C11 P2 Ti1 -60.9(2) . . . . ?
C13 C11 P2 Ti1 179.91(19) . . . . ?
C10 C7 P2 O1 158.17(16) . . . . ?
C9 C7 P2 O1 32.96(19) . . . . ?
C8 C7 P2 O1 -85.40(18) . . . . ?
C10 C7 P2 C11 52.1(2) . . . . ?
C9 C7 P2 C11 -73.1(2) . . . . ?
C8 C7 P2 C11 168.55(17) . . . . ?
C10 C7 P2 Ti1 -91.50(16) . . . . ?
C9 C7 P2 Ti1 143.29(15) . . . . ?
C8 C7 P2 Ti1 24.92(19) . . . . ?
Ti1 C23 Si1 C25 -76.97(19) . . . . ?
Ti1 C23 Si1 C24 165.07(15) . . . . ?
Ti1 C23 Si1 C26 45.9(2) . . . . ?
Ti1 C27 Si2 C29 112.8(2) . . . . ?
Ti1 C27 Si2 C30 -8.3(2) . . . . ?
Ti1 C27 Si2 C28 -129.75(19) . . . . ?

_refine_diff_density_max         0.279
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.040



####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2163361'
loop_
_audit_author_name
_audit_author_address
'Jiayu Zhang'
;College of Chemistry, Beijing Normal University,
China
;
_audit_update_record             
;
2022-03-30 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H65 P2 Sc Si2'
_chemical_formula_weight         612.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 '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'

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

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

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

_cell_length_a                   16.7335(7)
_cell_length_b                   13.2393(6)
_cell_length_c                   16.9263(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.212(4)
_cell_angle_gamma                90
_cell_volume                     3720.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8847
_cell_measurement_theta_min      4.1740
_cell_measurement_theta_max      29.3810

_exptl_crystal_description       Block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.366
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  Rigaku
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19441
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.257
_diffrn_reflns_theta_max         29.751
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             8822
_reflns_number_gt                6858
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0446P)²+0.3596P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8822
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.1014
_refine_ls_wR_factor_gt          0.0936
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Sc1 Sc 0.73274(2) 0.51041(2) 0.64984(2) 0.01559(8) Uani 1 1 d . . . . .
P2 P 0.75766(2) 0.71696(3) 0.63450(2) 0.01624(10) Uani 1 1 d . . . . .
P1 P 0.73407(2) 0.31959(3) 0.56985(2) 0.01975(11) Uani 1 1 d . . . . .
Si1 Si 0.53596(3) 0.49392(4) 0.72846(3) 0.02168(12) Uani 1 1 d . . . . .
Si2 Si 0.90054(3) 0.47837(4) 0.82107(3) 0.02391(12) Uani 1 1 d . . . . .
C25 C 0.59969(9) 0.53583(14) 0.65343(10) 0.0219(4) Uani 1 1 d . . . . .
H25A H 0.592690 0.608518 0.650374 0.026 Uiso 1 1 calc R U . . .
H25B H 0.573617 0.509397 0.603263 0.026 Uiso 1 1 calc R U . . .
C1 C 0.81232(9) 0.53325(13) 0.54731(9) 0.0186(3) Uani 1 1 d . . . . .
C6 C 0.82133(9) 0.46007(13) 0.48765(9) 0.0200(3) Uani 1 1 d . . . . .
C29 C 0.79410(9) 0.48432(13) 0.77311(9) 0.0213(4) Uani 1 1 d . . . . .
H29A H 0.770175 0.534895 0.804322 0.026 Uiso 1 1 calc R U . . .
H29B H 0.771740 0.420469 0.787920 0.026 Uiso 1 1 calc R U . . .
C2 C 0.86198(9) 0.61986(13) 0.54440(9) 0.0190(3) Uani 1 1 d . . . . .
C8 C 0.85846(9) 0.70515(13) 0.60354(10) 0.0219(4) Uani 1 1 d . . . . .
H8A H 0.872802 0.768065 0.579546 0.026 Uiso 1 1 calc R U . . .
H8B H 0.897395 0.692721 0.649983 0.026 Uiso 1 1 calc R U . . .
C17 C 0.77295(10) 0.80565(13) 0.72237(9) 0.0221(4) Uani 1 1 d . . . . .
C21 C 0.69425(10) 0.77858(14) 0.54691(9) 0.0219(4) Uani 1 1 d . . . . .
C24 C 0.62056(10) 0.83173(15) 0.57357(11) 0.0304(4) Uani 1 1 d . . . . .
H24A H 0.638079 0.887367 0.607809 0.046 Uiso 1 1 calc R U . . .
H24B H 0.590968 0.784745 0.601896 0.046 Uiso 1 1 calc R U . . .
H24C H 0.586581 0.856303 0.527685 0.046 Uiso 1 1 calc R U . . .
C13 C 0.81691(10) 0.23239(14) 0.61299(10) 0.0248(4) Uani 1 1 d . . . . .
C5 C 0.87675(11) 0.47116(14) 0.43304(10) 0.0264(4) Uani 1 1 d . . . . .
H3 H 0.881137 0.421006 0.395363 0.032 Uiso 1 1 calc R U . . .
C22 C 0.66277(10) 0.69506(15) 0.48770(10) 0.0268(4) Uani 1 1 d . . . . .
H22A H 0.629234 0.724586 0.443516 0.040 Uiso 1 1 calc R U . . .
H22B H 0.631955 0.647173 0.513886 0.040 Uiso 1 1 calc R U . . .
H22C H 0.707486 0.661362 0.468789 0.040 Uiso 1 1 calc R U . . .
C7 C 0.76731(10) 0.36799(14) 0.47755(9) 0.0241(4) Uani 1 1 d . . . . .
H7A H 0.795792 0.314505 0.453632 0.029 Uiso 1 1 calc R U . . .
H7B H 0.720017 0.384621 0.440637 0.029 Uiso 1 1 calc R U . . .
C3 C 0.91671(10) 0.63065(14) 0.48939(10) 0.0248(4) Uani 1 1 d . . . . .
H5 H 0.947916 0.688817 0.489705 0.030 Uiso 1 1 calc R U . . .
C32 C 0.91822(11) 0.55240(17) 0.91684(10) 0.0328(4) Uani 1 1 d . . . . .
H32A H 0.904537 0.621973 0.906460 0.049 Uiso 1 1 calc R U . . .
H32B H 0.973906 0.547443 0.938536 0.049 Uiso 1 1 calc R U . . .
H32C H 0.885213 0.525477 0.954282 0.049 Uiso 1 1 calc R U . . .
C26 C 0.53535(11) 0.35306(15) 0.74070(11) 0.0322(4) Uani 1 1 d . . . . .
H26A H 0.509654 0.322504 0.692678 0.048 Uiso 1 1 calc R U . . .
H26B H 0.506349 0.335677 0.784254 0.048 Uiso 1 1 calc R U . . .
H26C H 0.589731 0.328941 0.751447 0.048 Uiso 1 1 calc R U . . .
C14 C 0.80131(12) 0.20021(15) 0.69729(11) 0.0323(4) Uani 1 1 d . . . . .
H14A H 0.847153 0.163853 0.722635 0.048 Uiso 1 1 calc R U . . .
H14B H 0.754563 0.157615 0.693608 0.048 Uiso 1 1 calc R U . . .
H14C H 0.792504 0.259143 0.728098 0.048 Uiso 1 1 calc R U . . .
C18 C 0.84449(11) 0.76536(16) 0.77903(10) 0.0336(4) Uani 1 1 d . . . . .
H18A H 0.893765 0.781216 0.758175 0.050 Uiso 1 1 calc R U . . .
H18B H 0.839746 0.693447 0.783997 0.050 Uiso 1 1 calc R U . . .
H18C H 0.844765 0.796192 0.830395 0.050 Uiso 1 1 calc R U . . .
C30 C 0.97500(10) 0.52985(17) 0.75664(11) 0.0339(5) Uani 1 1 d . . . . .
H30A H 0.959830 0.508948 0.702522 0.051 Uiso 1 1 calc R U . . .
H30B H 1.027800 0.504558 0.775162 0.051 Uiso 1 1 calc R U . . .
H30C H 0.975308 0.602275 0.759388 0.051 Uiso 1 1 calc R U . . .
C27 C 0.42765(10) 0.53502(17) 0.70444(12) 0.0356(5) Uani 1 1 d . . . . .
H27A H 0.425411 0.607088 0.698311 0.053 Uiso 1 1 calc R U . . .
H27B H 0.397993 0.515380 0.746960 0.053 Uiso 1 1 calc R U . . .
H27C H 0.404459 0.503496 0.655831 0.053 Uiso 1 1 calc R U . . .
C9 C 0.64156(11) 0.24537(15) 0.52907(11) 0.0301(4) Uani 1 1 d . . . . .
C16 C 0.89538(10) 0.29490(15) 0.62098(11) 0.0308(4) Uani 1 1 d . . . . .
H16A H 0.938903 0.255017 0.646893 0.046 Uiso 1 1 calc R U . . .
H16B H 0.888830 0.354364 0.651982 0.046 Uiso 1 1 calc R U . . .
H16C H 0.907193 0.314205 0.569015 0.046 Uiso 1 1 calc R U . . .
C20 C 0.79067(12) 0.91553(14) 0.70290(11) 0.0323(4) Uani 1 1 d . . . . .
H20A H 0.804076 0.952660 0.751473 0.048 Uiso 1 1 calc R U . . .
H20B H 0.743960 0.944955 0.672841 0.048 Uiso 1 1 calc R U . . .
H20C H 0.835092 0.917987 0.672153 0.048 Uiso 1 1 calc R U . . .
C23 C 0.74250(11) 0.85393(16) 0.50304(11) 0.0353(5) Uani 1 1 d . . . . .
H23A H 0.783466 0.818541 0.479205 0.053 Uiso 1 1 calc R U . . .
H23B H 0.767202 0.902989 0.540119 0.053 Uiso 1 1 calc R U . . .
H23C H 0.707047 0.887453 0.462301 0.053 Uiso 1 1 calc R U . . .
C19 C 0.69804(12) 0.79909(16) 0.76639(11) 0.0346(5) Uani 1 1 d . . . . .
H19A H 0.705404 0.841574 0.812699 0.052 Uiso 1 1 calc R U . . .
H19B H 0.690454 0.730505 0.782283 0.052 Uiso 1 1 calc R U . . .
H19C H 0.651526 0.821113 0.731651 0.052 Uiso 1 1 calc R U . . .
C4 C 0.92492(10) 0.55556(15) 0.43444(10) 0.0287(4) Uani 1 1 d . . . . .
H4 H 0.962588 0.561921 0.398744 0.034 Uiso 1 1 calc R U . . .
C28 C 0.57354(11) 0.54977(17) 0.82825(10) 0.0338(4) Uani 1 1 d . . . . .
H28A H 0.628162 0.528796 0.843856 0.051 Uiso 1 1 calc R U . . .
H28B H 0.540353 0.526942 0.867001 0.051 Uiso 1 1 calc R U . . .
H28C H 0.571328 0.622122 0.824881 0.051 Uiso 1 1 calc R U . . .
C15 C 0.82870(12) 0.13896(15) 0.56319(11) 0.0363(5) Uani 1 1 d . . . . .
H15A H 0.835664 0.159059 0.509988 0.054 Uiso 1 1 calc R U . . .
H15B H 0.782270 0.096092 0.561756 0.054 Uiso 1 1 calc R U . . .
H15C H 0.875596 0.102859 0.586441 0.054 Uiso 1 1 calc R U . . .
C11 C 0.57419(11) 0.32475(17) 0.51251(12) 0.0383(5) Uani 1 1 d . . . . .
H11A H 0.526262 0.292905 0.486897 0.057 Uiso 1 1 calc R U . . .
H11B H 0.590990 0.376510 0.478456 0.057 Uiso 1 1 calc R U . . .
H11C H 0.563349 0.354274 0.561862 0.057 Uiso 1 1 calc R U . . .
C31 C 0.93269(12) 0.34527(16) 0.84774(12) 0.0389(5) Uani 1 1 d . . . . .
H31A H 0.891927 0.312648 0.873786 0.058 Uiso 1 1 calc R U . . .
H31B H 0.982411 0.346416 0.882857 0.058 Uiso 1 1 calc R U . . .
H31C H 0.940143 0.308799 0.800192 0.058 Uiso 1 1 calc R U . . .
C10 C 0.61722(12) 0.17041(16) 0.59013(12) 0.0401(5) Uani 1 1 d . . . . .
H10A H 0.564380 0.144655 0.572405 0.060 Uiso 1 1 calc R U . . .
H10B H 0.616913 0.203791 0.640438 0.060 Uiso 1 1 calc R U . . .
H10C H 0.655057 0.115592 0.595985 0.060 Uiso 1 1 calc R U . . .
C12 C 0.64922(13) 0.18909(17) 0.45092(12) 0.0435(5) Uani 1 1 d . . . . .
H12A H 0.693631 0.142775 0.459025 0.065 Uiso 1 1 calc R U . . .
H12B H 0.658358 0.236910 0.410378 0.065 Uiso 1 1 calc R U . . .
H12C H 0.600436 0.152437 0.434575 0.065 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sc1 C29 2.2338(16) . ?
Sc1 C25 2.2601(15) . ?
Sc1 C1 2.3359(15) . ?
Sc1 P2 2.7831(5) . ?
Sc1 P1 2.8677(5) . ?
P2 C8 1.8346(16) . ?
P2 C17 1.8871(17) . ?
P2 C21 1.8959(16) . ?
P1 C7 1.8382(16) . ?
P1 C13 1.8797(18) . ?
P1 C9 1.8895(18) . ?
Si1 C25 1.8434(16) . ?
Si1 C26 1.877(2) . ?
Si1 C28 1.8784(18) . ?
Si1 C27 1.8870(18) . ?
Si2 C29 1.8639(16) . ?
Si2 C31 1.881(2) . ?
Si2 C30 1.8835(19) . ?
Si2 C32 1.8856(18) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C1 C2 1.421(2) . ?
C1 C6 1.421(2) . ?
C6 C5 1.397(2) . ?
C6 C7 1.514(2) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C2 C3 1.393(2) . ?
C2 C8 1.515(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C17 C20 1.529(2) . ?
C17 C18 1.533(2) . ?
C17 C19 1.539(2) . ?
C21 C23 1.533(2) . ?
C21 C24 1.536(2) . ?
C21 C22 1.540(2) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C13 C15 1.524(2) . ?
C13 C14 1.542(2) . ?
C13 C16 1.544(2) . ?
C5 C4 1.376(3) . ?
C5 H3 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C3 C4 1.380(3) . ?
C3 H5 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C9 C10 1.525(3) . ?
C9 C12 1.537(3) . ?
C9 C11 1.541(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C4 H4 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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
C29 Sc1 C25 109.68(6) . . ?
C29 Sc1 C1 118.42(6) . . ?
C25 Sc1 C1 131.00(6) . . ?
C29 Sc1 P2 100.51(5) . . ?
C25 Sc1 P2 90.91(5) . . ?
C1 Sc1 P2 72.39(4) . . ?
C29 Sc1 P1 105.95(5) . . ?
C25 Sc1 P1 102.12(5) . . ?
C1 Sc1 P1 74.00(4) . . ?
P2 Sc1 P1 144.234(16) . . ?
C8 P2 C17 103.86(7) . . ?
C8 P2 C21 104.94(7) . . ?
C17 P2 C21 110.84(8) . . ?
C8 P2 Sc1 95.56(6) . . ?
C17 P2 Sc1 123.02(6) . . ?
C21 P2 Sc1 114.84(6) . . ?
C7 P1 C13 104.91(8) . . ?
C7 P1 C9 101.08(8) . . ?
C13 P1 C9 110.67(9) . . ?
C7 P1 Sc1 96.62(6) . . ?
C13 P1 Sc1 114.00(6) . . ?
C9 P1 Sc1 125.17(6) . . ?
C25 Si1 C26 112.76(8) . . ?
C25 Si1 C28 110.10(8) . . ?
C26 Si1 C28 107.32(9) . . ?
C25 Si1 C27 112.82(8) . . ?
C26 Si1 C27 106.98(9) . . ?
C28 Si1 C27 106.52(9) . . ?
C29 Si2 C31 111.90(9) . . ?
C29 Si2 C30 113.45(8) . . ?
C31 Si2 C30 106.73(9) . . ?
C29 Si2 C32 113.00(8) . . ?
C31 Si2 C32 105.75(9) . . ?
C30 Si2 C32 105.42(9) . . ?
Si1 C25 Sc1 129.11(9) . . ?
Si1 C25 H25A 105.0 . . ?
Sc1 C25 H25A 105.0 . . ?
Si1 C25 H25B 105.0 . . ?
Sc1 C25 H25B 105.0 . . ?
H25A C25 H25B 105.9 . . ?
C2 C1 C6 114.27(14) . . ?
C2 C1 Sc1 121.38(11) . . ?
C6 C1 Sc1 124.12(12) . . ?
C5 C6 C1 122.48(16) . . ?
C5 C6 C7 116.51(15) . . ?
C1 C6 C7 120.93(14) . . ?
Si2 C29 Sc1 135.68(8) . . ?
Si2 C29 H29A 103.2 . . ?
Sc1 C29 H29A 103.2 . . ?
Si2 C29 H29B 103.2 . . ?
Sc1 C29 H29B 103.2 . . ?
H29A C29 H29B 105.2 . . ?
C3 C2 C1 122.86(15) . . ?
C3 C2 C8 116.65(14) . . ?
C1 C2 C8 120.48(13) . . ?
C2 C8 P2 111.45(11) . . ?
C2 C8 H8A 109.3 . . ?
P2 C8 H8A 109.3 . . ?
C2 C8 H8B 109.3 . . ?
P2 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C20 C17 C18 107.98(15) . . ?
C20 C17 C19 110.47(15) . . ?
C18 C17 C19 107.29(14) . . ?
C20 C17 P2 115.65(12) . . ?
C18 C17 P2 107.13(12) . . ?
C19 C17 P2 107.96(12) . . ?
C23 C21 C24 109.59(16) . . ?
C23 C21 C22 108.06(14) . . ?
C24 C21 C22 107.37(14) . . ?
C23 C21 P2 112.45(11) . . ?
C24 C21 P2 111.01(11) . . ?
C22 C21 P2 108.18(12) . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C15 C13 C14 109.65(15) . . ?
C15 C13 C16 108.42(15) . . ?
C14 C13 C16 107.94(15) . . ?
C15 C13 P1 115.09(13) . . ?
C14 C13 P1 109.08(12) . . ?
C16 C13 P1 106.40(12) . . ?
C4 C5 C6 120.67(16) . . ?
C4 C5 H3 119.7 . . ?
C6 C5 H3 119.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C6 C7 P1 115.12(11) . . ?
C6 C7 H7A 108.5 . . ?
P1 C7 H7A 108.5 . . ?
C6 C7 H7B 108.5 . . ?
P1 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C4 C3 C2 120.40(16) . . ?
C4 C3 H5 119.8 . . ?
C2 C3 H5 119.8 . . ?
Si2 C32 H32A 109.5 . . ?
Si2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
Si2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si1 C26 H26A 109.5 . . ?
Si1 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si1 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C30 H30A 109.5 . . ?
Si2 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si2 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si1 C27 H27A 109.5 . . ?
Si1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C10 C9 C12 109.02(17) . . ?
C10 C9 C11 108.40(16) . . ?
C12 C9 C11 108.19(16) . . ?
C10 C9 P1 111.54(13) . . ?
C12 C9 P1 114.42(13) . . ?
C11 C9 P1 105.01(13) . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C5 C4 C3 119.26(15) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
Si1 C28 H28A 109.5 . . ?
Si1 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si1 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si2 C31 H31A 109.5 . . ?
Si2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_refine_diff_density_max         0.411
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.062



####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2168774'
loop_
_audit_author_name
_audit_author_address
'Jiayu Zhang'
;College of Chemistry, Beijing Normal University,
China
;
_audit_update_record             
;
2022-04-26 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H39 Cl2 O2 P2 Ti'
_chemical_formula_weight         516.27

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.6740(6)
_cell_length_b                   16.1874(9)
_cell_length_c                   15.2797(10)
_cell_angle_alpha                90
_cell_angle_beta                 91.080(6)
_cell_angle_gamma                90
_cell_volume                     2639.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1825
_cell_measurement_theta_min      3.9970
_cell_measurement_theta_max      24.5980

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_F_000             1092
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.663
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  Rigaku
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14374
_diffrn_reflns_av_unetI/netI     0.1634
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.415
_diffrn_reflns_theta_max         29.838
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6321
_reflns_number_gt                3692
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0535P)²+1.0794P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6321
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0726
_refine_ls_wR_factor_ref         0.1798
_refine_ls_wR_factor_gt          0.1369
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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
Ti1 Ti 0.49708(7) 0.38996(5) 0.21999(5) 0.0137(2) Uani 1 1 d . . . . .
Cl2 Cl 0.62304(10) 0.49095(6) 0.15922(7) 0.0166(3) Uani 1 1 d . . . . .
Cl1 Cl 0.49354(10) 0.29015(7) 0.11318(7) 0.0190(3) Uani 1 1 d . . . . .
P1 P 0.66015(11) 0.33961(7) 0.33499(8) 0.0145(3) Uani 1 1 d . . . . .
P2 P 0.27934(11) 0.46139(7) 0.20530(8) 0.0148(3) Uani 1 1 d . . . . .
O1 O 0.5757(3) 0.29598(19) 0.4108(2) 0.0195(7) Uani 1 1 d . . . . .
O2 O 0.2037(3) 0.4313(2) 0.2921(2) 0.0214(8) Uani 1 1 d . . . . .
C1 C 0.3964(4) 0.3638(3) 0.3411(3) 0.0149(10) Uani 1 1 d . . . . .
C2 C 0.2692(4) 0.3812(3) 0.3523(3) 0.0153(10) Uani 1 1 d . . . . .
C7 C 0.7641(4) 0.2531(3) 0.3023(3) 0.0170(10) Uani 1 1 d . . . . .
C6 C 0.4480(4) 0.3160(3) 0.4101(3) 0.0191(11) Uani 1 1 d . . . . .
C15 C 0.1717(4) 0.4232(3) 0.1173(3) 0.0180(10) Uani 1 1 d . . . . .
C3 C 0.1989(4) 0.3550(3) 0.4223(3) 0.0174(10) Uani 1 1 d . . . . .
H3 H 0.114868 0.369644 0.426151 0.021 Uiso 1 1 calc R U . . .
C4 C 0.2554(4) 0.3068(3) 0.4865(3) 0.0177(10) Uani 1 1 d . . . . .
H4 H 0.209147 0.287980 0.533396 0.021 Uiso 1 1 calc R U . . .
C9 C 0.8298(4) 0.2781(3) 0.2181(3) 0.0234(11) Uani 1 1 d . . . . .
H9A H 0.882870 0.324896 0.229604 0.035 Uiso 1 1 calc R U . . .
H9B H 0.768219 0.292247 0.174079 0.035 Uiso 1 1 calc R U . . .
H9C H 0.879635 0.232784 0.197959 0.035 Uiso 1 1 calc R U . . .
C5 C 0.3829(4) 0.2863(3) 0.4807(3) 0.0205(11) Uani 1 1 d . . . . .
H5 H 0.422145 0.253680 0.523131 0.025 Uiso 1 1 calc R U . . .
C13 C 0.8519(4) 0.4574(3) 0.3470(3) 0.0247(12) Uani 1 1 d . . . . .
H13A H 0.884756 0.505319 0.376351 0.037 Uiso 1 1 calc R U . . .
H13B H 0.820861 0.472662 0.289849 0.037 Uiso 1 1 calc R U . . .
H13C H 0.917079 0.416952 0.341383 0.037 Uiso 1 1 calc R U . . .
C8 C 0.6768(4) 0.1786(3) 0.2835(3) 0.0245(12) Uani 1 1 d . . . . .
H8A H 0.613616 0.194193 0.241100 0.037 Uiso 1 1 calc R U . . .
H8B H 0.637538 0.161862 0.336673 0.037 Uiso 1 1 calc R U . . .
H8C H 0.725025 0.133536 0.261066 0.037 Uiso 1 1 calc R U . . .
C11 C 0.7446(4) 0.4208(3) 0.4002(3) 0.0208(11) Uani 1 1 d . . . . .
C16 C 0.1593(5) 0.3301(3) 0.1332(4) 0.0289(13) Uani 1 1 d . . . . .
H16A H 0.110792 0.305661 0.086408 0.043 Uiso 1 1 calc R U . . .
H16B H 0.118183 0.320833 0.187706 0.043 Uiso 1 1 calc R U . . .
H16C H 0.241064 0.305419 0.135531 0.043 Uiso 1 1 calc R U . . .
C17 C 0.0415(4) 0.4631(3) 0.1171(3) 0.0271(12) Uani 1 1 d . . . . .
H17A H -0.013570 0.433274 0.078095 0.041 Uiso 1 1 calc R U . . .
H17B H 0.047662 0.519437 0.098004 0.041 Uiso 1 1 calc R U . . .
H17C H 0.008849 0.461645 0.175230 0.041 Uiso 1 1 calc R U . . .
C10 C 0.8616(5) 0.2275(3) 0.3726(4) 0.0275(12) Uani 1 1 d . . . . .
H10A H 0.895549 0.174456 0.358149 0.041 Uiso 1 1 calc R U . . .
H10B H 0.822240 0.224532 0.428530 0.041 Uiso 1 1 calc R U . . .
H10C H 0.927782 0.267646 0.375091 0.041 Uiso 1 1 calc R U . . .
C19 C 0.2751(5) 0.5758(3) 0.2197(4) 0.0255(12) Uani 1 1 d . . . . .
C14 C 0.6454(5) 0.4885(3) 0.4147(4) 0.0311(13) Uani 1 1 d . . . . .
H14A H 0.683174 0.534136 0.445499 0.047 Uiso 1 1 calc R U . . .
H14B H 0.578311 0.466447 0.448566 0.047 Uiso 1 1 calc R U . . .
H14C H 0.612915 0.507162 0.359123 0.047 Uiso 1 1 calc R U . . .
C18 C 0.2339(5) 0.4377(3) 0.0289(3) 0.0289(13) Uani 1 1 d . . . . .
H18A H 0.317062 0.415061 0.030528 0.043 Uiso 1 1 calc R U . . .
H18B H 0.238203 0.495970 0.017420 0.043 Uiso 1 1 calc R U . . .
H18C H 0.185510 0.411246 -0.016676 0.043 Uiso 1 1 calc R U . . .
C20 C 0.3759(5) 0.5938(3) 0.2903(4) 0.0336(14) Uani 1 1 d . . . . .
H20A H 0.457061 0.581001 0.267880 0.050 Uiso 1 1 calc R U . . .
H20B H 0.360794 0.560395 0.340969 0.050 Uiso 1 1 calc R U . . .
H20C H 0.372833 0.651095 0.306160 0.050 Uiso 1 1 calc R U . . .
C12 C 0.7933(5) 0.3907(3) 0.4895(3) 0.0326(13) Uani 1 1 d . . . . .
H12A H 0.862354 0.353657 0.481491 0.049 Uiso 1 1 calc R U . . .
H12B H 0.727390 0.362350 0.519155 0.049 Uiso 1 1 calc R U . . .
H12C H 0.820553 0.437150 0.523953 0.049 Uiso 1 1 calc R U . . .
C22 C 0.3081(5) 0.6187(3) 0.1340(4) 0.0390(15) Uani 1 1 d . . . . .
H22A H 0.325356 0.675946 0.145193 0.059 Uiso 1 1 calc R U . . .
H22B H 0.238979 0.614017 0.093240 0.059 Uiso 1 1 calc R U . . .
H22C H 0.380785 0.592956 0.109900 0.059 Uiso 1 1 calc R U . . .
C21 C 0.1483(5) 0.6072(3) 0.2531(4) 0.0416(16) Uani 1 1 d . . . . .
H21A H 0.154620 0.665022 0.266382 0.062 Uiso 1 1 calc R U . . .
H21B H 0.126637 0.577323 0.304903 0.062 Uiso 1 1 calc R U . . .
H21C H 0.084688 0.598821 0.208698 0.062 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
Ti1 C1 2.199(4) . ?
Ti1 Cl1 2.2963(14) . ?
Ti1 Cl2 2.3215(13) . ?
Ti1 P1 2.5818(14) . ?
Ti1 P2 2.6018(14) . ?
P1 O1 1.641(3) . ?
P1 C7 1.860(4) . ?
P1 C11 1.871(5) . ?
P2 O2 1.640(3) . ?
P2 C15 1.858(5) . ?
P2 C19 1.865(5) . ?
O1 C6 1.401(5) . ?
O2 C2 1.402(5) . ?
C1 C2 1.400(6) . ?
C1 C6 1.412(6) . ?
C2 C3 1.385(6) . ?
C7 C9 1.532(7) . ?
C7 C10 1.538(6) . ?
C7 C8 1.547(6) . ?
C6 C5 1.380(6) . ?
C15 C16 1.533(7) . ?
C15 C17 1.532(6) . ?
C15 C18 1.535(6) . ?
C3 C4 1.383(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.404(6) . ?
C4 H4 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C5 H5 0.9300 . ?
C13 C11 1.536(7) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C11 C12 1.530(7) . ?
C11 C14 1.544(6) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C19 C22 1.529(7) . ?
C19 C20 1.538(7) . ?
C19 C21 1.541(7) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?

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 Ti1 Cl1 117.47(12) . . ?
C1 Ti1 Cl2 140.18(12) . . ?
Cl1 Ti1 Cl2 102.30(5) . . ?
C1 Ti1 P1 72.57(12) . . ?
Cl1 Ti1 P1 105.27(5) . . ?
Cl2 Ti1 P1 96.11(5) . . ?
C1 Ti1 P2 73.02(12) . . ?
Cl1 Ti1 P2 104.40(5) . . ?
Cl2 Ti1 P2 100.12(5) . . ?
P1 Ti1 P2 142.06(5) . . ?
O1 P1 C7 101.74(19) . . ?
O1 P1 C11 101.0(2) . . ?
C7 P1 C11 112.8(2) . . ?
O1 P1 Ti1 104.15(12) . . ?
C7 P1 Ti1 116.93(15) . . ?
C11 P1 Ti1 116.93(15) . . ?
O2 P2 C15 100.36(19) . . ?
O2 P2 C19 100.7(2) . . ?
C15 P2 C19 113.5(2) . . ?
O2 P2 Ti1 104.52(12) . . ?
C15 P2 Ti1 116.99(15) . . ?
C19 P2 Ti1 117.06(16) . . ?
C6 O1 P1 116.2(3) . . ?
C2 O2 P2 117.1(3) . . ?
C2 C1 C6 112.6(4) . . ?
C2 C1 Ti1 123.7(3) . . ?
C6 C1 Ti1 123.0(3) . . ?
C3 C2 C1 125.0(4) . . ?
C3 C2 O2 114.4(4) . . ?
C1 C2 O2 120.6(4) . . ?
C9 C7 C10 110.0(4) . . ?
C9 C7 C8 109.5(4) . . ?
C10 C7 C8 108.5(4) . . ?
C9 C7 P1 108.1(3) . . ?
C10 C7 P1 114.5(3) . . ?
C8 C7 P1 106.1(3) . . ?
C5 C6 O1 114.7(4) . . ?
C5 C6 C1 125.4(4) . . ?
O1 C6 C1 119.9(4) . . ?
C16 C15 C17 109.5(4) . . ?
C16 C15 C18 109.3(4) . . ?
C17 C15 C18 110.0(4) . . ?
C16 C15 P2 105.4(3) . . ?
C17 C15 P2 114.2(3) . . ?
C18 C15 P2 108.3(3) . . ?
C2 C3 C4 119.0(4) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C5 C4 118.0(4) . . ?
C6 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C12 C11 C13 110.6(4) . . ?
C12 C11 C14 108.7(4) . . ?
C13 C11 C14 108.8(4) . . ?
C12 C11 P1 113.8(3) . . ?
C13 C11 P1 110.2(3) . . ?
C14 C11 P1 104.5(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C22 C19 C20 110.2(4) . . ?
C22 C19 C21 110.6(4) . . ?
C20 C19 C21 108.2(4) . . ?
C22 C19 P2 110.1(4) . . ?
C20 C19 P2 104.6(3) . . ?
C21 C19 P2 113.0(4) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

_refine_diff_density_max         0.782
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.132



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

data_exp_3918
_database_code_depnum_ccdc_archive 'CCDC 2161786'
loop_
_audit_author_name
_audit_author_address
'Wenshuang Huang'
;College of Chemistry, Beijing Normal University,
China
;
_audit_update_record             
;
2022-04-25 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;
_audit_creation_date             2022-04-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H57 P2 Si2 Ti'
_chemical_formula_sum            'C32 H57 P2 Si2 Ti'
_chemical_formula_weight         607.79
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H  P Ti Si'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ti Ti 0.2191 1.8069 '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           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   16.1352(2)
_cell_length_b                   13.17667(18)
_cell_length_c                   17.2700(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3671.75(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10628
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.2460
_cell_measurement_theta_min      4.3020
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.542
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13581
_diffrn_reflns_point_group_measured_fraction_full 0.837
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.437
_diffrn_reflns_theta_min         3.354
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00  25.00   0.50    0.10    --   46.95 -23.00-154.00  104
  2  ω    -21.00  12.00   0.50    0.10    --   46.95 -19.00 -30.00   66
  3  ω    -15.00  28.00   0.50    0.10    --   46.95 -19.00  60.00   86
  4  ω     95.00 162.00   0.50    0.50    --  104.75  23.00  10.00  134
  5  ω    -57.00 -32.00   0.50    0.50    -- -102.00  61.00 -60.00   50
  6  ω   -109.00 -32.00   0.50    0.50    -- -102.00 101.00 172.00  154
  7  ω   -116.00 -59.00   0.50    0.50    -- -102.00-144.00-177.00  114
  8  ω   -116.00 -78.00   0.50    0.10    --  -46.95-125.00 -60.00   76
  9  ω     60.00  90.00   0.50    0.10    --   46.95-125.00 -60.00   60
 10  ω     43.00  93.00   0.50    0.50    --  104.75 -77.00  90.00  100
 11  ω     36.00  72.00   0.50    0.50    --  104.75 -61.00 120.00   72
 12  ω     38.00  69.00   0.50    0.50    --  104.75 -61.00 -30.00   62
 13  ω     47.00  72.00   0.50    0.50    --  104.75 -61.00 -60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0830583000
_diffrn_orient_matrix_UB_12      -0.0107509000
_diffrn_orient_matrix_UB_13      0.0431897000
_diffrn_orient_matrix_UB_21      0.0465805000
_diffrn_orient_matrix_UB_22      0.0337748000
_diffrn_orient_matrix_UB_23      -0.0734250000
_diffrn_orient_matrix_UB_31      -0.0061051000
_diffrn_orient_matrix_UB_32      0.1115076000
_diffrn_orient_matrix_UB_33      0.0264149000
_diffrn_oxdiff_digest_frames     
;
01ca102ad8e7877c90162d2f76ee1b6e9b00104edfb
;
_diffrn_oxdiff_digest_hkl        
;
01a03a7c38b437d160dd0a3be3fbfd4073df9f
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.571
_reflns_Friedel_fraction_full    0.662
_reflns_Friedel_fraction_max     0.588
_reflns_number_gt                5838
_reflns_number_total             6009
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 
;
 Flack x determined using 2021 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6009
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0460
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0906P)²+1.2290P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1257
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3534(2) 0.1762(3) 0.4163(2) 0.0151(7) Uani 1 1 d . . . . .
C2 C 0.3049(2) 0.2461(3) 0.4590(2) 0.0183(8) Uani 1 1 d . . . . .
C3 C 0.2596(3) 0.2172(3) 0.5247(2) 0.0224(8) Uani 1 1 d . . . . .
H3 H 0.2278 0.2652 0.5507 0.027 Uiso 1 1 calc R . . . .
C4 C 0.2617(3) 0.1185(3) 0.5512(3) 0.0263(9) Uani 1 1 d . . . . .
H4 H 0.2338 0.1004 0.5962 0.032 Uiso 1 1 calc R . . . .
C5 C 0.3062(2) 0.0465(3) 0.5094(2) 0.0217(8) Uani 1 1 d . . . . .
H5 H 0.3080 -0.0203 0.5266 0.026 Uiso 1 1 calc R . . . .
C6 C 0.3483(2) 0.0738(3) 0.4419(2) 0.0164(7) Uani 1 1 d . . . . .
C7 C 0.3016(3) 0.3583(3) 0.4375(2) 0.0225(8) Uani 1 1 d . . . . .
C8 C 0.3832(2) -0.0120(3) 0.3932(2) 0.0191(7) Uani 1 1 d . . . . .
C9 C 0.2468(2) 0.3469(3) 0.2730(2) 0.0197(8) Uani 1 1 d . . . . .
C10 C 0.1632(3) 0.3774(3) 0.3089(3) 0.0252(9) Uani 1 1 d . . . . .
H10A H 0.1191 0.3584 0.2746 0.038 Uiso 1 1 calc GR . . . .
H10B H 0.1621 0.4495 0.3170 0.038 Uiso 1 1 calc GR . . . .
H10C H 0.1563 0.3434 0.3576 0.038 Uiso 1 1 calc GR . . . .
C11 C 0.2463(3) 0.2311(3) 0.2590(3) 0.0232(8) Uani 1 1 d . . . . .
H11A H 0.2969 0.2114 0.2341 0.035 Uiso 1 1 calc GR . . . .
H11B H 0.2001 0.2136 0.2265 0.035 Uiso 1 1 calc GR . . . .
H11C H 0.2414 0.1965 0.3077 0.035 Uiso 1 1 calc GR . . . .
C12 C 0.2573(3) 0.3966(3) 0.1937(2) 0.0225(8) Uani 1 1 d . . . . .
H12A H 0.2127 0.3761 0.1604 0.034 Uiso 1 1 calc GR . . . .
H12B H 0.3091 0.3758 0.1714 0.034 Uiso 1 1 calc GR . . . .
H12C H 0.2567 0.4691 0.1993 0.034 Uiso 1 1 calc GR . . . .
C13 C 0.3643(3) 0.5166(3) 0.3329(3) 0.0240(8) Uani 1 1 d . . . . .
C14 C 0.2887(3) 0.5872(3) 0.3356(3) 0.0308(9) Uani 1 1 d . . . . .
H14A H 0.3069 0.6561 0.3420 0.046 Uiso 1 1 calc GR . . . .
H14B H 0.2539 0.5686 0.3783 0.046 Uiso 1 1 calc GR . . . .
H14C H 0.2581 0.5812 0.2882 0.046 Uiso 1 1 calc GR . . . .
C15 C 0.4156(3) 0.5370(3) 0.2599(3) 0.0299(10) Uani 1 1 d . . . . .
H15A H 0.4338 0.6063 0.2597 0.045 Uiso 1 1 calc GR . . . .
H15B H 0.3822 0.5245 0.2149 0.045 Uiso 1 1 calc GR . . . .
H15C H 0.4629 0.4929 0.2592 0.045 Uiso 1 1 calc GR . . . .
C16 C 0.4193(4) 0.5420(4) 0.4032(3) 0.0366(12) Uani 1 1 d . . . . .
H16A H 0.3856 0.5455 0.4489 0.055 Uiso 1 1 calc GR . . . .
H16B H 0.4460 0.6061 0.3949 0.055 Uiso 1 1 calc GR . . . .
H16C H 0.4604 0.4900 0.4094 0.055 Uiso 1 1 calc GR . . . .
C17 C 0.4545(3) -0.0519(3) 0.2434(2) 0.0198(8) Uani 1 1 d . . . . .
C18 C 0.3780(3) -0.0080(3) 0.2017(3) 0.0267(9) Uani 1 1 d . . . . .
H18A H 0.3679 -0.0458 0.1551 0.040 Uiso 1 1 calc GR . . . .
H18B H 0.3880 0.0618 0.1889 0.040 Uiso 1 1 calc GR . . . .
H18C H 0.3306 -0.0127 0.2350 0.040 Uiso 1 1 calc GR . . . .
C19 C 0.4356(3) -0.1645(3) 0.2593(3) 0.0278(9) Uani 1 1 d . . . . .
H19A H 0.4843 -0.1971 0.2794 0.042 Uiso 1 1 calc GR . . . .
H19B H 0.4193 -0.1971 0.2119 0.042 Uiso 1 1 calc GR . . . .
H19C H 0.3915 -0.1697 0.2963 0.042 Uiso 1 1 calc GR . . . .
C20 C 0.5295(3) -0.0436(3) 0.1900(3) 0.0266(9) Uani 1 1 d . . . . .
H20A H 0.5166 -0.0736 0.1408 0.040 Uiso 1 1 calc GR . . . .
H20B H 0.5757 -0.0785 0.2128 0.040 Uiso 1 1 calc GR . . . .
H20C H 0.5434 0.0266 0.1828 0.040 Uiso 1 1 calc GR . . . .
C21 C 0.5633(2) -0.0167(3) 0.3902(2) 0.0198(8) Uani 1 1 d . . . . .
C22 C 0.5514(3) 0.0252(3) 0.4729(3) 0.0253(9) Uani 1 1 d . . . . .
H22A H 0.6002 0.0116 0.5030 0.038 Uiso 1 1 calc GR . . . .
H22B H 0.5045 -0.0071 0.4966 0.038 Uiso 1 1 calc GR . . . .
H22C H 0.5422 0.0971 0.4706 0.038 Uiso 1 1 calc GR . . . .
C23 C 0.5739(3) -0.1329(3) 0.3949(3) 0.0252(9) Uani 1 1 d . . . . .
H23A H 0.5230 -0.1632 0.4121 0.038 Uiso 1 1 calc GR . . . .
H23B H 0.6174 -0.1489 0.4309 0.038 Uiso 1 1 calc GR . . . .
H23C H 0.5880 -0.1589 0.3447 0.038 Uiso 1 1 calc GR . . . .
C24 C 0.6434(3) 0.0294(3) 0.3567(3) 0.0277(9) Uani 1 1 d . . . . .
H24A H 0.6897 0.0099 0.3883 0.042 Uiso 1 1 calc GR . . . .
H24B H 0.6389 0.1020 0.3560 0.042 Uiso 1 1 calc GR . . . .
H24C H 0.6516 0.0049 0.3049 0.042 Uiso 1 1 calc GR . . . .
C25 C 0.4768(3) 0.2535(3) 0.2087(2) 0.0201(8) Uani 1 1 d . . . . .
C26 C 0.5546(2) 0.3081(3) 0.3872(3) 0.0214(8) Uani 1 1 d . . . . .
C27 C 0.5978(3) 0.4168(3) 0.1530(3) 0.0323(10) Uani 1 1 d . . . . .
H27A H 0.6074 0.4422 0.2044 0.048 Uiso 1 1 calc GR . . . .
H27B H 0.5514 0.4516 0.1305 0.048 Uiso 1 1 calc GR . . . .
H27C H 0.6462 0.4281 0.1218 0.048 Uiso 1 1 calc GR . . . .
C28 C 0.5691(3) 0.2322(4) 0.0550(3) 0.0289(10) Uani 1 1 d . . . . .
H28A H 0.5231 0.2643 0.0296 0.043 Uiso 1 1 calc GR . . . .
H28B H 0.5615 0.1599 0.0542 0.043 Uiso 1 1 calc GR . . . .
H28C H 0.6195 0.2493 0.0284 0.043 Uiso 1 1 calc GR . . . .
C29 C 0.6698(3) 0.2134(4) 0.1995(3) 0.0326(10) Uani 1 1 d . . . . .
H29A H 0.6643 0.1411 0.1946 0.049 Uiso 1 1 calc GR . . . .
H29B H 0.6750 0.2311 0.2532 0.049 Uiso 1 1 calc GR . . . .
H29C H 0.7182 0.2355 0.1719 0.049 Uiso 1 1 calc GR . . . .
C30 C 0.6086(4) 0.4703(4) 0.5095(3) 0.0363(11) Uani 1 1 d . . . . .
H30A H 0.5607 0.5127 0.5032 0.054 Uiso 1 1 calc GR . . . .
H30B H 0.6507 0.4906 0.4735 0.054 Uiso 1 1 calc GR . . . .
H30C H 0.6294 0.4769 0.5614 0.054 Uiso 1 1 calc GR . . . .
C31 C 0.4924(3) 0.3050(3) 0.5599(3) 0.0298(9) Uani 1 1 d . . . . .
H31A H 0.4732 0.2369 0.5516 0.045 Uiso 1 1 calc GR . . . .
H31B H 0.4477 0.3517 0.5513 0.045 Uiso 1 1 calc GR . . . .
H31C H 0.5119 0.3117 0.6122 0.045 Uiso 1 1 calc GR . . . .
C32 C 0.6723(3) 0.2566(4) 0.5212(3) 0.0409(12) Uani 1 1 d . . . . .
H32A H 0.7186 0.2736 0.4889 0.061 Uiso 1 1 calc GR . . . .
H32B H 0.6600 0.1857 0.5160 0.061 Uiso 1 1 calc GR . . . .
H32C H 0.6856 0.2714 0.5742 0.061 Uiso 1 1 calc GR . . . .
Si1 Si 0.57528(7) 0.27706(8) 0.15768(6) 0.0190(2) Uani 1 1 d . . . . .
Si2 Si 0.57920(7) 0.33359(9) 0.49096(7) 0.0236(3) Uani 1 1 d . . . . .
P1 P 0.33908(5) 0.37616(6) 0.33802(6) 0.0167(2) Uani 1 1 d . . . . .
P2 P 0.47110(5) 0.02806(6) 0.33339(6) 0.0150(2) Uani 1 1 d . . . . .
Ti1 Ti 0.45228(4) 0.23264(4) 0.33372(4) 0.01371(17) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.415(5) . ?
C1 C6 1.423(5) . ?
C1 Ti1 2.265(4) . ?
C2 C3 1.402(6) . ?
C2 C7 1.526(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.379(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.392(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.396(5) . ?
C6 C8 1.518(5) . ?
C7 P1 1.835(4) . ?
C8 P2 1.832(4) . ?
C9 C10 1.537(5) . ?
C9 C11 1.545(5) . ?
C9 C12 1.527(6) . ?
C9 P1 1.905(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.534(6) . ?
C13 C15 1.533(7) . ?
C13 C16 1.539(6) . ?
C13 P1 1.897(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.541(6) . ?
C17 C19 1.539(5) . ?
C17 C20 1.526(6) . ?
C17 P2 1.897(4) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.543(6) . ?
C21 C23 1.543(5) . ?
C21 C24 1.542(6) . ?
C21 P2 1.877(4) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 Si1 1.843(4) . ?
C25 Ti1 2.213(4) . ?
C26 Si2 1.867(4) . ?
C26 Ti1 2.136(4) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C27 Si1 1.879(4) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C28 Si1 1.873(5) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C29 Si1 1.884(5) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C30 Si2 1.890(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C31 Si2 1.876(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C32 Si2 1.886(5) . ?
P1 Ti1 2.6302(10) . ?
P2 Ti1 2.7128(10) . ?

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
C2 C1 C6 115.0(3) . . ?
C2 C1 Ti1 120.3(3) . . ?
C6 C1 Ti1 123.2(3) . . ?
C1 C2 C7 121.5(3) . . ?
C3 C2 C1 122.3(4) . . ?
C3 C2 C7 116.2(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.7(4) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 118.9(4) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.6(4) . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C8 120.9(3) . . ?
C5 C6 C1 122.2(4) . . ?
C5 C6 C8 116.8(3) . . ?
C2 C7 P1 109.9(3) . . ?
C6 C8 P2 112.7(3) . . ?
C10 C9 C11 108.4(3) . . ?
C10 C9 P1 113.3(3) . . ?
C11 C9 P1 107.2(3) . . ?
C12 C9 C10 110.3(3) . . ?
C12 C9 C11 106.5(3) . . ?
C12 C9 P1 110.8(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C16 107.6(4) . . ?
C14 C13 P1 114.8(3) . . ?
C15 C13 C14 110.4(4) . . ?
C15 C13 C16 107.4(4) . . ?
C15 C13 P1 108.9(3) . . ?
C16 C13 P1 107.4(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 P2 106.7(3) . . ?
C19 C17 C18 106.7(3) . . ?
C19 C17 P2 114.7(3) . . ?
C20 C17 C18 109.0(3) . . ?
C20 C17 C19 109.5(3) . . ?
C20 C17 P2 110.1(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C23 108.6(3) . . ?
C22 C21 P2 105.9(3) . . ?
C23 C21 P2 115.3(3) . . ?
C24 C21 C22 108.1(4) . . ?
C24 C21 C23 108.5(3) . . ?
C24 C21 P2 110.2(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si1 C25 Ti1 129.9(2) . . ?
Si2 C26 Ti1 131.5(2) . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si1 C27 H27A 109.5 . . ?
Si1 C27 H27B 109.5 . . ?
Si1 C27 H27C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si1 C28 H28A 109.5 . . ?
Si1 C28 H28B 109.5 . . ?
Si1 C28 H28C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si1 C29 H29A 109.5 . . ?
Si1 C29 H29B 109.5 . . ?
Si1 C29 H29C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si2 C30 H30A 109.5 . . ?
Si2 C30 H30B 109.5 . . ?
Si2 C30 H30C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si2 C31 H31A 109.5 . . ?
Si2 C31 H31B 109.5 . . ?
Si2 C31 H31C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si2 C32 H32A 109.5 . . ?
Si2 C32 H32B 109.5 . . ?
Si2 C32 H32C 109.5 . . ?
C25 Si1 C27 110.6(2) . . ?
C25 Si1 C28 110.7(2) . . ?
C25 Si1 C29 116.08(19) . . ?
C27 Si1 C29 107.2(2) . . ?
C28 Si1 C27 106.2(2) . . ?
C28 Si1 C29 105.4(2) . . ?
C26 Si2 C30 112.8(2) . . ?
C26 Si2 C31 114.47(19) . . ?
C26 Si2 C32 109.8(2) . . ?
C31 Si2 C30 105.7(2) . . ?
C31 Si2 C32 108.1(2) . . ?
C32 Si2 C30 105.4(3) . . ?
C7 P1 C9 105.57(19) . . ?
C7 P1 C13 103.8(2) . . ?
C7 P1 Ti1 99.39(13) . . ?
C9 P1 Ti1 112.40(12) . . ?
C13 P1 C9 109.74(18) . . ?
C13 P1 Ti1 123.44(13) . . ?
C8 P2 C17 101.11(18) . . ?
C8 P2 C21 103.17(18) . . ?
C8 P2 Ti1 101.45(12) . . ?
C17 P2 Ti1 122.55(13) . . ?
C21 P2 C17 111.46(18) . . ?
C21 P2 Ti1 113.57(13) . . ?
C1 Ti1 P1 74.27(9) . . ?
C1 Ti1 P2 75.77(9) . . ?
C25 Ti1 C1 141.35(15) . . ?
C25 Ti1 P1 93.57(11) . . ?
C25 Ti1 P2 95.82(11) . . ?
C26 Ti1 C1 115.15(15) . . ?
C26 Ti1 C25 103.05(16) . . ?
C26 Ti1 P1 100.94(12) . . ?
C26 Ti1 P2 112.14(12) . . ?
P1 Ti1 P2 142.39(4) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.836
_oxdiff_exptl_absorpt_empirical_full_min 0.598
####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2169339'
loop_
_audit_author_name
_audit_author_address
'Jiayu Zhang'
;College of Chemistry, Beijing Normal University,
China
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H43 Cl2 P2 Ti'
_chemical_formula_weight         512.32

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'
P P 0.1023 0.0942 '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'

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

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

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

_cell_length_a                   12.1470(7)
_cell_length_b                   15.8810(7)
_cell_length_c                   14.4631(11)
_cell_angle_alpha                90
_cell_angle_beta                 105.389(7)
_cell_angle_gamma                90
_cell_volume                     2690.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8828
_cell_measurement_theta_min      3.8840
_cell_measurement_theta_max      29.6780

_exptl_crystal_description       Block
_exptl_crystal_colour            Purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_F_000             1092
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.645
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  Rigaku
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18427
_diffrn_reflns_av_unetI/netI     0.1057
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.479
_diffrn_reflns_theta_max         29.747
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6450
_reflns_number_gt                4764
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0847P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6450
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1703
_refine_ls_wR_factor_gt          0.1369
_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
Ti1 Ti 0.11207(4) 0.45916(3) 0.28145(4) 0.01170(15) Uani 1 1 d . . . . .
Cl2 Cl 0.19659(6) 0.56118(4) 0.39171(6) 0.0212(2) Uani 1 1 d . . . . .
Cl1 Cl 0.09310(6) 0.52626(4) 0.13595(6) 0.02081(19) Uani 1 1 d . . . . .
P1 P -0.10312(5) 0.47347(4) 0.27004(5) 0.01024(18) Uani 1 1 d . . . . .
P2 P 0.28426(6) 0.35694(4) 0.28587(5) 0.01178(18) Uani 1 1 d . . . . .
C13 C -0.1948(2) 0.41418(16) 0.1636(2) 0.0149(6) Uani 1 1 d . . . . .
C4 C 0.0010(2) 0.18779(17) 0.4177(2) 0.0172(6) Uani 1 1 d . . . . .
H4 H -0.016673 0.139080 0.446489 0.021 Uiso 1 1 calc R U . . .
C5 C 0.0908(2) 0.18847(16) 0.3744(2) 0.0172(6) Uani 1 1 d . . . . .
H5 H 0.131967 0.139383 0.372677 0.021 Uiso 1 1 calc R U . . .
C9 C -0.1706(2) 0.57688(16) 0.2869(2) 0.0128(6) Uani 1 1 d . . . . .
C2 C -0.0327(2) 0.33485(17) 0.3768(2) 0.0126(6) Uani 1 1 d . . . . .
C3 C -0.0614(2) 0.26097(17) 0.4172(2) 0.0169(6) Uani 1 1 d . . . . .
H3 H -0.123028 0.260819 0.444094 0.020 Uiso 1 1 calc R U . . .
C17 C 0.3410(2) 0.35602(17) 0.1775(2) 0.0141(6) Uani 1 1 d . . . . .
C7 C -0.1059(2) 0.41147(17) 0.3763(2) 0.0156(6) Uani 1 1 d . . . . .
H7A H -0.076090 0.444401 0.433991 0.019 Uiso 1 1 calc R U . . .
H7B H -0.183481 0.394837 0.373578 0.019 Uiso 1 1 calc R U . . .
C1 C 0.0604(2) 0.33884(16) 0.3357(2) 0.0133(6) Uani 1 1 d . . . . .
C12 C -0.2984(2) 0.57092(18) 0.2812(2) 0.0191(6) Uani 1 1 d . . . . .
H12A H -0.326653 0.625672 0.291318 0.029 Uiso 1 1 calc R U . . .
H12B H -0.309296 0.532986 0.329733 0.029 Uiso 1 1 calc R U . . .
H12C H -0.339110 0.550388 0.219162 0.029 Uiso 1 1 calc R U . . .
C20 C 0.4338(2) 0.28968(17) 0.1827(2) 0.0201(6) Uani 1 1 d . . . . .
H20A H 0.407029 0.235959 0.198171 0.030 Uiso 1 1 calc R U . . .
H20B H 0.501200 0.305218 0.231426 0.030 Uiso 1 1 calc R U . . .
H20C H 0.451306 0.286219 0.121913 0.030 Uiso 1 1 calc R U . . .
C6 C 0.1193(2) 0.26179(17) 0.3337(2) 0.0148(6) Uani 1 1 d . . . . .
C15 C -0.2972(3) 0.37162(18) 0.1862(2) 0.0224(7) Uani 1 1 d . . . . .
H15A H -0.341713 0.343305 0.130054 0.034 Uiso 1 1 calc R U . . .
H15B H -0.343466 0.413336 0.206041 0.034 Uiso 1 1 calc R U . . .
H15C H -0.270942 0.331454 0.236906 0.034 Uiso 1 1 calc R U . . .
C23 C 0.4624(3) 0.2646(2) 0.4185(3) 0.0346(9) Uani 1 1 d . . . . .
H23A H 0.500173 0.253844 0.369216 0.052 Uiso 1 1 calc R U . . .
H23B H 0.406614 0.221478 0.417257 0.052 Uiso 1 1 calc R U . . .
H23C H 0.517471 0.264699 0.479890 0.052 Uiso 1 1 calc R U . . .
C10 C -0.1080(2) 0.60992(18) 0.3864(2) 0.0190(6) Uani 1 1 d . . . . .
H10A H -0.027137 0.607769 0.393980 0.028 Uiso 1 1 calc R U . . .
H10B H -0.127093 0.575655 0.434582 0.028 Uiso 1 1 calc R U . . .
H10C H -0.130655 0.667050 0.392933 0.028 Uiso 1 1 calc R U . . .
C8 C 0.2094(2) 0.25592(17) 0.2796(3) 0.0206(7) Uani 1 1 d . . . . .
H8A H 0.174032 0.241623 0.213108 0.025 Uiso 1 1 calc R U . . .
H8B H 0.263501 0.211882 0.307141 0.025 Uiso 1 1 calc R U . . .
C11 C -0.1509(2) 0.63966(16) 0.2126(2) 0.0171(6) Uani 1 1 d . . . . .
H11A H -0.177122 0.694385 0.225333 0.026 Uiso 1 1 calc R U . . .
H11B H -0.192443 0.621761 0.149560 0.026 Uiso 1 1 calc R U . . .
H11C H -0.070945 0.642220 0.216196 0.026 Uiso 1 1 calc R U . . .
C19 C 0.3858(2) 0.44435(17) 0.1630(2) 0.0187(6) Uani 1 1 d . . . . .
H19A H 0.411206 0.444974 0.105578 0.028 Uiso 1 1 calc R U . . .
H19B H 0.448431 0.458343 0.216950 0.028 Uiso 1 1 calc R U . . .
H19C H 0.325720 0.484839 0.157525 0.028 Uiso 1 1 calc R U . . .
C14 C -0.2368(3) 0.47351(17) 0.0779(2) 0.0219(7) Uani 1 1 d . . . . .
H14A H -0.276164 0.441557 0.022655 0.033 Uiso 1 1 calc R U . . .
H14B H -0.172747 0.501768 0.064807 0.033 Uiso 1 1 calc R U . . .
H14C H -0.287942 0.514388 0.092572 0.033 Uiso 1 1 calc R U . . .
C16 C -0.1236(3) 0.34565(18) 0.1312(3) 0.0243(7) Uani 1 1 d . . . . .
H16A H -0.101068 0.303952 0.180725 0.036 Uiso 1 1 calc R U . . .
H16B H -0.056771 0.370648 0.119193 0.036 Uiso 1 1 calc R U . . .
H16C H -0.168443 0.319579 0.073634 0.036 Uiso 1 1 calc R U . . .
C21 C 0.4026(2) 0.35100(19) 0.4009(2) 0.0195(6) Uani 1 1 d . . . . .
C24 C 0.4906(3) 0.4201(2) 0.4027(2) 0.0281(8) Uani 1 1 d . . . . .
H24A H 0.541410 0.424118 0.465919 0.042 Uiso 1 1 calc R U . . .
H24B H 0.452163 0.472955 0.385610 0.042 Uiso 1 1 calc R U . . .
H24C H 0.533538 0.406767 0.357651 0.042 Uiso 1 1 calc R U . . .
C18 C 0.2416(3) 0.33603(19) 0.0898(2) 0.0237(7) Uani 1 1 d . . . . .
H18A H 0.265076 0.345505 0.032308 0.036 Uiso 1 1 calc R U . . .
H18B H 0.177947 0.371861 0.089918 0.036 Uiso 1 1 calc R U . . .
H18C H 0.219445 0.278219 0.092314 0.036 Uiso 1 1 calc R U . . .
C22 C 0.3484(3) 0.36606(19) 0.4834(2) 0.0222(7) Uani 1 1 d . . . . .
H22A H 0.405645 0.361234 0.543389 0.033 Uiso 1 1 calc R U . . .
H22B H 0.289681 0.324949 0.480887 0.033 Uiso 1 1 calc R U . . .
H22C H 0.315630 0.421461 0.477914 0.033 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
Ti1 C1 2.218(3) . ?
Ti1 Cl2 2.3138(8) . ?
Ti1 Cl1 2.3151(9) . ?
Ti1 P1 2.5851(8) . ?
Ti1 P2 2.6349(8) . ?
P1 C7 1.833(3) . ?
P1 C9 1.880(3) . ?
P1 C13 1.894(3) . ?
P2 C8 1.835(3) . ?
P2 C17 1.873(3) . ?
P2 C21 1.891(3) . ?
C13 C15 1.526(4) . ?
C13 C14 1.532(4) . ?
C13 C16 1.538(4) . ?
C4 C3 1.387(4) . ?
C4 C5 1.395(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.389(4) . ?
C5 H5 0.9300 . ?
C9 C11 1.531(4) . ?
C9 C10 1.530(4) . ?
C9 C12 1.536(4) . ?
C2 C3 1.396(4) . ?
C2 C1 1.413(4) . ?
C2 C7 1.506(4) . ?
C3 H3 0.9300 . ?
C17 C20 1.530(4) . ?
C17 C18 1.534(4) . ?
C17 C19 1.539(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C1 C6 1.421(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C6 C8 1.508(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C23 C21 1.541(4) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C21 C24 1.528(4) . ?
C21 C22 1.528(4) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?

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 Ti1 Cl2 118.35(8) . . ?
C1 Ti1 Cl1 138.47(8) . . ?
Cl2 Ti1 Cl1 102.89(3) . . ?
C1 Ti1 P1 73.88(7) . . ?
Cl2 Ti1 P1 103.81(3) . . ?
Cl1 Ti1 P1 92.66(3) . . ?
C1 Ti1 P2 75.99(7) . . ?
Cl2 Ti1 P2 102.15(3) . . ?
Cl1 Ti1 P2 101.10(3) . . ?
P1 Ti1 P2 146.97(3) . . ?
C7 P1 C9 104.78(13) . . ?
C7 P1 C13 106.08(13) . . ?
C9 P1 C13 110.93(12) . . ?
C7 P1 Ti1 98.17(9) . . ?
C9 P1 Ti1 122.46(8) . . ?
C13 P1 Ti1 112.00(9) . . ?
C8 P2 C17 103.84(13) . . ?
C8 P2 C21 104.55(15) . . ?
C17 P2 C21 111.94(13) . . ?
C8 P2 Ti1 99.08(9) . . ?
C17 P2 Ti1 116.78(9) . . ?
C21 P2 Ti1 117.74(10) . . ?
C15 C13 C14 109.3(2) . . ?
C15 C13 C16 108.0(2) . . ?
C14 C13 C16 106.4(3) . . ?
C15 C13 P1 112.5(2) . . ?
C14 C13 P1 110.46(18) . . ?
C16 C13 P1 110.00(19) . . ?
C3 C4 C5 118.9(3) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 120.6(3) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C11 C9 C10 107.8(2) . . ?
C11 C9 C12 110.3(2) . . ?
C10 C9 C12 108.3(2) . . ?
C11 C9 P1 108.87(19) . . ?
C10 C9 P1 107.26(18) . . ?
C12 C9 P1 114.12(18) . . ?
C3 C2 C1 122.1(3) . . ?
C3 C2 C7 118.0(2) . . ?
C1 C2 C7 119.9(2) . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C20 C17 C18 107.9(2) . . ?
C20 C17 C19 110.6(2) . . ?
C18 C17 C19 107.8(2) . . ?
C20 C17 P2 113.2(2) . . ?
C18 C17 P2 108.0(2) . . ?
C19 C17 P2 109.17(19) . . ?
C2 C7 P1 107.3(2) . . ?
C2 C7 H7A 110.3 . . ?
P1 C7 H7A 110.3 . . ?
C2 C7 H7B 110.3 . . ?
P1 C7 H7B 110.3 . . ?
H7A C7 H7B 108.5 . . ?
C2 C1 C6 115.7(2) . . ?
C2 C1 Ti1 121.39(19) . . ?
C6 C1 Ti1 122.9(2) . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C5 C6 C1 122.0(3) . . ?
C5 C6 C8 117.7(2) . . ?
C1 C6 C8 120.1(2) . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C8 P2 109.79(19) . . ?
C6 C8 H8A 109.7 . . ?
P2 C8 H8A 109.7 . . ?
C6 C8 H8B 109.7 . . ?
P2 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C24 C21 C22 108.6(3) . . ?
C24 C21 C23 109.9(3) . . ?
C22 C21 C23 107.0(3) . . ?
C24 C21 P2 110.1(2) . . ?
C22 C21 P2 107.1(2) . . ?
C23 C21 P2 113.8(2) . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_refine_diff_density_max         0.752
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.147



####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2161776'
loop_
_audit_author_name
_audit_author_address
'Jiayu Zhang'
;College of Chemistry, Beijing Normal University,
China
;
_audit_update_record             
;
2022-04-25 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H61 O2 P2 Sc Si2'
_chemical_formula_weight         616.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

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

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

_cell_length_a                   16.3488(9)
_cell_length_b                   13.2688(8)
_cell_length_c                   16.9093(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3668.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5959
_cell_measurement_theta_min      3.9240
_cell_measurement_theta_max      28.9270

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.376
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  Rigku
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15172
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.165
_diffrn_reflns_theta_max         29.876
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.710
_diffrn_reflns_point_group_measured_fraction_full 0.886
_reflns_number_total             7508
_reflns_number_gt                6627
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.624
_reflns_Friedel_fraction_max     0.564
_reflns_Friedel_fraction_full    0.767

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0472P)²+1.9836P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.28(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7508
_refine_ls_number_parameters     353
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.1014
_refine_ls_wR_factor_gt          0.0946
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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
Sc1 Sc 0.54181(4) 0.73576(4) 0.47351(4) 0.01534(14) Uani 1 1 d . . . . .
P1 P 0.67107(5) 0.86920(6) 0.46912(6) 0.01734(18) Uani 1 1 d . . . . .
P2 P 0.52730(5) 0.52817(7) 0.45417(6) 0.0197(2) Uani 1 1 d . . . . .
Si1 Si 0.42259(7) 0.77234(9) 0.65294(7) 0.0263(3) Uani 1 1 d . . . . .
Si2 Si 0.42560(7) 0.84664(10) 0.30323(7) 0.0314(3) Uani 1 1 d . . . . .
O1 O 0.71141(16) 0.8411(2) 0.38288(15) 0.0241(6) Uani 1 1 d . . . . .
O2 O 0.59496(17) 0.5039(2) 0.38542(17) 0.0270(6) Uani 1 1 d . . . . .
C6 C 0.6986(2) 0.7428(3) 0.3530(2) 0.0181(7) Uani 1 1 d . . . . .
C1 C 0.6436(2) 0.6773(3) 0.3895(2) 0.0167(7) Uani 1 1 d . . . . .
C2 C 0.6429(2) 0.5821(3) 0.3547(2) 0.0210(8) Uani 1 1 d . . . . .
C23 C 0.4429(2) 0.8163(3) 0.4094(2) 0.0248(8) Uani 1 1 d . . . . .
H26A H 0.393516 0.780871 0.424977 0.030 Uiso 1 1 calc R U . . .
H26B H 0.439961 0.881235 0.435587 0.030 Uiso 1 1 calc R U . . .
C7 C 0.7579(2) 0.8475(3) 0.5385(2) 0.0197(7) Uani 1 1 d . . . . .
C8 C 0.7595(2) 0.7335(3) 0.5550(2) 0.0229(8) Uani 1 1 d . . . . .
H8A H 0.802653 0.718517 0.591665 0.034 Uiso 1 1 calc R U . . .
H8B H 0.768795 0.697781 0.506466 0.034 Uiso 1 1 calc R U . . .
H8C H 0.708044 0.713059 0.577187 0.034 Uiso 1 1 calc R U . . .
C10 C 0.7428(2) 0.9020(3) 0.6169(2) 0.0244(8) Uani 1 1 d . . . . .
H10A H 0.688991 0.886224 0.635798 0.037 Uiso 1 1 calc R U . . .
H10B H 0.747449 0.973400 0.608943 0.037 Uiso 1 1 calc R U . . .
H10C H 0.782682 0.880522 0.655020 0.037 Uiso 1 1 calc R U . . .
C27 C 0.5196(2) 0.7392(3) 0.6047(2) 0.0223(8) Uani 1 1 d . . . . .
H30A H 0.533637 0.672575 0.623925 0.027 Uiso 1 1 calc R U . . .
H30B H 0.560164 0.784823 0.626313 0.027 Uiso 1 1 calc R U . . .
C11 C 0.6506(2) 1.0064(3) 0.4567(3) 0.0268(8) Uani 1 1 d . . . . .
C19 C 0.4322(2) 0.4811(3) 0.4061(3) 0.0287(9) Uani 1 1 d . . . . .
C9 C 0.8406(2) 0.8772(3) 0.5026(3) 0.0265(9) Uani 1 1 d . . . . .
H9A H 0.842135 0.948828 0.494434 0.040 Uiso 1 1 calc R U . . .
H9B H 0.847705 0.843480 0.452812 0.040 Uiso 1 1 calc R U . . .
H9C H 0.883836 0.858018 0.537929 0.040 Uiso 1 1 calc R U . . .
C5 C 0.7457(2) 0.7204(3) 0.2870(2) 0.0248(8) Uani 1 1 d . . . . .
H5 H 0.780599 0.768266 0.265236 0.030 Uiso 1 1 calc R U . . .
C3 C 0.6881(2) 0.5545(3) 0.2883(2) 0.0254(8) Uani 1 1 d . . . . .
H3 H 0.683848 0.489966 0.267207 0.030 Uiso 1 1 calc R U . . .
C4 C 0.7393(3) 0.6254(3) 0.2546(2) 0.0273(9) Uani 1 1 d . . . . .
H4 H 0.769606 0.608943 0.209845 0.033 Uiso 1 1 calc R U . . .
C17 C 0.6408(3) 0.4942(3) 0.5684(3) 0.0290(9) Uani 1 1 d . . . . .
H17A H 0.626273 0.558765 0.589841 0.043 Uiso 1 1 calc R U . . .
H17B H 0.680503 0.503061 0.527108 0.043 Uiso 1 1 calc R U . . .
H17C H 0.663634 0.452857 0.609432 0.043 Uiso 1 1 calc R U . . .
C13 C 0.7255(3) 1.0762(3) 0.4549(3) 0.0371(11) Uani 1 1 d . . . . .
H13A H 0.708083 1.144155 0.445230 0.056 Uiso 1 1 calc R U . . .
H13B H 0.761914 1.055094 0.413570 0.056 Uiso 1 1 calc R U . . .
H13C H 0.753327 1.072886 0.504847 0.056 Uiso 1 1 calc R U . . .
C30 C 0.4208(3) 0.7397(3) 0.7607(3) 0.0347(10) Uani 1 1 d . . . . .
H29A H 0.427356 0.668222 0.766927 0.052 Uiso 1 1 calc R U . . .
H29B H 0.369440 0.760086 0.783154 0.052 Uiso 1 1 calc R U . . .
H29C H 0.464569 0.773983 0.787253 0.052 Uiso 1 1 calc R U . . .
C15 C 0.5641(2) 0.4429(3) 0.5344(2) 0.0256(8) Uani 1 1 d . . . . .
C25 C 0.5153(3) 0.8134(4) 0.2385(3) 0.0365(10) Uani 1 1 d . . . . .
H23A H 0.561745 0.853246 0.253517 0.055 Uiso 1 1 calc R U . . .
H23B H 0.501774 0.826641 0.184253 0.055 Uiso 1 1 calc R U . . .
H23C H 0.528071 0.743189 0.244755 0.055 Uiso 1 1 calc R U . . .
C22 C 0.3586(2) 0.5236(3) 0.4512(3) 0.0365(10) Uani 1 1 d . . . . .
H22A H 0.308930 0.500975 0.426646 0.055 Uiso 1 1 calc R U . . .
H22B H 0.360535 0.595891 0.450278 0.055 Uiso 1 1 calc R U . . .
H22C H 0.360148 0.500543 0.505023 0.055 Uiso 1 1 calc R U . . .
C21 C 0.4335(3) 0.5258(4) 0.3228(3) 0.0380(11) Uani 1 1 d . . . . .
H21A H 0.475889 0.494131 0.292432 0.057 Uiso 1 1 calc R U . . .
H21B H 0.443790 0.596936 0.325962 0.057 Uiso 1 1 calc R U . . .
H21C H 0.381596 0.514493 0.297782 0.057 Uiso 1 1 calc R U . . .
C16 C 0.5900(3) 0.3379(3) 0.5051(3) 0.0417(12) Uani 1 1 d . . . . .
H16A H 0.619997 0.303971 0.545962 0.063 Uiso 1 1 calc R U . . .
H16B H 0.623974 0.344914 0.459081 0.063 Uiso 1 1 calc R U . . .
H16C H 0.542234 0.299382 0.491837 0.063 Uiso 1 1 calc R U . . .
C24 C 0.4027(3) 0.9839(4) 0.2863(3) 0.0429(12) Uani 1 1 d . . . . .
H25A H 0.351002 1.000416 0.309795 0.064 Uiso 1 1 calc R U . . .
H25B H 0.400618 0.997069 0.230504 0.064 Uiso 1 1 calc R U . . .
H25C H 0.444929 1.024192 0.309920 0.064 Uiso 1 1 calc R U . . .
C14 C 0.5925(3) 1.0378(3) 0.5232(3) 0.0399(12) Uani 1 1 d . . . . .
H14A H 0.620245 1.032526 0.573045 0.060 Uiso 1 1 calc R U . . .
H14B H 0.545561 0.994363 0.523201 0.060 Uiso 1 1 calc R U . . .
H14C H 0.575356 1.106172 0.514977 0.060 Uiso 1 1 calc R U . . .
C18 C 0.4996(3) 0.4344(3) 0.5991(3) 0.0350(10) Uani 1 1 d . . . . .
H18A H 0.523035 0.402488 0.644752 0.053 Uiso 1 1 calc R U . . .
H18B H 0.454462 0.394812 0.580228 0.053 Uiso 1 1 calc R U . . .
H18C H 0.480585 0.500469 0.613141 0.053 Uiso 1 1 calc R U . . .
C20 C 0.4237(3) 0.3668(3) 0.4005(3) 0.0358(10) Uani 1 1 d . . . . .
H20A H 0.418145 0.338994 0.452676 0.054 Uiso 1 1 calc R U . . .
H20B H 0.471528 0.339134 0.375661 0.054 Uiso 1 1 calc R U . . .
H20C H 0.376261 0.350270 0.369747 0.054 Uiso 1 1 calc R U . . .
C12 C 0.6063(3) 1.0154(3) 0.3772(3) 0.0470(13) Uani 1 1 d . . . . .
H12A H 0.561007 0.969423 0.376036 0.071 Uiso 1 1 calc R U . . .
H12B H 0.643597 0.999308 0.335185 0.071 Uiso 1 1 calc R U . . .
H12C H 0.586714 1.083034 0.370596 0.071 Uiso 1 1 calc R U . . .
C29 C 0.4055(3) 0.9113(4) 0.6461(3) 0.0488(14) Uani 1 1 d . . . . .
H28A H 0.451462 0.946109 0.668536 0.073 Uiso 1 1 calc R U . . .
H28B H 0.356809 0.928917 0.674721 0.073 Uiso 1 1 calc R U . . .
H28C H 0.399413 0.930276 0.591670 0.073 Uiso 1 1 calc R U . . .
C28 C 0.3325(3) 0.7057(5) 0.6089(3) 0.0584(17) Uani 1 1 d . . . . .
H27A H 0.326927 0.724593 0.554319 0.088 Uiso 1 1 calc R U . . .
H27B H 0.283822 0.724088 0.637134 0.088 Uiso 1 1 calc R U . . .
H27C H 0.340550 0.634154 0.612503 0.088 Uiso 1 1 calc R U . . .
C26 C 0.3347(3) 0.7770(5) 0.2631(4) 0.0612(17) Uani 1 1 d . . . . .
H24A H 0.342378 0.705907 0.270548 0.092 Uiso 1 1 calc R U . . .
H24B H 0.329003 0.791200 0.207712 0.092 Uiso 1 1 calc R U . . .
H24C H 0.286303 0.798300 0.290536 0.092 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
Sc1 C23 2.221(4) . ?
Sc1 C27 2.248(4) . ?
Sc1 C1 2.320(4) . ?
Sc1 P1 2.7579(10) . ?
Sc1 P2 2.7840(11) . ?
P1 O1 1.643(3) . ?
P1 C11 1.863(4) . ?
P1 C7 1.864(4) . ?
P2 O2 1.637(3) . ?
P2 C19 1.863(4) . ?
P2 C15 1.866(4) . ?
Si1 C27 1.836(4) . ?
Si1 C29 1.869(5) . ?
Si1 C28 1.873(5) . ?
Si1 C30 1.873(5) . ?
Si2 C23 1.862(4) . ?
Si2 C26 1.876(5) . ?
Si2 C24 1.881(5) . ?
Si2 C25 1.882(5) . ?
O1 C6 1.414(4) . ?
O2 C2 1.400(5) . ?
C6 C5 1.388(5) . ?
C6 C1 1.394(5) . ?
C1 C2 1.394(5) . ?
C2 C3 1.393(5) . ?
C23 H26A 0.9700 . ?
C23 H26B 0.9700 . ?
C7 C10 1.529(5) . ?
C7 C9 1.535(5) . ?
C7 C8 1.539(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C27 H30A 0.9700 . ?
C27 H30B 0.9700 . ?
C11 C14 1.528(6) . ?
C11 C12 1.531(6) . ?
C11 C13 1.536(5) . ?
C19 C20 1.526(6) . ?
C19 C21 1.529(6) . ?
C19 C22 1.532(6) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C5 C4 1.379(6) . ?
C5 H5 0.9300 . ?
C3 C4 1.383(6) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C17 C15 1.539(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C30 H29A 0.9600 . ?
C30 H29B 0.9600 . ?
C30 H29C 0.9600 . ?
C15 C18 1.524(6) . ?
C15 C16 1.538(6) . ?
C25 H23A 0.9600 . ?
C25 H23B 0.9600 . ?
C25 H23C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C24 H25A 0.9600 . ?
C24 H25B 0.9600 . ?
C24 H25C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C29 H28A 0.9600 . ?
C29 H28B 0.9600 . ?
C29 H28C 0.9600 . ?
C28 H27A 0.9600 . ?
C28 H27B 0.9600 . ?
C28 H27C 0.9600 . ?
C26 H24A 0.9600 . ?
C26 H24B 0.9600 . ?
C26 H24C 0.9600 . ?

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
C23 Sc1 C27 110.71(14) . . ?
C23 Sc1 C1 112.60(14) . . ?
C27 Sc1 C1 136.60(13) . . ?
C23 Sc1 P1 103.66(11) . . ?
C27 Sc1 P1 97.90(10) . . ?
C1 Sc1 P1 69.43(9) . . ?
C23 Sc1 P2 110.89(11) . . ?
C27 Sc1 P2 97.02(10) . . ?
C1 Sc1 P2 70.04(9) . . ?
P1 Sc1 P2 134.21(3) . . ?
O1 P1 C11 101.19(17) . . ?
O1 P1 C7 102.61(16) . . ?
C11 P1 C7 111.03(17) . . ?
O1 P1 Sc1 100.70(10) . . ?
C11 P1 Sc1 119.50(12) . . ?
C7 P1 Sc1 117.86(11) . . ?
O2 P2 C19 100.87(17) . . ?
O2 P2 C15 100.35(17) . . ?
C19 P2 C15 112.50(18) . . ?
O2 P2 Sc1 102.72(10) . . ?
C19 P2 Sc1 117.02(14) . . ?
C15 P2 Sc1 119.14(12) . . ?
C27 Si1 C29 109.8(2) . . ?
C27 Si1 C28 112.9(2) . . ?
C29 Si1 C28 108.9(3) . . ?
C27 Si1 C30 113.00(19) . . ?
C29 Si1 C30 106.6(2) . . ?
C28 Si1 C30 105.4(2) . . ?
C23 Si2 C26 111.2(3) . . ?
C23 Si2 C24 112.7(2) . . ?
C26 Si2 C24 105.3(3) . . ?
C23 Si2 C25 113.07(18) . . ?
C26 Si2 C25 106.9(2) . . ?
C24 Si2 C25 107.1(2) . . ?
C6 O1 P1 117.8(2) . . ?
C2 O2 P2 119.7(2) . . ?
C5 C6 C1 125.5(3) . . ?
C5 C6 O1 113.7(3) . . ?
C1 C6 O1 120.8(3) . . ?
C2 C1 C6 112.5(3) . . ?
C2 C1 Sc1 123.8(2) . . ?
C6 C1 Sc1 121.7(3) . . ?
C3 C2 C1 125.1(4) . . ?
C3 C2 O2 113.6(3) . . ?
C1 C2 O2 121.3(3) . . ?
Si2 C23 Sc1 133.2(2) . . ?
Si2 C23 H26A 103.9 . . ?
Sc1 C23 H26A 103.9 . . ?
Si2 C23 H26B 103.9 . . ?
Sc1 C23 H26B 103.9 . . ?
H26A C23 H26B 105.4 . . ?
C10 C7 C9 111.3(3) . . ?
C10 C7 C8 108.1(3) . . ?
C9 C7 C8 108.0(3) . . ?
C10 C7 P1 110.5(3) . . ?
C9 C7 P1 112.5(3) . . ?
C8 C7 P1 106.2(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C27 Sc1 125.7(2) . . ?
Si1 C27 H30A 105.9 . . ?
Sc1 C27 H30A 105.9 . . ?
Si1 C27 H30B 105.9 . . ?
Sc1 C27 H30B 105.9 . . ?
H30A C27 H30B 106.2 . . ?
C14 C11 C12 109.3(4) . . ?
C14 C11 C13 110.2(4) . . ?
C12 C11 C13 108.2(4) . . ?
C14 C11 P1 107.2(3) . . ?
C12 C11 P1 105.1(3) . . ?
C13 C11 P1 116.6(3) . . ?
C20 C19 C21 109.3(4) . . ?
C20 C19 C22 109.0(3) . . ?
C21 C19 C22 109.1(4) . . ?
C20 C19 P2 115.8(3) . . ?
C21 C19 P2 105.1(3) . . ?
C22 C19 P2 108.4(3) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C5 C6 118.3(4) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C4 C3 C2 118.3(4) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C5 C4 C3 120.2(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si1 C30 H29A 109.5 . . ?
Si1 C30 H29B 109.5 . . ?
H29A C30 H29B 109.5 . . ?
Si1 C30 H29C 109.5 . . ?
H29A C30 H29C 109.5 . . ?
H29B C30 H29C 109.5 . . ?
C18 C15 C16 110.8(4) . . ?
C18 C15 C17 109.2(3) . . ?
C16 C15 C17 107.2(3) . . ?
C18 C15 P2 110.1(3) . . ?
C16 C15 P2 113.8(3) . . ?
C17 C15 P2 105.4(3) . . ?
Si2 C25 H23A 109.5 . . ?
Si2 C25 H23B 109.5 . . ?
H23A C25 H23B 109.5 . . ?
Si2 C25 H23C 109.5 . . ?
H23A C25 H23C 109.5 . . ?
H23B C25 H23C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si2 C24 H25A 109.5 . . ?
Si2 C24 H25B 109.5 . . ?
H25A C24 H25B 109.5 . . ?
Si2 C24 H25C 109.5 . . ?
H25A C24 H25C 109.5 . . ?
H25B C24 H25C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C29 H28A 109.5 . . ?
Si1 C29 H28B 109.5 . . ?
H28A C29 H28B 109.5 . . ?
Si1 C29 H28C 109.5 . . ?
H28A C29 H28C 109.5 . . ?
H28B C29 H28C 109.5 . . ?
Si1 C28 H27A 109.5 . . ?
Si1 C28 H27B 109.5 . . ?
H27A C28 H27B 109.5 . . ?
Si1 C28 H27C 109.5 . . ?
H27A C28 H27C 109.5 . . ?
H27B C28 H27C 109.5 . . ?
Si2 C26 H24A 109.5 . . ?
Si2 C26 H24B 109.5 . . ?
H24A C26 H24B 109.5 . . ?
Si2 C26 H24C 109.5 . . ?
H24A C26 H24C 109.5 . . ?
H24B C26 H24C 109.5 . . ?

_refine_diff_density_max         0.409
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.059



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

data_shelx_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 2168775'
loop_
_audit_author_name
_audit_author_address
'Jiayu Zhang'
;College of Chemistry, Beijing Normal University,
China
;
_audit_update_record             
;
2022-04-26 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H39 Cl2 O2 P2 V'
_chemical_formula_weight         519.31

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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'

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

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

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

_cell_length_a                   10.6403(4)
_cell_length_b                   16.2799(8)
_cell_length_c                   15.1343(8)
_cell_angle_alpha                90
_cell_angle_beta                 90.332(4)
_cell_angle_gamma                90
_cell_volume                     2621.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9637
_cell_measurement_theta_min      3.9730
_cell_measurement_theta_max      29.2880

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_F_000             1096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.720
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  Rigaku
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31769
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.422
_diffrn_reflns_theta_max         29.778
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6664
_reflns_number_gt                5399
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0500P)²+2.8716P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6664
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1285
_refine_ls_wR_factor_gt          0.1169
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.49583(4) 0.60629(3) 0.22583(3) 0.01381(11) Uani 1 1 d . . . . .
Cl1 Cl 0.61818(5) 0.50427(4) 0.17030(4) 0.01931(14) Uani 1 1 d . . . . .
Cl2 Cl 0.49139(6) 0.70638(4) 0.12259(4) 0.02053(15) Uani 1 1 d . . . . .
P1 P 0.66114(6) 0.65973(4) 0.33100(4) 0.01520(15) Uani 1 1 d . . . . .
P2 P 0.28273(6) 0.53836(4) 0.20189(4) 0.01565(15) Uani 1 1 d . . . . .
O1 O 0.57498(16) 0.70334(12) 0.40829(13) 0.0220(4) Uani 1 1 d . . . . .
O2 O 0.20523(16) 0.56822(12) 0.29043(12) 0.0226(4) Uani 1 1 d . . . . .
C1 C 0.3968(2) 0.63480(15) 0.34041(17) 0.0164(5) Uani 1 1 d . . . . .
C5 C 0.1968(2) 0.64352(16) 0.42210(18) 0.0194(5) Uani 1 1 d . . . . .
H5 H 0.112541 0.629016 0.426720 0.023 Uiso 1 1 calc R U . . .
C6 C 0.2686(2) 0.61662(15) 0.35138(17) 0.0169(5) Uani 1 1 d . . . . .
C11 C 0.7655(2) 0.74573(15) 0.29836(18) 0.0184(5) Uani 1 1 d . . . . .
C2 C 0.4479(2) 0.68276(16) 0.40832(18) 0.0178(5) Uani 1 1 d . . . . .
C4 C 0.2536(2) 0.69233(16) 0.48538(18) 0.0201(5) Uani 1 1 d . . . . .
H4 H 0.206452 0.712027 0.532381 0.024 Uiso 1 1 calc R U . . .
C15 C 0.1761(2) 0.57693(17) 0.11354(18) 0.0209(5) Uani 1 1 d . . . . .
C3 C 0.3800(2) 0.71241(17) 0.47990(18) 0.0208(5) Uani 1 1 d . . . . .
H3 H 0.418301 0.744817 0.522888 0.025 Uiso 1 1 calc R U . . .
C14 C 0.6792(3) 0.82009(17) 0.2798(2) 0.0261(6) Uani 1 1 d . . . . .
H14A H 0.641395 0.837937 0.333896 0.039 Uiso 1 1 calc R U . . .
H14B H 0.614661 0.804482 0.238491 0.039 Uiso 1 1 calc R U . . .
H14C H 0.728005 0.864095 0.255317 0.039 Uiso 1 1 calc R U . . .
C7 C 0.7462(2) 0.58046(17) 0.39847(18) 0.0215(6) Uani 1 1 d . . . . .
C8 C 0.6470(3) 0.51402(18) 0.4179(2) 0.0281(6) Uani 1 1 d . . . . .
H8A H 0.684054 0.471529 0.453505 0.042 Uiso 1 1 calc R U . . .
H8B H 0.617260 0.490929 0.363294 0.042 Uiso 1 1 calc R U . . .
H8C H 0.577904 0.538203 0.449030 0.042 Uiso 1 1 calc R U . . .
C13 C 0.8281(3) 0.72002(18) 0.2113(2) 0.0250(6) Uani 1 1 d . . . . .
H13A H 0.877228 0.764847 0.189083 0.038 Uiso 1 1 calc R U . . .
H13B H 0.764511 0.705628 0.168826 0.038 Uiso 1 1 calc R U . . .
H13C H 0.881641 0.673520 0.221797 0.038 Uiso 1 1 calc R U . . .
C9 C 0.8535(2) 0.54231(17) 0.3454(2) 0.0245(6) Uani 1 1 d . . . . .
H9A H 0.918942 0.582190 0.337651 0.037 Uiso 1 1 calc R U . . .
H9B H 0.822388 0.525209 0.288629 0.037 Uiso 1 1 calc R U . . .
H9C H 0.886310 0.495606 0.376616 0.037 Uiso 1 1 calc R U . . .
C12 C 0.8646(2) 0.77067(17) 0.3661(2) 0.0271(6) Uani 1 1 d . . . . .
H12A H 0.927849 0.728765 0.369872 0.041 Uiso 1 1 calc R U . . .
H12B H 0.825843 0.777452 0.422784 0.041 Uiso 1 1 calc R U . . .
H12C H 0.902528 0.821530 0.348430 0.041 Uiso 1 1 calc R U . . .
C19 C 0.2746(3) 0.42531(17) 0.2163(2) 0.0275(6) Uani 1 1 d . . . . .
C16 C 0.1625(3) 0.66969(18) 0.1311(2) 0.0295(7) Uani 1 1 d . . . . .
H16A H 0.115974 0.694573 0.083559 0.044 Uiso 1 1 calc R U . . .
H16B H 0.244342 0.694274 0.134921 0.044 Uiso 1 1 calc R U . . .
H16C H 0.118685 0.678041 0.185598 0.044 Uiso 1 1 calc R U . . .
C17 C 0.0450(2) 0.53785(19) 0.1127(2) 0.0281(6) Uani 1 1 d . . . . .
H17A H -0.008522 0.567436 0.072621 0.042 Uiso 1 1 calc R U . . .
H17B H 0.010274 0.539953 0.171090 0.042 Uiso 1 1 calc R U . . .
H17C H 0.051299 0.481661 0.094018 0.042 Uiso 1 1 calc R U . . .
C22 C 0.3693(3) 0.40521(19) 0.2906(2) 0.0324(7) Uani 1 1 d . . . . .
H22A H 0.361827 0.348356 0.306508 0.049 Uiso 1 1 calc R U . . .
H22B H 0.352128 0.438878 0.341133 0.049 Uiso 1 1 calc R U . . .
H22C H 0.453099 0.415862 0.270287 0.049 Uiso 1 1 calc R U . . .
C10 C 0.7955(3) 0.6127(2) 0.4873(2) 0.0303(7) Uani 1 1 d . . . . .
H10A H 0.822781 0.567369 0.523154 0.045 Uiso 1 1 calc R U . . .
H10B H 0.729668 0.641805 0.517028 0.045 Uiso 1 1 calc R U . . .
H10C H 0.864954 0.649121 0.477314 0.045 Uiso 1 1 calc R U . . .
C18 C 0.2403(3) 0.5637(2) 0.0246(2) 0.0352(7) Uani 1 1 d . . . . .
H18A H 0.248297 0.505882 0.013495 0.053 Uiso 1 1 calc R U . . .
H18B H 0.322206 0.588416 0.025939 0.053 Uiso 1 1 calc R U . . .
H18C H 0.190775 0.588469 -0.021410 0.053 Uiso 1 1 calc R U . . .
C21 C 0.3135(3) 0.38175(19) 0.1319(3) 0.0395(8) Uani 1 1 d . . . . .
H21A H 0.390563 0.405010 0.110761 0.059 Uiso 1 1 calc R U . . .
H21B H 0.248934 0.388380 0.087934 0.059 Uiso 1 1 calc R U . . .
H21C H 0.325511 0.324350 0.143807 0.059 Uiso 1 1 calc R U . . .
C20 C 0.1451(3) 0.3945(2) 0.2469(3) 0.0468(10) Uani 1 1 d . . . . .
H20A H 0.086269 0.397909 0.198664 0.070 Uiso 1 1 calc R U . . .
H20B H 0.116243 0.427837 0.294959 0.070 Uiso 1 1 calc R U . . .
H20C H 0.151974 0.338416 0.266017 0.070 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
V1 C1 2.087(2) . ?
V1 Cl2 2.2577(7) . ?
V1 Cl1 2.2742(7) . ?
V1 P1 2.5203(8) . ?
V1 P2 2.5467(7) . ?
P1 O1 1.6508(18) . ?
P1 C11 1.855(3) . ?
P1 C7 1.875(3) . ?
P2 O2 1.6507(19) . ?
P2 C19 1.855(3) . ?
P2 C15 1.858(3) . ?
O1 C2 1.393(3) . ?
O2 C6 1.385(3) . ?
C1 C2 1.398(4) . ?
C1 C6 1.407(3) . ?
C5 C4 1.381(4) . ?
C5 C6 1.390(4) . ?
C5 H5 0.9300 . ?
C11 C12 1.522(4) . ?
C11 C13 1.537(4) . ?
C11 C14 1.544(4) . ?
C2 C3 1.392(4) . ?
C4 C3 1.386(4) . ?
C4 H4 0.9300 . ?
C15 C18 1.528(4) . ?
C15 C17 1.532(4) . ?
C15 C16 1.540(4) . ?
C3 H3 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C7 C9 1.531(4) . ?
C7 C10 1.533(4) . ?
C7 C8 1.541(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C19 C21 1.520(5) . ?
C19 C22 1.540(4) . ?
C19 C20 1.541(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?

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 V1 Cl2 113.95(7) . . ?
C1 V1 Cl1 139.68(7) . . ?
Cl2 V1 Cl1 106.33(3) . . ?
C1 V1 P1 75.66(7) . . ?
Cl2 V1 P1 101.51(3) . . ?
Cl1 V1 P1 94.96(3) . . ?
C1 V1 P2 76.19(7) . . ?
Cl2 V1 P2 101.53(3) . . ?
Cl1 V1 P2 98.13(3) . . ?
P1 V1 P2 149.01(3) . . ?
O1 P1 C11 101.52(11) . . ?
O1 P1 C7 100.28(12) . . ?
C11 P1 C7 112.12(12) . . ?
O1 P1 V1 101.98(7) . . ?
C11 P1 V1 120.58(9) . . ?
C7 P1 V1 116.06(9) . . ?
O2 P2 C19 99.95(12) . . ?
O2 P2 C15 100.29(11) . . ?
C19 P2 C15 113.04(13) . . ?
O2 P2 V1 101.84(7) . . ?
C19 P2 V1 117.12(9) . . ?
C15 P2 V1 119.68(9) . . ?
C2 O1 P1 116.09(16) . . ?
C6 O2 P2 117.68(15) . . ?
C2 C1 C6 113.8(2) . . ?
C2 C1 V1 122.62(17) . . ?
C6 C1 V1 123.09(19) . . ?
C4 C5 C6 118.3(2) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
O2 C6 C5 115.1(2) . . ?
O2 C6 C1 120.6(2) . . ?
C5 C6 C1 124.2(2) . . ?
C12 C11 C13 110.3(2) . . ?
C12 C11 C14 108.8(2) . . ?
C13 C11 C14 108.5(2) . . ?
C12 C11 P1 115.80(19) . . ?
C13 C11 P1 106.59(18) . . ?
C14 C11 P1 106.52(17) . . ?
C3 C2 O1 115.2(2) . . ?
C3 C2 C1 124.4(2) . . ?
O1 C2 C1 120.5(2) . . ?
C5 C4 C3 121.0(2) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C18 C15 C17 110.2(2) . . ?
C18 C15 C16 109.4(2) . . ?
C17 C15 C16 108.8(2) . . ?
C18 C15 P2 108.15(19) . . ?
C17 C15 P2 114.7(2) . . ?
C16 C15 P2 105.37(18) . . ?
C4 C3 C2 118.2(2) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C9 C7 C10 110.3(2) . . ?
C9 C7 C8 109.2(2) . . ?
C10 C7 C8 107.7(2) . . ?
C9 C7 P1 110.63(19) . . ?
C10 C7 P1 113.8(2) . . ?
C8 C7 P1 104.94(18) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C21 C19 C22 109.5(3) . . ?
C21 C19 C20 110.4(3) . . ?
C22 C19 C20 107.1(3) . . ?
C21 C19 P2 110.5(2) . . ?
C22 C19 P2 105.43(19) . . ?
C20 C19 P2 113.6(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_refine_diff_density_max         0.706
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.098



####################################################################### 
# 
# 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_shelx_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 2162723'
loop_
_audit_author_name
_audit_author_address
'Jiayu Zhang'
;College of Chemistry, Beijing Normal University,
China
;
_audit_update_record             
;
2022-03-29 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H61 O2 P2 Si2 V'
_chemical_formula_weight         622.84

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

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

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

_cell_length_a                   16.1044(4)
_cell_length_b                   13.1750(3)
_cell_length_c                   16.9968(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3606.30(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17314
_cell_measurement_theta_min      3.9940
_cell_measurement_theta_max      29.2130

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_F_000             1352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.453
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  Rigaku
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42226
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.341
_diffrn_reflns_theta_max         29.810
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_point_group_measured_fraction_full 0.961
_reflns_number_total             8658
_reflns_number_gt                7629
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_max     0.736
_reflns_Friedel_fraction_full    0.922

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0469P)²+0.8663P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.06(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8658
_refine_ls_number_parameters     353
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0929
_refine_ls_wR_factor_gt          0.0866
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.981
_refine_ls_shift/su_max          0.007
_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
V1 V 0.45351(3) 0.26608(3) 0.47533(3) 0.01848(11) Uani 1 1 d . . . . .
P1 P 0.34115(4) 0.12854(5) 0.47229(6) 0.02263(15) Uani 1 1 d . . . . .
P2 P 0.47807(4) 0.46297(5) 0.46209(5) 0.02327(17) Uani 1 1 d . . . . .
Si1 Si 0.57145(5) 0.22554(7) 0.64963(5) 0.0273(2) Uani 1 1 d . . . . .
Si2 Si 0.57613(6) 0.16212(8) 0.31409(6) 0.0361(2) Uani 1 1 d . . . . .
O1 O 0.29710(14) 0.15210(17) 0.38674(14) 0.0321(5) Uani 1 1 d . . . . .
O2 O 0.40785(14) 0.49348(16) 0.39554(15) 0.0319(5) Uani 1 1 d . . . . .
C11 C 0.25095(18) 0.1495(2) 0.54081(19) 0.0239(6) Uani 1 1 d . . . . .
C14 C 0.2470(2) 0.2638(2) 0.5588(2) 0.0283(7) Uani 1 1 d . . . . .
H14A H 0.201233 0.277228 0.593402 0.042 Uiso 1 1 calc R U . . .
H14B H 0.239540 0.300815 0.510605 0.042 Uiso 1 1 calc R U . . .
H14C H 0.297809 0.284801 0.583439 0.042 Uiso 1 1 calc R U . . .
C6 C 0.36107(18) 0.4155(2) 0.36214(19) 0.0245(6) Uani 1 1 d . . . . .
C1 C 0.36079(17) 0.3187(2) 0.39573(18) 0.0213(6) Uani 1 1 d . . . . .
C2 C 0.30646(19) 0.2512(2) 0.35746(19) 0.0244(6) Uani 1 1 d . . . . .
C27 C 0.55325(19) 0.1917(3) 0.4201(2) 0.0290(7) Uani 1 1 d . . . . .
H27A H 0.601891 0.228558 0.437880 0.035 Uiso 1 1 calc R U . . .
H27B H 0.555905 0.126248 0.446118 0.035 Uiso 1 1 calc R U . . .
C23 C 0.47303(19) 0.2589(2) 0.59886(19) 0.0244(6) Uani 1 1 d . . . . .
H23A H 0.457418 0.325105 0.618990 0.029 Uiso 1 1 calc R U . . .
H23B H 0.431856 0.211625 0.618658 0.029 Uiso 1 1 calc R U . . .
C12 C 0.2643(2) 0.0934(2) 0.6185(2) 0.0322(7) Uani 1 1 d . . . . .
H12A H 0.317405 0.111578 0.640003 0.048 Uiso 1 1 calc R U . . .
H12B H 0.262556 0.021534 0.609433 0.048 Uiso 1 1 calc R U . . .
H12C H 0.221351 0.111924 0.654970 0.048 Uiso 1 1 calc R U . . .
C15 C 0.5734(2) 0.5128(3) 0.4125(2) 0.0316(7) Uani 1 1 d . . . . .
C5 C 0.3161(2) 0.4432(2) 0.29567(19) 0.0309(7) Uani 1 1 d . . . . .
H5 H 0.319593 0.508572 0.275259 0.037 Uiso 1 1 calc R U . . .
C13 C 0.1675(2) 0.1191(3) 0.5034(2) 0.0349(8) Uani 1 1 d . . . . .
H13A H 0.167072 0.047290 0.493795 0.052 Uiso 1 1 calc R U . . .
H13B H 0.160447 0.154697 0.454605 0.052 Uiso 1 1 calc R U . . .
H13C H 0.123022 0.136316 0.538548 0.052 Uiso 1 1 calc R U . . .
C3 C 0.2602(2) 0.2743(3) 0.2918(2) 0.0314(7) Uani 1 1 d . . . . .
H3 H 0.225856 0.225946 0.268823 0.038 Uiso 1 1 calc R U . . .
C7 C 0.3615(2) -0.0107(2) 0.4620(3) 0.0361(8) Uani 1 1 d . . . . .
C4 C 0.2659(2) 0.3708(3) 0.2608(2) 0.0351(8) Uani 1 1 d . . . . .
H4 H 0.235714 0.387356 0.215923 0.042 Uiso 1 1 calc R U . . .
C24 C 0.5645(2) 0.2632(3) 0.7553(2) 0.0389(9) Uani 1 1 d . . . . .
H24A H 0.558059 0.335445 0.759035 0.058 Uiso 1 1 calc R U . . .
H24B H 0.614334 0.243036 0.782121 0.058 Uiso 1 1 calc R U . . .
H24C H 0.517593 0.230377 0.779131 0.058 Uiso 1 1 calc R U . . .
C29 C 0.6036(3) 0.0243(3) 0.2972(2) 0.0479(10) Uani 1 1 d . . . . .
H29A H 0.648605 0.005449 0.331268 0.072 Uiso 1 1 calc R U . . .
H29B H 0.620089 0.014890 0.243384 0.072 Uiso 1 1 calc R U . . .
H29C H 0.556200 -0.017425 0.308309 0.072 Uiso 1 1 calc R U . . .
C10 C 0.2857(2) -0.0813(2) 0.4608(3) 0.0462(10) Uani 1 1 d . . . . .
H10A H 0.303741 -0.150077 0.453157 0.069 Uiso 1 1 calc R U . . .
H10B H 0.249411 -0.061955 0.418643 0.069 Uiso 1 1 calc R U . . .
H10C H 0.256629 -0.076111 0.509966 0.069 Uiso 1 1 calc R U . . .
C17 C 0.5689(2) 0.4703(3) 0.3286(2) 0.0422(9) Uani 1 1 d . . . . .
H17A H 0.524618 0.502961 0.300520 0.063 Uiso 1 1 calc R U . . .
H17B H 0.558808 0.398572 0.330688 0.063 Uiso 1 1 calc R U . . .
H17C H 0.620546 0.482834 0.302069 0.063 Uiso 1 1 calc R U . . .
C16 C 0.6499(2) 0.4704(3) 0.4542(2) 0.0427(9) Uani 1 1 d . . . . .
H16A H 0.699145 0.493742 0.427922 0.064 Uiso 1 1 calc R U . . .
H16B H 0.648257 0.397613 0.453018 0.064 Uiso 1 1 calc R U . . .
H16C H 0.650481 0.493299 0.507802 0.064 Uiso 1 1 calc R U . . .
C18 C 0.5807(2) 0.6284(3) 0.4081(2) 0.0425(9) Uani 1 1 d . . . . .
H18A H 0.590252 0.655183 0.459835 0.064 Uiso 1 1 calc R U . . .
H18B H 0.530241 0.656305 0.387218 0.064 Uiso 1 1 calc R U . . .
H18C H 0.626303 0.646380 0.374433 0.064 Uiso 1 1 calc R U . . .
C20 C 0.3622(2) 0.5034(3) 0.5757(2) 0.0363(8) Uani 1 1 d . . . . .
H20A H 0.341541 0.545271 0.617554 0.054 Uiso 1 1 calc R U . . .
H20B H 0.373518 0.436557 0.595470 0.054 Uiso 1 1 calc R U . . .
H20C H 0.321482 0.499383 0.534605 0.054 Uiso 1 1 calc R U . . .
C19 C 0.4428(2) 0.5499(2) 0.5428(2) 0.0312(7) Uani 1 1 d . . . . .
C28 C 0.4883(3) 0.1929(3) 0.2453(2) 0.0456(9) Uani 1 1 d . . . . .
H28A H 0.441828 0.149737 0.256697 0.068 Uiso 1 1 calc R U . . .
H28B H 0.505920 0.182125 0.191975 0.068 Uiso 1 1 calc R U . . .
H28C H 0.472358 0.262562 0.252044 0.068 Uiso 1 1 calc R U . . .
C21 C 0.4208(3) 0.6586(3) 0.5155(3) 0.0504(11) Uani 1 1 d . . . . .
H21A H 0.388168 0.655211 0.468304 0.076 Uiso 1 1 calc R U . . .
H21B H 0.470968 0.695667 0.505301 0.076 Uiso 1 1 calc R U . . .
H21C H 0.389655 0.692263 0.555940 0.076 Uiso 1 1 calc R U . . .
C22 C 0.5087(2) 0.5538(3) 0.6076(2) 0.0409(9) Uani 1 1 d . . . . .
H22A H 0.487637 0.591355 0.651688 0.061 Uiso 1 1 calc R U . . .
H22B H 0.557757 0.586487 0.587823 0.061 Uiso 1 1 calc R U . . .
H22C H 0.522162 0.486018 0.623942 0.061 Uiso 1 1 calc R U . . .
C25 C 0.5908(3) 0.0861(3) 0.6483(3) 0.0488(10) Uani 1 1 d . . . . .
H25A H 0.543856 0.051328 0.670222 0.073 Uiso 1 1 calc R U . . .
H25B H 0.639418 0.071050 0.678876 0.073 Uiso 1 1 calc R U . . .
H25C H 0.599262 0.064057 0.595031 0.073 Uiso 1 1 calc R U . . .
C26 C 0.6666(2) 0.2899(4) 0.6106(3) 0.0565(13) Uani 1 1 d . . . . .
H26A H 0.676991 0.267362 0.557785 0.085 Uiso 1 1 calc R U . . .
H26B H 0.713322 0.273387 0.643227 0.085 Uiso 1 1 calc R U . . .
H26C H 0.658266 0.362093 0.610703 0.085 Uiso 1 1 calc R U . . .
C9 C 0.4202(3) -0.0409(3) 0.5287(3) 0.0506(11) Uani 1 1 d . . . . .
H9A H 0.390848 -0.038514 0.577863 0.076 Uiso 1 1 calc R U . . .
H9B H 0.466161 0.005411 0.530369 0.076 Uiso 1 1 calc R U . . .
H9C H 0.440299 -0.108490 0.519815 0.076 Uiso 1 1 calc R U . . .
C8 C 0.4069(3) -0.0219(3) 0.3834(3) 0.0639(15) Uani 1 1 d . . . . .
H8A H 0.428906 -0.089350 0.379019 0.096 Uiso 1 1 calc R U . . .
H8B H 0.451529 0.026356 0.380879 0.096 Uiso 1 1 calc R U . . .
H8C H 0.368791 -0.009590 0.341067 0.096 Uiso 1 1 calc R U . . .
C30 C 0.6712(3) 0.2334(4) 0.2801(3) 0.0653(14) Uani 1 1 d . . . . .
H30A H 0.661525 0.305037 0.284459 0.098 Uiso 1 1 calc R U . . .
H30B H 0.682696 0.216494 0.226201 0.098 Uiso 1 1 calc R U . . .
H30C H 0.717826 0.214812 0.312209 0.098 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
V1 C27 2.103(3) . ?
V1 C23 2.125(3) . ?
V1 C1 2.131(3) . ?
V1 P1 2.5614(8) . ?
V1 P2 2.6336(8) . ?
P1 O1 1.647(3) . ?
P1 C7 1.872(3) . ?
P1 C11 1.882(3) . ?
P2 O2 1.649(2) . ?
P2 C15 1.871(3) . ?
P2 C19 1.875(4) . ?
Si1 C23 1.857(3) . ?
Si1 C25 1.864(4) . ?
Si1 C24 1.867(4) . ?
Si1 C26 1.873(4) . ?
Si2 C27 1.880(3) . ?
Si2 C28 1.879(4) . ?
Si2 C30 1.887(4) . ?
Si2 C29 1.891(4) . ?
O1 C2 1.405(4) . ?
O2 C6 1.395(4) . ?
C11 C12 1.529(5) . ?
C11 C14 1.538(4) . ?
C11 C13 1.539(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C6 C5 1.391(4) . ?
C6 C1 1.398(4) . ?
C1 C2 1.407(4) . ?
C2 C3 1.376(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C15 C16 1.528(5) . ?
C15 C18 1.529(5) . ?
C15 C17 1.533(5) . ?
C5 C4 1.384(5) . ?
C5 H5 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C3 C4 1.379(5) . ?
C3 H3 0.9300 . ?
C7 C9 1.528(6) . ?
C7 C8 1.530(6) . ?
C7 C10 1.535(4) . ?
C4 H4 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 C19 1.540(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C19 C22 1.532(5) . ?
C19 C21 1.545(4) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C27 V1 C23 107.91(12) . . ?
C27 V1 C1 113.79(12) . . ?
C23 V1 C1 138.19(12) . . ?
C27 V1 P1 101.59(10) . . ?
C23 V1 P1 95.33(9) . . ?
C1 V1 P1 73.86(8) . . ?
C27 V1 P2 107.83(10) . . ?
C23 V1 P2 96.08(9) . . ?
C1 V1 P2 74.38(8) . . ?
P1 V1 P2 143.24(3) . . ?
O1 P1 C7 100.26(15) . . ?
O1 P1 C11 100.73(14) . . ?
C7 P1 C11 109.68(14) . . ?
O1 P1 V1 100.88(8) . . ?
C7 P1 V1 124.84(11) . . ?
C11 P1 V1 115.40(9) . . ?
O2 P2 C15 99.65(14) . . ?
O2 P2 C19 98.31(14) . . ?
C15 P2 C19 111.34(15) . . ?
O2 P2 V1 101.29(8) . . ?
C15 P2 V1 120.52(12) . . ?
C19 P2 V1 119.59(11) . . ?
C23 Si1 C25 111.76(17) . . ?
C23 Si1 C24 109.46(16) . . ?
C25 Si1 C24 106.48(18) . . ?
C23 Si1 C26 115.23(16) . . ?
C25 Si1 C26 107.8(2) . . ?
C24 Si1 C26 105.6(2) . . ?
C27 Si2 C28 113.85(16) . . ?
C27 Si2 C30 110.5(2) . . ?
C28 Si2 C30 108.2(2) . . ?
C27 Si2 C29 112.99(17) . . ?
C28 Si2 C29 106.79(19) . . ?
C30 Si2 C29 103.9(2) . . ?
C2 O1 P1 116.20(19) . . ?
C6 O2 P2 118.04(19) . . ?
C12 C11 C14 107.9(3) . . ?
C12 C11 C13 110.7(3) . . ?
C14 C11 C13 107.5(3) . . ?
C12 C11 P1 110.8(2) . . ?
C14 C11 P1 107.3(2) . . ?
C13 C11 P1 112.3(2) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C6 C5 114.8(3) . . ?
O2 C6 C1 120.5(3) . . ?
C5 C6 C1 124.7(3) . . ?
C6 C1 C2 113.0(3) . . ?
C6 C1 V1 123.6(2) . . ?
C2 C1 V1 121.6(2) . . ?
C3 C2 O1 115.8(3) . . ?
C3 C2 C1 124.9(3) . . ?
O1 C2 C1 119.3(3) . . ?
Si2 C27 V1 132.39(18) . . ?
Si2 C27 H27A 104.1 . . ?
V1 C27 H27A 104.1 . . ?
Si2 C27 H27B 104.1 . . ?
V1 C27 H27B 104.1 . . ?
H27A C27 H27B 105.5 . . ?
Si1 C23 V1 126.56(16) . . ?
Si1 C23 H23A 105.7 . . ?
V1 C23 H23A 105.7 . . ?
Si1 C23 H23B 105.7 . . ?
V1 C23 H23B 105.7 . . ?
H23A C23 H23B 106.1 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C16 C15 C18 108.9(3) . . ?
C16 C15 C17 109.6(3) . . ?
C18 C15 C17 108.8(3) . . ?
C16 C15 P2 108.9(2) . . ?
C18 C15 P2 115.8(3) . . ?
C17 C15 P2 104.6(2) . . ?
C4 C5 C6 118.1(3) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C2 C3 C4 118.6(3) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C9 C7 C8 109.1(3) . . ?
C9 C7 C10 110.1(3) . . ?
C8 C7 C10 108.1(3) . . ?
C9 C7 P1 107.1(2) . . ?
C8 C7 P1 105.0(2) . . ?
C10 C7 P1 117.1(2) . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
Si1 C24 H24A 109.5 . . ?
Si1 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si1 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si2 C29 H29A 109.5 . . ?
Si2 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si2 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C19 C20 109.6(3) . . ?
C22 C19 C21 110.1(3) . . ?
C20 C19 C21 106.6(3) . . ?
C22 C19 P2 109.6(2) . . ?
C20 C19 P2 106.1(2) . . ?
C21 C19 P2 114.6(3) . . ?
Si2 C28 H28A 109.5 . . ?
Si2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C25 H25A 109.5 . . ?
Si1 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si1 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si1 C26 H26A 109.5 . . ?
Si1 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si1 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C30 H30A 109.5 . . ?
Si2 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si2 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

_refine_diff_density_max         0.289
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.054



