# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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. 
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data_Compound_5b
_database_code_depnum_ccdc_archive 'CCDC 1851868'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-10-11 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         'C26 H34 B N6 O2 P W'
_chemical_formula_sum            'C26 H34 B N6 O2 P W'
_chemical_formula_weight         688.22

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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.0730(4)
_cell_length_b                   20.5330(5)
_cell_length_c                   20.5731(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6367.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    3538
_cell_measurement_theta_min      4.2510
_cell_measurement_theta_max      71.6770

_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_F_000             2736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.062
_exptl_absorpt_coefficient_mu    7.441
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.40485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_reflns_number            9401
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.226
_diffrn_reflns_theta_max         66.588
_diffrn_reflns_theta_full        66.588
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measured_fraction_theta_full 0.866
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_Laue_measured_fraction_full 0.866
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_point_group_measured_fraction_full 0.866
_reflns_number_total             4874
_reflns_number_gt                3858
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_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)+(0.1117P)²+11.7065P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4874
_refine_ls_number_parameters     346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0580
_refine_ls_wR_factor_ref         0.1676
_refine_ls_wR_factor_gt          0.1504
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
W W 0.70427(2) 0.69042(2) 0.60156(2) 0.02764(18) Uani 1 1 d . . . . .
P P 0.74989(15) 0.60410(10) 0.45433(11) 0.0417(5) Uani 1 1 d . . . . .
N3 N 0.5592(5) 0.6907(3) 0.6101(3) 0.0309(14) Uani 1 1 d . . . . .
N4 N 0.5180(4) 0.6953(2) 0.6704(3) 0.0275(12) Uani 1 1 d . . . . .
O1 O 0.7101(5) 0.7951(3) 0.4901(3) 0.0568(18) Uani 1 1 d . . . . .
O2 O 0.9108(4) 0.7020(3) 0.6087(3) 0.0488(16) Uani 1 1 d . . . . .
C3 C 0.8391(6) 0.6981(3) 0.6070(4) 0.0300(17) Uani 1 1 d . . . . .
N6 N 0.6364(4) 0.6397(3) 0.7368(3) 0.0290(12) Uani 1 1 d . . . . .
N2 N 0.6333(4) 0.7611(3) 0.7295(3) 0.0294(12) Uani 1 1 d . . . . .
N5 N 0.6933(4) 0.6246(3) 0.6868(3) 0.0295(13) Uani 1 1 d . . . . .
N1 N 0.6927(4) 0.7709(3) 0.6785(3) 0.0273(13) Uani 1 1 d . . . . .
C20 C 0.4277(5) 0.6979(3) 0.6636(4) 0.0347(16) Uani 1 1 d . . . . .
C18 C 0.4922(6) 0.6896(3) 0.5658(4) 0.0363(17) Uani 1 1 d . . . . .
C24 C 0.7103(6) 0.5529(4) 0.7670(4) 0.049(2) Uani 1 1 d . . . . .
H24 H 0.7306 0.5175 0.7910 0.058 Uiso 1 1 calc R U . . .
C14 C 0.7004(5) 0.8547(4) 0.7487(4) 0.0400(18) Uani 1 1 d . . . . .
H14 H 0.7183 0.8937 0.7675 0.048 Uiso 1 1 calc R U . . .
C2 C 0.7067(5) 0.7592(4) 0.5291(4) 0.0383(18) Uani 1 1 d . . . . .
C19 C 0.4102(6) 0.6937(3) 0.5974(4) 0.0361(18) Uani 1 1 d . . . . .
H19 H 0.3546 0.6936 0.5778 0.043 Uiso 1 1 calc R U . . .
B B 0.5749(6) 0.6994(4) 0.7329(4) 0.0288(16) Uani 1 1 d . . . . .
C13 C 0.7319(6) 0.8264(3) 0.6906(4) 0.0375(17) Uani 1 1 d . . . . .
C23 C 0.7394(5) 0.5721(3) 0.7048(4) 0.0339(16) Uani 1 1 d . . . . .
C17 C 0.5108(6) 0.6847(4) 0.4947(4) 0.048(2) Uani 1 1 d . . . . .
H17A H 0.5414 0.7232 0.4805 0.072 Uiso 1 1 calc R U . . .
H17B H 0.4559 0.6806 0.4714 0.072 Uiso 1 1 calc R U . . .
H17C H 0.5471 0.6472 0.4865 0.072 Uiso 1 1 calc R U . . .
C7 C 0.9326(6) 0.5859(4) 0.4905(4) 0.0433(18) Uani 1 1 d . . . . .
H7A H 0.9166 0.5962 0.5349 0.052 Uiso 1 1 calc R U . . .
H7B H 0.9265 0.5392 0.4846 0.052 Uiso 1 1 calc R U . . .
C6 C 0.8699(5) 0.6211(4) 0.4441(4) 0.0390(17) Uani 1 1 d . . . . .
H6 H 0.8774 0.6677 0.4529 0.047 Uiso 1 1 calc R U . . .
C25 C 0.6464(6) 0.5965(4) 0.7851(4) 0.0398(17) Uani 1 1 d . . . . .
C11 C 0.8980(6) 0.6109(4) 0.3732(4) 0.049(2) Uani 1 1 d . . . . .
H11A H 0.8872 0.5659 0.3611 0.059 Uiso 1 1 calc R U . . .
H11B H 0.8620 0.6383 0.3454 0.059 Uiso 1 1 calc R U . . .
C12 C 0.8031(5) 0.8551(4) 0.6472(5) 0.046(2) Uani 1 1 d . . . . .
H12A H 0.8456 0.8220 0.6364 0.068 Uiso 1 1 calc R U . . .
H12B H 0.8324 0.8900 0.6696 0.068 Uiso 1 1 calc R U . . .
H12C H 0.7765 0.8714 0.6081 0.068 Uiso 1 1 calc R U . . .
C9 C 1.0551(7) 0.5925(5) 0.4102(5) 0.054(2) Uani 1 1 d . . . . .
H9A H 1.0532 0.5459 0.4021 0.065 Uiso 1 1 calc R U . . .
H9B H 1.1157 0.6070 0.4037 0.065 Uiso 1 1 calc R U . . .
C1 C 0.7277(6) 0.6352(4) 0.5326(4) 0.0393(17) Uani 1 1 d . . . . .
C26 C 0.5949(7) 0.5987(4) 0.8472(4) 0.054(2) Uani 1 1 d . . . . .
H26A H 0.6071 0.6388 0.8695 0.081 Uiso 1 1 calc R U . . .
H26B H 0.6120 0.5626 0.8742 0.081 Uiso 1 1 calc R U . . .
H26C H 0.5327 0.5959 0.8378 0.081 Uiso 1 1 calc R U . . .
C10 C 0.9954(7) 0.6267(4) 0.3623(5) 0.056(2) Uani 1 1 d . . . . .
H10A H 1.0119 0.6141 0.3185 0.067 Uiso 1 1 calc R U . . .
H10B H 1.0039 0.6734 0.3661 0.067 Uiso 1 1 calc R U . . .
C22 C 0.8066(6) 0.5406(4) 0.6615(5) 0.047(2) Uani 1 1 d . . . . .
H22A H 0.7796 0.5298 0.6206 0.070 Uiso 1 1 calc R U . . .
H22B H 0.8283 0.5016 0.6817 0.070 Uiso 1 1 calc R U . . .
H22C H 0.8551 0.5701 0.6544 0.070 Uiso 1 1 calc R U . . .
C21 C 0.3655(5) 0.7049(4) 0.7184(4) 0.0440(18) Uani 1 1 d . . . . .
H21A H 0.3753 0.6705 0.7491 0.066 Uiso 1 1 calc R U . . .
H21B H 0.3056 0.7027 0.7026 0.066 Uiso 1 1 calc R U . . .
H21C H 0.3749 0.7462 0.7393 0.066 Uiso 1 1 calc R U . . .
C4 C 0.7510(6) 0.5193(4) 0.4694(5) 0.049(2) Uani 1 1 d . . . . .
C15 C 0.6375(6) 0.8121(3) 0.7713(4) 0.0359(17) Uani 1 1 d . . . . .
C8 C 1.0284(6) 0.6054(4) 0.4786(5) 0.050(2) Uani 1 1 d . . . . .
H8A H 1.0356 0.6514 0.4879 0.061 Uiso 1 1 calc R U . . .
H8B H 1.0667 0.5812 0.5077 0.061 Uiso 1 1 calc R U . . .
C5 C 0.7474(7) 0.4620(5) 0.4748(6) 0.072(3) Uani 1 1 d . . . . .
H5 H 0.7445 0.4170 0.4790 0.086 Uiso 1 1 calc R U . . .
C16 C 0.5838(7) 0.8163(4) 0.8308(4) 0.052(2) Uani 1 1 d . . . . .
H16A H 0.5229 0.8238 0.8194 0.078 Uiso 1 1 calc R U . . .
H16B H 0.6049 0.8517 0.8572 0.078 Uiso 1 1 calc R U . . .
H16C H 0.5886 0.7763 0.8547 0.078 Uiso 1 1 calc R U . . .
H99 H 0.535(6) 0.705(4) 0.777(4) 0.04(2) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W C1 1.850(8) . ?
W C3 2.041(9) . ?
W C2 2.055(8) . ?
W N3 2.194(8) . ?
W N5 2.220(5) . ?
W N1 2.295(5) . ?
P C1 1.764(8) . ?
P C4 1.769(9) . ?
P C6 1.854(8) . ?
N3 C18 1.360(11) . ?
N3 N4 1.392(9) . ?
N4 C20 1.369(10) . ?
N4 B 1.548(11) . ?
O1 C2 1.091(10) . ?
O2 C3 1.085(11) . ?
N6 C25 1.341(9) . ?
N6 N5 1.375(8) . ?
N6 B 1.537(9) . ?
N2 C15 1.356(9) . ?
N2 N1 1.394(8) . ?
N2 B 1.544(10) . ?
N5 C23 1.334(9) . ?
N1 C13 1.307(11) . ?
C20 C19 1.390(11) . ?
C20 C21 1.475(12) . ?
C18 C19 1.399(12) . ?
C18 C17 1.492(11) . ?
C24 C25 1.368(12) . ?
C24 C23 1.409(12) . ?
C24 H24 0.9300 . ?
C14 C15 1.371(11) . ?
C14 C13 1.411(12) . ?
C14 H14 0.9300 . ?
C19 H19 0.9300 . ?
B H99 1.10(9) . ?
C13 C12 1.517(12) . ?
C23 C22 1.496(11) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C7 C8 1.517(12) . ?
C7 C6 1.525(11) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C6 C11 1.533(11) . ?
C6 H6 0.9800 . ?
C25 C26 1.495(11) . ?
C11 C10 1.520(13) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C9 C8 1.488(12) . ?
C9 C10 1.509(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C4 C5 1.182(14) . ?
C15 C16 1.471(12) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C5 H5 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 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 W C3 84.2(3) . . ?
C1 W C2 82.0(3) . . ?
C3 W C2 88.3(3) . . ?
C1 W N3 104.7(3) . . ?
C3 W N3 171.0(3) . . ?
C2 W N3 94.2(3) . . ?
C1 W N5 104.3(3) . . ?
C3 W N5 94.4(2) . . ?
C2 W N5 173.3(3) . . ?
N3 W N5 82.2(2) . . ?
C1 W N1 170.0(3) . . ?
C3 W N1 89.0(2) . . ?
C2 W N1 90.4(3) . . ?
N3 W N1 82.4(2) . . ?
N5 W N1 83.6(2) . . ?
C1 P C4 101.4(4) . . ?
C1 P C6 102.7(4) . . ?
C4 P C6 101.3(4) . . ?
C18 N3 N4 105.5(7) . . ?
C18 N3 W 133.4(6) . . ?
N4 N3 W 121.0(5) . . ?
C20 N4 N3 110.7(6) . . ?
C20 N4 B 129.4(7) . . ?
N3 N4 B 119.9(6) . . ?
O2 C3 W 178.6(8) . . ?
C25 N6 N5 109.5(6) . . ?
C25 N6 B 129.3(6) . . ?
N5 N6 B 121.2(5) . . ?
C15 N2 N1 109.6(6) . . ?
C15 N2 B 129.2(6) . . ?
N1 N2 B 121.2(6) . . ?
C23 N5 N6 107.5(6) . . ?
C23 N5 W 132.2(5) . . ?
N6 N5 W 119.9(4) . . ?
C13 N1 N2 105.8(6) . . ?
C13 N1 W 136.5(5) . . ?
N2 N1 W 117.7(4) . . ?
N4 C20 C19 106.7(7) . . ?
N4 C20 C21 123.9(7) . . ?
C19 C20 C21 129.4(8) . . ?
N3 C18 C19 110.1(7) . . ?
N3 C18 C17 121.2(8) . . ?
C19 C18 C17 128.7(8) . . ?
C25 C24 C23 106.5(7) . . ?
C25 C24 H24 126.7 . . ?
C23 C24 H24 126.7 . . ?
C15 C14 C13 104.8(7) . . ?
C15 C14 H14 127.6 . . ?
C13 C14 H14 127.6 . . ?
O1 C2 W 178.1(7) . . ?
C20 C19 C18 106.9(8) . . ?
C20 C19 H19 126.5 . . ?
C18 C19 H19 126.5 . . ?
N6 B N2 108.2(6) . . ?
N6 B N4 109.5(6) . . ?
N2 B N4 108.8(6) . . ?
N6 B H99 112(4) . . ?
N2 B H99 105(4) . . ?
N4 B H99 113(5) . . ?
N1 C13 C14 111.7(7) . . ?
N1 C13 C12 123.1(7) . . ?
C14 C13 C12 125.2(8) . . ?
N5 C23 C24 108.4(7) . . ?
N5 C23 C22 122.5(7) . . ?
C24 C23 C22 129.1(7) . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C8 C7 C6 111.3(7) . . ?
C8 C7 H7A 109.4 . . ?
C6 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C6 C11 111.0(7) . . ?
C7 C6 P 116.4(6) . . ?
C11 C6 P 110.6(6) . . ?
C7 C6 H6 106.0 . . ?
C11 C6 H6 106.0 . . ?
P C6 H6 106.0 . . ?
N6 C25 C24 108.1(7) . . ?
N6 C25 C26 123.8(7) . . ?
C24 C25 C26 128.2(7) . . ?
C10 C11 C6 112.2(8) . . ?
C10 C11 H11A 109.2 . . ?
C6 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
C6 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C8 C9 C10 111.9(8) . . ?
C8 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
P C1 W 163.4(5) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C9 C10 C11 112.3(7) . . ?
C9 C10 H10A 109.1 . . ?
C11 C10 H10A 109.1 . . ?
C9 C10 H10B 109.1 . . ?
C11 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C5 C4 P 174.2(10) . . ?
N2 C15 C14 108.1(7) . . ?
N2 C15 C16 123.2(7) . . ?
C14 C15 C16 128.7(7) . . ?
C9 C8 C7 111.3(8) . . ?
C9 C8 H8A 109.4 . . ?
C7 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
C7 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C4 C5 H5 180.0 . . ?
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 . . ?

_refine_diff_density_max         2.576
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.173




####################################################################### 
# 
# 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_Compound_10
_database_code_depnum_ccdc_archive 'CCDC 1851874'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H45 B2 N12 O4 P W2'
_chemical_formula_sum            'C38 H45 B2 N12 O4 P W2'
_chemical_formula_weight         1154.15

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   15.2850(6)
_cell_length_b                   10.7644(5)
_cell_length_c                   27.3927(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.766(4)
_cell_angle_gamma                90
_cell_volume                     4497.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    6452
_cell_measurement_theta_min      3.8390
_cell_measurement_theta_max      28.2530

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_F_000             2248
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.021
_exptl_absorpt_coefficient_mu    5.199
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.54791
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_reflns_number            14491
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.318
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4587
_reflns_number_gt                3737
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0370P)²+5.8432P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4587
_refine_ls_number_parameters     290
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0753
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.019
_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
C4 C 0.1525(8) 1.0127(9) 0.5052(3) 0.040(3) Uani 0.5 1 d D . P . .
C5 C 0.0855(14) 1.070(2) 0.5120(7) 0.058(6) Uani 0.339(16) 1 d D U P A 1
H5 H 0.034513 1.114162 0.517062 0.069 Uiso 0.339(16) 1 calc R U P A 1
C5A C 0.0715(15) 1.009(4) 0.5030(16) 0.058(6) Uani 0.161(16) 1 d D U P A 2
H5A H 0.010589 1.006917 0.501244 0.069 Uiso 0.161(16) 1 calc R U P A 2
C3 C 0.2525(3) 0.9177(5) 0.36157(18) 0.0342(11) Uani 1 1 d . . . . .
O2 O 0.2717(3) 1.0135(3) 0.34597(15) 0.0579(11) Uani 1 1 d . . . . .
H99 H 0.261(2) 0.383(4) 0.3371(14) 0.016(10) Uiso 1 1 d . . . . .
C1 C 0.2381(3) 0.8423(4) 0.44960(17) 0.0300(11) Uani 1 1 d . . . . .
C2 C 0.0964(3) 0.8347(5) 0.39368(19) 0.0374(12) Uani 1 1 d . . . . .
C6 C 0.1526(3) 0.5140(4) 0.26714(17) 0.0289(11) Uani 1 1 d . . . . .
C7 C 0.1171(3) 0.6171(5) 0.24451(18) 0.0331(11) Uani 1 1 d . . . . .
H7 H 0.086827 0.619809 0.213935 0.040 Uiso 1 1 calc R U . . .
C8 C 0.1344(3) 0.7164(4) 0.27541(17) 0.0281(10) Uani 1 1 d . . . . .
C9 C 0.1119(3) 0.8507(5) 0.26750(19) 0.0414(13) Uani 1 1 d . . . . .
H9A H 0.085848 0.882752 0.295851 0.062 Uiso 1 1 calc R U . . .
H9B H 0.071224 0.858763 0.239458 0.062 Uiso 1 1 calc R U . . .
H9C H 0.164259 0.896597 0.262125 0.062 Uiso 1 1 calc R U . . .
C10 C 0.2108(4) 0.2400(4) 0.4120(3) 0.0476(15) Uani 1 1 d . . . . .
H10A H 0.180073 0.217832 0.381503 0.071 Uiso 1 1 calc R U . . .
H10B H 0.194468 0.184034 0.437118 0.071 Uiso 1 1 calc R U . . .
H10C H 0.272792 0.234597 0.408706 0.071 Uiso 1 1 calc R U . . .
C11 C 0.1874(3) 0.3693(4) 0.42526(18) 0.0305(11) Uani 1 1 d . . . . .
C12 C 0.1452(3) 0.4122(4) 0.46464(18) 0.0318(11) Uani 1 1 d . . . . .
H12 H 0.124841 0.364530 0.489848 0.038 Uiso 1 1 calc R U . . .
C13 C 0.1389(3) 0.5397(4) 0.45965(17) 0.0297(11) Uani 1 1 d . . . . .
C14 C 0.0980(3) 0.6312(5) 0.49287(18) 0.0419(13) Uani 1 1 d . . . . .
H14A H 0.142892 0.682299 0.508606 0.063 Uiso 1 1 calc R U . . .
H14B H 0.067845 0.587065 0.517197 0.063 Uiso 1 1 calc R U . . .
H14C H 0.057032 0.682515 0.473998 0.063 Uiso 1 1 calc R U . . .
C15 C 0.4385(3) 0.3815(5) 0.3312(2) 0.0448(14) Uani 1 1 d . . . . .
H15A H 0.415626 0.317874 0.351362 0.067 Uiso 1 1 calc R U . . .
H15B H 0.500789 0.371258 0.330261 0.067 Uiso 1 1 calc R U . . .
H15C H 0.411541 0.375143 0.298643 0.067 Uiso 1 1 calc R U . . .
C16 C 0.4194(3) 0.5051(4) 0.35176(17) 0.0303(11) Uani 1 1 d . . . . .
C17 C 0.4744(3) 0.5994(5) 0.36666(17) 0.0323(11) Uani 1 1 d . . . . .
H17 H 0.535138 0.598741 0.366094 0.039 Uiso 1 1 calc R U . . .
C18 C 0.4245(3) 0.6958(5) 0.38271(17) 0.0299(11) Uani 1 1 d . . . . .
C19 C 0.4522(3) 0.8196(5) 0.4028(2) 0.0414(13) Uani 1 1 d . . . . .
H19A H 0.440199 0.882192 0.378280 0.062 Uiso 1 1 calc R U . . .
H19B H 0.513939 0.818218 0.411926 0.062 Uiso 1 1 calc R U . . .
H19C H 0.420425 0.837922 0.430954 0.062 Uiso 1 1 calc R U . . .
C20 C 0.1522(4) 0.3814(5) 0.2503(2) 0.0464(14) Uani 1 1 d . . . . .
H20A H 0.210954 0.356098 0.244844 0.070 Uiso 1 1 calc R U . . .
H20B H 0.116159 0.373902 0.220382 0.070 Uiso 1 1 calc R U . . .
H20C H 0.129148 0.329431 0.274872 0.070 Uiso 1 1 calc R U . . .
B B 0.2496(3) 0.4749(5) 0.3489(2) 0.0237(11) Uani 1 1 d . . . . .
N1 N 0.3387(2) 0.6627(3) 0.37778(13) 0.0245(8) Uani 1 1 d . . . . .
N2 N 0.3365(2) 0.5444(3) 0.35821(14) 0.0253(8) Uani 1 1 d . . . . .
N3 N 0.1783(2) 0.6764(3) 0.31641(13) 0.0222(8) Uani 1 1 d . . . . .
N4 N 0.1902(2) 0.5495(3) 0.31080(14) 0.0235(8) Uani 1 1 d . . . . .
N5 N 0.1761(2) 0.5749(3) 0.41881(13) 0.0236(8) Uani 1 1 d . . . . .
N6 N 0.2051(2) 0.4682(3) 0.39734(13) 0.0244(8) Uani 1 1 d . . . . .
O1 O 0.0290(3) 0.8819(4) 0.39448(16) 0.0596(12) Uani 1 1 d . . . . .
P P 0.250000 0.94783(16) 0.500000 0.0385(5) Uani 1 2 d S T P A .
W W 0.21538(2) 0.75992(2) 0.39185(2) 0.02324(8) 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
C4 C5 1.221(17) . ?
C4 C5A 1.24(2) . ?
C4 P 1.660(10) . ?
C3 O2 1.161(6) . ?
C3 W 1.989(5) . ?
C1 P 1.788(5) . ?
C1 W 1.827(5) . ?
C2 O1 1.150(5) . ?
C2 W 1.992(5) . ?
C6 N4 1.348(6) . ?
C6 C7 1.366(7) . ?
C6 C20 1.500(6) . ?
C7 C8 1.378(6) . ?
C8 N3 1.340(6) . ?
C8 C9 1.499(6) . ?
C10 C11 1.489(6) . ?
C11 N6 1.348(6) . ?
C11 C12 1.372(7) . ?
C12 C13 1.382(6) . ?
C13 N5 1.343(6) . ?
C13 C14 1.505(6) . ?
C15 C16 1.482(6) . ?
C16 N2 1.359(5) . ?
C16 C17 1.363(6) . ?
C17 C18 1.376(6) . ?
C18 N1 1.357(5) . ?
C18 C19 1.492(7) . ?
B N2 1.531(6) . ?
B N6 1.532(6) . ?
B N4 1.560(6) . ?
N1 N2 1.381(5) . ?
N1 W 2.212(3) . ?
N3 N4 1.389(5) . ?
N3 W 2.291(3) . ?
N5 N6 1.377(5) . ?
N5 W 2.221(4) . ?

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
C5 C4 P 173.0(16) . . ?
C5A C4 P 152(2) . . ?
O2 C3 W 176.0(4) . . ?
P C1 W 168.8(3) . . ?
O1 C2 W 177.6(5) . . ?
N4 C6 C7 107.9(4) . . ?
N4 C6 C20 122.3(4) . . ?
C7 C6 C20 129.8(5) . . ?
C6 C7 C8 107.2(4) . . ?
N3 C8 C7 109.4(4) . . ?
N3 C8 C9 121.9(4) . . ?
C7 C8 C9 128.8(4) . . ?
N6 C11 C12 107.6(4) . . ?
N6 C11 C10 122.6(5) . . ?
C12 C11 C10 129.7(5) . . ?
C11 C12 C13 106.8(4) . . ?
N5 C13 C12 109.4(4) . . ?
N5 C13 C14 122.3(4) . . ?
C12 C13 C14 128.3(4) . . ?
N2 C16 C17 106.9(4) . . ?
N2 C16 C15 122.5(4) . . ?
C17 C16 C15 130.5(4) . . ?
C16 C17 C18 108.3(4) . . ?
N1 C18 C17 108.8(4) . . ?
N1 C18 C19 121.4(4) . . ?
C17 C18 C19 129.8(4) . . ?
N2 B N6 107.9(4) . . ?
N2 B N4 108.7(4) . . ?
N6 B N4 109.4(4) . . ?
C18 N1 N2 106.2(3) . . ?
C18 N1 W 133.4(3) . . ?
N2 N1 W 120.3(2) . . ?
C16 N2 N1 109.7(3) . . ?
C16 N2 B 129.3(4) . . ?
N1 N2 B 121.0(3) . . ?
C8 N3 N4 106.6(4) . . ?
C8 N3 W 135.3(3) . . ?
N4 N3 W 117.3(3) . . ?
C6 N4 N3 109.0(4) . . ?
C6 N4 B 130.1(4) . . ?
N3 N4 B 120.5(3) . . ?
C13 N5 N6 106.6(4) . . ?
C13 N5 W 132.0(3) . . ?
N6 N5 W 120.3(3) . . ?
C11 N6 N5 109.5(4) . . ?
C11 N6 B 130.2(4) . . ?
N5 N6 B 120.3(3) . . ?
C4 P C4 130.3(8) 2_556 . ?
C4 P C1 104.3(4) 2_556 . ?
C4 P C1 106.7(4) . . ?
C4 P C1 106.7(4) 2_556 2_556 ?
C4 P C1 104.3(4) . 2_556 ?
C1 P C1 101.1(3) . 2_556 ?
C1 W C3 84.5(2) . . ?
C1 W C2 84.5(2) . . ?
C3 W C2 87.2(2) . . ?
C1 W N1 105.37(17) . . ?
C3 W N1 93.52(17) . . ?
C2 W N1 170.15(17) . . ?
C1 W N5 100.82(17) . . ?
C3 W N5 174.44(15) . . ?
C2 W N5 94.99(17) . . ?
N1 W N5 83.43(13) . . ?
C1 W N3 173.44(16) . . ?
C3 W N3 91.09(17) . . ?
C2 W N3 90.50(17) . . ?
N1 W N3 79.66(12) . . ?
N5 W N3 83.79(13) . . ?

_refine_diff_density_max         1.899
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.125



####################################################################### 
# 
# 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_Compound_13
_database_code_depnum_ccdc_archive 'CCDC 1851877'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-10-11 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         'C50 H54 As B2 N12 O4 P W2'
_chemical_formula_sum            'C50 H54 As B2 N12 O4 P W2'
_chemical_formula_weight         1382.26

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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2582(3)
_cell_length_b                   11.6958(4)
_cell_length_c                   22.3488(6)
_cell_angle_alpha                83.656(3)
_cell_angle_beta                 81.841(2)
_cell_angle_gamma                71.230(3)
_cell_volume                     2751.44(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    10309
_cell_measurement_theta_min      3.9870
_cell_measurement_theta_max      73.5500

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_F_000             1352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.077
_exptl_absorpt_coefficient_mu    8.990
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.66275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_reflns_number            17344
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         4.002
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_full        66.599
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             9655
_reflns_number_gt                8716
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_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)+(0.0949P)²+3.7623P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9655
_refine_ls_number_parameters     669
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1423
_refine_ls_wR_factor_gt          0.1363
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.047
_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
W1 W 0.67999(2) 0.22038(2) 0.88086(2) 0.03506(11) Uani 1 1 d . . . . .
W2 W 0.74311(3) 0.29619(2) 0.61499(2) 0.03899(11) Uani 1 1 d . . . . .
As As 0.24974(8) 0.66541(8) 0.69661(4) 0.0549(2) Uani 1 1 d . . . . .
P P 0.52722(15) 0.26339(14) 0.74584(7) 0.0398(3) Uani 1 1 d . . . . .
N5 N 0.6785(5) 0.3980(4) 0.9063(2) 0.0372(10) Uani 1 1 d . . . . .
O3 O 0.5657(5) 0.5674(5) 0.6138(3) 0.0628(14) Uani 1 1 d . . . . .
N9 N 0.8842(5) 0.1164(4) 0.6040(2) 0.0385(11) Uani 1 1 d . . . . .
N6 N 0.7782(5) 0.4063(5) 0.9342(2) 0.0383(10) Uani 1 1 d . . . . .
N11 N 0.8989(6) 0.3358(5) 0.6497(2) 0.0454(12) Uani 1 1 d . . . . .
N8 N 0.9754(5) 0.3047(5) 0.5176(2) 0.0420(11) Uani 1 1 d . . . . .
N3 N 0.8813(4) 0.1947(5) 0.8500(2) 0.0355(10) Uani 1 1 d . . . . .
O2 O 0.4041(5) 0.2447(6) 0.9412(3) 0.0638(14) Uani 1 1 d . . . . .
N7 N 0.8463(5) 0.3391(5) 0.5234(2) 0.0403(11) Uani 1 1 d . . . . .
N10 N 1.0056(5) 0.1065(5) 0.5794(2) 0.0417(11) Uani 1 1 d . . . . .
N4 N 0.9513(5) 0.2433(5) 0.8800(2) 0.0383(10) Uani 1 1 d . . . . .
O4 O 0.5372(5) 0.2379(6) 0.5524(3) 0.0630(14) Uani 1 1 d . . . . .
O1 O 0.6791(6) -0.0438(5) 0.8664(3) 0.0669(15) Uani 1 1 d . . . . .
N12 N 1.0217(5) 0.2851(5) 0.6259(3) 0.0453(12) Uani 1 1 d . . . . .
N2 N 0.8570(5) 0.1979(5) 0.9845(2) 0.0436(12) Uani 1 1 d . . . . .
N1 N 0.7574(5) 0.1625(5) 0.9728(2) 0.0409(11) Uani 1 1 d . . . . .
C3 C 0.5041(6) 0.2388(6) 0.9199(3) 0.0417(13) Uani 1 1 d . . . . .
C29 C 1.0703(6) 0.2160(6) 0.8515(3) 0.0443(14) Uani 1 1 d . . . . .
C27 C 0.9584(6) 0.1375(6) 0.8042(3) 0.0436(14) Uani 1 1 d . . . . .
C44 C 1.0700(7) -0.0107(6) 0.5718(3) 0.0482(15) Uani 1 1 d . . . . .
C39 C 1.0196(7) 0.3524(6) 0.4647(3) 0.0455(14) Uani 1 1 d . . . . .
C5 C 0.6307(7) 0.4693(6) 0.6143(3) 0.0492(15) Uani 1 1 d . . . . .
C1 C 0.6074(6) 0.2573(6) 0.8100(3) 0.0399(12) Uani 1 1 d . . . . .
C28 C 1.0779(6) 0.1505(6) 0.8035(3) 0.0437(14) Uani 1 1 d . . . . .
H28 H 1.1484 0.1204 0.7758 0.052 Uiso 1 1 calc R U . . .
C43 C 0.9880(8) -0.0782(6) 0.5925(3) 0.0511(16) Uani 1 1 d . . . . .
H43 H 1.0066 -0.1617 0.5929 0.061 Uiso 1 1 calc R U . . .
C36 C 0.6754(7) 0.4605(7) 0.4629(3) 0.0550(17) Uani 1 1 d . . . . .
H36A H 0.6363 0.3978 0.4664 0.082 Uiso 1 1 calc R U . . .
H36B H 0.6700 0.5005 0.4230 0.082 Uiso 1 1 calc R U . . .
H36C H 0.6327 0.5181 0.4924 0.082 Uiso 1 1 calc R U . . .
C48 C 1.0283(8) 0.3844(7) 0.7018(3) 0.0538(17) Uani 1 1 d . . . . .
H48 H 1.0574 0.4179 0.7303 0.065 Uiso 1 1 calc R U . . .
C37 C 0.8088(7) 0.4070(5) 0.4732(3) 0.0444(14) Uani 1 1 d . . . . .
C47 C 0.9026(8) 0.3973(6) 0.6966(3) 0.0532(17) Uani 1 1 d . . . . .
C24 C 0.9003(7) 0.1415(7) 1.0366(3) 0.0506(16) Uani 1 1 d . . . . .
C49 C 1.0993(7) 0.3146(6) 0.6581(3) 0.0511(16) Uani 1 1 d . . . . .
C38 C 0.9155(7) 0.4186(5) 0.4355(3) 0.0451(14) Uani 1 1 d . . . . .
H38 H 0.9163 0.4622 0.3981 0.054 Uiso 1 1 calc R U . . .
C33 C 0.6260(7) 0.5808(6) 0.9404(4) 0.0548(17) Uani 1 1 d . . . . .
H33 H 0.5799 0.6600 0.9490 0.066 Uiso 1 1 calc R U . . .
C32 C 0.5891(6) 0.5039(6) 0.9092(3) 0.0457(14) Uani 1 1 d . . . . .
C45 C 1.2051(8) -0.0563(7) 0.5452(4) 0.064(2) Uani 1 1 d . . . . .
H45A H 1.2136 -0.0231 0.5041 0.096 Uiso 1 1 calc R U . . .
H45B H 1.2314 -0.1430 0.5458 0.096 Uiso 1 1 calc R U . . .
H45C H 1.2570 -0.0319 0.5686 0.096 Uiso 1 1 calc R U . . .
C26 C 0.9170(7) 0.0750(7) 0.7601(3) 0.0555(17) Uani 1 1 d . . . . .
H26A H 0.8898 0.0100 0.7811 0.083 Uiso 1 1 calc R U . . .
H26B H 0.9863 0.0431 0.7299 0.083 Uiso 1 1 calc R U . . .
H26C H 0.8484 0.1317 0.7409 0.083 Uiso 1 1 calc R U . . .
C34 C 0.7452(6) 0.5162(7) 0.9562(3) 0.0507(16) Uani 1 1 d . . . . .
C42 C 0.8742(7) 0.0039(6) 0.6123(3) 0.0440(14) Uani 1 1 d . . . . .
C7 C 0.4250(6) 0.4140(6) 0.7393(3) 0.0460(14) Uani 1 1 d . . . . .
C2 C 0.6442(6) 0.2739(6) 0.6849(3) 0.0413(13) Uani 1 1 d . . . . .
C40 C 1.1554(7) 0.3361(7) 0.4453(4) 0.0556(17) Uani 1 1 d . . . . .
H40A H 1.1881 0.3720 0.4731 0.083 Uiso 1 1 calc R U . . .
H40B H 1.1648 0.3745 0.4054 0.083 Uiso 1 1 calc R U . . .
H40C H 1.2011 0.2513 0.4447 0.083 Uiso 1 1 calc R U . . .
C2A C 0.6854(6) 0.0500(6) 0.8713(3) 0.0460(14) Uani 1 1 d . . . . .
C4 C 0.6161(7) 0.2573(6) 0.5736(3) 0.0457(14) Uani 1 1 d . . . . .
C22 C 0.7384(8) 0.0841(7) 1.0202(3) 0.0557(18) Uani 1 1 d . . . . .
C41 C 0.7549(8) -0.0193(7) 0.6388(3) 0.0575(17) Uani 1 1 d . . . . .
H41A H 0.7226 0.0231 0.6750 0.086 Uiso 1 1 calc R U . . .
H41B H 0.7709 -0.1045 0.6485 0.086 Uiso 1 1 calc R U . . .
H41C H 0.6942 0.0086 0.6101 0.086 Uiso 1 1 calc R U . . .
C8 C 0.3566(7) 0.5116(7) 0.7260(3) 0.0514(16) Uani 1 1 d . . . . .
C31 C 0.4655(7) 0.5286(7) 0.8841(4) 0.063(2) Uani 1 1 d . . . . .
H31A H 0.4807 0.4962 0.8451 0.095 Uiso 1 1 calc R U . . .
H31B H 0.4245 0.6144 0.8801 0.095 Uiso 1 1 calc R U . . .
H31C H 0.4125 0.4911 0.9111 0.095 Uiso 1 1 calc R U . . .
C9 C 0.1016(7) 0.6707(6) 0.7563(3) 0.0493(15) Uani 1 1 d . . . . .
C50 C 1.2406(8) 0.2712(8) 0.6426(4) 0.068(2) Uani 1 1 d . . . . .
H50A H 1.2709 0.1845 0.6482 0.102 Uiso 1 1 calc R U . . .
H50B H 1.2791 0.3055 0.6687 0.102 Uiso 1 1 calc R U . . .
H50C H 1.2618 0.2960 0.6012 0.102 Uiso 1 1 calc R U . . .
B1 B 0.8956(6) 0.2963(7) 0.9414(3) 0.0394(14) Uani 1 1 d . . . . .
C12 C -0.1199(8) 0.6731(8) 0.8276(4) 0.0631(19) Uani 1 1 d . . . . .
H12 H -0.1943 0.6744 0.8521 0.076 Uiso 1 1 calc R U . . .
C30 C 1.1715(6) 0.2535(7) 0.8727(4) 0.0573(18) Uani 1 1 d . . . . .
H30A H 1.1456 0.3402 0.8728 0.086 Uiso 1 1 calc R U . . .
H30B H 1.2480 0.2262 0.8459 0.086 Uiso 1 1 calc R U . . .
H30C H 1.1858 0.2183 0.9129 0.086 Uiso 1 1 calc R U . . .
C46 C 0.7865(9) 0.4626(7) 0.7352(3) 0.064(2) Uani 1 1 d . . . . .
H46A H 0.7352 0.5285 0.7114 0.096 Uiso 1 1 calc R U . . .
H46B H 0.8096 0.4934 0.7684 0.096 Uiso 1 1 calc R U . . .
H46C H 0.7398 0.4078 0.7506 0.096 Uiso 1 1 calc R U . . .
B2 B 1.0496(7) 0.2187(7) 0.5667(3) 0.0432(15) Uani 1 1 d . . . . .
C23 C 0.8294(8) 0.0688(8) 1.0599(4) 0.062(2) Uani 1 1 d . . . . .
H23 H 0.8394 0.0185 1.0954 0.075 Uiso 1 1 calc R U . . .
C35 C 0.8267(7) 0.5528(8) 0.9927(4) 0.066(2) Uani 1 1 d . . . . .
H35A H 0.8231 0.5143 1.0328 0.099 Uiso 1 1 calc R U . . .
H35B H 0.7970 0.6391 0.9948 0.099 Uiso 1 1 calc R U . . .
H35C H 0.9123 0.5285 0.9738 0.099 Uiso 1 1 calc R U . . .
C10 C 0.1029(9) 0.5902(8) 0.8065(4) 0.064(2) Uani 1 1 d . . . . .
H10 H 0.1787 0.5355 0.8169 0.077 Uiso 1 1 calc R U . . .
C21 C 0.6390(9) 0.0249(9) 1.0236(4) 0.070(2) Uani 1 1 d . . . . .
H21A H 0.5640 0.0822 1.0098 0.105 Uiso 1 1 calc R U . . .
H21B H 0.6205 -0.0033 1.0648 0.105 Uiso 1 1 calc R U . . .
H21C H 0.6681 -0.0424 0.9985 0.105 Uiso 1 1 calc R U . . .
C13 C -0.1225(9) 0.7528(9) 0.7787(4) 0.073(2) Uani 1 1 d . . . . .
H13 H -0.1984 0.8091 0.7695 0.088 Uiso 1 1 calc R U . . .
C25 C 1.0090(8) 0.1602(9) 1.0626(4) 0.067(2) Uani 1 1 d . . . . .
H25A H 1.0797 0.1503 1.0319 0.101 Uiso 1 1 calc R U . . .
H25B H 1.0325 0.1019 1.0960 0.101 Uiso 1 1 calc R U . . .
H25C H 0.9838 0.2404 1.0763 0.101 Uiso 1 1 calc R U . . .
C11 C -0.0093(9) 0.5915(8) 0.8410(4) 0.070(2) Uani 1 1 d . . . . .
H11 H -0.0089 0.5355 0.8740 0.084 Uiso 1 1 calc R U . . .
C14 C -0.0112(9) 0.7497(7) 0.7424(4) 0.067(2) Uani 1 1 d . . . . .
H14 H -0.0135 0.8025 0.7080 0.081 Uiso 1 1 calc R U . . .
C15 C 0.3257(9) 0.7723(8) 0.7288(4) 0.067(2) Uani 1 1 d . U . . .
C16 C 0.3090(12) 0.7985(11) 0.7891(5) 0.089(3) Uani 1 1 d . U . . .
H16 H 0.2584 0.7657 0.8178 0.106 Uiso 1 1 calc R U . . .
C17 C 0.3673(15) 0.8721(13) 0.8053(7) 0.111(4) Uani 1 1 d . U . . .
H17 H 0.3543 0.8921 0.8453 0.134 Uiso 1 1 calc R U . . .
C18 C 0.4459(16) 0.9189(13) 0.7642(7) 0.119(4) Uani 1 1 d . U . . .
H18 H 0.4926 0.9622 0.7772 0.143 Uiso 1 1 calc R U . . .
C19 C 0.454(2) 0.9012(16) 0.7048(9) 0.147(5) Uani 1 1 d . U . . .
H19 H 0.5039 0.9357 0.6763 0.176 Uiso 1 1 calc R U . . .
C20 C 0.3886(15) 0.8306(14) 0.6863(7) 0.116(4) Uani 1 1 d . U . . .
H20 H 0.3879 0.8237 0.6454 0.139 Uiso 1 1 calc R U . . .
H99 H 0.968(7) 0.331(7) 0.960(3) 0.044(19) Uiso 1 1 d . . . . .
H98 H 1.160(9) 0.199(8) 0.549(4) 0.07(3) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C1 1.831(6) . ?
W1 C3 2.002(6) . ?
W1 C2A 2.007(7) . ?
W1 N3 2.206(5) . ?
W1 N5 2.208(5) . ?
W1 N1 2.295(5) . ?
W2 C2 1.830(7) . ?
W2 C4 1.997(7) . ?
W2 C5 2.012(7) . ?
W2 N9 2.205(5) . ?
W2 N11 2.209(6) . ?
W2 N7 2.294(5) . ?
As C8 1.919(7) . ?
As C15 1.969(9) . ?
As C9 1.972(7) . ?
P C7 1.770(7) . ?
P C2 1.779(7) . ?
P C1 1.783(6) . ?
N5 C32 1.322(9) . ?
N5 N6 1.393(7) . ?
O3 C5 1.146(9) . ?
N9 C42 1.346(8) . ?
N9 N10 1.372(8) . ?
N6 C34 1.345(9) . ?
N6 B1 1.533(9) . ?
N11 C47 1.348(8) . ?
N11 N12 1.371(8) . ?
N8 C39 1.348(9) . ?
N8 N7 1.369(8) . ?
N8 B2 1.545(9) . ?
N3 C27 1.332(8) . ?
N3 N4 1.383(7) . ?
O2 C3 1.142(8) . ?
N7 C37 1.338(8) . ?
N10 C44 1.346(9) . ?
N10 B2 1.531(9) . ?
N4 C29 1.353(8) . ?
N4 B1 1.535(9) . ?
O4 C4 1.158(9) . ?
O1 C2A 1.141(9) . ?
N12 C49 1.351(9) . ?
N12 B2 1.551(9) . ?
N2 C24 1.348(8) . ?
N2 N1 1.379(7) . ?
N2 B1 1.549(9) . ?
N1 C22 1.362(9) . ?
C29 C28 1.364(10) . ?
C29 C30 1.494(10) . ?
C27 C28 1.400(10) . ?
C27 C26 1.493(10) . ?
C44 C43 1.399(11) . ?
C44 C45 1.498(11) . ?
C39 C38 1.387(10) . ?
C39 C40 1.485(10) . ?
C28 H28 0.9300 . ?
C43 C42 1.379(10) . ?
C43 H43 0.9300 . ?
C36 C37 1.471(10) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C48 C49 1.340(11) . ?
C48 C47 1.394(12) . ?
C48 H48 0.9300 . ?
C37 C38 1.402(10) . ?
C47 C46 1.489(12) . ?
C24 C23 1.361(11) . ?
C24 C25 1.511(9) . ?
C49 C50 1.506(12) . ?
C38 H38 0.9300 . ?
C33 C34 1.385(10) . ?
C33 C32 1.390(10) . ?
C33 H33 0.9300 . ?
C32 C31 1.503(9) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C34 C35 1.494(10) . ?
C42 C41 1.483(11) . ?
C7 C8 1.188(10) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C22 C23 1.405(10) . ?
C22 C21 1.484(10) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C9 C14 1.362(11) . ?
C9 C10 1.381(11) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
B1 H99 1.17(8) . ?
C12 C11 1.352(13) . ?
C12 C13 1.353(13) . ?
C12 H12 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
B2 H98 1.21(9) . ?
C23 H23 0.9300 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C10 C11 1.380(13) . ?
C10 H10 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C13 C14 1.385(13) . ?
C13 H13 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C11 H11 0.9300 . ?
C14 H14 0.9300 . ?
C15 C20 1.358(15) . ?
C15 C16 1.389(14) . ?
C16 C17 1.342(17) . ?
C16 H16 0.9300 . ?
C17 C18 1.376(19) . ?
C17 H17 0.9300 . ?
C18 C19 1.35(2) . ?
C18 H18 0.9300 . ?
C19 C20 1.40(2) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?

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 W1 C3 84.6(3) . . ?
C1 W1 C2A 85.2(3) . . ?
C3 W1 C2A 84.2(3) . . ?
C1 W1 N3 102.9(2) . . ?
C3 W1 N3 172.4(2) . . ?
C2A W1 N3 96.4(2) . . ?
C1 W1 N5 103.4(2) . . ?
C3 W1 N5 93.8(2) . . ?
C2A W1 N5 171.0(2) . . ?
N3 W1 N5 84.47(19) . . ?
C1 W1 N1 174.2(2) . . ?
C3 W1 N1 90.9(2) . . ?
C2A W1 N1 90.7(2) . . ?
N3 W1 N1 81.58(18) . . ?
N5 W1 N1 80.56(19) . . ?
C2 W2 C4 84.8(3) . . ?
C2 W2 C5 85.2(3) . . ?
C4 W2 C5 88.3(3) . . ?
C2 W2 N9 103.6(2) . . ?
C4 W2 N9 93.7(2) . . ?
C5 W2 N9 171.2(3) . . ?
C2 W2 N11 102.2(2) . . ?
C4 W2 N11 172.8(2) . . ?
C5 W2 N11 94.0(3) . . ?
N9 W2 N11 83.0(2) . . ?
C2 W2 N7 173.4(2) . . ?
C4 W2 N7 91.1(2) . . ?
C5 W2 N7 89.6(2) . . ?
N9 W2 N7 81.79(19) . . ?
N11 W2 N7 82.1(2) . . ?
C8 As C15 99.3(4) . . ?
C8 As C9 96.7(3) . . ?
C15 As C9 102.8(3) . . ?
C7 P C2 98.6(3) . . ?
C7 P C1 104.8(3) . . ?
C2 P C1 101.7(3) . . ?
C32 N5 N6 107.3(5) . . ?
C32 N5 W1 132.1(4) . . ?
N6 N5 W1 119.8(4) . . ?
C42 N9 N10 107.5(5) . . ?
C42 N9 W2 132.0(5) . . ?
N10 N9 W2 120.2(4) . . ?
C34 N6 N5 108.9(5) . . ?
C34 N6 B1 130.1(5) . . ?
N5 N6 B1 120.7(5) . . ?
C47 N11 N12 106.4(6) . . ?
C47 N11 W2 132.5(5) . . ?
N12 N11 W2 120.8(4) . . ?
C39 N8 N7 110.3(5) . . ?
C39 N8 B2 129.2(6) . . ?
N7 N8 B2 120.5(5) . . ?
C27 N3 N4 107.0(5) . . ?
C27 N3 W1 132.2(4) . . ?
N4 N3 W1 120.8(4) . . ?
C37 N7 N8 107.4(5) . . ?
C37 N7 W2 133.9(4) . . ?
N8 N7 W2 118.1(4) . . ?
C44 N10 N9 109.3(6) . . ?
C44 N10 B2 130.1(6) . . ?
N9 N10 B2 120.6(5) . . ?
C29 N4 N3 108.9(5) . . ?
C29 N4 B1 130.6(5) . . ?
N3 N4 B1 119.6(5) . . ?
C49 N12 N11 109.4(6) . . ?
C49 N12 B2 130.9(6) . . ?
N11 N12 B2 119.3(5) . . ?
C24 N2 N1 110.2(5) . . ?
C24 N2 B1 130.6(5) . . ?
N1 N2 B1 119.1(5) . . ?
C22 N1 N2 106.1(5) . . ?
C22 N1 W1 134.3(4) . . ?
N2 N1 W1 119.1(4) . . ?
O2 C3 W1 177.0(6) . . ?
N4 C29 C28 108.3(6) . . ?
N4 C29 C30 122.9(6) . . ?
C28 C29 C30 128.7(6) . . ?
N3 C27 C28 109.4(6) . . ?
N3 C27 C26 123.3(6) . . ?
C28 C27 C26 127.2(6) . . ?
N10 C44 C43 107.7(6) . . ?
N10 C44 C45 124.5(7) . . ?
C43 C44 C45 127.8(7) . . ?
N8 C39 C38 106.9(6) . . ?
N8 C39 C40 124.1(6) . . ?
C38 C39 C40 129.0(6) . . ?
O3 C5 W2 179.3(7) . . ?
P C1 W1 167.2(4) . . ?
C29 C28 C27 106.3(6) . . ?
C29 C28 H28 126.9 . . ?
C27 C28 H28 126.9 . . ?
C42 C43 C44 106.2(6) . . ?
C42 C43 H43 126.9 . . ?
C44 C43 H43 126.9 . . ?
C37 C36 H36A 109.5 . . ?
C37 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C37 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C49 C48 C47 107.2(6) . . ?
C49 C48 H48 126.4 . . ?
C47 C48 H48 126.4 . . ?
N7 C37 C38 108.8(6) . . ?
N7 C37 C36 123.2(6) . . ?
C38 C37 C36 128.0(6) . . ?
N11 C47 C48 108.6(7) . . ?
N11 C47 C46 122.3(7) . . ?
C48 C47 C46 129.0(7) . . ?
N2 C24 C23 108.2(6) . . ?
N2 C24 C25 123.7(7) . . ?
C23 C24 C25 128.1(7) . . ?
C48 C49 N12 108.3(7) . . ?
C48 C49 C50 130.1(7) . . ?
N12 C49 C50 121.6(7) . . ?
C39 C38 C37 106.6(6) . . ?
C39 C38 H38 126.7 . . ?
C37 C38 H38 126.7 . . ?
C34 C33 C32 106.3(6) . . ?
C34 C33 H33 126.8 . . ?
C32 C33 H33 126.8 . . ?
N5 C32 C33 109.7(6) . . ?
N5 C32 C31 122.5(6) . . ?
C33 C32 C31 127.7(6) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C27 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N6 C34 C33 107.7(6) . . ?
N6 C34 C35 123.1(6) . . ?
C33 C34 C35 129.1(7) . . ?
N9 C42 C43 109.3(6) . . ?
N9 C42 C41 122.0(6) . . ?
C43 C42 C41 128.6(6) . . ?
C8 C7 P 170.0(6) . . ?
P C2 W2 170.8(4) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O1 C2A W1 175.0(6) . . ?
O4 C4 W2 176.0(6) . . ?
N1 C22 C23 108.6(6) . . ?
N1 C22 C21 122.1(6) . . ?
C23 C22 C21 129.2(7) . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C7 C8 As 174.6(6) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C14 C9 C10 118.7(8) . . ?
C14 C9 As 116.7(6) . . ?
C10 C9 As 124.1(6) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N6 B1 N4 110.5(5) . . ?
N6 B1 N2 108.8(5) . . ?
N4 B1 N2 108.3(5) . . ?
N6 B1 H99 106(4) . . ?
N4 B1 H99 110(4) . . ?
N2 B1 H99 113(4) . . ?
C11 C12 C13 120.2(9) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C47 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N10 B2 N8 109.6(5) . . ?
N10 B2 N12 108.5(6) . . ?
N8 B2 N12 108.8(5) . . ?
N10 B2 H98 115(4) . . ?
N8 B2 H98 107(4) . . ?
N12 B2 H98 108(4) . . ?
C24 C23 C22 106.9(6) . . ?
C24 C23 H23 126.6 . . ?
C22 C23 H23 126.6 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C11 C10 C9 119.5(8) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C12 C13 C14 119.5(8) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C12 C11 C10 121.0(9) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C9 C14 C13 121.1(8) . . ?
C9 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C20 C15 C16 120.1(11) . . ?
C20 C15 As 115.0(9) . . ?
C16 C15 As 124.7(7) . . ?
C17 C16 C15 118.7(11) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C16 C17 C18 121.9(13) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 H17 119.1 . . ?
C19 C18 C17 119.3(14) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C20 119.7(15) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C15 C20 C19 119.4(14) . . ?
C15 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?

_refine_diff_density_max         2.320
_refine_diff_density_min         -1.746
_refine_diff_density_rms         0.170



####################################################################### 
# 
# 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_Compound_2a
_database_code_depnum_ccdc_archive 'CCDC 1851869'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H36 B Mo N6 O2 P Si'
_chemical_formula_sum            'C29 H36 B Mo N6 O2 P Si'
_chemical_formula_weight         666.45

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   17.0572(4)
_cell_length_b                   10.5503(2)
_cell_length_c                   17.9411(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3228.65(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.01(1)
_cell_measurement_reflns_used    14075
_cell_measurement_theta_min      3.7910
_cell_measurement_theta_max      28.0630

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_F_000             1376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.129
_exptl_absorpt_coefficient_mu    0.528
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.01(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_reflns_number            28899
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.275
_diffrn_reflns_theta_max         28.892
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             6939
_reflns_number_gt                6359
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_max     0.745
_reflns_Friedel_fraction_full    0.949

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0312P)²+1.4771P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2648 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6939
_refine_ls_number_parameters     383
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0696
_refine_ls_wR_factor_gt          0.0657
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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
N2 N 0.37698(18) 0.1918(3) 0.15425(17) 0.0224(7) Uani 1 1 d . . . . .
N6 N 0.25994(18) 0.0549(3) 0.18129(18) 0.0248(7) Uani 1 1 d . . . . .
N4 N 0.24417(17) 0.2528(3) 0.10435(17) 0.0231(7) Uani 1 1 d . . . . .
C50 C 0.4790(2) 0.3808(4) 0.2912(2) 0.0344(10) Uani 1 1 d . . . . .
H50A H 0.458195 0.464427 0.283873 0.052 Uiso 1 1 calc R U . . .
H50B H 0.535183 0.384621 0.292536 0.052 Uiso 1 1 calc R U . . .
H50C H 0.459875 0.347176 0.337524 0.052 Uiso 1 1 calc R U . . .
C53 C 0.4502(2) 0.1801(4) 0.1265(2) 0.0282(8) Uani 1 1 d . . . . .
C51 C 0.4536(2) 0.2973(4) 0.2288(2) 0.0269(8) Uani 1 1 d . . . . .
C52 C 0.5000(2) 0.2457(4) 0.1732(2) 0.0302(9) Uani 1 1 d . . . . .
H52 H 0.554079 0.253720 0.168305 0.036 Uiso 1 1 calc R U . . .
P P 0.13001(6) 0.43336(9) 0.40971(6) 0.0263(2) Uani 1 1 d . . . . .
C56 C 0.2106(2) 0.0037(3) 0.2887(2) 0.0284(9) Uani 1 1 d . . . . .
C63 C 0.2178(2) 0.2937(4) 0.0373(2) 0.0282(9) Uani 1 1 d . . . . .
C4 C 0.0803(2) 0.3052(4) 0.4524(2) 0.0293(9) Uani 1 1 d . . . . .
C58 C 0.2476(2) -0.0719(4) 0.1795(2) 0.0307(9) Uani 1 1 d . . . . .
C61 C 0.1793(2) 0.4258(4) 0.1258(2) 0.0274(8) Uani 1 1 d . . . . .
C62 C 0.1767(2) 0.4043(4) 0.0495(2) 0.0306(9) Uani 1 1 d . . . . .
H62 H 0.152217 0.454499 0.013831 0.037 Uiso 1 1 calc R U . . .
C57 C 0.2158(2) -0.1058(4) 0.2471(2) 0.0315(9) Uani 1 1 d . . . . .
H57 H 0.200726 -0.186679 0.261802 0.038 Uiso 1 1 calc R U . . .
C64 C 0.2323(3) 0.2255(5) -0.0340(3) 0.0399(10) Uani 1 1 d . . . . .
H64A H 0.287219 0.228199 -0.045486 0.060 Uiso 1 1 calc R U . . .
H64B H 0.203186 0.265441 -0.073281 0.060 Uiso 1 1 calc R U . . .
H64C H 0.215813 0.138915 -0.029065 0.060 Uiso 1 1 calc R U . . .
C5 C 0.0544(2) 0.2173(4) 0.4867(2) 0.0323(9) Uani 1 1 d . . . . .
C55 C 0.1830(3) 0.0200(4) 0.3674(2) 0.0340(9) Uani 1 1 d . . . . .
H55A H 0.227493 0.029847 0.399708 0.051 Uiso 1 1 calc R U . . .
H55B H 0.153544 -0.053225 0.382219 0.051 Uiso 1 1 calc R U . . .
H55C H 0.150414 0.093976 0.370679 0.051 Uiso 1 1 calc R U . . .
C60 C 0.1413(3) 0.5309(4) 0.1687(2) 0.0366(10) Uani 1 1 d . . . . .
H60A H 0.101703 0.496441 0.200872 0.055 Uiso 1 1 calc R U . . .
H60B H 0.117835 0.589917 0.134703 0.055 Uiso 1 1 calc R U . . .
H60C H 0.180164 0.573690 0.198206 0.055 Uiso 1 1 calc R U . . .
C9 C 0.0511(2) 0.5201(4) 0.3634(2) 0.0267(8) Uani 1 1 d . . . . .
C54 C 0.4676(3) 0.1086(5) 0.0570(3) 0.0448(12) Uani 1 1 d . . . . .
H54A H 0.454624 0.020889 0.064031 0.067 Uiso 1 1 calc R U . . .
H54B H 0.522284 0.116304 0.045350 0.067 Uiso 1 1 calc R U . . .
H54C H 0.436968 0.142548 0.016755 0.067 Uiso 1 1 calc R U . . .
C59 C 0.2686(3) -0.1524(4) 0.1140(3) 0.0471(13) Uani 1 1 d . . . . .
H59A H 0.238619 -0.126019 0.071462 0.071 Uiso 1 1 calc R U . . .
H59B H 0.257230 -0.239500 0.125022 0.071 Uiso 1 1 calc R U . . .
H59C H 0.323488 -0.143300 0.103421 0.071 Uiso 1 1 calc R U . . .
C10 C 0.0657(3) 0.6464(4) 0.3434(2) 0.0351(10) Uani 1 1 d . . . . .
H10 H 0.114233 0.682104 0.354229 0.042 Uiso 1 1 calc R U . . .
Si Si 0.02477(7) 0.07835(11) 0.54341(7) 0.0332(3) Uani 1 1 d . . . . .
C6 C -0.0244(4) -0.0397(5) 0.4827(3) 0.0602(15) Uani 1 1 d . . . . .
H6A H 0.011952 -0.069612 0.445858 0.090 Uiso 1 1 calc R U . . .
H6B H -0.068423 -0.000799 0.458443 0.090 Uiso 1 1 calc R U . . .
H6C H -0.042182 -0.109663 0.512429 0.090 Uiso 1 1 calc R U . . .
O2 O 0.3088(2) 0.5876(3) 0.30093(18) 0.0516(9) Uani 1 1 d . . . . .
C14 C -0.0212(3) 0.4692(4) 0.3468(3) 0.0428(11) Uani 1 1 d . . . . .
H14 H -0.032659 0.386246 0.360557 0.051 Uiso 1 1 calc R U . . .
O1 O 0.3346(2) 0.2542(4) 0.43333(18) 0.0505(8) Uani 1 1 d . . . . .
C12 C -0.0619(3) 0.6642(5) 0.2912(3) 0.0529(14) Uani 1 1 d . . . . .
H12 H -0.099800 0.712530 0.267114 0.063 Uiso 1 1 calc R U . . .
C13 C -0.0771(3) 0.5410(5) 0.3096(3) 0.0566(14) Uani 1 1 d . . . . .
H13 H -0.125057 0.505008 0.297045 0.068 Uiso 1 1 calc R U . . .
C8 C 0.1163(3) 0.0141(5) 0.5824(3) 0.0530(14) Uani 1 1 d . . . . .
H8A H 0.138664 0.074429 0.616347 0.079 Uiso 1 1 calc R U . . .
H8B H 0.152737 -0.002282 0.542718 0.079 Uiso 1 1 calc R U . . .
H8C H 0.105386 -0.063421 0.608414 0.079 Uiso 1 1 calc R U . . .
C11 C 0.0106(3) 0.7171(4) 0.3088(3) 0.0485(13) Uani 1 1 d . . . . .
H11 H 0.021132 0.801153 0.296754 0.058 Uiso 1 1 calc R U . . .
C7 C -0.0434(4) 0.1342(6) 0.6147(3) 0.0669(17) Uani 1 1 d . . . . .
H7A H -0.064137 0.062932 0.641473 0.100 Uiso 1 1 calc R U . . .
H7B H -0.085517 0.179660 0.591372 0.100 Uiso 1 1 calc R U . . .
H7C H -0.016317 0.189246 0.648598 0.100 Uiso 1 1 calc R U . . .
B B 0.2991(2) 0.1401(4) 0.1222(2) 0.0236(9) Uani 1 1 d . . . . .
H99 H 0.308(2) 0.093(3) 0.070(2) 0.018(9) Uiso 1 1 d . . . . .
Mo1 Mo 0.26007(2) 0.30493(2) 0.27588(2) 0.02178(8) Uani 1 1 d . . . . .
N5 N 0.23783(18) 0.1024(3) 0.24901(18) 0.0243(7) Uani 1 1 d . . . . .
C1 C 0.1789(2) 0.3546(4) 0.3336(2) 0.0249(8) Uani 1 1 d . . . . .
C3 C 0.2927(2) 0.4853(4) 0.2899(2) 0.0318(9) Uani 1 1 d . . . . .
N1 N 0.37815(19) 0.2640(3) 0.21781(17) 0.0247(7) Uani 1 1 d . . . . .
N3 N 0.22055(19) 0.3344(3) 0.15936(18) 0.0241(7) Uani 1 1 d . . . . .
C2 C 0.3092(2) 0.2697(4) 0.3757(2) 0.0325(9) 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
N2 C53 1.351(5) . ?
N2 N1 1.372(4) . ?
N2 B 1.547(5) . ?
N6 C58 1.355(5) . ?
N6 N5 1.367(4) . ?
N6 B 1.542(5) . ?
N4 C63 1.355(5) . ?
N4 N3 1.370(5) . ?
N4 B 1.547(5) . ?
C50 C51 1.489(5) . ?
C53 C52 1.380(6) . ?
C53 C54 1.486(6) . ?
C51 N1 1.349(5) . ?
C51 C52 1.385(6) . ?
P C4 1.770(4) . ?
P C1 1.803(4) . ?
P C9 1.828(4) . ?
C56 N5 1.344(5) . ?
C56 C57 1.379(6) . ?
C56 C55 1.498(6) . ?
C63 C62 1.379(6) . ?
C63 C64 1.487(6) . ?
C4 C5 1.198(6) . ?
C58 C57 1.374(6) . ?
C58 C59 1.494(6) . ?
C61 N3 1.337(5) . ?
C61 C62 1.387(6) . ?
C61 C60 1.498(6) . ?
C5 Si 1.855(4) . ?
C9 C14 1.378(6) . ?
C9 C10 1.402(6) . ?
C10 C11 1.351(7) . ?
Si C7 1.825(5) . ?
Si C8 1.841(5) . ?
Si C6 1.854(5) . ?
O2 C3 1.130(5) . ?
C14 C13 1.388(7) . ?
O1 C2 1.133(5) . ?
C12 C13 1.365(7) . ?
C12 C11 1.394(7) . ?
Mo1 C1 1.807(4) . ?
Mo1 C3 1.999(4) . ?
Mo1 C2 2.011(5) . ?
Mo1 N3 2.218(3) . ?
Mo1 N5 2.223(3) . ?
Mo1 N1 2.308(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C53 N2 N1 110.1(3) . . ?
C53 N2 B 128.7(3) . . ?
N1 N2 B 121.1(3) . . ?
C58 N6 N5 109.8(3) . . ?
C58 N6 B 128.9(3) . . ?
N5 N6 B 121.1(3) . . ?
C63 N4 N3 110.0(3) . . ?
C63 N4 B 129.0(3) . . ?
N3 N4 B 120.8(3) . . ?
N2 C53 C52 107.4(3) . . ?
N2 C53 C54 122.7(3) . . ?
C52 C53 C54 129.9(4) . . ?
N1 C51 C52 109.7(3) . . ?
N1 C51 C50 122.8(4) . . ?
C52 C51 C50 127.5(4) . . ?
C53 C52 C51 106.4(3) . . ?
C4 P C1 101.37(18) . . ?
C4 P C9 103.04(18) . . ?
C1 P C9 103.13(18) . . ?
N5 C56 C57 109.9(4) . . ?
N5 C56 C55 121.3(4) . . ?
C57 C56 C55 128.8(4) . . ?
N4 C63 C62 107.3(3) . . ?
N4 C63 C64 123.6(4) . . ?
C62 C63 C64 129.1(4) . . ?
C5 C4 P 172.1(4) . . ?
N6 C58 C57 107.3(4) . . ?
N6 C58 C59 122.8(4) . . ?
C57 C58 C59 129.9(4) . . ?
N3 C61 C62 110.1(4) . . ?
N3 C61 C60 122.0(4) . . ?
C62 C61 C60 127.9(4) . . ?
C63 C62 C61 106.2(4) . . ?
C58 C57 C56 106.6(3) . . ?
C4 C5 Si 174.0(4) . . ?
C14 C9 C10 118.4(4) . . ?
C14 C9 P 124.2(3) . . ?
C10 C9 P 117.4(3) . . ?
C11 C10 C9 121.2(4) . . ?
C7 Si C8 113.1(3) . . ?
C7 Si C6 109.9(3) . . ?
C8 Si C6 111.1(3) . . ?
C7 Si C5 107.6(2) . . ?
C8 Si C5 105.6(2) . . ?
C6 Si C5 109.4(2) . . ?
C9 C14 C13 120.3(4) . . ?
C13 C12 C11 119.7(4) . . ?
C12 C13 C14 120.4(5) . . ?
C10 C11 C12 120.0(4) . . ?
N6 B N2 108.8(3) . . ?
N6 B N4 109.2(3) . . ?
N2 B N4 109.0(3) . . ?
C1 Mo1 C3 82.28(16) . . ?
C1 Mo1 C2 82.12(16) . . ?
C3 Mo1 C2 87.00(17) . . ?
C1 Mo1 N3 105.45(14) . . ?
C3 Mo1 N3 94.02(14) . . ?
C2 Mo1 N3 172.43(14) . . ?
C1 Mo1 N5 105.78(14) . . ?
C3 Mo1 N5 171.89(14) . . ?
C2 Mo1 N5 94.96(15) . . ?
N3 Mo1 N5 83.02(12) . . ?
C1 Mo1 N1 169.02(14) . . ?
C3 Mo1 N1 89.52(14) . . ?
C2 Mo1 N1 90.21(14) . . ?
N3 Mo1 N1 82.30(11) . . ?
N5 Mo1 N1 82.61(11) . . ?
C56 N5 N6 106.4(3) . . ?
C56 N5 Mo1 133.5(3) . . ?
N6 N5 Mo1 119.9(2) . . ?
P C1 Mo1 157.2(2) . . ?
O2 C3 Mo1 176.5(4) . . ?
C51 N1 N2 106.3(3) . . ?
C51 N1 Mo1 135.9(3) . . ?
N2 N1 Mo1 117.8(2) . . ?
C61 N3 N4 106.5(3) . . ?
C61 N3 Mo1 133.3(3) . . ?
N4 N3 Mo1 120.1(2) . . ?
O1 C2 Mo1 176.7(4) . . ?

_refine_diff_density_max         0.488
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.066



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

data_Compound_9
_database_code_depnum_ccdc_archive 'CCDC 1851875'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-10-11 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         'C41 H53 B2 N12 O4 P Si W2, 0.667(C H Cl3)'
_chemical_formula_sum            'C41.67 H53.67 B2 Cl2 N12 O4 P Si W2'
_chemical_formula_weight         1305.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.7758(4)
_cell_length_b                   10.9760(2)
_cell_length_c                   24.1570(8)
_cell_angle_alpha                90
_cell_angle_beta                 115.485(2)
_cell_angle_gamma                90
_cell_volume                     5212.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    23320
_cell_measurement_theta_min      4.0700
_cell_measurement_theta_max      73.7010

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_F_000             2563
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.032
_exptl_absorpt_coefficient_mu    9.907
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_reflns_number            51072
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         4.055
_diffrn_reflns_theta_max         73.898
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5275
_reflns_number_gt                4892
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_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)+(0.0496P)²+29.6616P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5275
_refine_ls_number_parameters     317
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.1076
_refine_ls_wR_factor_gt          0.1043
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.114
_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
W1 W 0.91174(2) 0.97492(2) 0.11720(2) 0.04443(10) Uani 1 1 d . . . . .
P P 1.0000 0.78864(18) 0.2500 0.0530(5) Uani 1 2 d S T P . .
O1 O 0.9052(3) 0.7237(4) 0.0525(2) 0.0799(14) Uani 1 1 d . . . . .
O2 O 0.7865(3) 0.8683(5) 0.1333(3) 0.0777(13) Uani 1 1 d . . . . .
N1 N 0.8418(2) 1.0679(4) 0.02811(19) 0.0464(9) Uani 1 1 d . . . . .
N2 N 0.8555(2) 1.1869(4) 0.01959(19) 0.0465(9) Uani 1 1 d . . . . .
N3 N 0.9077(2) 1.1553(4) 0.15561(19) 0.0463(9) Uani 1 1 d . . . . .
N4 N 0.9156(2) 1.2593(4) 0.1291(2) 0.0500(10) Uani 1 1 d . . . . .
N5 N 0.9882(2) 1.0602(4) 0.09154(19) 0.0456(9) Uani 1 1 d . . . . .
N6 N 0.9825(2) 1.1809(4) 0.0755(2) 0.0485(10) Uani 1 1 d . . . . .
C1 C 0.9619(3) 0.8880(5) 0.1866(2) 0.0480(11) Uani 1 1 d . . . . .
C3 C 0.9083(3) 0.8173(5) 0.0742(3) 0.0573(14) Uani 1 1 d . . . . .
C4 C 0.8308(3) 0.9090(6) 0.1276(3) 0.0561(13) Uani 1 1 d . . . . .
C50 C 0.7555(4) 0.9100(7) -0.0290(3) 0.0692(17) Uani 1 1 d . . . . .
H50A H 0.7899 0.8499 -0.0227 0.104 Uiso 1 1 calc R U . . .
H50B H 0.7196 0.9016 -0.0696 0.104 Uiso 1 1 calc R U . . .
H50C H 0.7374 0.8988 0.0005 0.104 Uiso 1 1 calc R U . . .
C51 C 0.7862(3) 1.0355(5) -0.0217(3) 0.0527(12) Uani 1 1 d . . . . .
C52 C 0.7637(3) 1.1320(6) -0.0620(3) 0.0586(14) Uani 1 1 d . . . . .
H52 H 0.7258 1.1329 -0.0997 0.070 Uiso 1 1 calc R U . . .
C53 C 0.8078(3) 1.2266(6) -0.0357(2) 0.0536(13) Uani 1 1 d . . . . .
C54 C 0.8078(4) 1.3514(6) -0.0590(3) 0.0723(19) Uani 1 1 d . . . . .
H54A H 0.8105 1.4097 -0.0285 0.108 Uiso 1 1 calc R U . . .
H54B H 0.7666 1.3643 -0.0956 0.108 Uiso 1 1 calc R U . . .
H54C H 0.8462 1.3612 -0.0682 0.108 Uiso 1 1 calc R U . . .
C55 C 0.9278(4) 1.4835(6) 0.1478(4) 0.076(2) Uani 1 1 d . . . . .
H55A H 0.9735 1.4921 0.1522 0.114 Uiso 1 1 calc R U . . .
H55B H 0.9201 1.5399 0.1745 0.114 Uiso 1 1 calc R U . . .
H55C H 0.8964 1.5000 0.1061 0.114 Uiso 1 1 calc R U . . .
C56 C 0.9172(3) 1.3566(6) 0.1641(3) 0.0562(13) Uani 1 1 d . . . . .
C57 C 0.9095(3) 1.3127(6) 0.2137(3) 0.0587(15) Uani 1 1 d . . . . .
H57 H 0.9086 1.3589 0.2456 0.070 Uiso 1 1 calc R U . . .
C58 C 0.9034(3) 1.1883(6) 0.2079(2) 0.0533(13) Uani 1 1 d . . . . .
C59 C 0.8956(4) 1.0993(7) 0.2507(3) 0.0681(17) Uani 1 1 d . . . . .
H59A H 0.8541 1.0544 0.2297 0.102 Uiso 1 1 calc R U . . .
H59B H 0.8941 1.1419 0.2849 0.102 Uiso 1 1 calc R U . . .
H59C H 0.9334 1.0440 0.2653 0.102 Uiso 1 1 calc R U . . .
C60 C 1.0676(4) 0.8900(7) 0.1041(3) 0.0723(18) Uani 1 1 d . . . . .
H60A H 1.0716 0.8696 0.1442 0.108 Uiso 1 1 calc R U . . .
H60B H 1.1109 0.8805 0.1031 0.108 Uiso 1 1 calc R U . . .
H60C H 1.0349 0.8370 0.0743 0.108 Uiso 1 1 calc R U . . .
C61 C 1.0447(3) 1.0180(6) 0.0898(3) 0.0543(13) Uani 1 1 d . . . . .
C62 C 1.0366(3) 1.2142(6) 0.0652(3) 0.0622(15) Uani 1 1 d . . . . .
C63 C 1.0449(5) 1.3425(7) 0.0480(5) 0.096(3) Uani 1 1 d . . . . .
H63A H 1.0123 1.3583 0.0066 0.144 Uiso 1 1 calc R U . . .
H63B H 1.0900 1.3530 0.0509 0.144 Uiso 1 1 calc R U . . .
H63C H 1.0379 1.3983 0.0753 0.144 Uiso 1 1 calc R U . . .
C72 C 1.0765(3) 1.1137(7) 0.0739(3) 0.0631(15) Uani 1 1 d . . . . .
H72 H 1.1171 1.1096 0.0700 0.076 Uiso 1 1 calc R U . . .
B1 B 0.9193(4) 1.2542(6) 0.0669(3) 0.0504(14) Uani 1 1 d . . . . .
C7 C 0.9422(5) 0.7117(8) 0.2576(4) 0.0377(9) Uani 0.5 1 d . . P A 1
C8 C 0.8903(5) 0.6779(8) 0.2615(4) 0.0377(9) Uani 0.5 1 d . . P A 1
Si Si 0.8130(3) 0.6196(7) 0.2640(3) 0.0710(12) Uani 0.5 1 d D . P A 1
C9 C 0.7538(5) 0.5749(12) 0.1862(6) 0.0377(9) Uani 0.5 1 d D . P A 1
H10A H 0.7441 0.6441 0.1594 0.057 Uiso 0.5 1 calc R U P A 1
H10B H 0.7739 0.5116 0.1720 0.057 Uiso 0.5 1 calc R U P A 1
H10C H 0.7124 0.5456 0.1864 0.057 Uiso 0.5 1 calc R U P A 1
C10 C 0.8349(5) 0.5039(9) 0.3170(4) 0.0377(9) Uani 0.5 1 d D . P A 1
H11A H 0.7947 0.4724 0.3188 0.057 Uiso 0.5 1 calc R U P A 1
H11B H 0.8571 0.4400 0.3053 0.057 Uiso 0.5 1 calc R U P A 1
H11C H 0.8653 0.5348 0.3566 0.057 Uiso 0.5 1 calc R U P A 1
C11 C 0.7728(6) 0.7510(11) 0.2844(5) 0.0377(9) Uani 0.5 1 d D . P A 1
H12A H 0.7615 0.8129 0.2535 0.057 Uiso 0.5 1 calc R U P A 1
H12B H 0.7321 0.7243 0.2870 0.057 Uiso 0.5 1 calc R U P A 1
H12C H 0.8039 0.7837 0.3232 0.057 Uiso 0.5 1 calc R U P A 1
C99 C 0.8036(15) 0.627(2) 0.2600(9) 0.0377(9) Uani 0.3333 1 d D . P B 2
H99 H 0.8370 0.6698 0.2500 0.045 Uiso 0.3333 1 calc R U P B 2
Cl1 Cl 0.7669(6) 0.5594(10) 0.1909(5) 0.1132(17) Uani 0.3333 1 d D . P B 2
Cl3 Cl 0.8615(5) 0.5533(8) 0.3163(4) 0.1132(17) Uani 0.3333 1 d D . P B 2
Cl2 Cl 0.7693(6) 0.7570(10) 0.2698(4) 0.1132(17) Uani 0.3333 1 d D . P B 2
H98 H 0.924(3) 1.335(6) 0.055(3) 0.045(14) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C1 1.827(5) . ?
W1 C3 2.003(6) . ?
W1 C4 2.019(6) . ?
W1 N3 2.204(4) . ?
W1 N5 2.219(4) . ?
W1 N1 2.274(4) . ?
P C7 1.590(9) 2_755 ?
P C7 1.590(9) . ?
P C1 1.769(6) . ?
P C1 1.769(6) 2_755 ?
O1 C3 1.142(7) . ?
O2 C4 1.124(7) . ?
N1 C51 1.336(7) . ?
N1 N2 1.375(6) . ?
N2 C53 1.363(7) . ?
N2 B1 1.553(8) . ?
N3 C58 1.355(6) . ?
N3 N4 1.355(7) . ?
N4 C56 1.352(7) . ?
N4 B1 1.540(7) . ?
N5 C61 1.332(7) . ?
N5 N6 1.371(6) . ?
N6 C62 1.354(7) . ?
N6 B1 1.530(8) . ?
C50 C51 1.508(9) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 C52 1.379(9) . ?
C52 C53 1.371(9) . ?
C52 H52 0.9300 . ?
C53 C54 1.481(9) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 C56 1.492(10) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 C57 1.367(9) . ?
C57 C58 1.374(9) . ?
C57 H57 0.9300 . ?
C58 C59 1.486(9) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C60 C61 1.480(9) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C61 C72 1.400(9) . ?
C62 C72 1.363(10) . ?
C62 C63 1.502(10) . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C72 H72 0.9300 . ?
B1 H98 0.95(6) . ?
C7 C8 1.232(13) . ?
C8 Si 1.826(13) . ?
Si C10 1.719(11) . ?
Si C9 1.830(11) . ?
Si C11 1.861(11) . ?
C9 H10A 0.9600 . ?
C9 H10B 0.9600 . ?
C9 H10C 0.9600 . ?
C10 H11A 0.9600 . ?
C10 H11B 0.9600 . ?
C10 H11C 0.9600 . ?
C11 H12A 0.9600 . ?
C11 H12B 0.9600 . ?
C11 H12C 0.9600 . ?
C99 Cl3 1.620(16) . ?
C99 Cl2 1.673(16) . ?
C99 Cl1 1.682(16) . ?
C99 H99 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W1 C3 84.2(2) . . ?
C1 W1 C4 84.7(2) . . ?
C3 W1 C4 85.1(3) . . ?
C1 W1 N3 101.47(19) . . ?
C3 W1 N3 174.2(2) . . ?
C4 W1 N3 94.3(2) . . ?
C1 W1 N5 104.6(2) . . ?
C3 W1 N5 94.8(2) . . ?
C4 W1 N5 170.6(2) . . ?
N3 W1 N5 84.81(16) . . ?
C1 W1 N1 174.4(2) . . ?
C3 W1 N1 92.1(2) . . ?
C4 W1 N1 90.8(2) . . ?
N3 W1 N1 82.16(15) . . ?
N5 W1 N1 79.85(16) . . ?
C7 P C7 115.8(7) 2_755 . ?
C7 P C1 109.1(3) 2_755 . ?
C7 P C1 109.2(4) . . ?
C7 P C1 109.2(4) 2_755 2_755 ?
C7 P C1 109.1(3) . 2_755 ?
C1 P C1 103.8(4) . 2_755 ?
C51 N1 N2 106.8(4) . . ?
C51 N1 W1 135.3(4) . . ?
N2 N1 W1 117.9(3) . . ?
C53 N2 N1 109.1(5) . . ?
C53 N2 B1 129.2(5) . . ?
N1 N2 B1 121.6(4) . . ?
C58 N3 N4 106.7(5) . . ?
C58 N3 W1 131.6(4) . . ?
N4 N3 W1 121.5(3) . . ?
C56 N4 N3 110.2(5) . . ?
C56 N4 B1 129.8(5) . . ?
N3 N4 B1 120.0(4) . . ?
C61 N5 N6 107.5(5) . . ?
C61 N5 W1 132.6(4) . . ?
N6 N5 W1 119.9(3) . . ?
C62 N6 N5 109.4(5) . . ?
C62 N6 B1 129.5(5) . . ?
N5 N6 B1 120.9(4) . . ?
P C1 W1 171.3(4) . . ?
O1 C3 W1 175.4(5) . . ?
O2 C4 W1 177.6(6) . . ?
C51 C50 H50A 109.5 . . ?
C51 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C51 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N1 C51 C52 109.9(5) . . ?
N1 C51 C50 122.2(5) . . ?
C52 C51 C50 127.9(6) . . ?
C53 C52 C51 106.8(5) . . ?
C53 C52 H52 126.6 . . ?
C51 C52 H52 126.6 . . ?
N2 C53 C52 107.4(5) . . ?
N2 C53 C54 123.0(6) . . ?
C52 C53 C54 129.7(6) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C56 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C56 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N4 C56 C57 106.8(6) . . ?
N4 C56 C55 122.5(6) . . ?
C57 C56 C55 130.6(6) . . ?
C56 C57 C58 107.7(5) . . ?
C56 C57 H57 126.2 . . ?
C58 C57 H57 126.2 . . ?
N3 C58 C57 108.6(5) . . ?
N3 C58 C59 123.2(6) . . ?
C57 C58 C59 128.2(5) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N5 C61 C72 108.6(6) . . ?
N5 C61 C60 123.0(6) . . ?
C72 C61 C60 128.4(6) . . ?
N6 C62 C72 107.4(6) . . ?
N6 C62 C63 121.6(6) . . ?
C72 C62 C63 131.0(6) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C72 C61 107.0(5) . . ?
C62 C72 H72 126.5 . . ?
C61 C72 H72 126.5 . . ?
N6 B1 N4 108.0(5) . . ?
N6 B1 N2 108.5(4) . . ?
N4 B1 N2 109.3(5) . . ?
N6 B1 H98 109(3) . . ?
N4 B1 H98 108(3) . . ?
N2 B1 H98 114(3) . . ?
C8 C7 P 165.2(9) . . ?
C7 C8 Si 176.3(8) . . ?
C10 Si C8 108.6(5) . . ?
C10 Si C9 114.5(7) . . ?
C8 Si C9 108.2(6) . . ?
C10 Si C11 112.7(7) . . ?
C8 Si C11 106.4(6) . . ?
C9 Si C11 106.0(6) . . ?
Si C9 H10A 109.5 . . ?
Si C9 H10B 109.5 . . ?
H10A C9 H10B 109.5 . . ?
Si C9 H10C 109.5 . . ?
H10A C9 H10C 109.5 . . ?
H10B C9 H10C 109.5 . . ?
Si C10 H11A 109.5 . . ?
Si C10 H11B 109.5 . . ?
H11A C10 H11B 109.5 . . ?
Si C10 H11C 109.5 . . ?
H11A C10 H11C 109.5 . . ?
H11B C10 H11C 109.5 . . ?
Si C11 H12A 109.5 . . ?
Si C11 H12B 109.5 . . ?
H12A C11 H12B 109.5 . . ?
Si C11 H12C 109.5 . . ?
H12A C11 H12C 109.5 . . ?
H12B C11 H12C 109.5 . . ?
Cl3 C99 Cl2 122.8(12) . . ?
Cl3 C99 Cl1 118.5(12) . . ?
Cl2 C99 Cl1 117.8(11) . . ?
Cl3 C99 H99 93.0 . . ?
Cl2 C99 H99 93.0 . . ?
Cl1 C99 H99 93.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C51 N1 N2 C53 0.1(6) . . . . ?
W1 N1 N2 C53 -179.2(3) . . . . ?
C51 N1 N2 B1 -176.7(5) . . . . ?
W1 N1 N2 B1 4.0(6) . . . . ?
C58 N3 N4 C56 0.8(6) . . . . ?
W1 N3 N4 C56 -174.5(4) . . . . ?
C58 N3 N4 B1 -177.6(5) . . . . ?
W1 N3 N4 B1 7.2(6) . . . . ?
C61 N5 N6 C62 -1.5(6) . . . . ?
W1 N5 N6 C62 176.5(4) . . . . ?
C61 N5 N6 B1 174.1(5) . . . . ?
W1 N5 N6 B1 -7.9(6) . . . . ?
N2 N1 C51 C52 -0.4(6) . . . . ?
W1 N1 C51 C52 178.7(4) . . . . ?
N2 N1 C51 C50 -180.0(5) . . . . ?
W1 N1 C51 C50 -0.9(9) . . . . ?
N1 C51 C52 C53 0.6(7) . . . . ?
C50 C51 C52 C53 -179.9(6) . . . . ?
N1 N2 C53 C52 0.3(6) . . . . ?
B1 N2 C53 C52 176.8(5) . . . . ?
N1 N2 C53 C54 180.0(5) . . . . ?
B1 N2 C53 C54 -3.6(9) . . . . ?
C51 C52 C53 N2 -0.5(6) . . . . ?
C51 C52 C53 C54 179.9(6) . . . . ?
N3 N4 C56 C57 -0.6(6) . . . . ?
B1 N4 C56 C57 177.6(6) . . . . ?
N3 N4 C56 C55 177.9(6) . . . . ?
B1 N4 C56 C55 -4.0(10) . . . . ?
N4 C56 C57 C58 0.1(6) . . . . ?
C55 C56 C57 C58 -178.1(6) . . . . ?
N4 N3 C58 C57 -0.7(6) . . . . ?
W1 N3 C58 C57 173.9(4) . . . . ?
N4 N3 C58 C59 -179.0(5) . . . . ?
W1 N3 C58 C59 -4.4(8) . . . . ?
C56 C57 C58 N3 0.4(6) . . . . ?
C56 C57 C58 C59 178.6(6) . . . . ?
N6 N5 C61 C72 1.5(6) . . . . ?
W1 N5 C61 C72 -176.2(4) . . . . ?
N6 N5 C61 C60 -179.6(5) . . . . ?
W1 N5 C61 C60 2.7(9) . . . . ?
N5 N6 C62 C72 0.9(6) . . . . ?
B1 N6 C62 C72 -174.2(5) . . . . ?
N5 N6 C62 C63 -178.8(6) . . . . ?
B1 N6 C62 C63 6.2(10) . . . . ?
N6 C62 C72 C61 0.1(7) . . . . ?
C63 C62 C72 C61 179.6(7) . . . . ?
N5 C61 C72 C62 -1.0(7) . . . . ?
C60 C61 C72 C62 -179.8(6) . . . . ?
C62 N6 B1 N4 -121.8(6) . . . . ?
N5 N6 B1 N4 63.6(6) . . . . ?
C62 N6 B1 N2 119.8(6) . . . . ?
N5 N6 B1 N2 -54.8(6) . . . . ?
C56 N4 B1 N6 118.8(6) . . . . ?
N3 N4 B1 N6 -63.2(6) . . . . ?
C56 N4 B1 N2 -123.3(6) . . . . ?
N3 N4 B1 N2 54.7(6) . . . . ?
C53 N2 B1 N6 -119.5(6) . . . . ?
N1 N2 B1 N6 56.6(6) . . . . ?
C53 N2 B1 N4 122.9(6) . . . . ?
N1 N2 B1 N4 -61.0(6) . . . . ?
C7 P C7 C8 -169(3) 2_755 . . . ?
C1 P C7 C8 -46(3) . . . . ?
C1 P C7 C8 67(3) 2_755 . . . ?

_refine_diff_density_max         1.903
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.110



####################################################################### 
# 
# 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_Compound_3a
_database_code_depnum_ccdc_archive 'CCDC 1851872'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-10-11 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         'C29 H42 B Mo N6 O2 P Si'
_chemical_formula_sum            'C29 H42 B Mo N6 O2 P Si'
_chemical_formula_weight         672.49

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   17.5232(3)
_cell_length_b                   10.5308(2)
_cell_length_c                   18.0406(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3329.09(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    33283
_cell_measurement_theta_min      3.7610
_cell_measurement_theta_max      29.5130

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_F_000             1400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.617
_exptl_crystal_size_mid          0.463
_exptl_crystal_size_min          0.133
_exptl_absorpt_coefficient_mu    0.513
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84332
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_reflns_number            70511
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.241
_diffrn_reflns_theta_max         29.893
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             8728
_reflns_number_gt                7898
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_max     0.869
_reflns_Friedel_fraction_full    0.996

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_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)+(0.0303P)²+1.9295P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3328 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8728
_refine_ls_number_parameters     410
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0720
_refine_ls_wR_factor_gt          0.0692
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.003
_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
C4A C 0.3935(7) 0.9823(18) -0.0703(13) 0.079(5) Uani 0.73(4) 1 d D U P A 1
H4A H 0.4061 1.0530 -0.1016 0.119 Uiso 0.73(4) 1 calc R U P A 1
H4B H 0.3778 0.9118 -0.1004 0.119 Uiso 0.73(4) 1 calc R U P A 1
H4C H 0.3526 1.0057 -0.0377 0.119 Uiso 0.73(4) 1 calc R U P A 1
C5A C 0.5108(11) 1.0678(13) 0.0446(9) 0.077(5) Uani 0.73(4) 1 d D U P A 1
H5A H 0.5546 1.0402 0.0722 0.115 Uiso 0.73(4) 1 calc R U P A 1
H5B H 0.5244 1.1396 0.0146 0.115 Uiso 0.73(4) 1 calc R U P A 1
H5C H 0.4709 1.0916 0.0783 0.115 Uiso 0.73(4) 1 calc R U P A 1
C6A C 0.5571(8) 0.8835(16) -0.0750(8) 0.068(4) Uani 0.73(4) 1 d D U P A 1
H6A H 0.5998 0.8607 -0.0445 0.102 Uiso 0.73(4) 1 calc R U P A 1
H6B H 0.5412 0.8111 -0.1034 0.102 Uiso 0.73(4) 1 calc R U P A 1
H6C H 0.5716 0.9509 -0.1079 0.102 Uiso 0.73(4) 1 calc R U P A 1
C6B C 0.531(3) 0.883(5) -0.097(2) 0.12(2) Uani 0.27(4) 1 d D U P A 3
H6B1 H 0.5011 0.8233 -0.1244 0.187 Uiso 0.27(4) 1 calc R U P A 3
H6B2 H 0.5434 0.9543 -0.1276 0.187 Uiso 0.27(4) 1 calc R U P A 3
H6B3 H 0.5776 0.8427 -0.0807 0.187 Uiso 0.27(4) 1 calc R U P A 3
C4B C 0.3848(14) 1.007(5) -0.044(3) 0.066(10) Uani 0.27(4) 1 d D U P A 3
H4B1 H 0.3575 1.0350 -0.0006 0.100 Uiso 0.27(4) 1 calc R U P A 3
H4B2 H 0.3939 1.0785 -0.0758 0.100 Uiso 0.27(4) 1 calc R U P A 3
H4B3 H 0.3552 0.9447 -0.0697 0.100 Uiso 0.27(4) 1 calc R U P A 3
C5B C 0.533(3) 1.052(4) 0.039(3) 0.097(17) Uani 0.27(4) 1 d D U P A 3
H5B1 H 0.5041 1.0791 0.0811 0.145 Uiso 0.27(4) 1 calc R U P A 3
H5B2 H 0.5797 1.0124 0.0555 0.145 Uiso 0.27(4) 1 calc R U P A 3
H5B3 H 0.5454 1.1240 0.0086 0.145 Uiso 0.27(4) 1 calc R U P A 3
H99 H 0.1860(17) 0.925(3) 0.4409(18) 0.008(7) Uiso 1 1 d . . . . .
C1 C 0.33030(18) 0.6587(3) 0.19809(18) 0.0247(6) Uani 1 1 d . . . . .
C4 C 0.4255(2) 0.7149(3) 0.08038(19) 0.0293(7) Uani 1 1 d . . . . .
C5 C 0.4485(2) 0.8012(4) 0.0429(2) 0.0347(8) Uani 1 1 d . . . . .
C7 C 0.46437(19) 0.5124(3) 0.1804(2) 0.0286(7) Uani 1 1 d . . . . .
H7 H 0.4679 0.5573 0.2279 0.034 Uiso 1 1 calc R U . . .
C8 C 0.54127(19) 0.5211(4) 0.1418(2) 0.0358(8) Uani 1 1 d . . . . .
H8A H 0.5544 0.6094 0.1335 0.043 Uiso 1 1 calc R U . . .
H8B H 0.5388 0.4788 0.0942 0.043 Uiso 1 1 calc R U . . .
C9 C 0.6021(2) 0.4581(4) 0.1904(3) 0.0432(10) Uani 1 1 d . . . . .
H9A H 0.6509 0.4609 0.1650 0.052 Uiso 1 1 calc R U . . .
H9B H 0.6072 0.5054 0.2363 0.052 Uiso 1 1 calc R U . . .
C10 C 0.5824(3) 0.3218(4) 0.2080(3) 0.0550(12) Uani 1 1 d . . . . .
H10A H 0.5826 0.2724 0.1626 0.066 Uiso 1 1 calc R U . . .
H10B H 0.6208 0.2867 0.2409 0.066 Uiso 1 1 calc R U . . .
C11 C 0.5056(3) 0.3120(4) 0.2440(4) 0.0591(13) Uani 1 1 d . . . . .
H11A H 0.5071 0.3535 0.2920 0.071 Uiso 1 1 calc R U . . .
H11B H 0.4932 0.2232 0.2519 0.071 Uiso 1 1 calc R U . . .
C12 C 0.4433(2) 0.3738(4) 0.1960(2) 0.0388(9) Uani 1 1 d . . . . .
H12A H 0.4385 0.3279 0.1496 0.047 Uiso 1 1 calc R U . . .
H12B H 0.3947 0.3700 0.2215 0.047 Uiso 1 1 calc R U . . .
C13 C 0.3300(2) 0.9912(4) 0.1668(2) 0.0389(9) Uani 1 1 d . . . . .
H13A H 0.3605 0.9155 0.1660 0.058 Uiso 1 1 calc R U . . .
H13B H 0.3614 1.0633 0.1553 0.058 Uiso 1 1 calc R U . . .
H13C H 0.2900 0.9842 0.1306 0.058 Uiso 1 1 calc R U . . .
C14 C 0.29591(18) 1.0076(3) 0.2418(2) 0.0296(7) Uani 1 1 d . . . . .
C15 C 0.2867(2) 1.1175(3) 0.2819(2) 0.0371(8) Uani 1 1 d . . . . .
H15 H 0.3021 1.1985 0.2678 0.045 Uiso 1 1 calc R U . . .
C16 C 0.2505(2) 1.0847(3) 0.3467(2) 0.0341(8) Uani 1 1 d . . . . .
C17 C 0.2250(3) 1.1659(4) 0.4102(3) 0.0553(13) Uani 1 1 d . . . . .
H17A H 0.1713 1.1539 0.4183 0.083 Uiso 1 1 calc R U . . .
H17B H 0.2347 1.2535 0.3989 0.083 Uiso 1 1 calc R U . . .
H17C H 0.2525 1.1424 0.4541 0.083 Uiso 1 1 calc R U . . .
C18 C 0.2536(2) 0.7926(5) 0.5611(2) 0.0478(11) Uani 1 1 d . . . . .
H18A H 0.2731 0.8777 0.5581 0.072 Uiso 1 1 calc R U . . .
H18B H 0.2760 0.7501 0.6029 0.072 Uiso 1 1 calc R U . . .
H18C H 0.1992 0.7951 0.5668 0.072 Uiso 1 1 calc R U . . .
C19 C 0.2732(2) 0.7228(4) 0.4920(2) 0.0309(7) Uani 1 1 d . . . . .
C20 C 0.31448(19) 0.6126(4) 0.4833(2) 0.0339(8) Uani 1 1 d . . . . .
H20 H 0.3370 0.5644 0.5206 0.041 Uiso 1 1 calc R U . . .
C21 C 0.31590(18) 0.5875(3) 0.40806(19) 0.0274(7) Uani 1 1 d . . . . .
C22 C 0.3533(2) 0.4790(3) 0.3695(2) 0.0367(8) Uani 1 1 d . . . . .
H22A H 0.3161 0.4335 0.3409 0.055 Uiso 1 1 calc R U . . .
H22B H 0.3755 0.4230 0.4056 0.055 Uiso 1 1 calc R U . . .
H22C H 0.3925 0.5104 0.3372 0.055 Uiso 1 1 calc R U . . .
C23 C 0.0297(2) 0.9046(4) 0.4548(2) 0.0411(9) Uani 1 1 d . . . . .
H23A H 0.0564 0.8732 0.4975 0.062 Uiso 1 1 calc R U . . .
H23B H -0.0242 0.8963 0.4625 0.062 Uiso 1 1 calc R U . . .
H23C H 0.0423 0.9925 0.4474 0.062 Uiso 1 1 calc R U . . .
C24 C 0.05259(18) 0.8302(3) 0.38838(19) 0.0277(7) Uani 1 1 d . . . . .
C25 C 0.00793(18) 0.7607(3) 0.3401(2) 0.0313(7) Uani 1 1 d . . . . .
H25 H -0.0448 0.7511 0.3418 0.038 Uiso 1 1 calc R U . . .
C26 C 0.05720(19) 0.7084(3) 0.28861(19) 0.0273(7) Uani 1 1 d . . . . .
C27 C 0.0378(2) 0.6213(4) 0.2263(2) 0.0388(9) Uani 1 1 d . . . . .
H27A H 0.0632 0.6492 0.1821 0.058 Uiso 1 1 calc R U . . .
H27B H -0.0164 0.6219 0.2185 0.058 Uiso 1 1 calc R U . . .
H27C H 0.0541 0.5367 0.2383 0.058 Uiso 1 1 calc R U . . .
C2 C 0.2060(2) 0.7382(4) 0.1511(2) 0.0328(8) Uani 1 1 d . . . . .
C3 C 0.2196(2) 0.5252(3) 0.23699(19) 0.0312(8) Uani 1 1 d . . . . .
B B 0.1988(2) 0.8734(4) 0.4016(2) 0.0250(7) Uani 1 1 d . . . . .
N3 N 0.26710(15) 0.9094(3) 0.28009(16) 0.0235(5) Uani 1 1 d . . . . .
N4 N 0.23968(15) 0.9582(3) 0.34503(17) 0.0262(6) Uani 1 1 d . . . . .
N5 N 0.27794(16) 0.6782(3) 0.37161(15) 0.0239(5) Uani 1 1 d . . . . .
N6 N 0.25176(14) 0.7617(3) 0.42392(16) 0.0254(6) Uani 1 1 d . . . . .
N1 N 0.12943(16) 0.7436(3) 0.30367(15) 0.0239(5) Uani 1 1 d . . . . .
N2 N 0.12557(15) 0.8186(3) 0.36577(15) 0.0234(5) Uani 1 1 d . . . . .
O1 O 0.1838(2) 0.7516(4) 0.09224(16) 0.0566(8) Uani 1 1 d . . . . .
O2 O 0.2051(2) 0.4209(3) 0.22535(18) 0.0526(8) Uani 1 1 d . . . . .
Si Si 0.47721(6) 0.93713(11) -0.01553(6) 0.0371(2) Uani 1 1 d D . . . .
P P 0.38438(5) 0.58300(8) 0.12608(5) 0.02691(17) Uani 1 1 d . . . . .
Mo Mo 0.24823(2) 0.70585(2) 0.25261(3) 0.02186(7) 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
C4A Si 1.832(9) . ?
C5A Si 1.849(9) . ?
C6A Si 1.851(8) . ?
C6B Si 1.836(18) . ?
C4B Si 1.851(16) . ?
C5B Si 1.842(18) . ?
C1 P 1.795(3) . ?
C1 Mo 1.812(3) . ?
C4 C5 1.203(5) . ?
C4 P 1.768(4) . ?
C5 Si 1.847(4) . ?
C7 C8 1.519(5) . ?
C7 C12 1.532(5) . ?
C7 P 1.865(4) . ?
C8 C9 1.531(5) . ?
C9 C10 1.510(6) . ?
C10 C11 1.498(7) . ?
C11 C12 1.538(6) . ?
C13 C14 1.490(5) . ?
C14 N3 1.343(4) . ?
C14 C15 1.373(5) . ?
C15 C16 1.375(6) . ?
C16 N4 1.346(5) . ?
C16 C17 1.498(6) . ?
C18 C19 1.487(6) . ?
C19 N6 1.349(5) . ?
C19 C20 1.377(5) . ?
C20 C21 1.382(5) . ?
C21 N5 1.337(4) . ?
C21 C22 1.490(5) . ?
C23 C24 1.487(5) . ?
C24 N2 1.348(4) . ?
C24 C25 1.380(5) . ?
C25 C26 1.383(5) . ?
C26 N1 1.347(4) . ?
C26 C27 1.489(5) . ?
C2 O1 1.139(4) . ?
C2 Mo 2.005(4) . ?
C3 O2 1.147(4) . ?
C3 Mo 1.987(4) . ?
B N4 1.534(5) . ?
B N2 1.549(4) . ?
B N6 1.551(5) . ?
N3 N4 1.367(4) . ?
N3 Mo 2.225(3) . ?
N5 N6 1.369(4) . ?
N5 Mo 2.228(3) . ?
N1 N2 1.373(4) . ?
N1 Mo 2.311(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P C1 Mo 159.0(2) . . ?
C5 C4 P 172.9(3) . . ?
C4 C5 Si 176.2(3) . . ?
C8 C7 C12 110.8(3) . . ?
C8 C7 P 113.7(3) . . ?
C12 C7 P 107.2(2) . . ?
C7 C8 C9 109.2(3) . . ?
C10 C9 C8 111.9(3) . . ?
C11 C10 C9 111.3(3) . . ?
C10 C11 C12 111.3(4) . . ?
C7 C12 C11 109.6(3) . . ?
N3 C14 C15 109.5(3) . . ?
N3 C14 C13 121.9(3) . . ?
C15 C14 C13 128.5(3) . . ?
C14 C15 C16 106.9(3) . . ?
N4 C16 C15 107.1(3) . . ?
N4 C16 C17 122.7(4) . . ?
C15 C16 C17 130.2(4) . . ?
N6 C19 C20 107.3(3) . . ?
N6 C19 C18 123.3(3) . . ?
C20 C19 C18 129.4(4) . . ?
C19 C20 C21 106.5(3) . . ?
N5 C21 C20 109.7(3) . . ?
N5 C21 C22 122.5(3) . . ?
C20 C21 C22 127.8(3) . . ?
N2 C24 C25 107.4(3) . . ?
N2 C24 C23 123.1(3) . . ?
C25 C24 C23 129.4(3) . . ?
C24 C25 C26 106.3(3) . . ?
N1 C26 C25 110.0(3) . . ?
N1 C26 C27 122.5(3) . . ?
C25 C26 C27 127.6(3) . . ?
O1 C2 Mo 176.7(4) . . ?
O2 C3 Mo 177.0(3) . . ?
N4 B N2 109.0(3) . . ?
N4 B N6 109.6(3) . . ?
N2 B N6 108.8(3) . . ?
C14 N3 N4 106.4(3) . . ?
C14 N3 Mo 133.1(2) . . ?
N4 N3 Mo 120.1(2) . . ?
C16 N4 N3 110.0(3) . . ?
C16 N4 B 128.8(3) . . ?
N3 N4 B 121.0(3) . . ?
C21 N5 N6 106.6(3) . . ?
C21 N5 Mo 133.1(2) . . ?
N6 N5 Mo 120.1(2) . . ?
C19 N6 N5 109.8(3) . . ?
C19 N6 B 129.3(3) . . ?
N5 N6 B 120.6(3) . . ?
C26 N1 N2 106.1(3) . . ?
C26 N1 Mo 136.0(2) . . ?
N2 N1 Mo 117.96(19) . . ?
C24 N2 N1 110.2(3) . . ?
C24 N2 B 128.8(3) . . ?
N1 N2 B 121.0(3) . . ?
C6B Si C5B 110.8(13) . . ?
C4A Si C5 106.9(5) . . ?
C6B Si C5 110.8(17) . . ?
C5B Si C5 110.4(18) . . ?
C4A Si C5A 112.2(7) . . ?
C5 Si C5A 109.2(6) . . ?
C6B Si C4B 110.8(13) . . ?
C5B Si C4B 110.6(13) . . ?
C5 Si C4B 103.2(14) . . ?
C4A Si C6A 111.8(7) . . ?
C5 Si C6A 107.5(6) . . ?
C5A Si C6A 109.0(6) . . ?
C4 P C1 101.77(16) . . ?
C4 P C7 104.57(16) . . ?
C1 P C7 101.14(16) . . ?
C1 Mo C3 82.02(15) . . ?
C1 Mo C2 81.00(15) . . ?
C3 Mo C2 86.56(15) . . ?
C1 Mo N3 105.49(12) . . ?
C3 Mo N3 172.43(12) . . ?
C2 Mo N3 95.43(14) . . ?
C1 Mo N5 107.55(13) . . ?
C3 Mo N5 94.04(12) . . ?
C2 Mo N5 171.43(12) . . ?
N3 Mo N5 82.91(10) . . ?
C1 Mo N1 168.14(13) . . ?
C3 Mo N1 89.63(13) . . ?
C2 Mo N1 90.15(12) . . ?
N3 Mo N1 83.07(10) . . ?
N5 Mo N1 81.31(10) . . ?

_refine_diff_density_max         0.777
_refine_diff_density_min         -0.418
_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_Compound_6
_database_code_depnum_ccdc_archive 'CCDC 1851871'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H49 B2 N12 O4 P W2'
_chemical_formula_sum            'C44 H49 B2 N12 O4 P W2'
_chemical_formula_weight         1230.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.4317(10)
_cell_length_b                   10.8744(3)
_cell_length_c                   23.8394(10)
_cell_angle_alpha                90
_cell_angle_beta                 117.336(5)
_cell_angle_gamma                90
_cell_volume                     5165.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    17996
_cell_measurement_theta_min      4.6260
_cell_measurement_theta_max      71.7430

_exptl_crystal_description       block
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_F_000             2408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.025
_exptl_absorpt_coefficient_mu    8.815
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.278
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_reflns_number            36085
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         4.438
_diffrn_reflns_theta_max         72.253
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5069
_reflns_number_gt                4680
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0480P)²+48.2455P] 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         5069
_refine_ls_number_parameters     324
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1409
_refine_ls_wR_factor_gt          0.1373
_refine_ls_goodness_of_fit_ref   1.272
_refine_ls_restrained_S_all      1.270
_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
W1 W 0.58990(2) 0.02110(3) 0.88654(2) 0.04335(14) Uani 1 1 d . . . . .
P P 0.500000 0.2108(2) 0.750000 0.0513(7) Uani 1 2 d S T P . .
O1 O 0.7100(3) 0.1344(7) 0.8705(3) 0.0711(17) Uani 1 1 d . . . . .
O2 O 0.6014(4) 0.2756(6) 0.9538(3) 0.0745(19) Uani 1 1 d . . . . .
N1 N 0.6602(3) -0.0735(6) 0.9788(3) 0.0473(14) Uani 1 1 d . . . . .
N2 N 0.6464(3) -0.1918(6) 0.9878(3) 0.0500(15) Uani 1 1 d . . . . .
N3 N 0.5143(3) -0.0623(6) 0.9112(3) 0.0439(13) Uani 1 1 d . . . . .
N4 N 0.5209(4) -0.1847(6) 0.9292(3) 0.0520(15) Uani 1 1 d . . . . .
N5 N 0.5921(3) -0.1608(6) 0.8471(3) 0.0470(14) Uani 1 1 d . . . . .
N6 N 0.5842(3) -0.2666(6) 0.8748(3) 0.0502(15) Uani 1 1 d . . . . .
C1 C 0.5391(4) 0.1083(7) 0.8145(3) 0.0446(15) Uani 1 1 d . . . . .
C3 C 0.6672(4) 0.0881(7) 0.8754(4) 0.0505(18) Uani 1 1 d . . . . .
C4 C 0.5956(5) 0.1827(8) 0.9310(4) 0.057(2) Uani 1 1 d . . . . .
C7 C 0.5588(7) 0.2780(12) 0.7408(6) 0.040(3) Uani 0.5 1 d . . P . .
C8 C 0.6033(8) 0.3420(13) 0.7385(6) 0.047(3) Uani 0.5 1 d . . P . .
C9 C 0.6546(5) 0.4100(8) 0.7370(5) 0.045(3) Uani 0.5 1 d G U P . .
C10 C 0.7187(5) 0.4096(9) 0.7878(4) 0.056(4) Uani 0.5 1 d G U P . .
H10 H 0.729815 0.352504 0.820091 0.068 Uiso 0.5 1 calc R U P . .
C11 C 0.7661(4) 0.4947(11) 0.7902(4) 0.071(4) Uani 0.5 1 d G U P . .
H11 H 0.808918 0.494470 0.824183 0.085 Uiso 0.5 1 calc R U P . .
C12 C 0.7494(5) 0.5801(10) 0.7419(5) 0.057(4) Uani 0.5 1 d G U P . .
H12 H 0.781089 0.636994 0.743580 0.069 Uiso 0.5 1 calc R U P . .
C13 C 0.6853(5) 0.5804(9) 0.6912(4) 0.058(4) Uani 0.5 1 d G U P . .
H13 H 0.674157 0.637553 0.658885 0.070 Uiso 0.5 1 calc R U P . .
C14 C 0.6379(4) 0.4954(10) 0.6887(4) 0.064(4) Uani 0.5 1 d G U P . .
H14 H 0.595053 0.495588 0.654791 0.077 Uiso 0.5 1 calc R U P . .
C50 C 0.7469(5) 0.0845(10) 1.0373(4) 0.074(3) Uani 1 1 d . . . . .
H50A H 0.714128 0.145433 1.033222 0.111 Uiso 1 1 calc R U . . .
H50B H 0.761069 0.097569 1.005462 0.111 Uiso 1 1 calc R U . . .
H50C H 0.784829 0.090869 1.078343 0.111 Uiso 1 1 calc R U . . .
C51 C 0.7165(4) -0.0408(8) 1.0295(4) 0.0537(19) Uani 1 1 d . . . . .
C52 C 0.7393(4) -0.1392(9) 1.0711(4) 0.059(2) Uani 1 1 d . . . . .
H52 H 0.777561 -0.140589 1.109985 0.071 Uiso 1 1 calc R U . . .
C53 C 0.6948(5) -0.2342(8) 1.0441(4) 0.060(2) Uani 1 1 d . . . . .
C54 C 0.6949(6) -0.3610(10) 1.0684(5) 0.084(3) Uani 1 1 d . . . . .
H54A H 0.658577 -0.368951 1.078889 0.126 Uiso 1 1 calc R U . . .
H54B H 0.736688 -0.375420 1.105377 0.126 Uiso 1 1 calc R U . . .
H54C H 0.689510 -0.420051 1.036465 0.126 Uiso 1 1 calc R U . . .
C55 C 0.4620(7) -0.3452(10) 0.9593(6) 0.094(4) Uani 1 1 d . . . . .
H55A H 0.483032 -0.402797 0.943474 0.141 Uiso 1 1 calc R U . . .
H55B H 0.415250 -0.365055 0.942784 0.141 Uiso 1 1 calc R U . . .
H55C H 0.483114 -0.349468 1.004604 0.141 Uiso 1 1 calc R U . . .
C56 C 0.4692(5) -0.2167(9) 0.9391(4) 0.062(2) Uani 1 1 d . . . . .
C57 C 0.4284(5) -0.1157(10) 0.9275(4) 0.064(2) Uani 1 1 d . . . . .
H57 H 0.388404 -0.111722 0.930198 0.076 Uiso 1 1 calc R U . . .
C58 C 0.4587(4) -0.0204(8) 0.9109(3) 0.0510(18) Uani 1 1 d . . . . .
C59 C 0.5700(6) -0.4925(8) 0.8553(5) 0.077(3) Uani 1 1 d . . . . .
H59A H 0.597299 -0.506354 0.899694 0.116 Uiso 1 1 calc R U . . .
H59B H 0.582370 -0.549766 0.831791 0.116 Uiso 1 1 calc R U . . .
H59C H 0.523634 -0.503805 0.844809 0.116 Uiso 1 1 calc R U . . .
C60 C 0.5806(4) -0.3642(8) 0.8392(4) 0.057(2) Uani 1 1 d . . . . .
C61 C 0.5871(4) -0.3221(9) 0.7881(4) 0.061(2) Uani 1 1 d . . . . .
H61 H 0.586755 -0.369491 0.755439 0.073 Uiso 1 1 calc R U . . .
C62 C 0.5942(4) -0.1959(8) 0.7943(3) 0.0501(18) Uani 1 1 d . . . . .
C63 C 0.6031(5) -0.1067(9) 0.7517(4) 0.068(2) Uani 1 1 d . . . . .
H63A H 0.565570 -0.051418 0.734600 0.102 Uiso 1 1 calc R U . . .
H63B H 0.605842 -0.150157 0.717905 0.102 Uiso 1 1 calc R U . . .
H63C H 0.643664 -0.060824 0.775045 0.102 Uiso 1 1 calc R U . . .
C88 C 0.4352(4) 0.1083(8) 0.8937(4) 0.059(2) Uani 1 1 d . . . . .
H88A H 0.472064 0.163687 0.915430 0.089 Uiso 1 1 calc R U . . .
H88B H 0.400505 0.125353 0.905509 0.089 Uiso 1 1 calc R U . . .
H88C H 0.417835 0.119107 0.848915 0.089 Uiso 1 1 calc R U . . .
B1 B 0.5832(5) -0.2602(9) 0.9386(4) 0.053(2) Uani 1 1 d . . . . .
H1 H 0.580975 -0.343096 0.953640 0.064 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
W1 C1 1.831(7) . ?
W1 C3 2.008(9) . ?
W1 C4 2.025(9) . ?
W1 N5 2.201(6) . ?
W1 N3 2.226(6) . ?
W1 N1 2.280(6) . ?
P C7 1.608(14) . ?
P C7 1.608(14) 2_656 ?
P C1 1.771(7) 2_656 ?
P C1 1.771(7) . ?
O1 C3 1.136(10) . ?
O2 C4 1.127(10) . ?
N1 C51 1.334(10) . ?
N1 N2 1.362(9) . ?
N2 C53 1.362(10) . ?
N2 B1 1.553(11) . ?
N3 C58 1.325(11) . ?
N3 N4 1.386(9) . ?
N4 C56 1.331(11) . ?
N4 B1 1.546(12) . ?
N5 C62 1.337(9) . ?
N5 N6 1.378(9) . ?
N6 C60 1.337(10) . ?
N6 B1 1.534(11) . ?
C7 C8 1.24(2) . ?
C8 C9 1.382(18) . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 C11 1.3900 . ?
C10 H10 0.9300 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C50 C51 1.495(13) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 C52 1.388(12) . ?
C52 C53 1.374(13) . ?
C52 H52 0.9300 . ?
C53 C54 1.495(13) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 C56 1.511(13) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 C57 1.374(14) . ?
C57 C58 1.393(12) . ?
C57 H57 0.9300 . ?
C58 C88 1.485(12) . ?
C59 C60 1.494(13) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C60 C61 1.372(13) . ?
C61 C62 1.382(12) . ?
C61 H61 0.9300 . ?
C62 C63 1.482(12) . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C88 H88A 0.9600 . ?
C88 H88B 0.9600 . ?
C88 H88C 0.9600 . ?
B1 H1 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W1 C3 83.8(3) . . ?
C1 W1 C4 84.5(3) . . ?
C3 W1 C4 84.5(3) . . ?
C1 W1 N5 101.0(3) . . ?
C3 W1 N5 94.6(3) . . ?
C4 W1 N5 174.3(3) . . ?
C1 W1 N3 103.7(3) . . ?
C3 W1 N3 172.4(3) . . ?
C4 W1 N3 95.0(3) . . ?
N5 W1 N3 85.2(2) . . ?
C1 W1 N1 174.8(3) . . ?
C3 W1 N1 92.0(3) . . ?
C4 W1 N1 92.2(3) . . ?
N5 W1 N1 82.3(2) . . ?
N3 W1 N1 80.5(2) . . ?
C7 P C7 125.9(10) . 2_656 ?
C7 P C1 106.1(5) . 2_656 ?
C7 P C1 107.2(5) 2_656 2_656 ?
C7 P C1 107.2(5) . . ?
C7 P C1 106.1(5) 2_656 . ?
C1 P C1 102.0(5) 2_656 . ?
C51 N1 N2 107.4(6) . . ?
C51 N1 W1 134.5(6) . . ?
N2 N1 W1 118.1(4) . . ?
C53 N2 N1 109.8(7) . . ?
C53 N2 B1 128.4(7) . . ?
N1 N2 B1 121.8(6) . . ?
C58 N3 N4 107.3(6) . . ?
C58 N3 W1 133.5(5) . . ?
N4 N3 W1 119.2(5) . . ?
C56 N4 N3 109.2(7) . . ?
C56 N4 B1 129.7(8) . . ?
N3 N4 B1 121.0(6) . . ?
C62 N5 N6 106.3(6) . . ?
C62 N5 W1 132.6(5) . . ?
N6 N5 W1 120.8(4) . . ?
C60 N6 N5 110.0(7) . . ?
C60 N6 B1 129.9(7) . . ?
N5 N6 B1 120.1(6) . . ?
P C1 W1 170.8(5) . . ?
O1 C3 W1 174.9(7) . . ?
O2 C4 W1 175.1(8) . . ?
C8 C7 P 171.6(13) . . ?
C7 C8 C9 177.9(16) . . ?
C8 C9 C10 121.1(9) . . ?
C8 C9 C14 117.9(9) . . ?
C10 C9 C14 120.0 . . ?
C9 C10 C11 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C9 120.0 . . ?
C13 C14 H14 120.0 . . ?
C9 C14 H14 120.0 . . ?
C51 C50 H50A 109.5 . . ?
C51 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C51 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N1 C51 C52 109.0(8) . . ?
N1 C51 C50 123.0(8) . . ?
C52 C51 C50 128.0(8) . . ?
C53 C52 C51 107.2(7) . . ?
C53 C52 H52 126.4 . . ?
C51 C52 H52 126.4 . . ?
N2 C53 C52 106.6(7) . . ?
N2 C53 C54 123.5(9) . . ?
C52 C53 C54 129.9(8) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C56 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C56 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N4 C56 C57 108.0(8) . . ?
N4 C56 C55 121.9(10) . . ?
C57 C56 C55 130.1(9) . . ?
C56 C57 C58 106.6(8) . . ?
C56 C57 H57 126.7 . . ?
C58 C57 H57 126.7 . . ?
N3 C58 C57 108.9(8) . . ?
N3 C58 C88 122.6(7) . . ?
C57 C58 C88 128.5(8) . . ?
C60 C59 H59A 109.5 . . ?
C60 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C60 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
N6 C60 C61 107.4(8) . . ?
N6 C60 C59 123.3(9) . . ?
C61 C60 C59 129.3(8) . . ?
C60 C61 C62 106.9(8) . . ?
C60 C61 H61 126.5 . . ?
C62 C61 H61 126.5 . . ?
N5 C62 C61 109.4(8) . . ?
N5 C62 C63 122.1(8) . . ?
C61 C62 C63 128.5(8) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C58 C88 H88A 109.5 . . ?
C58 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C58 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
N6 B1 N4 107.7(6) . . ?
N6 B1 N2 110.3(7) . . ?
N4 B1 N2 107.9(7) . . ?
N6 B1 H1 110.3 . . ?
N4 B1 H1 110.3 . . ?
N2 B1 H1 110.3 . . ?

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
C51 N1 N2 C53 -0.7(9) . . . . ?
W1 N1 N2 C53 177.8(5) . . . . ?
C51 N1 N2 B1 178.8(7) . . . . ?
W1 N1 N2 B1 -2.7(9) . . . . ?
C58 N3 N4 C56 0.6(8) . . . . ?
W1 N3 N4 C56 -177.4(5) . . . . ?
C58 N3 N4 B1 -176.1(6) . . . . ?
W1 N3 N4 B1 5.9(8) . . . . ?
C62 N5 N6 C60 -0.8(9) . . . . ?
W1 N5 N6 C60 173.9(5) . . . . ?
C62 N5 N6 B1 177.0(7) . . . . ?
W1 N5 N6 B1 -8.4(9) . . . . ?
C8 C9 C10 C11 -168.4(11) . . . . ?
C14 C9 C10 C11 0.0 . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C9 0.0 . . . . ?
C8 C9 C14 C13 168.8(11) . . . . ?
C10 C9 C14 C13 0.0 . . . . ?
N2 N1 C51 C52 0.4(9) . . . . ?
W1 N1 C51 C52 -177.8(6) . . . . ?
N2 N1 C51 C50 -178.8(8) . . . . ?
W1 N1 C51 C50 3.0(13) . . . . ?
N1 C51 C52 C53 0.0(10) . . . . ?
C50 C51 C52 C53 179.2(9) . . . . ?
N1 N2 C53 C52 0.7(9) . . . . ?
B1 N2 C53 C52 -178.7(8) . . . . ?
N1 N2 C53 C54 -179.8(9) . . . . ?
B1 N2 C53 C54 0.7(14) . . . . ?
C51 C52 C53 N2 -0.4(10) . . . . ?
C51 C52 C53 C54 -179.8(10) . . . . ?
N3 N4 C56 C57 0.1(9) . . . . ?
B1 N4 C56 C57 176.4(7) . . . . ?
N3 N4 C56 C55 179.9(8) . . . . ?
B1 N4 C56 C55 -3.8(14) . . . . ?
N4 C56 C57 C58 -0.8(9) . . . . ?
C55 C56 C57 C58 179.4(10) . . . . ?
N4 N3 C58 C57 -1.1(8) . . . . ?
W1 N3 C58 C57 176.5(5) . . . . ?
N4 N3 C58 C88 -180.0(7) . . . . ?
W1 N3 C58 C88 -2.4(11) . . . . ?
C56 C57 C58 N3 1.2(9) . . . . ?
C56 C57 C58 C88 179.9(8) . . . . ?
N5 N6 C60 C61 0.7(9) . . . . ?
B1 N6 C60 C61 -176.8(8) . . . . ?
N5 N6 C60 C59 -178.2(8) . . . . ?
B1 N6 C60 C59 4.3(14) . . . . ?
N6 C60 C61 C62 -0.4(10) . . . . ?
C59 C60 C61 C62 178.5(9) . . . . ?
N6 N5 C62 C61 0.5(9) . . . . ?
W1 N5 C62 C61 -173.2(6) . . . . ?
N6 N5 C62 C63 -179.4(7) . . . . ?
W1 N5 C62 C63 6.9(12) . . . . ?
C60 C61 C62 N5 -0.1(10) . . . . ?
C60 C61 C62 C63 179.8(8) . . . . ?
C60 N6 B1 N4 -118.4(9) . . . . ?
N5 N6 B1 N4 64.3(9) . . . . ?
C60 N6 B1 N2 124.1(9) . . . . ?
N5 N6 B1 N2 -53.2(10) . . . . ?
C56 N4 B1 N6 121.2(8) . . . . ?
N3 N4 B1 N6 -62.9(9) . . . . ?
C56 N4 B1 N2 -119.7(8) . . . . ?
N3 N4 B1 N2 56.2(8) . . . . ?
C53 N2 B1 N6 -121.1(9) . . . . ?
N1 N2 B1 N6 59.5(10) . . . . ?
C53 N2 B1 N4 121.5(8) . . . . ?
N1 N2 B1 N4 -57.8(9) . . . . ?

_refine_diff_density_max         1.316
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.141



####################################################################### 
# 
# 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_Compound_12
_database_code_depnum_ccdc_archive 'CCDC 1851876'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT308_shelx               
;
PROBLEM: Single Bonded Metal Atom in Structure  (Unusual)         Au Check 
RESPONSE: Au is in fact doubly bonded (to P and Cl) but this is missed by checkcif.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H53 Au B2 Cl N12 O4 P Si W2'
_chemical_formula_sum            'C41 H53 Au B2 Cl N12 O4 P Si W2'
_chemical_formula_weight         1458.75

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.114(2)
_cell_length_b                   11.0992(5)
_cell_length_c                   23.9715(16)
_cell_angle_alpha                90
_cell_angle_beta                 114.633(9)
_cell_angle_gamma                90
_cell_volume                     5348.3(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    5010
_cell_measurement_theta_min      3.5260
_cell_measurement_theta_max      27.5960

_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_F_000             2792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.045
_exptl_absorpt_coefficient_mu    7.178
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_reflns_number            13179
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.372
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_full        25.025
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4708
_reflns_number_gt                3768
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_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)+310.7889P] 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         4708
_refine_ls_number_parameters     319
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0838
_refine_ls_wR_factor_ref         0.1791
_refine_ls_wR_factor_gt          0.1693
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_restrained_S_all      1.258
_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
W W 0.41106(4) 0.48149(6) 0.61684(3) 0.0395(2) Uani 1 1 d . . . . .
P P 0.5000 0.3019(5) 0.7500 0.0377(15) Uani 1 2 d DS T P . .
N3 N 0.4833(7) 0.5637(11) 0.5883(6) 0.035(3) Uani 1 1 d . . . . .
N2 N 0.3525(7) 0.6852(12) 0.5160(6) 0.039(3) Uani 1 1 d . . . . .
N1 N 0.3410(8) 0.5667(13) 0.5262(6) 0.045(4) Uani 1 1 d . . . . .
N4 N 0.4768(8) 0.6853(12) 0.5694(6) 0.046(4) Uani 1 1 d . . . . .
N5 N 0.4059(8) 0.6640(12) 0.6536(6) 0.043(4) Uani 1 1 d . . . . .
C2 C 0.4065(10) 0.3256(16) 0.5754(8) 0.048(5) Uani 1 1 d . . . . .
C1 C 0.4616(8) 0.4004(15) 0.6868(7) 0.039(4) Uani 1 1 d . . . . .
O1 O 0.4061(8) 0.2320(12) 0.5554(6) 0.070(4) Uani 1 1 d . . . . .
O2 O 0.2886(8) 0.3807(15) 0.6359(8) 0.085(5) Uani 1 1 d . . . . .
N6 N 0.4107(8) 0.7631(13) 0.6249(6) 0.048(4) Uani 1 1 d . . . . .
C3 C 0.3345(10) 0.4185(19) 0.6295(9) 0.057(5) Uani 1 1 d . . . . .
C15 C 0.4056(9) 0.6997(18) 0.7080(8) 0.051(5) Uani 1 1 d . . . . .
C20 C 0.2879(9) 0.5313(16) 0.4787(8) 0.048(4) Uani 1 1 d . . . . .
C22 C 0.3043(10) 0.7197(16) 0.4623(8) 0.046(5) Uani 1 1 d . . . . .
C10 C 0.5415(9) 0.5321(15) 0.5867(7) 0.044(4) Uani 1 1 d . . . . .
C12 C 0.5286(11) 0.7157(17) 0.5569(9) 0.054(5) Uani 1 1 d . . . . .
C16 C 0.4109(9) 0.8220(18) 0.7121(8) 0.053(5) Uani 1 1 d . . . . .
H16 H 0.4124 0.8696 0.7446 0.063 Uiso 1 1 calc R U . . .
C11 C 0.5712(11) 0.6209(19) 0.5703(8) 0.057(5) Uani 1 1 d . . . . .
H11 H 0.6123 0.6185 0.5684 0.068 Uiso 1 1 calc R U . . .
C14 C 0.3999(11) 0.6107(19) 0.7514(9) 0.067(6) Uani 1 1 d . . . . .
H14A H 0.3994 0.6519 0.7864 0.100 Uiso 1 1 calc R U . . .
H14B H 0.4372 0.5568 0.7645 0.100 Uiso 1 1 calc R U . . .
H14C H 0.3595 0.5657 0.7315 0.100 Uiso 1 1 calc R U . . .
C17 C 0.4134(9) 0.8618(16) 0.6577(10) 0.054(5) Uani 1 1 d . . . . .
C9 C 0.5644(10) 0.4037(18) 0.6046(8) 0.055(5) Uani 1 1 d . . . . .
H9A H 0.6006 0.3861 0.5936 0.083 Uiso 1 1 calc R U . . .
H9B H 0.5283 0.3495 0.5834 0.083 Uiso 1 1 calc R U . . .
H9C H 0.5790 0.3942 0.6481 0.083 Uiso 1 1 calc R U . . .
C21 C 0.2625(10) 0.6239(19) 0.4368(9) 0.055(5) Uani 1 1 d . . . . .
H21 H 0.2252 0.6218 0.3995 0.066 Uiso 1 1 calc R U . . .
C19 C 0.2557(10) 0.4080(17) 0.4721(10) 0.063(6) Uani 1 1 d . . . . .
H19A H 0.2890 0.3496 0.4947 0.094 Uiso 1 1 calc R U . . .
H19B H 0.2355 0.3858 0.4295 0.094 Uiso 1 1 calc R U . . .
H19C H 0.2224 0.4108 0.4879 0.094 Uiso 1 1 calc R U . . .
B B 0.4128(12) 0.7547(19) 0.5612(9) 0.048(5) Uani 1 1 d . . . . .
H H 0.4136 0.8358 0.5454 0.058 Uiso 1 1 calc R U . . .
C18 C 0.4187(12) 0.9833(18) 0.6381(12) 0.087(8) Uani 1 1 d . . . . .
H18A H 0.4638 0.9985 0.6441 0.130 Uiso 1 1 calc R U . . .
H18B H 0.4061 1.0398 0.6617 0.130 Uiso 1 1 calc R U . . .
H18C H 0.3897 0.9922 0.5954 0.130 Uiso 1 1 calc R U . . .
C23 C 0.3023(12) 0.8447(18) 0.4356(9) 0.068(6) Uani 1 1 d . . . . .
H23A H 0.2726 0.8950 0.4452 0.102 Uiso 1 1 calc R U . . .
H23B H 0.2869 0.8390 0.3919 0.102 Uiso 1 1 calc R U . . .
H23C H 0.3461 0.8791 0.4529 0.102 Uiso 1 1 calc R U . . .
C13 C 0.5358(15) 0.8386(19) 0.5381(13) 0.099(10) Uani 1 1 d . . . . .
H13A H 0.4941 0.8652 0.5069 0.148 Uiso 1 1 calc R U . . .
H13B H 0.5690 0.8395 0.5221 0.148 Uiso 1 1 calc R U . . .
H13C H 0.5490 0.8914 0.5729 0.148 Uiso 1 1 calc R U . . .
Au Au 0.43489(10) 0.17732(14) 0.77855(8) 0.0544(5) Uani 0.5 1 d . . P A 2
Cl Cl 0.3918(13) 0.0452(17) 0.8255(12) 0.069(5) Uani 0.329(15) 1 d . . P A 2
Cl1 Cl 0.356(3) 0.071(4) 0.799(3) 0.069(5) Uani 0.171(15) 1 d . . P A 3
Si Si 0.3125(6) 0.1304(11) 0.7652(5) 0.052(3) Uani 0.5 1 d . . P A 1
C5 C 0.386(2) 0.197(4) 0.7543(18) 0.053(5) Uani 0.5 1 d . . P A 1
C6 C 0.2683(19) 0.262(3) 0.7762(16) 0.053(5) Uani 0.5 1 d . . P A 1
H6A H 0.2295 0.2777 0.7391 0.080 Uiso 0.5 1 calc R U P A 1
H6B H 0.2971 0.3312 0.7862 0.080 Uiso 0.5 1 calc R U P A 1
H6C H 0.2553 0.2467 0.8091 0.080 Uiso 0.5 1 calc R U P A 1
C7 C 0.2597(19) 0.081(3) 0.6887(16) 0.053(5) Uani 0.5 1 d . . P A 1
H7A H 0.2494 -0.0029 0.6895 0.080 Uiso 0.5 1 calc R U P A 1
H7B H 0.2824 0.0921 0.6625 0.080 Uiso 0.5 1 calc R U P A 1
H7C H 0.2193 0.1270 0.6732 0.080 Uiso 0.5 1 calc R U P A 1
C4 C 0.4302(14) 0.233(3) 0.7506(18) 0.053(5) Uani 0.5 1 d D . P A 1
C8 C 0.337(2) 0.010(4) 0.8227(16) 0.053(5) Uani 0.5 1 d . . P A 1
H8A H 0.3547 -0.0561 0.8087 0.080 Uiso 0.5 1 calc R U P A 1
H8B H 0.2988 -0.0157 0.8288 0.080 Uiso 0.5 1 calc R U P A 1
H8C H 0.3702 0.0403 0.8607 0.080 Uiso 0.5 1 calc R U P A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W C1 1.819(17) . ?
W C3 1.97(2) . ?
W C2 1.977(19) . ?
W N3 2.183(13) . ?
W N5 2.231(13) . ?
W N1 2.282(14) . ?
P C4 1.726(19) . ?
P C4 1.726(19) 2_656 ?
P C1 1.772(18) 2_656 ?
P C1 1.772(17) . ?
P Au 2.297(4) . ?
P Au 2.297(4) 2_656 ?
N3 C10 1.35(2) . ?
N3 N4 1.411(18) . ?
N2 C22 1.34(2) . ?
N2 N1 1.381(19) . ?
N2 B 1.53(3) . ?
N1 C20 1.31(2) . ?
N4 C12 1.34(2) . ?
N4 B 1.55(3) . ?
N5 N6 1.326(19) . ?
N5 C15 1.37(2) . ?
C2 O1 1.14(2) . ?
O2 C3 1.17(2) . ?
N6 C17 1.34(2) . ?
N6 B 1.55(2) . ?
C15 C16 1.36(3) . ?
C15 C14 1.48(3) . ?
C20 C21 1.38(2) . ?
C20 C19 1.52(2) . ?
C22 C21 1.37(3) . ?
C22 C23 1.52(2) . ?
C10 C11 1.33(3) . ?
C10 C9 1.51(2) . ?
C12 C11 1.36(3) . ?
C12 C13 1.47(3) . ?
C16 C17 1.40(3) . ?
C16 H16 0.9300 . ?
C11 H11 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C17 C18 1.45(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C21 H21 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
B H 0.9800 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
Au Cl 2.285(18) . ?
Si C7 1.80(4) . ?
Si C8 1.83(4) . ?
Si C6 1.84(4) . ?
Si C5 1.89(5) . ?
C5 C4 1.10(5) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 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 W C3 85.4(8) . . ?
C1 W C2 85.1(7) . . ?
C3 W C2 84.2(9) . . ?
C1 W N3 104.3(6) . . ?
C3 W N3 170.3(6) . . ?
C2 W N3 95.7(6) . . ?
C1 W N5 101.4(6) . . ?
C3 W N5 94.2(7) . . ?
C2 W N5 173.2(6) . . ?
N3 W N5 84.8(5) . . ?
C1 W N1 174.3(7) . . ?
C3 W N1 90.4(7) . . ?
C2 W N1 90.7(6) . . ?
N3 W N1 79.8(5) . . ?
N5 W N1 82.7(5) . . ?
C4 P C4 128(3) . 2_656 ?
C4 P C1 112.1(14) . 2_656 ?
C4 P C1 99.6(15) 2_656 2_656 ?
C4 P C1 99.6(15) . . ?
C4 P C1 112.1(14) 2_656 . ?
C1 P C1 103.8(11) 2_656 . ?
C1 P Au 104.7(5) 2_656 . ?
C1 P Au 119.3(6) . . ?
C1 P Au 119.3(6) 2_656 2_656 ?
C1 P Au 104.7(5) . 2_656 ?
Au P Au 106.0(2) . 2_656 ?
C10 N3 N4 102.2(13) . . ?
C10 N3 W 137.0(11) . . ?
N4 N3 W 120.6(10) . . ?
C22 N2 N1 108.1(14) . . ?
C22 N2 B 130.2(15) . . ?
N1 N2 B 121.7(14) . . ?
C20 N1 N2 107.2(14) . . ?
C20 N1 W 135.3(12) . . ?
N2 N1 W 117.5(11) . . ?
C12 N4 N3 109.2(15) . . ?
C12 N4 B 131.7(16) . . ?
N3 N4 B 118.8(14) . . ?
N6 N5 C15 106.9(14) . . ?
N6 N5 W 121.3(10) . . ?
C15 N5 W 131.4(12) . . ?
O1 C2 W 175.1(16) . . ?
P C1 W 170.0(11) . . ?
N5 N6 C17 111.5(15) . . ?
N5 N6 B 120.3(14) . . ?
C17 N6 B 128.2(17) . . ?
O2 C3 W 178.8(19) . . ?
C16 C15 N5 108.9(17) . . ?
C16 C15 C14 130.1(17) . . ?
N5 C15 C14 121.0(18) . . ?
N1 C20 C21 110.8(17) . . ?
N1 C20 C19 124.9(16) . . ?
C21 C20 C19 124.2(18) . . ?
N2 C22 C21 108.9(15) . . ?
N2 C22 C23 122.5(18) . . ?
C21 C22 C23 128.6(18) . . ?
C11 C10 N3 114.2(16) . . ?
C11 C10 C9 129.2(18) . . ?
N3 C10 C9 116.6(16) . . ?
N4 C12 C11 109.0(17) . . ?
N4 C12 C13 121.0(19) . . ?
C11 C12 C13 130(2) . . ?
C15 C16 C17 106.4(16) . . ?
C15 C16 H16 126.8 . . ?
C17 C16 H16 126.8 . . ?
C10 C11 C12 105.2(18) . . ?
C10 C11 H11 127.4 . . ?
C12 C11 H11 127.4 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C17 C16 106.4(17) . . ?
N6 C17 C18 124(2) . . ?
C16 C17 C18 129.5(18) . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C10 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C22 C21 C20 104.9(17) . . ?
C22 C21 H21 127.5 . . ?
C20 C21 H21 127.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 B N6 110.8(15) . . ?
N2 B N4 108.6(14) . . ?
N6 B N4 107.7(16) . . ?
N2 B H 109.9 . . ?
N6 B H 109.9 . . ?
N4 B H 109.9 . . ?
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 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Cl Au P 167.3(7) . . ?
C7 Si C8 114.1(18) . . ?
C7 Si C6 103.4(18) . . ?
C8 Si C6 118.7(17) . . ?
C7 Si C5 101.9(18) . . ?
C8 Si C5 113(2) . . ?
C6 Si C5 104.1(19) . . ?
C4 C5 Si 177(4) . . ?
Si C6 H6A 109.5 . . ?
Si C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si C7 H7A 109.5 . . ?
Si C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C4 P 174(4) . . ?
Si C8 H8A 109.5 . . ?
Si C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

_refine_diff_density_max         1.548
_refine_diff_density_min         -1.896
_refine_diff_density_rms         0.211



####################################################################### 
# 
# 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_Compound_7
_database_code_depnum_ccdc_archive 'CCDC 1851870'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H51 B2 N12 O4 P W2'
_chemical_formula_sum            'C45 H51 B2 N12 O4 P W2'
_chemical_formula_weight         1244.26

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7103(8)
_cell_length_b                   12.8936(5)
_cell_length_c                   19.5744(8)
_cell_angle_alpha                77.598(4)
_cell_angle_beta                 78.252(5)
_cell_angle_gamma                70.388(5)
_cell_volume                     2461.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    12876
_cell_measurement_theta_min      3.7150
_cell_measurement_theta_max      28.6470

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_F_000             1220
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.039
_exptl_absorpt_coefficient_mu    4.757
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_reflns_number            35346
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.388
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             10039
_reflns_number_gt                8161
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0375P)²+3.1559P] 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         10039
_refine_ls_number_parameters     569
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0865
_refine_ls_wR_factor_gt          0.0798
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.006
_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
W1 W 0.27620(2) 0.76382(2) 0.65024(2) 0.02636(7) Uani 1 1 d . . . . .
W2 W 0.31789(2) 1.06252(2) 0.80845(2) 0.02170(7) Uani 1 1 d . . . . .
P P 0.31774(15) 0.78070(12) 0.82447(7) 0.0295(3) Uani 1 1 d . . . . .
O4 O 0.0179(4) 1.0689(4) 0.8237(2) 0.0560(13) Uani 1 1 d . . . . .
O3 O 0.3478(5) 1.0862(4) 0.6429(2) 0.0470(11) Uani 1 1 d . . . . .
O1 O 0.0965(5) 1.0094(4) 0.6671(2) 0.0487(11) Uani 1 1 d . . . . .
O2 O 0.5409(5) 0.8313(5) 0.6072(3) 0.0636(15) Uani 1 1 d . . . . .
N1 N 0.2418(5) 0.8062(4) 0.5346(2) 0.0400(13) Uani 1 1 d . . . . .
N2 N 0.2018(5) 0.7341(4) 0.5072(2) 0.0312(11) Uani 1 1 d . . . . .
N5 N 0.0947(4) 0.7098(3) 0.6660(2) 0.0243(10) Uani 1 1 d . . . . .
N6 N 0.0755(4) 0.6571(4) 0.6166(2) 0.0266(10) Uani 1 1 d . . . . .
N3 N 0.3721(5) 0.5934(4) 0.6252(2) 0.0294(10) Uani 1 1 d . . . . .
N4 N 0.3179(5) 0.5532(4) 0.5822(2) 0.0302(10) Uani 1 1 d . . . . .
N11 N 0.5178(4) 1.0803(3) 0.8013(2) 0.0241(9) Uani 1 1 d . . . . .
N12 N 0.5358(4) 1.1604(3) 0.8318(2) 0.0243(9) Uani 1 1 d . . . . .
N7 N 0.2535(4) 1.2540(4) 0.7969(2) 0.0283(10) Uani 1 1 d . . . . .
N8 N 0.3076(4) 1.3005(3) 0.8363(2) 0.0260(10) Uani 1 1 d . . . . .
N9 N 0.3069(4) 1.0754(4) 0.9200(2) 0.0245(9) Uani 1 1 d . . . . .
N10 N 0.3642(4) 1.1451(3) 0.9381(2) 0.0258(10) Uani 1 1 d . . . . .
C68 C 0.3642(7) 0.3772(5) 0.5330(3) 0.0473(16) Uani 1 1 d . . . . .
H68A H 0.434987 0.307732 0.532696 0.071 Uiso 1 1 calc R U . . .
H68B H 0.359299 0.416365 0.485558 0.071 Uiso 1 1 calc R U . . .
H68C H 0.280662 0.362936 0.552612 0.071 Uiso 1 1 calc R U . . .
C1 C 0.3052(5) 0.7580(4) 0.7393(3) 0.0243(11) Uani 1 1 d . . . . .
C2 C 0.3433(5) 0.9133(4) 0.8129(3) 0.0258(12) Uani 1 1 d . . . . .
C7 C 0.4733(6) 0.6856(5) 0.8435(3) 0.0361(14) Uani 1 1 d . . . . .
C8 C 0.5668(7) 0.6158(5) 0.8673(3) 0.0399(15) Uani 1 1 d . . . . .
C6 C 0.1259(6) 1.0694(5) 0.8177(3) 0.0326(13) Uani 1 1 d . . . . .
C5 C 0.3359(6) 1.0767(5) 0.7029(3) 0.0305(13) Uani 1 1 d . . . . .
C4 C 0.4428(7) 0.8084(5) 0.6220(3) 0.0414(15) Uani 1 1 d . . . . .
C3 C 0.1631(6) 0.9217(5) 0.6597(3) 0.0335(13) Uani 1 1 d . . . . .
C150 C 0.1221(7) 0.7245(6) 0.3978(3) 0.0449(16) Uani 1 1 d . . . . .
H15D H 0.125586 0.762449 0.349886 0.067 Uiso 1 1 calc R U . . .
H15E H 0.031448 0.726166 0.416569 0.067 Uiso 1 1 calc R U . . .
H15F H 0.177969 0.648466 0.398982 0.067 Uiso 1 1 calc R U . . .
C151 C 0.1707(6) 0.7812(5) 0.4414(3) 0.0386(15) Uani 1 1 d . . . . .
C152 C 0.1919(8) 0.8823(6) 0.4258(3) 0.054(2) Uani 1 1 d . . . . .
H152 H 0.179606 0.932205 0.383936 0.065 Uiso 1 1 calc R U . . .
C153 C 0.2354(8) 0.8972(6) 0.4845(3) 0.0524(19) Uani 1 1 d . . . . .
C154 C 0.5615(6) 0.5242(6) 0.6944(3) 0.0466(17) Uani 1 1 d . . . . .
H15G H 0.639199 0.459854 0.698044 0.070 Uiso 1 1 calc R U . . .
H15H H 0.510406 0.531864 0.740406 0.070 Uiso 1 1 calc R U . . .
H15I H 0.588905 0.589558 0.675383 0.070 Uiso 1 1 calc R U . . .
C155 C 0.4775(6) 0.5108(5) 0.6467(3) 0.0364(14) Uani 1 1 d . . . . .
C156 C 0.4935(6) 0.4171(5) 0.6170(3) 0.0404(15) Uani 1 1 d . . . . .
H156 H 0.559813 0.348739 0.623125 0.048 Uiso 1 1 calc R U . . .
C157 C 0.3914(6) 0.4458(5) 0.5765(3) 0.0382(14) Uani 1 1 d . . . . .
C158 C -0.0279(6) 0.7777(5) 0.7781(3) 0.0386(14) Uani 1 1 d . . . . .
H15J H -0.113525 0.781901 0.806295 0.058 Uiso 1 1 calc R U . . .
H15K H -0.019628 0.851383 0.763354 0.058 Uiso 1 1 calc R U . . .
H15L H 0.041879 0.732703 0.805464 0.058 Uiso 1 1 calc R U . . .
C159 C -0.0162(6) 0.7260(4) 0.7136(3) 0.0293(12) Uani 1 1 d . . . . .
C160 C -0.1072(6) 0.6858(5) 0.6945(3) 0.0342(13) Uani 1 1 d . . . . .
H160 H -0.191889 0.687025 0.718559 0.041 Uiso 1 1 calc R U . . .
C161 C -0.0473(6) 0.6440(5) 0.6328(3) 0.0316(13) Uani 1 1 d . . . . .
C162 C -0.1027(6) 0.5950(6) 0.5867(3) 0.0447(16) Uani 1 1 d . . . . .
H16A H -0.185931 0.583916 0.610664 0.067 Uiso 1 1 calc R U . . .
H16B H -0.039946 0.524798 0.576921 0.067 Uiso 1 1 calc R U . . .
H16C H -0.117550 0.645239 0.543053 0.067 Uiso 1 1 calc R U . . .
C163 C 0.0918(7) 1.3207(5) 0.7096(4) 0.0512(18) Uani 1 1 d . . . . .
H16D H 0.042866 1.391728 0.685997 0.077 Uiso 1 1 calc R U . . .
H16E H 0.030107 1.282536 0.736625 0.077 Uiso 1 1 calc R U . . .
H16F H 0.150648 1.276854 0.675265 0.077 Uiso 1 1 calc R U . . .
C164 C 0.1722(6) 1.3379(5) 0.7580(3) 0.0351(13) Uani 1 1 d . . . . .
C165 C 0.1762(6) 1.4379(5) 0.7716(3) 0.0387(14) Uani 1 1 d . . . . .
H165 H 0.130252 1.508975 0.750878 0.046 Uiso 1 1 calc R U . . .
C166 C 0.2604(5) 1.4129(4) 0.8212(3) 0.0315(13) Uani 1 1 d . . . . .
C167 C 0.2941(6) 1.4881(5) 0.8572(4) 0.0462(16) Uani 1 1 d . . . . .
H16G H 0.260008 1.563808 0.834728 0.069 Uiso 1 1 calc R U . . .
H16H H 0.389533 1.468219 0.854396 0.069 Uiso 1 1 calc R U . . .
H16I H 0.254363 1.480940 0.905939 0.069 Uiso 1 1 calc R U . . .
C168 C 0.1907(6) 0.9368(5) 0.9827(3) 0.0417(15) Uani 1 1 d . . . . .
H16J H 0.155019 0.914334 1.030620 0.063 Uiso 1 1 calc R U . . .
H16K H 0.253540 0.872979 0.964028 0.063 Uiso 1 1 calc R U . . .
H16L H 0.119168 0.969335 0.954665 0.063 Uiso 1 1 calc R U . . .
C169 C 0.2600(5) 1.0207(4) 0.9809(3) 0.0294(12) Uani 1 1 d . . . . .
C170 C 0.6537(6) 0.9442(5) 0.7219(3) 0.0389(14) Uani 1 1 d . . . . .
H17A H 0.747146 0.913679 0.705038 0.058 Uiso 1 1 calc R U . . .
H17B H 0.604679 0.973665 0.682448 0.058 Uiso 1 1 calc R U . . .
H17C H 0.621356 0.886597 0.752088 0.058 Uiso 1 1 calc R U . . .
C171 C 0.6351(5) 1.0355(5) 0.7626(3) 0.0284(12) Uani 1 1 d . . . . .
C172 C 0.7282(5) 1.0867(5) 0.7685(3) 0.0294(12) Uani 1 1 d . . . . .
H172 H 0.817154 1.070629 0.747497 0.035 Uiso 1 1 calc R U . . .
C173 C 0.6611(5) 1.1657(4) 0.8118(3) 0.0270(12) Uani 1 1 d . . . . .
C174 C 0.7104(6) 1.2463(5) 0.8343(3) 0.0400(15) Uani 1 1 d . . . . .
H17D H 0.801863 1.237244 0.813279 0.060 Uiso 1 1 calc R U . . .
H17E H 0.704891 1.232753 0.884847 0.060 Uiso 1 1 calc R U . . .
H17F H 0.656377 1.320950 0.819297 0.060 Uiso 1 1 calc R U . . .
C175 C 0.4075(7) 1.1936(6) 1.0464(3) 0.0467(16) Uani 1 1 d . . . . .
H17G H 0.391431 1.169904 1.096518 0.070 Uiso 1 1 calc R U . . .
H17H H 0.363097 1.272042 1.035474 0.070 Uiso 1 1 calc R U . . .
H17I H 0.502031 1.178820 1.031327 0.070 Uiso 1 1 calc R U . . .
C176 C 0.3546(6) 1.1312(5) 1.0091(3) 0.0320(13) Uani 1 1 d . . . . .
C177 C 0.2893(6) 1.0526(5) 1.0378(3) 0.0349(13) Uani 1 1 d . . . . .
H177 H 0.268958 1.026236 1.085544 0.042 Uiso 1 1 calc R U . . .
C180 C 0.2749(11) 0.9940(7) 0.4937(4) 0.093(4) Uani 1 1 d . . . . .
H18A H 0.286611 1.039672 0.448608 0.140 Uiso 1 1 calc R U . . .
H18B H 0.357319 0.966876 0.513232 0.140 Uiso 1 1 calc R U . . .
H18C H 0.205940 1.037460 0.525042 0.140 Uiso 1 1 calc R U . . .
B1 B 0.1860(7) 0.6251(5) 0.5538(3) 0.0315(15) Uani 1 1 d . . . . .
H1 H 0.159534 0.582748 0.526242 0.038 Uiso 1 1 calc R U . . .
B2 B 0.4186(6) 1.2267(5) 0.8810(3) 0.0267(13) Uani 1 1 d . . . . .
H2 H 0.449370 1.273556 0.902936 0.032 Uiso 1 1 calc R U . . .
C9 C 0.6746(10) 0.5257(10) 0.8981(7) 0.0448(8) Uani 0.413(10) 1 d G . P A 1
C10 C 0.8074(12) 0.5170(10) 0.8706(5) 0.0448(8) Uani 0.413(10) 1 d G . P A 1
H10 H 0.827673 0.565311 0.830458 0.054 Uiso 0.413(10) 1 calc R U P A 1
C11 C 0.9099(9) 0.4361(11) 0.9033(6) 0.0448(8) Uani 0.413(10) 1 d G . P A 1
H11 H 0.998737 0.430232 0.884919 0.054 Uiso 0.413(10) 1 calc R U P A 1
C12 C 0.8795(11) 0.3638(9) 0.9633(6) 0.0448(8) Uani 0.413(10) 1 d G . P A 1
C13 C 0.7467(13) 0.3725(10) 0.9907(5) 0.0448(8) Uani 0.413(10) 1 d G . P A 1
H13 H 0.726444 0.324182 1.030926 0.054 Uiso 0.413(10) 1 calc R U P A 1
C14 C 0.6442(10) 0.4534(12) 0.9581(7) 0.0448(8) Uani 0.413(10) 1 d G . P A 1
H14 H 0.555377 0.459261 0.976466 0.054 Uiso 0.413(10) 1 calc R U P A 1
C15 C 0.9930(17) 0.2711(15) 0.9919(9) 0.0448(8) Uani 0.413(10) 1 d . . P A 1
H15A H 0.958896 0.227593 1.033085 0.067 Uiso 0.413(10) 1 calc R U P A 1
H15B H 1.038946 0.224424 0.956612 0.067 Uiso 0.413(10) 1 calc R U P A 1
H15C H 1.054176 0.301587 1.004298 0.067 Uiso 0.413(10) 1 calc R U P A 1
C9A C 0.6840(7) 0.5360(7) 0.8981(5) 0.0448(8) Uani 0.587(10) 1 d G . P A 2
C10A C 0.8058(8) 0.5582(7) 0.8860(4) 0.0448(8) Uani 0.587(10) 1 d G . P A 2
H10A H 0.815999 0.621833 0.855552 0.054 Uiso 0.587(10) 1 calc R U P A 2
C11A C 0.9122(7) 0.4851(7) 0.9194(4) 0.0448(8) Uani 0.587(10) 1 d G . P A 2
H11A H 0.993624 0.499894 0.911298 0.054 Uiso 0.587(10) 1 calc R U P A 2
C12A C 0.8969(8) 0.3899(6) 0.9649(4) 0.0448(8) Uani 0.587(10) 1 d G . P A 2
C13A C 0.7751(9) 0.3678(6) 0.9770(4) 0.0448(8) Uani 0.587(10) 1 d G . P A 2
H13A H 0.764908 0.304108 1.007411 0.054 Uiso 0.587(10) 1 calc R U P A 2
C14A C 0.6687(7) 0.4408(8) 0.9436(5) 0.0448(8) Uani 0.587(10) 1 d G . P A 2
H14A H 0.587281 0.426045 0.951665 0.054 Uiso 0.587(10) 1 calc R U P A 2
C15A C 1.0118(12) 0.3089(10) 1.0019(6) 0.0448(8) Uani 0.587(10) 1 d . . P A 2
H15M H 0.983403 0.248493 1.031010 0.067 Uiso 0.587(10) 1 calc R U P A 2
H15N H 1.086134 0.280078 0.967245 0.067 Uiso 0.587(10) 1 calc R U P A 2
H15O H 1.038513 0.346887 1.030815 0.067 Uiso 0.587(10) 1 calc R U P A 2


_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
W1 C1 1.813(5) . ?
W1 C4 1.992(6) . ?
W1 C3 2.015(6) . ?
W1 N3 2.206(5) . ?
W1 N5 2.221(4) . ?
W1 N1 2.286(4) . ?
W2 C2 1.836(5) . ?
W2 C6 2.001(6) . ?
W2 C5 2.010(5) . ?
W2 N9 2.201(4) . ?
W2 N11 2.202(4) . ?
W2 N7 2.302(4) . ?
P C7 1.762(6) . ?
P C2 1.781(5) . ?
P C1 1.793(5) . ?
O4 C6 1.140(6) . ?
O3 C5 1.139(6) . ?
O1 C3 1.138(7) . ?
O2 C4 1.150(7) . ?
N1 C153 1.351(7) . ?
N1 N2 1.383(6) . ?
N2 C151 1.357(7) . ?
N2 B1 1.543(8) . ?
N5 C159 1.337(7) . ?
N5 N6 1.377(5) . ?
N6 C161 1.347(7) . ?
N6 B1 1.543(8) . ?
N3 C155 1.334(7) . ?
N3 N4 1.380(6) . ?
N4 C157 1.360(7) . ?
N4 B1 1.544(8) . ?
N11 C171 1.342(7) . ?
N11 N12 1.380(5) . ?
N12 C173 1.340(6) . ?
N12 B2 1.542(7) . ?
N7 C164 1.338(7) . ?
N7 N8 1.380(5) . ?
N8 C166 1.353(7) . ?
N8 B2 1.546(7) . ?
N9 C169 1.343(6) . ?
N9 N10 1.380(5) . ?
N10 C176 1.349(6) . ?
N10 B2 1.529(7) . ?
C68 C157 1.479(8) . ?
C7 C8 1.198(8) . ?
C8 C9 1.458(11) . ?
C8 C9A 1.473(9) . ?
C150 C151 1.496(7) . ?
C151 C152 1.357(8) . ?
C152 C153 1.394(8) . ?
C153 C180 1.501(8) . ?
C154 C155 1.492(8) . ?
C155 C156 1.397(8) . ?
C156 C157 1.384(8) . ?
C158 C159 1.514(7) . ?
C159 C160 1.389(7) . ?
C160 C161 1.375(8) . ?
C161 C162 1.511(7) . ?
C163 C164 1.496(8) . ?
C164 C165 1.388(8) . ?
C165 C166 1.373(8) . ?
C166 C167 1.483(8) . ?
C168 C169 1.494(8) . ?
C169 C177 1.391(7) . ?
C170 C171 1.496(7) . ?
C171 C172 1.402(7) . ?
C172 C173 1.380(7) . ?
C173 C174 1.488(7) . ?
C175 C176 1.493(7) . ?
C176 C177 1.380(8) . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 C11 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C12 C15 1.495(18) . ?
C13 C14 1.3900 . ?
C9A C10A 1.3900 . ?
C9A C14A 1.3900 . ?
C10A C11A 1.3900 . ?
C11A C12A 1.3900 . ?
C12A C13A 1.3900 . ?
C12A C15A 1.519(12) . ?
C13A C14A 1.3900 . ?

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 W1 C4 83.9(2) . . ?
C1 W1 C3 84.1(2) . . ?
C4 W1 C3 91.8(2) . . ?
C1 W1 N3 106.04(19) . . ?
C4 W1 N3 94.9(2) . . ?
C3 W1 N3 168.40(19) . . ?
C1 W1 N5 103.95(19) . . ?
C4 W1 N5 171.87(19) . . ?
C3 W1 N5 91.18(19) . . ?
N3 W1 N5 81.04(16) . . ?
C1 W1 N1 168.73(19) . . ?
C4 W1 N1 89.5(2) . . ?
C3 W1 N1 87.0(2) . . ?
N3 W1 N1 83.58(17) . . ?
N5 W1 N1 83.06(16) . . ?
C2 W2 C6 81.8(2) . . ?
C2 W2 C5 87.5(2) . . ?
C6 W2 C5 90.5(2) . . ?
C2 W2 N9 102.18(19) . . ?
C6 W2 N9 94.41(19) . . ?
C5 W2 N9 169.68(18) . . ?
C2 W2 N11 106.36(19) . . ?
C6 W2 N11 171.61(19) . . ?
C5 W2 N11 91.61(19) . . ?
N9 W2 N11 82.30(15) . . ?
C2 W2 N7 170.73(18) . . ?
C6 W2 N7 89.60(19) . . ?
C5 W2 N7 89.01(19) . . ?
N9 W2 N7 81.95(15) . . ?
N11 W2 N7 82.32(15) . . ?
C7 P C2 103.7(3) . . ?
C7 P C1 103.8(3) . . ?
C2 P C1 107.3(2) . . ?
C153 N1 N2 106.4(4) . . ?
C153 N1 W1 134.1(4) . . ?
N2 N1 W1 118.9(3) . . ?
C151 N2 N1 109.4(4) . . ?
C151 N2 B1 130.5(4) . . ?
N1 N2 B1 119.9(4) . . ?
C159 N5 N6 106.7(4) . . ?
C159 N5 W1 132.9(3) . . ?
N6 N5 W1 120.1(3) . . ?
C161 N6 N5 109.6(4) . . ?
C161 N6 B1 130.1(4) . . ?
N5 N6 B1 120.3(4) . . ?
C155 N3 N4 107.2(4) . . ?
C155 N3 W1 132.3(4) . . ?
N4 N3 W1 120.4(3) . . ?
C157 N4 N3 109.6(5) . . ?
C157 N4 B1 129.9(5) . . ?
N3 N4 B1 120.3(4) . . ?
C171 N11 N12 106.6(4) . . ?
C171 N11 W2 131.5(3) . . ?
N12 N11 W2 121.2(3) . . ?
C173 N12 N11 110.1(4) . . ?
C173 N12 B2 130.5(4) . . ?
N11 N12 B2 119.4(4) . . ?
C164 N7 N8 107.4(4) . . ?
C164 N7 W2 134.6(4) . . ?
N8 N7 W2 118.0(3) . . ?
C166 N8 N7 109.3(4) . . ?
C166 N8 B2 129.4(4) . . ?
N7 N8 B2 120.8(4) . . ?
C169 N9 N10 106.5(4) . . ?
C169 N9 W2 132.7(3) . . ?
N10 N9 W2 120.7(3) . . ?
C176 N10 N9 109.5(4) . . ?
C176 N10 B2 130.1(4) . . ?
N9 N10 B2 120.3(4) . . ?
P C1 W1 168.9(3) . . ?
P C2 W2 163.6(3) . . ?
C8 C7 P 168.8(6) . . ?
C7 C8 C9 175.9(8) . . ?
C7 C8 C9A 176.1(7) . . ?
O4 C6 W2 177.3(5) . . ?
O3 C5 W2 178.5(5) . . ?
O2 C4 W1 177.8(6) . . ?
O1 C3 W1 177.5(6) . . ?
N2 C151 C152 108.0(5) . . ?
N2 C151 C150 122.5(5) . . ?
C152 C151 C150 129.5(5) . . ?
C151 C152 C153 107.1(5) . . ?
N1 C153 C152 109.1(5) . . ?
N1 C153 C180 122.6(5) . . ?
C152 C153 C180 128.3(6) . . ?
N3 C155 C156 109.4(5) . . ?
N3 C155 C154 122.2(6) . . ?
C156 C155 C154 128.3(6) . . ?
C157 C156 C155 106.6(6) . . ?
N4 C157 C156 107.1(5) . . ?
N4 C157 C68 124.4(6) . . ?
C156 C157 C68 128.4(6) . . ?
N5 C159 C160 109.6(5) . . ?
N5 C159 C158 121.3(5) . . ?
C160 C159 C158 129.1(5) . . ?
C161 C160 C159 106.4(5) . . ?
N6 C161 C160 107.7(5) . . ?
N6 C161 C162 122.9(5) . . ?
C160 C161 C162 129.3(5) . . ?
N7 C164 C165 108.6(5) . . ?
N7 C164 C163 123.3(5) . . ?
C165 C164 C163 128.1(5) . . ?
C166 C165 C164 107.5(5) . . ?
N8 C166 C165 107.2(5) . . ?
N8 C166 C167 122.9(5) . . ?
C165 C166 C167 129.9(5) . . ?
N9 C169 C177 109.9(5) . . ?
N9 C169 C168 122.2(5) . . ?
C177 C169 C168 127.8(5) . . ?
N11 C171 C172 109.3(5) . . ?
N11 C171 C170 121.8(5) . . ?
C172 C171 C170 129.0(5) . . ?
C173 C172 C171 106.1(5) . . ?
N12 C173 C172 107.9(5) . . ?
N12 C173 C174 123.0(5) . . ?
C172 C173 C174 129.1(5) . . ?
N10 C176 C177 108.1(5) . . ?
N10 C176 C175 123.4(5) . . ?
C177 C176 C175 128.5(5) . . ?
C176 C177 C169 105.9(5) . . ?
N6 B1 N2 107.7(5) . . ?
N6 B1 N4 109.2(4) . . ?
N2 B1 N4 110.9(5) . . ?
N10 B2 N12 109.1(4) . . ?
N10 B2 N8 109.6(4) . . ?
N12 B2 N8 108.3(4) . . ?
C10 C9 C14 120.0 . . ?
C10 C9 C8 120.1(9) . . ?
C14 C9 C8 119.7(9) . . ?
C11 C10 C9 120.0 . . ?
C12 C11 C10 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 C15 117.7(10) . . ?
C13 C12 C15 122.0(10) . . ?
C14 C13 C12 120.0 . . ?
C13 C14 C9 120.0 . . ?
C10A C9A C14A 120.0 . . ?
C10A C9A C8 121.1(6) . . ?
C14A C9A C8 118.7(6) . . ?
C11A C10A C9A 120.0 . . ?
C10A C11A C12A 120.0 . . ?
C11A C12A C13A 120.0 . . ?
C11A C12A C15A 120.9(7) . . ?
C13A C12A C15A 119.1(7) . . ?
C14A C13A C12A 120.0 . . ?
C13A C14A C9A 120.0 . . ?

_refine_diff_density_max         2.305
_refine_diff_density_min         -1.492
_refine_diff_density_rms         0.140



####################################################################### 
# 
# 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_Compound_8
_database_code_depnum_ccdc_archive 'CCDC 1851878'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-10-11 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         'C42 H53 B2 N12 O4 P W2, C H Cl3'
_chemical_formula_sum            'C43 H54 B2 Cl3 N12 O4 P W2'
_chemical_formula_weight         1329.62

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.4150(5)
_cell_length_b                   10.8991(2)
_cell_length_c                   24.0583(5)
_cell_angle_alpha                90
_cell_angle_beta                 115.668(3)
_cell_angle_gamma                90
_cell_volume                     5061.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    30131
_cell_measurement_theta_min      3.6250
_cell_measurement_theta_max      29.6310

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_F_000             2608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.291
_exptl_crystal_size_min          0.114
_exptl_absorpt_coefficient_mu    4.785
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.48028
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_reflns_number            51216
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.380
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5154
_reflns_number_gt                4941
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_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)+(0.0067P)²+21.1350P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5154
_refine_ls_number_parameters     349
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0198
_refine_ls_wR_factor_ref         0.0441
_refine_ls_wR_factor_gt          0.0432
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_restrained_S_all      1.240
_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
W W 0.58836(2) 0.53392(2) 0.38343(2) 0.02198(4) Uani 1 1 d . . . . .
P P 0.5000 0.72500(10) 0.2500 0.0280(2) Uani 1 2 d S T P . .
N5 N 0.50996(12) 0.4452(2) 0.40735(11) 0.0242(5) Uani 1 1 d . . . . .
N6 N 0.51378(13) 0.3219(2) 0.42041(11) 0.0258(5) Uani 1 1 d . . . . .
N3 N 0.59238(13) 0.3544(2) 0.34233(11) 0.0251(5) Uani 1 1 d . . . . .
O1 O 0.59245(15) 0.7860(2) 0.44781(12) 0.0471(7) Uani 1 1 d . . . . .
O2 O 0.71754(14) 0.6415(3) 0.37053(13) 0.0516(7) Uani 1 1 d . . . . .
N4 N 0.58362(13) 0.2465(2) 0.36738(11) 0.0253(5) Uani 1 1 d . . . . .
N1 N 0.65789(12) 0.4336(2) 0.47183(11) 0.0232(5) Uani 1 1 d . . . . .
N2 N 0.64299(13) 0.3134(2) 0.47872(11) 0.0235(5) Uani 1 1 d . . . . .
C1 C 0.53812(16) 0.6218(3) 0.31373(13) 0.0260(6) Uani 1 1 d . . . . .
C2 C 0.59022(18) 0.6911(3) 0.42634(14) 0.0324(7) Uani 1 1 d . . . . .
C3 C 0.67059(17) 0.5996(3) 0.37486(14) 0.0323(7) Uani 1 1 d . . . . .
C16 C 0.59789(15) 0.3249(3) 0.29040(13) 0.0274(6) Uani 1 1 d . . . . .
C11 C 0.45219(16) 0.4871(3) 0.40972(13) 0.0314(7) Uani 1 1 d . . . . .
C21 C 0.71417(15) 0.4646(3) 0.52339(13) 0.0268(6) Uani 1 1 d . . . . .
C23 C 0.68979(16) 0.2711(3) 0.53370(13) 0.0271(6) Uani 1 1 d . . . . .
C15 C 0.60788(19) 0.4180(3) 0.24963(15) 0.0391(8) Uani 1 1 d . . . . .
H15A H 0.5694 0.4738 0.2347 0.059 Uiso 1 1 calc R U . . .
H15B H 0.6108 0.3775 0.2154 0.059 Uiso 1 1 calc R U . . .
H15C H 0.6499 0.4626 0.2726 0.059 Uiso 1 1 calc R U . . .
C18 C 0.58276(15) 0.1518(3) 0.33136(14) 0.0292(7) Uani 1 1 d . . . . .
C20 C 0.74550(17) 0.5895(3) 0.53195(15) 0.0360(8) Uani 1 1 d . . . . .
H20A H 0.7648 0.6014 0.5031 0.054 Uiso 1 1 calc R U . . .
H20B H 0.7814 0.5972 0.5732 0.054 Uiso 1 1 calc R U . . .
H20C H 0.7104 0.6502 0.5251 0.054 Uiso 1 1 calc R U . . .
C13 C 0.45831(17) 0.2878(3) 0.42957(14) 0.0323(7) Uani 1 1 d . . . . .
C12 C 0.41881(17) 0.3901(4) 0.42308(15) 0.0371(8) Uani 1 1 d . . . . .
H12 H 0.3774 0.3941 0.4269 0.045 Uiso 1 1 calc R U . . .
C22 C 0.73546(16) 0.3643(3) 0.56272(13) 0.0287(7) Uani 1 1 d . . . . .
H22 H 0.7733 0.3609 0.6012 0.034 Uiso 1 1 calc R U . . .
C17 C 0.59230(16) 0.1986(3) 0.28266(14) 0.0314(7) Uani 1 1 d . . . . .
H17 H 0.5946 0.1542 0.2506 0.038 Uiso 1 1 calc R U . . .
C24 C 0.6886(2) 0.1436(3) 0.55582(16) 0.0386(8) Uani 1 1 d . . . . .
H24A H 0.6478 0.1326 0.5624 0.058 Uiso 1 1 calc R U . . .
H24B H 0.7290 0.1303 0.5938 0.058 Uiso 1 1 calc R U . . .
H24C H 0.6881 0.0861 0.5255 0.058 Uiso 1 1 calc R U . . .
C10 C 0.43105(19) 0.6181(4) 0.39926(17) 0.0443(9) Uani 1 1 d . . . . .
H10A H 0.4627 0.6666 0.4330 0.066 Uiso 1 1 calc R U . . .
H10B H 0.3852 0.6267 0.3964 0.066 Uiso 1 1 calc R U . . .
H10C H 0.4316 0.6457 0.3616 0.066 Uiso 1 1 calc R U . . .
C19 C 0.5714(2) 0.0222(3) 0.34534(18) 0.0432(9) Uani 1 1 d . . . . .
H19A H 0.6014 0.0040 0.3876 0.065 Uiso 1 1 calc R U . . .
H19B H 0.5814 -0.0325 0.3190 0.065 Uiso 1 1 calc R U . . .
H19C H 0.5240 0.0119 0.3384 0.065 Uiso 1 1 calc R U . . .
C14 C 0.4469(2) 0.1577(4) 0.44252(19) 0.0483(10) Uani 1 1 d . . . . .
H14A H 0.4530 0.1046 0.4133 0.072 Uiso 1 1 calc R U . . .
H14B H 0.4008 0.1486 0.4390 0.072 Uiso 1 1 calc R U . . .
H14C H 0.4798 0.1361 0.4835 0.072 Uiso 1 1 calc R U . . .
B B 0.57872(18) 0.2489(3) 0.42926(16) 0.0258(7) Uani 1 1 d . . . . .
C4 C 0.5754(4) 0.7794(6) 0.2441(3) 0.0426(19) Uani 0.5 1 d . . P A 1
C5 C 0.6229(4) 0.8229(7) 0.2414(4) 0.0451(18) Uani 0.5 1 d . . P A 1
C7 C 0.6685(5) 0.9647(9) 0.1889(4) 0.0526(18) Uani 0.5 1 d D U P A 1
H7A H 0.6380 0.9322 0.1493 0.079 Uiso 0.5 1 calc R U P A 1
H7B H 0.7104 0.9931 0.1879 0.079 Uiso 0.5 1 calc R U P A 1
H7C H 0.6462 1.0319 0.1990 0.079 Uiso 0.5 1 calc R U P A 1
C9 C 0.7274(9) 0.7623(15) 0.2314(10) 0.0526(18) Uani 0.5 1 d D U P A 1
H9A H 0.7008 0.7156 0.1949 0.079 Uiso 0.5 1 calc R U P A 1
H9B H 0.7398 0.7111 0.2671 0.079 Uiso 0.5 1 calc R U P A 1
H9C H 0.7687 0.7922 0.2296 0.079 Uiso 0.5 1 calc R U P A 1
C8 C 0.7297(8) 0.9342(15) 0.2922(6) 0.0526(18) Uani 0.5 1 d D U P A 1
H8A H 0.7657 0.9763 0.2862 0.079 Uiso 0.5 1 calc R U P A 1
H8B H 0.7501 0.8761 0.3252 0.079 Uiso 0.5 1 calc R U P A 1
H8C H 0.7027 0.9925 0.3024 0.079 Uiso 0.5 1 calc R U P A 1
C6 C 0.6849(7) 0.8694(11) 0.2354(5) 0.0526(18) Uani 0.5 1 d D U P A 1
C51 C 0.6838(5) 0.8499(8) 0.2493(3) 0.037(2) Uani 0.5 1 d D . P B 2
H51 H 0.6547 0.8031 0.2639 0.045 Uiso 0.5 1 calc R U P B 2
Cl1 Cl 0.62781(17) 0.9261(3) 0.18372(11) 0.0790(9) Uani 0.5 1 d D . P B 2
Cl2 Cl 0.7341(2) 0.9427(3) 0.30848(11) 0.0529(7) Uani 0.5 1 d D . P B 2
Cl3 Cl 0.7323(3) 0.7411(4) 0.2303(3) 0.0659(9) Uani 0.5 1 d D . P B 2
H99 H 0.5747(17) 0.155(3) 0.4437(15) 0.030(9) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W C1 1.823(3) . ?
W C2 1.992(3) . ?
W C3 1.992(3) . ?
W N3 2.211(3) . ?
W N5 2.219(2) . ?
W N1 2.279(2) . ?
P C4 1.783(8) 2_655 ?
P C4 1.783(8) . ?
P C1 1.788(3) 2_655 ?
P C1 1.788(3) . ?
N5 C11 1.343(4) . ?
N5 N6 1.374(3) . ?
N6 C13 1.351(4) . ?
N6 B 1.535(4) . ?
N3 C16 1.344(4) . ?
N3 N4 1.371(3) . ?
O1 C2 1.148(4) . ?
O2 C3 1.150(4) . ?
N4 C18 1.342(4) . ?
N4 B 1.537(4) . ?
N1 C21 1.346(4) . ?
N1 N2 1.374(3) . ?
N2 C23 1.348(4) . ?
N2 B 1.545(4) . ?
C16 C17 1.387(5) . ?
C16 C15 1.489(5) . ?
C11 C12 1.390(5) . ?
C11 C10 1.486(5) . ?
C21 C22 1.387(4) . ?
C21 C20 1.492(5) . ?
C23 C22 1.373(5) . ?
C23 C24 1.492(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C18 C17 1.372(5) . ?
C18 C19 1.496(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C13 C12 1.367(5) . ?
C13 C14 1.495(5) . ?
C12 H12 0.9300 . ?
C22 H22 0.9300 . ?
C17 H17 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 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 . ?
B H99 1.10(3) . ?
C4 C5 1.149(10) . ?
C5 C6 1.486(15) . ?
C7 C6 1.453(12) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C9 C6 1.509(13) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C8 C6 1.466(12) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C51 Cl2 1.697(9) . ?
C51 Cl1 1.726(7) . ?
C51 Cl3 1.763(8) . ?
C51 H51 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W C2 84.05(13) . . ?
C1 W C3 84.95(13) . . ?
C2 W C3 85.68(14) . . ?
C1 W N3 100.09(11) . . ?
C2 W N3 175.75(11) . . ?
C3 W N3 93.67(12) . . ?
C1 W N5 104.84(11) . . ?
C2 W N5 95.05(12) . . ?
C3 W N5 170.21(11) . . ?
N3 W N5 84.88(9) . . ?
C1 W N1 175.75(11) . . ?
C2 W N1 94.07(11) . . ?
C3 W N1 91.11(11) . . ?
N3 W N1 81.74(9) . . ?
N5 W N1 79.09(9) . . ?
C4 P C4 141.1(5) 2_655 . ?
C4 P C1 100.7(3) 2_655 2_655 ?
C4 P C1 103.5(2) . 2_655 ?
C4 P C1 103.5(2) 2_655 . ?
C4 P C1 100.7(3) . . ?
C1 P C1 102.0(2) 2_655 . ?
C11 N5 N6 106.7(3) . . ?
C11 N5 W 132.6(2) . . ?
N6 N5 W 120.57(18) . . ?
C13 N6 N5 109.7(3) . . ?
C13 N6 B 130.0(3) . . ?
N5 N6 B 120.0(2) . . ?
C16 N3 N4 106.7(2) . . ?
C16 N3 W 131.6(2) . . ?
N4 N3 W 121.57(18) . . ?
C18 N4 N3 110.0(2) . . ?
C18 N4 B 130.6(3) . . ?
N3 N4 B 119.4(2) . . ?
C21 N1 N2 106.9(2) . . ?
C21 N1 W 134.6(2) . . ?
N2 N1 W 118.55(17) . . ?
C23 N2 N1 109.3(2) . . ?
C23 N2 B 129.4(3) . . ?
N1 N2 B 121.1(2) . . ?
P C1 W 170.88(19) . . ?
O1 C2 W 174.8(3) . . ?
O2 C3 W 177.5(3) . . ?
N3 C16 C17 109.0(3) . . ?
N3 C16 C15 123.0(3) . . ?
C17 C16 C15 128.0(3) . . ?
N5 C11 C12 109.1(3) . . ?
N5 C11 C10 122.6(3) . . ?
C12 C11 C10 128.4(3) . . ?
N1 C21 C22 109.2(3) . . ?
N1 C21 C20 121.8(3) . . ?
C22 C21 C20 129.0(3) . . ?
N2 C23 C22 108.0(3) . . ?
N2 C23 C24 123.2(3) . . ?
C22 C23 C24 128.8(3) . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C18 C17 107.5(3) . . ?
N4 C18 C19 122.6(3) . . ?
C17 C18 C19 129.9(3) . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N6 C13 C12 107.6(3) . . ?
N6 C13 C14 121.9(3) . . ?
C12 C13 C14 130.5(3) . . ?
C13 C12 C11 107.0(3) . . ?
C13 C12 H12 126.5 . . ?
C11 C12 H12 126.5 . . ?
C23 C22 C21 106.5(3) . . ?
C23 C22 H22 126.7 . . ?
C21 C22 H22 126.7 . . ?
C18 C17 C16 106.9(3) . . ?
C18 C17 H17 126.6 . . ?
C16 C17 H17 126.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 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 . . ?
N6 B N4 108.2(2) . . ?
N6 B N2 108.8(2) . . ?
N4 B N2 110.0(2) . . ?
N6 B H99 109.7(17) . . ?
N4 B H99 109.9(17) . . ?
N2 B H99 110.3(17) . . ?
C5 C4 P 175.0(7) . . ?
C4 C5 C6 175.1(9) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C6 C8 102.4(11) . . ?
C7 C6 C5 112.9(9) . . ?
C8 C6 C5 109.0(10) . . ?
C7 C6 C9 117.1(12) . . ?
C8 C6 C9 105.2(13) . . ?
C5 C6 C9 109.4(11) . . ?
Cl2 C51 Cl1 114.7(5) . . ?
Cl2 C51 Cl3 112.7(6) . . ?
Cl1 C51 Cl3 109.9(4) . . ?
Cl2 C51 H51 106.3 . . ?
Cl1 C51 H51 106.3 . . ?
Cl3 C51 H51 106.3 . . ?

_refine_diff_density_max         0.924
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.073



####################################################################### 
# 
# 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_Compound_2b
_database_code_depnum_ccdc_archive 'CCDC 1851873'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H36 B N6 O2 P Si W'
_chemical_formula_sum            'C29 H36 B N6 O2 P Si W'
_chemical_formula_weight         754.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   17.0998(2)
_cell_length_b                   10.5256(2)
_cell_length_c                   17.8373(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3210.46(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    26329
_cell_measurement_theta_min      3.7930
_cell_measurement_theta_max      29.4640

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_F_000             1504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.067
_exptl_absorpt_coefficient_mu    3.721
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_reflns_number            55398
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.222
_diffrn_reflns_theta_max         30.095
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8485
_reflns_number_gt                7525
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_max     0.852
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0164P)²+1.7965P] 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 
;
 Flack x determined using 3219 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8485
_refine_ls_number_parameters     376
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0467
_refine_ls_wR_factor_gt          0.0425
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.003
_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
W W 0.73949(2) 0.19581(2) -0.00278(2) 0.01890(5) Uani 1 1 d . . . . .
P P 0.87076(7) 0.06801(11) 0.13140(7) 0.0234(2) Uani 1 1 d . . . . .
Si Si 0.97636(9) 0.42403(15) 0.26510(9) 0.0310(3) Uani 1 1 d . . . . .
C2 C 0.7068(3) 0.0160(5) 0.0110(3) 0.0282(12) Uani 1 1 d . . . . .
N1 N 0.6226(2) 0.2368(4) -0.06018(19) 0.0212(8) Uani 1 1 d . . . . .
N5 N 0.76179(19) 0.3970(4) -0.0296(2) 0.0217(8) Uani 1 1 d . . . . .
C1 C 0.8217(2) 0.1461(4) 0.0556(2) 0.0222(9) Uani 1 1 d . . . . .
C4 C 0.9210(3) 0.1958(4) 0.1740(3) 0.0265(10) Uani 1 1 d . . . . .
C9 C 0.9496(2) -0.0198(4) 0.0851(3) 0.0247(10) Uani 1 1 d . . . . .
C5 C 0.9468(3) 0.2849(5) 0.2083(3) 0.0311(11) Uani 1 1 d . . . . .
O2 O 0.6643(2) 0.2450(4) 0.1548(2) 0.0441(9) Uani 1 1 d . . . . .
C14 C 0.9339(3) -0.1447(5) 0.0647(3) 0.0336(11) Uani 1 1 d . . . . .
H51 H 0.885146 -0.179719 0.075004 0.040 Uiso 1 1 calc R U . . .
C13 C 0.9896(3) -0.2163(5) 0.0297(3) 0.0438(14) Uani 1 1 d . . . . .
H52 H 0.978585 -0.299756 0.016302 0.053 Uiso 1 1 calc R U . . .
C10 C 1.0222(3) 0.0295(5) 0.0702(3) 0.0390(13) Uani 1 1 d . . . . .
H53 H 1.034034 0.112029 0.085066 0.047 Uiso 1 1 calc R U . . .
N4 N 0.75509(19) 0.2496(4) -0.1751(2) 0.0214(8) Uani 1 1 d . . . . .
C41 C 0.7892(2) 0.4952(4) 0.0108(3) 0.0263(12) Uani 1 1 d . . . . .
N6 N 0.7396(2) 0.4468(4) -0.0977(2) 0.0228(8) Uani 1 1 d . . . . .
N3 N 0.7786(2) 0.1676(3) -0.1196(2) 0.0205(8) Uani 1 1 d . . . . .
N2 N 0.6231(2) 0.3100(3) -0.1241(2) 0.0200(8) Uani 1 1 d . . . . .
C38 C 0.5498(2) 0.3219(4) -0.1507(3) 0.0249(10) Uani 1 1 d . . . . .
C33 C 0.7817(3) 0.2074(4) -0.2421(3) 0.0249(10) Uani 1 1 d . . . . .
C35 C 0.5224(3) 0.1202(5) 0.0145(2) 0.0317(12) Uani 1 1 d . . . . .
H14A H 0.543890 0.036783 0.007433 0.048 Uiso 1 1 calc R U . . .
H14B H 0.466379 0.115151 0.015444 0.048 Uiso 1 1 calc R U . . .
H14C H 0.540816 0.154504 0.061191 0.048 Uiso 1 1 calc R U . . .
C36 C 0.5475(3) 0.2041(4) -0.0481(3) 0.0240(10) Uani 1 1 d . . . . .
C37 C 0.5009(2) 0.2553(4) -0.1034(3) 0.0285(11) Uani 1 1 d . . . . .
H16 H 0.446988 0.246652 -0.107881 0.034 Uiso 1 1 calc R U . . .
C43 C 0.7519(3) 0.5738(5) -0.0985(3) 0.0275(10) Uani 1 1 d . . . . .
C40 C 0.8169(3) 0.4780(5) 0.0904(3) 0.0303(11) Uani 1 1 d . . . . .
H9A H 0.772591 0.467679 0.122887 0.045 Uiso 1 1 calc R U . . .
H9B H 0.846280 0.551307 0.105608 0.045 Uiso 1 1 calc R U . . .
H9C H 0.849529 0.403898 0.093432 0.045 Uiso 1 1 calc R U . . .
C31 C 0.8196(2) 0.0748(5) -0.1531(3) 0.0248(10) Uani 1 1 d . . . . .
O1 O 0.6899(2) -0.0877(3) 0.0217(2) 0.0467(11) Uani 1 1 d . . . . .
C44 C 0.7313(3) 0.6548(5) -0.1637(3) 0.0409(14) Uani 1 1 d . . . . .
H13A H 0.758557 0.625161 -0.207326 0.061 Uiso 1 1 calc R U . . .
H13B H 0.746001 0.741110 -0.153493 0.061 Uiso 1 1 calc R U . . .
H13C H 0.675929 0.650521 -0.172314 0.061 Uiso 1 1 calc R U . . .
C42 C 0.7841(3) 0.6057(5) -0.0303(3) 0.0301(11) Uani 1 1 d . . . . .
H11 H 0.799483 0.686350 -0.014896 0.036 Uiso 1 1 calc R U . . .
B B 0.7005(3) 0.3622(5) -0.1565(3) 0.0206(10) Uani 1 1 d . . . . .
H0 H 0.689982 0.411520 -0.201956 0.025 Uiso 1 1 calc R U . . .
C32 C 0.8226(3) 0.0979(5) -0.2294(3) 0.0278(10) Uani 1 1 d . . . . .
H6 H 0.847753 0.048426 -0.265272 0.033 Uiso 1 1 calc R U . . .
C30 C 0.8573(3) -0.0298(5) -0.1096(3) 0.0315(11) Uani 1 1 d . . . . .
H4A H 0.898905 0.004310 -0.079679 0.047 Uiso 1 1 calc R U . . .
H4B H 0.877952 -0.091941 -0.143670 0.047 Uiso 1 1 calc R U . . .
H4C H 0.819153 -0.069064 -0.077605 0.047 Uiso 1 1 calc R U . . .
C12 C 1.0622(3) -0.1654(5) 0.0141(4) 0.0515(18) Uani 1 1 d . . . . .
H57 H 1.100125 -0.214494 -0.009524 0.062 Uiso 1 1 calc R U . . .
C34 C 0.7666(3) 0.2755(6) -0.3138(3) 0.0357(12) Uani 1 1 d . . . . .
H8A H 0.712073 0.269841 -0.326034 0.054 Uiso 1 1 calc R U . . .
H8B H 0.796965 0.237430 -0.353154 0.054 Uiso 1 1 calc R U . . .
H8C H 0.781155 0.363163 -0.308547 0.054 Uiso 1 1 calc R U . . .
C6 C 1.0257(4) 0.5426(6) 0.2041(4) 0.059(2) Uani 1 1 d . . . . .
H59A H 0.989987 0.571141 0.166162 0.089 Uiso 1 1 calc R U . . .
H59B H 1.042231 0.613737 0.233867 0.089 Uiso 1 1 calc R U . . .
H59C H 1.070477 0.504279 0.180771 0.089 Uiso 1 1 calc R U . . .
C7 C 0.8854(3) 0.4881(6) 0.3040(4) 0.0481(15) Uani 1 1 d . . . . .
H58A H 0.851918 0.515143 0.263826 0.072 Uiso 1 1 calc R U . . .
H58B H 0.859501 0.423499 0.332724 0.072 Uiso 1 1 calc R U . . .
H58C H 0.897119 0.559227 0.335727 0.072 Uiso 1 1 calc R U . . .
C11 C 1.0779(3) -0.0419(6) 0.0335(4) 0.0543(17) Uani 1 1 d . . . . .
H56 H 1.126232 -0.006362 0.021995 0.065 Uiso 1 1 calc R U . . .
C8 C 1.0445(4) 0.3696(7) 0.3375(4) 0.0626(19) Uani 1 1 d . . . . .
H60A H 1.090968 0.337077 0.314191 0.094 Uiso 1 1 calc R U . . .
H60B H 1.057908 0.439458 0.369597 0.094 Uiso 1 1 calc R U . . .
H60C H 1.020290 0.303730 0.366594 0.094 Uiso 1 1 calc R U . . .
C3 C 0.6904(3) 0.2301(5) 0.0968(3) 0.0274(10) Uani 1 1 d . . . . .
C39 C 0.5314(3) 0.3950(6) -0.2202(3) 0.0404(14) Uani 1 1 d . . . . .
H18A H 0.540203 0.483797 -0.211493 0.061 Uiso 1 1 calc R U . . .
H18B H 0.477645 0.381595 -0.233643 0.061 Uiso 1 1 calc R U . . .
H18C H 0.564495 0.366422 -0.260327 0.061 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
W C1 1.827(4) . ?
W C2 1.989(5) . ?
W C3 1.997(5) . ?
W N5 2.204(4) . ?
W N3 2.209(4) . ?
W N1 2.287(4) . ?
P C4 1.767(5) . ?
P C1 1.790(4) . ?
P C9 1.831(5) . ?
Si C8 1.831(6) . ?
Si C7 1.831(5) . ?
Si C5 1.851(5) . ?
Si C6 1.859(6) . ?
C2 O1 1.145(5) . ?
N1 C36 1.346(6) . ?
N1 N2 1.376(5) . ?
N5 C41 1.344(6) . ?
N5 N6 1.377(5) . ?
C4 C5 1.204(6) . ?
C9 C10 1.373(6) . ?
C9 C14 1.390(7) . ?
O2 C3 1.137(6) . ?
C14 C13 1.366(7) . ?
C13 C12 1.379(8) . ?
C10 C11 1.378(7) . ?
N4 C33 1.354(6) . ?
N4 N3 1.373(5) . ?
N4 B 1.544(6) . ?
C41 C42 1.377(7) . ?
C41 C40 1.509(7) . ?
N6 C43 1.353(6) . ?
N6 B 1.529(6) . ?
N3 C31 1.342(6) . ?
N2 C38 1.345(5) . ?
N2 B 1.546(6) . ?
C38 C37 1.380(6) . ?
C38 C39 1.493(6) . ?
C33 C32 1.367(6) . ?
C33 C34 1.489(7) . ?
C35 C36 1.488(6) . ?
C36 C37 1.377(7) . ?
C43 C42 1.377(7) . ?
C43 C44 1.484(7) . ?
C31 C32 1.385(6) . ?
C31 C30 1.492(7) . ?
C12 C11 1.372(8) . ?

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 W C2 82.74(19) . . ?
C1 W C3 82.44(19) . . ?
C2 W C3 86.8(2) . . ?
C1 W N5 105.39(16) . . ?
C2 W N5 171.79(16) . . ?
C3 W N5 95.27(17) . . ?
C1 W N3 105.46(16) . . ?
C2 W N3 94.23(17) . . ?
C3 W N3 172.10(16) . . ?
N5 W N3 82.67(13) . . ?
C1 W N1 169.20(16) . . ?
C2 W N1 89.37(16) . . ?
C3 W N1 89.78(16) . . ?
N5 W N1 82.70(13) . . ?
N3 W N1 82.40(13) . . ?
C4 P C1 101.7(2) . . ?
C4 P C9 102.7(2) . . ?
C1 P C9 103.6(2) . . ?
C8 Si C7 112.9(3) . . ?
C8 Si C5 108.2(3) . . ?
C7 Si C5 105.5(2) . . ?
C8 Si C6 109.5(3) . . ?
C7 Si C6 111.1(3) . . ?
C5 Si C6 109.6(3) . . ?
O1 C2 W 177.0(4) . . ?
C36 N1 N2 106.3(3) . . ?
C36 N1 W 135.5(3) . . ?
N2 N1 W 118.1(3) . . ?
C41 N5 N6 106.0(4) . . ?
C41 N5 W 133.1(3) . . ?
N6 N5 W 120.6(3) . . ?
P C1 W 157.3(3) . . ?
C5 C4 P 171.8(4) . . ?
C10 C9 C14 118.8(5) . . ?
C10 C9 P 124.2(4) . . ?
C14 C9 P 117.0(3) . . ?
C4 C5 Si 174.1(4) . . ?
C13 C14 C9 120.5(5) . . ?
C14 C13 C12 120.4(5) . . ?
C9 C10 C11 120.7(5) . . ?
C33 N4 N3 109.4(4) . . ?
C33 N4 B 130.1(4) . . ?
N3 N4 B 120.3(3) . . ?
N5 C41 C42 110.1(4) . . ?
N5 C41 C40 121.4(4) . . ?
C42 C41 C40 128.5(4) . . ?
C43 N6 N5 110.0(4) . . ?
C43 N6 B 129.5(4) . . ?
N5 N6 B 120.2(4) . . ?
C31 N3 N4 106.9(4) . . ?
C31 N3 W 132.5(3) . . ?
N4 N3 W 120.4(3) . . ?
C38 N2 N1 109.8(3) . . ?
C38 N2 B 129.3(4) . . ?
N1 N2 B 120.9(3) . . ?
N2 C38 C37 107.5(4) . . ?
N2 C38 C39 122.5(4) . . ?
C37 C38 C39 130.0(4) . . ?
N4 C33 C32 107.6(4) . . ?
N4 C33 C34 122.9(4) . . ?
C32 C33 C34 129.5(4) . . ?
N1 C36 C37 109.7(4) . . ?
N1 C36 C35 123.1(4) . . ?
C37 C36 C35 127.1(4) . . ?
C36 C37 C38 106.6(4) . . ?
N6 C43 C42 107.1(4) . . ?
N6 C43 C44 122.6(5) . . ?
C42 C43 C44 130.3(5) . . ?
N3 C31 C32 109.2(4) . . ?
N3 C31 C30 122.1(4) . . ?
C32 C31 C30 128.6(4) . . ?
C41 C42 C43 106.8(4) . . ?
N6 B N4 109.3(3) . . ?
N6 B N2 109.0(4) . . ?
N4 B N2 109.0(4) . . ?
C33 C32 C31 107.0(4) . . ?
C11 C12 C13 119.5(5) . . ?
C12 C11 C10 120.1(5) . . ?
O2 C3 W 176.8(4) . . ?

_refine_diff_density_max         0.777
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.107



