# 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. 
# 
#######################################################################

data_Compound_2a
_database_code_depnum_ccdc_archive 'CCDC 1588341'
_audit_update_record             
;
2017-11-29 deposited with the CCDC.
2018-01-22 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         ?
_chemical_formula_sum            'C30 H32 B Mo N7 O2'
_chemical_formula_weight         629.37

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'
Mo Mo -0.0483 2.7339 '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'

_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                   8.01890(10)
_cell_length_b                   10.2181(2)
_cell_length_c                   18.5046(4)
_cell_angle_alpha                77.570(2)
_cell_angle_beta                 87.661(2)
_cell_angle_gamma                80.033(2)
_cell_volume                     1458.33(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    18123
_cell_measurement_theta_min      4.4750
_cell_measurement_theta_max      73.6860

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_F_000             648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.456
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.045
_exptl_absorpt_coefficient_mu    4.002
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_T_max  0.933
_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            29604
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.445
_diffrn_reflns_theta_max         73.817
_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             5895
_reflns_number_gt                5651
_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    ?
_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)+(0.0277P)²+0.9136P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5895
_refine_ls_number_parameters     376
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.0634
_refine_ls_wR_factor_gt          0.0626
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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
Mo Mo 0.01641(2) 0.53814(2) 0.27409(2) 0.02017(5) Uani 1 1 d . . . . .
O1 O 0.3401(2) 0.34477(17) 0.23635(11) 0.0461(4) Uani 1 1 d . . . . .
O2 O -0.1227(3) 0.27324(17) 0.34995(9) 0.0489(4) Uani 1 1 d . . . . .
N1 N 0.1292(2) 0.56697(17) 0.38122(9) 0.0275(3) Uani 1 1 d . . . . .
N2 N 0.1187(2) 0.69645(18) 0.39273(9) 0.0275(3) Uani 1 1 d . . . . .
N3 N 0.1208(2) 0.72630(16) 0.22534(8) 0.0225(3) Uani 1 1 d . . . . .
N4 N 0.1071(2) 0.83112(16) 0.26239(9) 0.0238(3) Uani 1 1 d . . . . .
N5 N -0.1953(2) 0.68678(16) 0.30654(9) 0.0233(3) Uani 1 1 d . . . . .
N6 N -0.1632(2) 0.79585(16) 0.33311(9) 0.0252(3) Uani 1 1 d . . . . .
N7 N -0.1496(2) 0.48042(16) 0.13393(9) 0.0235(3) Uani 1 1 d . . . . .
C1 C -0.0785(2) 0.50918(18) 0.19206(10) 0.0223(3) Uani 1 1 d . . . . .
C2 C 0.2229(3) 0.4167(2) 0.25038(12) 0.0293(4) Uani 1 1 d . . . . .
C3 C -0.0736(3) 0.3720(2) 0.32573(11) 0.0305(4) Uani 1 1 d . . . . .
C4 C -0.1608(2) 0.34005(18) 0.13495(10) 0.0232(4) Uani 1 1 d . . . . .
C5 C -0.2715(3) 0.2764(2) 0.18381(11) 0.0293(4) Uani 1 1 d . . . . .
H5 H -0.338856 0.323383 0.215218 0.035 Uiso 1 1 calc R U . . .
C6 C -0.2808(3) 0.1410(2) 0.18541(13) 0.0376(5) Uani 1 1 d . . . . .
H6 H -0.354382 0.096917 0.218247 0.045 Uiso 1 1 calc R U . . .
C7 C -0.1817(3) 0.0724(2) 0.13861(14) 0.0421(6) Uani 1 1 d . . . . .
H7 H -0.187642 -0.018241 0.140219 0.051 Uiso 1 1 calc R U . . .
C8 C -0.0728(3) 0.1375(2) 0.08902(13) 0.0399(5) Uani 1 1 d . . . . .
H8 H -0.007985 0.090894 0.056735 0.048 Uiso 1 1 calc R U . . .
C9 C -0.0601(3) 0.2718(2) 0.08733(11) 0.0302(4) Uani 1 1 d . . . . .
H9 H 0.014506 0.315309 0.054850 0.036 Uiso 1 1 calc R U . . .
C10 C -0.2317(2) 0.58727(19) 0.07718(10) 0.0236(4) Uani 1 1 d . . . . .
C11 C -0.3048(2) 0.5580(2) 0.01680(11) 0.0265(4) Uani 1 1 d . . . . .
H11 H -0.299681 0.468252 0.012806 0.032 Uiso 1 1 calc R U . . .
C12 C -0.3854(3) 0.6635(2) -0.03755(11) 0.0304(4) Uani 1 1 d . . . . .
H12 H -0.433552 0.643652 -0.077941 0.036 Uiso 1 1 calc R U . . .
C13 C -0.3948(3) 0.7970(2) -0.03226(12) 0.0324(4) Uani 1 1 d . . . . .
H13 H -0.449474 0.866970 -0.068660 0.039 Uiso 1 1 calc R U . . .
C14 C -0.3218(3) 0.8262(2) 0.02804(12) 0.0341(4) Uani 1 1 d . . . . .
H14 H -0.327869 0.916182 0.031806 0.041 Uiso 1 1 calc R U . . .
C15 C -0.2397(3) 0.7224(2) 0.08278(11) 0.0304(4) Uani 1 1 d . . . . .
H15 H -0.190636 0.742750 0.122789 0.037 Uiso 1 1 calc R U . . .
C16 C 0.2517(4) 0.3332(3) 0.44625(15) 0.0502(6) Uani 1 1 d . . . . .
H16A H 0.299142 0.311525 0.400950 0.075 Uiso 1 1 calc R U . . .
H16B H 0.148195 0.297504 0.457073 0.075 Uiso 1 1 calc R U . . .
H16C H 0.330507 0.293773 0.485841 0.075 Uiso 1 1 calc R U . . .
C17 C 0.2161(3) 0.4841(2) 0.43827(12) 0.0350(5) Uani 1 1 d . . . . .
C18 C 0.2629(3) 0.5598(3) 0.48615(12) 0.0403(5) Uani 1 1 d . . . . .
H18 H 0.324323 0.526478 0.529719 0.048 Uiso 1 1 calc R U . . .
C19 C 0.2003(3) 0.6928(2) 0.45618(11) 0.0338(5) Uani 1 1 d . . . . .
C20 C 0.2139(3) 0.8195(3) 0.48298(13) 0.0444(6) Uani 1 1 d . . . . .
H20A H 0.104295 0.858882 0.498275 0.067 Uiso 1 1 calc R U . . .
H20B H 0.255855 0.883504 0.443668 0.067 Uiso 1 1 calc R U . . .
H20C H 0.290394 0.796835 0.524102 0.067 Uiso 1 1 calc R U . . .
C21 C 0.2524(3) 0.6735(2) 0.10867(11) 0.0338(4) Uani 1 1 d . . . . .
H21A H 0.153195 0.639498 0.098831 0.051 Uiso 1 1 calc R U . . .
H21B H 0.339788 0.598540 0.128019 0.051 Uiso 1 1 calc R U . . .
H21C H 0.291190 0.725763 0.063619 0.051 Uiso 1 1 calc R U . . .
C22 C 0.2108(2) 0.7612(2) 0.16381(10) 0.0263(4) Uani 1 1 d . . . . .
C23 C 0.2570(3) 0.8873(2) 0.16160(11) 0.0308(4) Uani 1 1 d . . . . .
H23 H 0.320727 0.934137 0.125027 0.037 Uiso 1 1 calc R U . . .
C24 C 0.1899(2) 0.9290(2) 0.22419(11) 0.0277(4) Uani 1 1 d . . . . .
C25 C 0.1964(3) 1.0586(2) 0.24803(13) 0.0358(5) Uani 1 1 d . . . . .
H25A H 0.250206 1.038685 0.295462 0.054 Uiso 1 1 calc R U . . .
H25B H 0.083378 1.106711 0.251519 0.054 Uiso 1 1 calc R U . . .
H25C H 0.259751 1.113778 0.212449 0.054 Uiso 1 1 calc R U . . .
C26 C -0.4476(3) 0.5881(2) 0.28600(13) 0.0356(5) Uani 1 1 d . . . . .
H26A H -0.408410 0.499667 0.315823 0.053 Uiso 1 1 calc R U . . .
H26B H -0.420798 0.587706 0.235007 0.053 Uiso 1 1 calc R U . . .
H26C H -0.567930 0.611188 0.291651 0.053 Uiso 1 1 calc R U . . .
C27 C -0.3629(2) 0.6907(2) 0.31017(11) 0.0271(4) Uani 1 1 d . . . . .
C28 C -0.4391(3) 0.8016(2) 0.33934(12) 0.0315(4) Uani 1 1 d . . . . .
H28 H -0.554185 0.827475 0.347413 0.038 Uiso 1 1 calc R U . . .
C29 C -0.3099(3) 0.8653(2) 0.35381(11) 0.0293(4) Uani 1 1 d . . . . .
C30 C -0.3189(3) 0.9869(2) 0.38746(14) 0.0401(5) Uani 1 1 d . . . . .
H30A H -0.264950 0.960094 0.434960 0.060 Uiso 1 1 calc R U . . .
H30B H -0.435342 1.025647 0.393267 0.060 Uiso 1 1 calc R U . . .
H30C H -0.262356 1.053145 0.355744 0.060 Uiso 1 1 calc R U . . .
B B 0.0203(3) 0.8193(2) 0.33883(12) 0.0265(4) Uani 1 1 d . . . . .
H98 H 0.028112 0.926477 0.360600 0.032 Uiso 1 1 d 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
Mo C1 1.8267(18) . ?
Mo C2 1.985(2) . ?
Mo C3 1.996(2) . ?
Mo N3 2.2271(15) . ?
Mo N5 2.2282(16) . ?
Mo N1 2.3077(16) . ?
O1 C2 1.146(3) . ?
O2 C3 1.142(3) . ?
N1 C17 1.337(3) . ?
N1 N2 1.373(2) . ?
N2 C19 1.358(3) . ?
N2 B 1.541(3) . ?
N3 C22 1.339(2) . ?
N3 N4 1.378(2) . ?
N4 C24 1.352(2) . ?
N4 B 1.541(3) . ?
N5 C27 1.337(2) . ?
N5 N6 1.377(2) . ?
N6 C29 1.351(3) . ?
N6 B 1.542(3) . ?
N7 C1 1.346(2) . ?
N7 C10 1.429(2) . ?
N7 C4 1.449(2) . ?
C4 C5 1.382(3) . ?
C4 C9 1.388(3) . ?
C5 C6 1.392(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.373(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.385(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.387(3) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.392(3) . ?
C10 C15 1.397(3) . ?
C11 C12 1.392(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.377(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.391(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.391(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.494(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.396(3) . ?
C18 C19 1.367(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.504(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.490(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.393(3) . ?
C23 C24 1.376(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.493(3) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.494(3) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.395(3) . ?
C28 C29 1.378(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.495(3) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
B H98 1.2577 . ?

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 Mo C2 86.90(8) . . ?
C1 Mo C3 84.16(8) . . ?
C2 Mo C3 87.95(8) . . ?
C1 Mo N3 100.30(7) . . ?
C2 Mo N3 93.21(7) . . ?
C3 Mo N3 175.44(7) . . ?
C1 Mo N5 98.91(7) . . ?
C2 Mo N5 173.28(7) . . ?
C3 Mo N5 95.95(7) . . ?
N3 Mo N5 82.48(6) . . ?
C1 Mo N1 177.20(7) . . ?
C2 Mo N1 93.58(7) . . ?
C3 Mo N1 93.10(7) . . ?
N3 Mo N1 82.43(6) . . ?
N5 Mo N1 80.78(6) . . ?
C17 N1 N2 106.42(17) . . ?
C17 N1 Mo 134.87(15) . . ?
N2 N1 Mo 118.62(12) . . ?
C19 N2 N1 109.77(17) . . ?
C19 N2 B 129.32(18) . . ?
N1 N2 B 120.89(15) . . ?
C22 N3 N4 106.87(15) . . ?
C22 N3 Mo 132.23(13) . . ?
N4 N3 Mo 120.78(11) . . ?
C24 N4 N3 109.57(15) . . ?
C24 N4 B 129.88(16) . . ?
N3 N4 B 120.34(15) . . ?
C27 N5 N6 106.79(15) . . ?
C27 N5 Mo 132.34(13) . . ?
N6 N5 Mo 120.75(12) . . ?
C29 N6 N5 109.76(16) . . ?
C29 N6 B 129.82(17) . . ?
N5 N6 B 120.36(15) . . ?
C1 N7 C10 120.51(15) . . ?
C1 N7 C4 118.57(15) . . ?
C10 N7 C4 120.43(15) . . ?
N7 C1 Mo 176.57(15) . . ?
O1 C2 Mo 178.53(18) . . ?
O2 C3 Mo 174.34(18) . . ?
C5 C4 C9 121.21(18) . . ?
C5 C4 N7 119.12(17) . . ?
C9 C4 N7 119.67(17) . . ?
C4 C5 C6 119.1(2) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C7 C6 C5 120.1(2) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C8 120.4(2) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C7 C8 C9 120.3(2) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C8 C9 C4 118.8(2) . . ?
C8 C9 H9 120.6 . . ?
C4 C9 H9 120.6 . . ?
C11 C10 C15 119.76(18) . . ?
C11 C10 N7 120.72(17) . . ?
C15 C10 N7 119.52(17) . . ?
C12 C11 C10 119.83(18) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C13 C12 C11 120.81(18) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 119.34(19) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C13 C14 C15 120.81(19) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C14 C15 C10 119.45(18) . . ?
C14 C15 H15 120.3 . . ?
C10 C15 H15 120.3 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C17 C18 109.9(2) . . ?
N1 C17 C16 122.5(2) . . ?
C18 C17 C16 127.7(2) . . ?
C19 C18 C17 106.24(19) . . ?
C19 C18 H18 126.9 . . ?
C17 C18 H18 126.9 . . ?
N2 C19 C18 107.67(19) . . ?
N2 C19 C20 122.4(2) . . ?
C18 C19 C20 129.9(2) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 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 . . ?
N3 C22 C23 109.44(17) . . ?
N3 C22 C21 123.02(18) . . ?
C23 C22 C21 127.53(18) . . ?
C24 C23 C22 106.51(17) . . ?
C24 C23 H23 126.7 . . ?
C22 C23 H23 126.7 . . ?
N4 C24 C23 107.62(17) . . ?
N4 C24 C25 123.44(19) . . ?
C23 C24 C25 128.91(19) . . ?
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 . . ?
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 . . ?
N5 C27 C28 109.57(17) . . ?
N5 C27 C26 122.86(18) . . ?
C28 C27 C26 127.56(19) . . ?
C29 C28 C27 106.31(18) . . ?
C29 C28 H28 126.8 . . ?
C27 C28 H28 126.8 . . ?
N6 C29 C28 107.56(18) . . ?
N6 C29 C30 123.36(19) . . ?
C28 C29 C30 129.1(2) . . ?
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 . . ?
N4 B N2 108.61(16) . . ?
N4 B N6 109.93(16) . . ?
N2 B N6 108.78(16) . . ?
N4 B H98 107.3 . . ?
N2 B H98 109.5 . . ?
N6 B H98 112.7 . . ?

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
C17 N1 N2 C19 0.6(2) . . . . ?
Mo N1 N2 C19 -176.48(13) . . . . ?
C17 N1 N2 B -177.66(17) . . . . ?
Mo N1 N2 B 5.2(2) . . . . ?
C22 N3 N4 C24 -0.7(2) . . . . ?
Mo N3 N4 C24 175.76(12) . . . . ?
C22 N3 N4 B -175.89(17) . . . . ?
Mo N3 N4 B 0.6(2) . . . . ?
C27 N5 N6 C29 0.8(2) . . . . ?
Mo N5 N6 C29 -175.67(13) . . . . ?
C27 N5 N6 B 178.15(17) . . . . ?
Mo N5 N6 B 1.7(2) . . . . ?
C1 N7 C4 C5 70.0(2) . . . . ?
C10 N7 C4 C5 -102.0(2) . . . . ?
C1 N7 C4 C9 -109.7(2) . . . . ?
C10 N7 C4 C9 78.3(2) . . . . ?
C9 C4 C5 C6 0.5(3) . . . . ?
N7 C4 C5 C6 -179.26(17) . . . . ?
C4 C5 C6 C7 -0.4(3) . . . . ?
C5 C6 C7 C8 -0.6(3) . . . . ?
C6 C7 C8 C9 1.5(3) . . . . ?
C7 C8 C9 C4 -1.3(3) . . . . ?
C5 C4 C9 C8 0.4(3) . . . . ?
N7 C4 C9 C8 -179.89(18) . . . . ?
C1 N7 C10 C11 179.72(17) . . . . ?
C4 N7 C10 C11 -8.4(3) . . . . ?
C1 N7 C10 C15 -0.8(3) . . . . ?
C4 N7 C10 C15 171.05(18) . . . . ?
C15 C10 C11 C12 0.0(3) . . . . ?
N7 C10 C11 C12 179.44(17) . . . . ?
C10 C11 C12 C13 -0.3(3) . . . . ?
C11 C12 C13 C14 0.4(3) . . . . ?
C12 C13 C14 C15 0.0(3) . . . . ?
C13 C14 C15 C10 -0.4(3) . . . . ?
C11 C10 C15 C14 0.4(3) . . . . ?
N7 C10 C15 C14 -179.09(19) . . . . ?
N2 N1 C17 C18 -0.6(2) . . . . ?
Mo N1 C17 C18 175.86(15) . . . . ?
N2 N1 C17 C16 179.0(2) . . . . ?
Mo N1 C17 C16 -4.6(3) . . . . ?
N1 C17 C18 C19 0.3(3) . . . . ?
C16 C17 C18 C19 -179.2(2) . . . . ?
N1 N2 C19 C18 -0.5(2) . . . . ?
B N2 C19 C18 177.6(2) . . . . ?
N1 N2 C19 C20 178.72(19) . . . . ?
B N2 C19 C20 -3.2(3) . . . . ?
C17 C18 C19 N2 0.1(3) . . . . ?
C17 C18 C19 C20 -179.0(2) . . . . ?
N4 N3 C22 C23 0.8(2) . . . . ?
Mo N3 C22 C23 -175.09(13) . . . . ?
N4 N3 C22 C21 -179.78(18) . . . . ?
Mo N3 C22 C21 4.3(3) . . . . ?
N3 C22 C23 C24 -0.6(2) . . . . ?
C21 C22 C23 C24 -180.0(2) . . . . ?
N3 N4 C24 C23 0.3(2) . . . . ?
B N4 C24 C23 174.91(19) . . . . ?
N3 N4 C24 C25 178.44(18) . . . . ?
B N4 C24 C25 -7.0(3) . . . . ?
C22 C23 C24 N4 0.2(2) . . . . ?
C22 C23 C24 C25 -177.8(2) . . . . ?
N6 N5 C27 C28 -0.3(2) . . . . ?
Mo N5 C27 C28 175.58(14) . . . . ?
N6 N5 C27 C26 179.96(18) . . . . ?
Mo N5 C27 C26 -4.2(3) . . . . ?
N5 C27 C28 C29 -0.3(2) . . . . ?
C26 C27 C28 C29 179.5(2) . . . . ?
N5 N6 C29 C28 -1.0(2) . . . . ?
B N6 C29 C28 -178.01(19) . . . . ?
N5 N6 C29 C30 177.90(19) . . . . ?
B N6 C29 C30 0.8(3) . . . . ?
C27 C28 C29 N6 0.8(2) . . . . ?
C27 C28 C29 C30 -178.0(2) . . . . ?
C24 N4 B N2 -113.7(2) . . . . ?
N3 N4 B N2 60.4(2) . . . . ?
C24 N4 B N6 127.4(2) . . . . ?
N3 N4 B N6 -58.5(2) . . . . ?
C19 N2 B N4 118.9(2) . . . . ?
N1 N2 B N4 -63.2(2) . . . . ?
C19 N2 B N6 -121.5(2) . . . . ?
N1 N2 B N6 56.4(2) . . . . ?
C29 N6 B N4 -126.1(2) . . . . ?
N5 N6 B N4 57.1(2) . . . . ?
C29 N6 B N2 115.1(2) . . . . ?
N5 N6 B N2 -61.7(2) . . . . ?

_refine_diff_density_max         0.713
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.055

####################################################################### 
# 
# 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_6b
_database_code_depnum_ccdc_archive 'CCDC 1588346'
_audit_update_record             
;
2017-11-29 deposited with the CCDC.
2018-01-22 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         'C30 H32 B Bi N6 O2 W'
_chemical_formula_sum            'C30 H32 B Bi N6 O2 W'
_chemical_formula_weight         912.25

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'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.0111 8.9310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   10.21600(10)
_cell_length_b                   14.1835(2)
_cell_length_c                   10.63590(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.0670(10)
_cell_angle_gamma                90
_cell_volume                     1541.13(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    16451
_cell_measurement_theta_min      4.1470
_cell_measurement_theta_max      71.8990

_exptl_crystal_description       needle
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.023
_exptl_absorpt_coefficient_mu    18.169
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72490
_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            29197
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.157
_diffrn_reflns_theta_max         72.109
_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 0.891
_diffrn_reflns_point_group_measured_fraction_full 0.903
_reflns_number_total             5420
_reflns_number_gt                5268
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.723
_reflns_Friedel_fraction_max     0.782
_reflns_Friedel_fraction_full    0.796

_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)+(0.0302P)²] 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 2136 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.035(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5420
_refine_ls_number_parameters     380
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0221
_refine_ls_wR_factor_ref         0.0532
_refine_ls_wR_factor_gt          0.0525
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
C2 C 1.0406(7) 0.7190(6) 0.2412(7) 0.0284(16) Uani 1 1 d . . . . .
C3 C 1.0912(7) 0.5586(6) 0.0994(7) 0.0296(16) Uani 1 1 d . . . . .
C4 C 0.9113(7) 0.7639(6) -0.2727(6) 0.0300(16) Uani 1 1 d . . . . .
C5 C 0.7839(8) 0.7612(7) -0.2241(7) 0.040(2) Uani 1 1 d . . . . .
H5 H 0.770071 0.773277 -0.139191 0.047 Uiso 1 1 calc R U . . .
C6 C 0.6783(9) 0.7408(9) -0.3016(9) 0.051(3) Uani 1 1 d . . . . .
H6 H 0.593773 0.739811 -0.269341 0.061 Uiso 1 1 calc R U . . .
C7 C 0.7004(10) 0.7219(9) -0.4281(9) 0.054(3) Uani 1 1 d . . . . .
H7 H 0.630179 0.708537 -0.480966 0.065 Uiso 1 1 calc R U . . .
C8 C 0.8231(10) 0.7229(8) -0.4744(8) 0.050(2) Uani 1 1 d . . . . .
H8 H 0.837191 0.707263 -0.558256 0.060 Uiso 1 1 calc R U . . .
C9 C 0.9285(8) 0.7469(8) -0.3993(7) 0.042(2) Uani 1 1 d . . . . .
H9 H 1.011588 0.751534 -0.434299 0.050 Uiso 1 1 calc R U . . .
C10 C 1.2290(8) 0.6997(7) -0.1881(7) 0.0306(17) Uani 1 1 d . . . . .
C11 C 1.2451(10) 0.6574(9) -0.3016(9) 0.055(3) Uani 1 1 d . . . . .
H11 H 1.185854 0.669605 -0.365972 0.066 Uiso 1 1 calc R U . . .
C12 C 1.3494(10) 0.5960(10) -0.3230(10) 0.060(3) Uani 1 1 d . . . . .
H12 H 1.359007 0.567446 -0.401153 0.072 Uiso 1 1 calc R U . . .
C13 C 1.4378(9) 0.5775(8) -0.2289(10) 0.050(2) Uani 1 1 d . . . . .
H13 H 1.507796 0.537003 -0.242898 0.060 Uiso 1 1 calc R U . . .
C14 C 1.4213(9) 0.6199(8) -0.1133(9) 0.048(2) Uani 1 1 d . . . . .
H14 H 1.481192 0.607966 -0.049273 0.057 Uiso 1 1 calc R U . . .
C15 C 1.3176(9) 0.6795(8) -0.0914(8) 0.044(2) Uani 1 1 d . . . . .
H15 H 1.306391 0.706434 -0.012346 0.052 Uiso 1 1 calc R U . . .
C16 C 0.4069(7) 0.6599(8) 0.2995(8) 0.043(2) Uani 1 1 d . . . . .
H16A H 0.377801 0.614932 0.238056 0.065 Uiso 1 1 calc R U . . .
H16B H 0.344065 0.709951 0.305982 0.065 Uiso 1 1 calc R U . . .
H16C H 0.415962 0.629347 0.379563 0.065 Uiso 1 1 calc R U . . .
C17 C 0.5355(6) 0.6993(6) 0.2605(6) 0.0279(16) Uani 1 1 d . . . . .
C18 C 0.5753(7) 0.7907(7) 0.2516(7) 0.0345(19) Uani 1 1 d . . . . .
H18 H 0.526192 0.844160 0.270230 0.041 Uiso 1 1 calc R U . . .
C19 C 0.7054(7) 0.7881(6) 0.2087(6) 0.0298(16) Uani 1 1 d . . . . .
C20 C 0.7955(8) 0.8702(6) 0.1839(8) 0.0393(18) Uani 1 1 d . . . . .
H20A H 0.859861 0.873896 0.249475 0.059 Uiso 1 1 calc R U . . .
H20B H 0.745526 0.927469 0.181816 0.059 Uiso 1 1 calc R U . . .
H20C H 0.838378 0.861360 0.104469 0.059 Uiso 1 1 calc R U . . .
C21 C 0.9098(7) 0.5148(6) -0.1697(6) 0.0333(16) Uani 1 1 d . . . . .
H21A H 0.892845 0.574350 -0.209460 0.050 Uiso 1 1 calc R U . . .
H21B H 0.911852 0.466019 -0.232284 0.050 Uiso 1 1 calc R U . . .
H21C H 0.992639 0.517306 -0.127187 0.050 Uiso 1 1 calc R U . . .
C22 C 0.8041(7) 0.4942(5) -0.0769(6) 0.026(2) Uani 1 1 d . . . . .
C23 C 0.7010(7) 0.4311(6) -0.0909(6) 0.0297(15) Uani 1 1 d . . . . .
H23 H 0.684083 0.392261 -0.159478 0.036 Uiso 1 1 calc R U . . .
C24 C 0.6281(6) 0.4382(6) 0.0200(6) 0.0291(16) Uani 1 1 d . . . . .
C25 C 0.5047(8) 0.3893(7) 0.0563(8) 0.0391(19) Uani 1 1 d . . . . .
H25A H 0.515300 0.361138 0.137774 0.059 Uiso 1 1 calc R U . . .
H25B H 0.485043 0.341233 -0.004302 0.059 Uiso 1 1 calc R U . . .
H25C H 0.434331 0.434130 0.058931 0.059 Uiso 1 1 calc R U . . .
C26 C 1.1000(8) 0.5141(7) 0.4101(8) 0.044(2) Uani 1 1 d . . . . .
H26A H 1.146806 0.472931 0.354369 0.065 Uiso 1 1 calc R U . . .
H26B H 1.125501 0.501234 0.495348 0.065 Uiso 1 1 calc R U . . .
H26C H 1.120066 0.578434 0.389989 0.065 Uiso 1 1 calc R U . . .
C27 C 0.9550(8) 0.4977(5) 0.3956(6) 0.031(2) Uani 1 1 d . . . . .
C28 C 0.8775(9) 0.4437(6) 0.4717(6) 0.037(2) Uani 1 1 d . . . . .
H28 H 0.903439 0.409323 0.541969 0.045 Uiso 1 1 calc R U . . .
C29 C 0.7525(8) 0.4507(6) 0.4225(6) 0.034(2) Uani 1 1 d . . . . .
C30 C 0.6291(10) 0.4060(9) 0.4670(10) 0.058(3) Uani 1 1 d . . . . .
H30A H 0.566214 0.454175 0.486520 0.088 Uiso 1 1 calc R U . . .
H30B H 0.646644 0.369302 0.540892 0.088 Uiso 1 1 calc R U . . .
H30C H 0.594707 0.365883 0.402213 0.088 Uiso 1 1 calc R U . . .
B B 0.6497(7) 0.5359(7) 0.2276(7) 0.0282(17) Uani 1 1 d . . . . .
N1 N 0.7427(6) 0.6985(5) 0.1931(6) 0.0230(13) Uani 1 1 d . . . . .
N2 N 0.6376(5) 0.6432(5) 0.2256(5) 0.0253(13) Uani 1 1 d . . . . .
N3 N 0.7962(5) 0.5368(5) 0.0356(5) 0.0240(12) Uani 1 1 d . . . . .
N4 N 0.6869(5) 0.5012(4) 0.0939(5) 0.0262(15) Uani 1 1 d . . . . .
N5 N 0.8846(6) 0.5370(5) 0.3028(5) 0.0257(13) Uani 1 1 d . . . . .
N6 N 0.7580(6) 0.5067(5) 0.3208(5) 0.0280(14) Uani 1 1 d . . . . .
O1 O 1.1066(5) 0.7681(5) 0.2995(5) 0.0391(14) Uani 1 1 d . . . . .
O2 O 1.1836(5) 0.5153(5) 0.0830(6) 0.0417(14) Uani 1 1 d . . . . .
H99 H 0.569(8) 0.502(6) 0.253(7) 0.03(2) Uiso 1 1 d . . . . .
C1 C 0.9858(9) 0.7113(8) 0.0078(9) 0.027(2) Uani 1 1 d . . . . .
W W 0.93070(3) 0.63572(2) 0.13383(3) 0.02071(13) Uani 1 1 d . . . . .
Bi Bi 1.07191(3) 0.80747(2) -0.13963(3) 0.02808(13) 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
C2 O1 1.151(10) . ?
C2 W 1.989(8) . ?
C3 O2 1.139(10) . ?
C3 W 2.005(8) . ?
C4 C9 1.378(10) . ?
C4 C5 1.401(11) . ?
C4 Bi 2.252(7) . ?
C5 C6 1.388(12) . ?
C6 C7 1.391(13) . ?
C7 C8 1.348(14) . ?
C8 C9 1.382(12) . ?
C10 C11 1.358(13) . ?
C10 C15 1.399(12) . ?
C10 Bi 2.276(9) . ?
C11 C12 1.395(14) . ?
C12 C13 1.372(14) . ?
C13 C14 1.379(15) . ?
C14 C15 1.377(14) . ?
C16 C17 1.487(10) . ?
C17 C18 1.362(13) . ?
C17 N2 1.364(9) . ?
C18 C19 1.407(10) . ?
C19 N1 1.337(11) . ?
C19 C20 1.507(12) . ?
C21 C22 1.493(9) . ?
C22 N3 1.343(8) . ?
C22 C23 1.390(10) . ?
C23 C24 1.400(10) . ?
C24 N4 1.332(9) . ?
C24 C25 1.490(10) . ?
C26 C27 1.507(11) . ?
C27 N5 1.342(9) . ?
C27 C28 1.369(11) . ?
C28 C29 1.383(11) . ?
C29 N6 1.343(9) . ?
C29 C30 1.488(12) . ?
B N2 1.526(11) . ?
B N6 1.541(10) . ?
B N4 1.553(9) . ?
N1 N2 1.375(9) . ?
N1 W 2.210(6) . ?
N3 N4 1.374(8) . ?
N3 W 2.223(6) . ?
N5 N6 1.377(8) . ?
N5 W 2.327(6) . ?
C1 W 1.807(9) . ?
C1 Bi 2.258(9) . ?

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
O1 C2 W 177.6(7) . . ?
O2 C3 W 178.1(6) . . ?
C9 C4 C5 118.4(7) . . ?
C9 C4 Bi 124.6(6) . . ?
C5 C4 Bi 116.8(5) . . ?
C6 C5 C4 120.5(7) . . ?
C5 C6 C7 119.2(8) . . ?
C8 C7 C6 120.2(8) . . ?
C7 C8 C9 121.0(8) . . ?
C4 C9 C8 120.5(8) . . ?
C11 C10 C15 119.0(9) . . ?
C11 C10 Bi 125.8(7) . . ?
C15 C10 Bi 115.2(6) . . ?
C10 C11 C12 121.0(10) . . ?
C13 C12 C11 120.1(10) . . ?
C12 C13 C14 119.1(9) . . ?
C15 C14 C13 120.9(9) . . ?
C14 C15 C10 119.9(9) . . ?
C18 C17 N2 108.0(6) . . ?
C18 C17 C16 129.8(8) . . ?
N2 C17 C16 122.1(8) . . ?
C17 C18 C19 106.2(7) . . ?
N1 C19 C18 109.5(8) . . ?
N1 C19 C20 122.6(7) . . ?
C18 C19 C20 127.9(8) . . ?
N3 C22 C23 109.8(6) . . ?
N3 C22 C21 123.0(6) . . ?
C23 C22 C21 127.2(6) . . ?
C22 C23 C24 105.5(6) . . ?
N4 C24 C23 107.8(6) . . ?
N4 C24 C25 122.7(6) . . ?
C23 C24 C25 129.5(7) . . ?
N5 C27 C28 110.9(7) . . ?
N5 C27 C26 122.5(7) . . ?
C28 C27 C26 126.5(7) . . ?
C27 C28 C29 105.7(6) . . ?
N6 C29 C28 107.9(7) . . ?
N6 C29 C30 122.9(8) . . ?
C28 C29 C30 129.1(8) . . ?
N2 B N6 109.6(6) . . ?
N2 B N4 108.9(6) . . ?
N6 B N4 109.1(6) . . ?
C19 N1 N2 106.8(6) . . ?
C19 N1 W 131.8(6) . . ?
N2 N1 W 121.4(5) . . ?
C17 N2 N1 109.4(6) . . ?
C17 N2 B 129.8(6) . . ?
N1 N2 B 120.6(5) . . ?
C22 N3 N4 106.6(5) . . ?
C22 N3 W 131.7(5) . . ?
N4 N3 W 121.5(4) . . ?
C24 N4 N3 110.3(5) . . ?
C24 N4 B 130.0(6) . . ?
N3 N4 B 119.8(5) . . ?
C27 N5 N6 105.8(6) . . ?
C27 N5 W 135.2(5) . . ?
N6 N5 W 119.1(4) . . ?
C29 N6 N5 109.7(6) . . ?
C29 N6 B 130.3(6) . . ?
N5 N6 B 120.0(6) . . ?
W C1 Bi 174.7(5) . . ?
C1 W C2 84.1(4) . . ?
C1 W C3 86.1(4) . . ?
C2 W C3 88.1(3) . . ?
C1 W N1 104.1(4) . . ?
C2 W N1 95.0(3) . . ?
C3 W N1 169.5(3) . . ?
C1 W N3 102.6(3) . . ?
C2 W N3 173.0(2) . . ?
C3 W N3 94.3(3) . . ?
N1 W N3 81.5(2) . . ?
C1 W N5 173.5(3) . . ?
C2 W N5 91.6(3) . . ?
C3 W N5 88.8(3) . . ?
N1 W N5 81.1(2) . . ?
N3 W N5 81.8(2) . . ?
C4 Bi C1 89.2(3) . . ?
C4 Bi C10 100.7(3) . . ?
C1 Bi C10 91.5(3) . . ?

_refine_diff_density_max         0.921
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.100

####################################################################### 
# 
# 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 1588342'
_audit_update_record             
;
2017-11-29 deposited with the CCDC.
2018-01-22 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         ?
_chemical_formula_sum            'C30 H32 B N7 O2 W'
_chemical_formula_weight         717.28

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'
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                   7.9985(3)
_cell_length_b                   10.1857(3)
_cell_length_c                   18.5100(6)
_cell_angle_alpha                77.580(3)
_cell_angle_beta                 87.554(3)
_cell_angle_gamma                79.822(3)
_cell_volume                     1449.53(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    10209
_cell_measurement_theta_min      4.0450
_cell_measurement_theta_max      27.9880

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_F_000             712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.633
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.032
_exptl_absorpt_coefficient_mu    4.025
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95233
_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            22569
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.374
_diffrn_reflns_theta_max         28.771
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6466
_reflns_number_gt                5820
_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    ?
_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)+(0.0182P)²+0.8734P] 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         6466
_refine_ls_number_parameters     380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0594
_refine_ls_wR_factor_gt          0.0557
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 0.48326(2) -0.03877(2) 0.72571(2) 0.01656(5) Uani 1 1 d . . . . .
O1 O 0.1560(3) 0.1552(3) 0.76160(18) 0.0391(8) Uani 1 1 d . . . . .
O2 O 0.6234(4) 0.2259(3) 0.64890(16) 0.0414(8) Uani 1 1 d . . . . .
N5 N 0.3799(3) -0.2268(3) 0.77361(16) 0.0172(6) Uani 1 1 d . . . . .
N6 N 0.3932(3) -0.3330(3) 0.73680(16) 0.0185(6) Uani 1 1 d . . . . .
N3 N 0.3712(3) -0.0671(3) 0.61913(17) 0.0216(7) Uani 1 1 d . . . . .
N4 N 0.3810(3) -0.1966(3) 0.60673(17) 0.0229(7) Uani 1 1 d . . . . .
N1 N 0.6943(3) -0.1877(3) 0.69325(17) 0.0191(7) Uani 1 1 d . . . . .
N2 N 0.6638(3) -0.2973(3) 0.66639(17) 0.0199(7) Uani 1 1 d . . . . .
N7 N 0.6492(3) 0.0197(3) 0.86685(16) 0.0179(6) Uani 1 1 d . . . . .
C1 C 0.5775(4) -0.0093(3) 0.80835(19) 0.0180(8) Uani 1 1 d . . . . .
C3 C 0.5721(4) 0.1268(4) 0.6745(2) 0.0225(8) Uani 1 1 d . . . . .
C2 C 0.2764(4) 0.0825(4) 0.7483(2) 0.0219(8) Uani 1 1 d . . . . .
C21 C 0.2472(6) 0.1687(4) 0.5556(3) 0.0421(11) Uani 1 1 d . . . . .
H20A H 0.350571 0.204917 0.544779 0.063 Uiso 1 1 calc R U . . .
H20B H 0.200130 0.189007 0.601310 0.063 Uiso 1 1 calc R U . . .
H20C H 0.167399 0.209168 0.516410 0.063 Uiso 1 1 calc R U . . .
C26 C 0.2475(5) -0.1721(4) 0.8902(2) 0.0289(9) Uani 1 1 d . . . . .
H22A H 0.160741 -0.096318 0.870486 0.043 Uiso 1 1 calc R U . . .
H22B H 0.347573 -0.139013 0.899951 0.043 Uiso 1 1 calc R U . . .
H22C H 0.207648 -0.223508 0.935331 0.043 Uiso 1 1 calc R U . . .
C27 C 0.2884(4) -0.2613(4) 0.8357(2) 0.0208(8) Uani 1 1 d . . . . .
C24 C 0.2986(5) -0.1902(4) 0.5435(2) 0.0276(9) Uani 1 1 d . . . . .
C22 C 0.2840(4) 0.0172(4) 0.5623(2) 0.0287(9) Uani 1 1 d . . . . .
C16 C 0.9462(4) -0.0867(4) 0.7144(2) 0.0300(9) Uani 1 1 d . . . . .
H22D H 0.923662 -0.089610 0.766051 0.045 Uiso 1 1 calc R U . . .
H22E H 0.901014 0.002427 0.686315 0.045 Uiso 1 1 calc R U . . .
H22F H 1.066581 -0.105844 0.706391 0.045 Uiso 1 1 calc R U . . .
C17 C 0.8629(4) -0.1924(4) 0.6899(2) 0.0215(8) Uani 1 1 d . . . . .
C10 C 0.7307(4) -0.0875(4) 0.92349(19) 0.0183(8) Uani 1 1 d . . . . .
C11 C 0.8045(4) -0.0591(4) 0.98399(19) 0.0187(8) Uani 1 1 d . . . . .
H331 H 0.799546 0.030943 0.988014 0.022 Uiso 1 1 calc R U . . .
C5 C 0.5615(4) 0.2300(4) 0.9134(2) 0.0232(8) Uani 1 1 d . . . . .
H332 H 0.487506 0.186484 0.946394 0.028 Uiso 1 1 calc R U . . .
C4 C 0.6603(4) 0.1604(4) 0.8653(2) 0.0185(8) Uani 1 1 d . . . . .
C29 C 0.3104(4) -0.4309(4) 0.7759(2) 0.0212(8) Uani 1 1 d . . . . .
C18 C 0.9391(4) -0.3025(4) 0.6613(2) 0.0251(9) Uani 1 1 d . . . . .
H335 H 1.054808 -0.328242 0.653547 0.030 Uiso 1 1 calc R U . . .
C19 C 0.8120(4) -0.3668(4) 0.6464(2) 0.0233(8) Uani 1 1 d . . . . .
C20 C 0.8231(5) -0.4894(4) 0.6125(2) 0.0333(10) Uani 1 1 d . . . . .
H33A H 0.771768 -0.462192 0.564424 0.050 Uiso 1 1 calc R U . . .
H33B H 0.764489 -0.555249 0.643456 0.050 Uiso 1 1 calc R U . . .
H33C H 0.940174 -0.529050 0.607872 0.050 Uiso 1 1 calc R U . . .
C23 C 0.2375(5) -0.0588(5) 0.5149(2) 0.0331(10) Uani 1 1 d . . . . .
H338 H 0.175548 -0.024919 0.471508 0.040 Uiso 1 1 calc R U . . .
C25 C 0.2842(5) -0.3175(5) 0.5163(2) 0.0372(11) Uani 1 1 d . . . . .
H33D H 0.239750 -0.380947 0.555138 0.056 Uiso 1 1 calc R U . . .
H33E H 0.394431 -0.358474 0.501764 0.056 Uiso 1 1 calc R U . . .
H33F H 0.209258 -0.293772 0.474554 0.056 Uiso 1 1 calc R U . . .
C12 C 0.8848(4) -0.1639(4) 1.0380(2) 0.0245(8) Uani 1 1 d . . . . .
H350 H 0.932701 -0.143624 1.078298 0.029 Uiso 1 1 calc R U . . .
C13 C 0.8952(4) -0.2994(4) 1.0329(2) 0.0258(9) Uani 1 1 d . . . . .
H351 H 0.949370 -0.369802 1.069365 0.031 Uiso 1 1 calc R U . . .
C14 C 0.8235(5) -0.3274(4) 0.9727(2) 0.0285(9) Uani 1 1 d . . . . .
H352 H 0.831171 -0.417539 0.968363 0.034 Uiso 1 1 calc R U . . .
C15 C 0.7405(4) -0.2238(4) 0.9185(2) 0.0240(8) Uani 1 1 d . . . . .
H353 H 0.691066 -0.244723 0.878751 0.029 Uiso 1 1 calc R U . . .
C9 C 0.7699(4) 0.2232(4) 0.8167(2) 0.0229(8) Uani 1 1 d . . . . .
H354 H 0.837153 0.175714 0.785252 0.027 Uiso 1 1 calc R U . . .
C6 C 0.5739(5) 0.3642(4) 0.9118(2) 0.0345(10) Uani 1 1 d . . . . .
H355 H 0.509599 0.411135 0.944336 0.041 Uiso 1 1 calc R U . . .
C28 C 0.2434(4) -0.3878(4) 0.8380(2) 0.0254(9) Uani 1 1 d . . . . .
H356 H 0.179766 -0.434463 0.874708 0.031 Uiso 1 1 calc R U . . .
C30 C 0.3054(5) -0.5615(4) 0.7524(2) 0.0310(9) Uani 1 1 d . . . . .
H35A H 0.419000 -0.610026 0.749581 0.046 Uiso 1 1 calc R U . . .
H35B H 0.252784 -0.542024 0.704742 0.046 Uiso 1 1 calc R U . . .
H35C H 0.241035 -0.616362 0.787795 0.046 Uiso 1 1 calc R U . . .
C8 C 0.7798(5) 0.3596(4) 0.8148(2) 0.0319(10) Uani 1 1 d . . . . .
H380 H 0.852906 0.403480 0.781424 0.038 Uiso 1 1 calc R U . . .
C7 C 0.6828(5) 0.4284(4) 0.8615(2) 0.0357(11) Uani 1 1 d . . . . .
H381 H 0.689601 0.519271 0.859665 0.043 Uiso 1 1 calc R U . . .
B B 0.4800(5) -0.3210(5) 0.6605(3) 0.0243(10) Uani 1 1 d . . . . .
H99 H 0.479(4) -0.415(4) 0.638(2) 0.021(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 1.837(3) . ?
W C2 1.970(4) . ?
W C3 1.981(4) . ?
W N5 2.214(3) . ?
W N1 2.216(3) . ?
W N3 2.295(3) . ?
O1 C2 1.158(4) . ?
O2 C3 1.156(4) . ?
N5 C27 1.350(4) . ?
N5 N6 1.384(4) . ?
N6 C29 1.356(4) . ?
N6 B 1.538(5) . ?
N3 C22 1.339(5) . ?
N3 N4 1.375(4) . ?
N4 C24 1.351(4) . ?
N4 B 1.547(6) . ?
N1 C17 1.340(4) . ?
N1 N2 1.377(4) . ?
N2 C19 1.350(4) . ?
N2 B 1.544(5) . ?
N7 C1 1.356(4) . ?
N7 C10 1.425(5) . ?
N7 C4 1.446(4) . ?
C21 C22 1.498(6) . ?
C26 C27 1.487(5) . ?
C27 C28 1.389(5) . ?
C24 C23 1.340(6) . ?
C24 C25 1.513(5) . ?
C22 C23 1.388(5) . ?
C16 C17 1.516(5) . ?
C17 C18 1.377(5) . ?
C10 C11 1.393(5) . ?
C10 C15 1.400(5) . ?
C11 C12 1.380(5) . ?
C5 C6 1.382(5) . ?
C5 C4 1.390(5) . ?
C4 C9 1.368(5) . ?
C29 C28 1.371(5) . ?
C29 C30 1.493(5) . ?
C18 C19 1.370(5) . ?
C19 C20 1.501(5) . ?
C12 C13 1.392(5) . ?
C13 C14 1.378(5) . ?
C14 C15 1.383(5) . ?
C9 C8 1.398(5) . ?
C6 C7 1.388(6) . ?
C8 C7 1.361(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W C2 87.18(15) . . ?
C1 W C3 84.25(15) . . ?
C2 W C3 87.77(15) . . ?
C1 W N5 100.48(13) . . ?
C2 W N5 93.43(12) . . ?
C3 W N5 175.17(12) . . ?
C1 W N1 99.35(13) . . ?
C2 W N1 172.66(12) . . ?
C3 W N1 96.17(13) . . ?
N5 W N1 82.14(10) . . ?
C1 W N3 177.23(13) . . ?
C2 W N3 92.99(13) . . ?
C3 W N3 92.99(13) . . ?
N5 W N3 82.28(10) . . ?
N1 W N3 80.64(10) . . ?
C27 N5 N6 106.7(3) . . ?
C27 N5 W 131.6(2) . . ?
N6 N5 W 121.5(2) . . ?
C29 N6 N5 109.4(3) . . ?
C29 N6 B 130.6(3) . . ?
N5 N6 B 119.8(3) . . ?
C22 N3 N4 106.1(3) . . ?
C22 N3 W 134.5(3) . . ?
N4 N3 W 119.3(2) . . ?
C24 N4 N3 109.4(3) . . ?
C24 N4 B 130.1(3) . . ?
N3 N4 B 120.5(3) . . ?
C17 N1 N2 106.3(3) . . ?
C17 N1 W 132.2(2) . . ?
N2 N1 W 121.38(19) . . ?
C19 N2 N1 109.7(3) . . ?
C19 N2 B 130.1(3) . . ?
N1 N2 B 120.2(3) . . ?
C1 N7 C10 120.4(3) . . ?
C1 N7 C4 118.3(3) . . ?
C10 N7 C4 120.8(3) . . ?
N7 C1 W 176.5(3) . . ?
O2 C3 W 175.6(3) . . ?
O1 C2 W 179.1(3) . . ?
N5 C27 C28 109.1(3) . . ?
N5 C27 C26 122.6(3) . . ?
C28 C27 C26 128.3(3) . . ?
C23 C24 N4 108.1(3) . . ?
C23 C24 C25 130.3(4) . . ?
N4 C24 C25 121.6(4) . . ?
N3 C22 C23 109.2(4) . . ?
N3 C22 C21 122.2(3) . . ?
C23 C22 C21 128.5(4) . . ?
N1 C17 C18 109.7(3) . . ?
N1 C17 C16 122.0(3) . . ?
C18 C17 C16 128.3(3) . . ?
C11 C10 C15 118.8(3) . . ?
C11 C10 N7 121.0(3) . . ?
C15 C10 N7 120.2(3) . . ?
C12 C11 C10 120.4(3) . . ?
C6 C5 C4 119.6(4) . . ?
C9 C4 C5 120.7(3) . . ?
C9 C4 N7 119.3(3) . . ?
C5 C4 N7 120.1(3) . . ?
N6 C29 C28 107.7(3) . . ?
N6 C29 C30 122.9(3) . . ?
C28 C29 C30 129.4(3) . . ?
C19 C18 C17 106.9(3) . . ?
N2 C19 C18 107.4(3) . . ?
N2 C19 C20 123.3(3) . . ?
C18 C19 C20 129.3(3) . . ?
C24 C23 C22 107.1(4) . . ?
C11 C12 C13 120.9(3) . . ?
C14 C13 C12 118.7(4) . . ?
C13 C14 C15 121.2(4) . . ?
C14 C15 C10 120.0(3) . . ?
C4 C9 C8 119.3(4) . . ?
C5 C6 C7 119.5(4) . . ?
C29 C28 C27 107.2(3) . . ?
C7 C8 C9 120.2(4) . . ?
C8 C7 C6 120.6(4) . . ?
N6 B N2 109.7(3) . . ?
N6 B N4 108.5(3) . . ?
N2 B N4 108.5(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
C27 N5 N6 C29 0.1(4) . . . . ?
W N5 N6 C29 -176.1(2) . . . . ?
C27 N5 N6 B 175.7(3) . . . . ?
W N5 N6 B -0.6(4) . . . . ?
C22 N3 N4 C24 -0.8(4) . . . . ?
W N3 N4 C24 176.2(2) . . . . ?
C22 N3 N4 B 177.7(3) . . . . ?
W N3 N4 B -5.3(4) . . . . ?
C17 N1 N2 C19 -0.6(4) . . . . ?
W N1 N2 C19 176.1(2) . . . . ?
C17 N1 N2 B -178.4(3) . . . . ?
W N1 N2 B -1.8(4) . . . . ?
N6 N5 C27 C28 -0.3(4) . . . . ?
W N5 C27 C28 175.4(2) . . . . ?
N6 N5 C27 C26 179.8(3) . . . . ?
W N5 C27 C26 -4.5(5) . . . . ?
N3 N4 C24 C23 0.5(4) . . . . ?
B N4 C24 C23 -177.7(3) . . . . ?
N3 N4 C24 C25 -178.6(3) . . . . ?
B N4 C24 C25 3.2(6) . . . . ?
N4 N3 C22 C23 0.7(4) . . . . ?
W N3 C22 C23 -175.6(2) . . . . ?
N4 N3 C22 C21 -179.7(4) . . . . ?
W N3 C22 C21 4.0(6) . . . . ?
N2 N1 C17 C18 0.2(4) . . . . ?
W N1 C17 C18 -175.9(3) . . . . ?
N2 N1 C17 C16 179.5(3) . . . . ?
W N1 C17 C16 3.4(6) . . . . ?
C1 N7 C10 C11 -179.8(3) . . . . ?
C4 N7 C10 C11 8.3(5) . . . . ?
C1 N7 C10 C15 1.3(5) . . . . ?
C4 N7 C10 C15 -170.6(3) . . . . ?
C15 C10 C11 C12 -0.3(5) . . . . ?
N7 C10 C11 C12 -179.2(3) . . . . ?
C6 C5 C4 C9 0.2(5) . . . . ?
C6 C5 C4 N7 179.5(3) . . . . ?
C1 N7 C4 C9 -69.9(4) . . . . ?
C10 N7 C4 C9 102.2(4) . . . . ?
C1 N7 C4 C5 110.8(4) . . . . ?
C10 N7 C4 C5 -77.2(4) . . . . ?
N5 N6 C29 C28 0.1(4) . . . . ?
B N6 C29 C28 -174.8(3) . . . . ?
N5 N6 C29 C30 -178.0(3) . . . . ?
B N6 C29 C30 7.1(6) . . . . ?
N1 C17 C18 C19 0.2(5) . . . . ?
C16 C17 C18 C19 -179.0(4) . . . . ?
N1 N2 C19 C18 0.7(4) . . . . ?
B N2 C19 C18 178.3(4) . . . . ?
N1 N2 C19 C20 -177.9(4) . . . . ?
B N2 C19 C20 -0.2(6) . . . . ?
C17 C18 C19 N2 -0.6(4) . . . . ?
C17 C18 C19 C20 177.9(4) . . . . ?
N4 C24 C23 C22 -0.1(4) . . . . ?
C25 C24 C23 C22 178.9(4) . . . . ?
N3 C22 C23 C24 -0.4(5) . . . . ?
C21 C22 C23 C24 -180.0(4) . . . . ?
C10 C11 C12 C13 0.6(5) . . . . ?
C11 C12 C13 C14 0.0(5) . . . . ?
C12 C13 C14 C15 -0.9(6) . . . . ?
C13 C14 C15 C10 1.2(6) . . . . ?
C11 C10 C15 C14 -0.6(5) . . . . ?
N7 C10 C15 C14 178.3(3) . . . . ?
C5 C4 C9 C8 -1.1(5) . . . . ?
N7 C4 C9 C8 179.5(3) . . . . ?
C4 C5 C6 C7 1.0(6) . . . . ?
N6 C29 C28 C27 -0.3(4) . . . . ?
C30 C29 C28 C27 177.7(3) . . . . ?
N5 C27 C28 C29 0.4(4) . . . . ?
C26 C27 C28 C29 -179.7(4) . . . . ?
C4 C9 C8 C7 0.8(5) . . . . ?
C9 C8 C7 C6 0.4(6) . . . . ?
C5 C6 C7 C8 -1.3(6) . . . . ?
C29 N6 B N2 -127.3(4) . . . . ?
N5 N6 B N2 58.2(4) . . . . ?
C29 N6 B N4 114.3(4) . . . . ?
N5 N6 B N4 -60.2(4) . . . . ?
C19 N2 B N6 125.6(4) . . . . ?
N1 N2 B N6 -56.9(4) . . . . ?
C19 N2 B N4 -116.0(4) . . . . ?
N1 N2 B N4 61.4(4) . . . . ?
C24 N4 B N6 -118.8(4) . . . . ?
N3 N4 B N6 63.1(4) . . . . ?
C24 N4 B N2 122.0(4) . . . . ?
N3 N4 B N2 -56.1(4) . . . . ?

_refine_diff_density_max         1.244
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.139

####################################################################### 
# 
# 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_6a
_database_code_depnum_ccdc_archive 'CCDC 1588345'
_audit_update_record             
;
2017-11-29 deposited with the CCDC.
2018-01-22 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         ?
_chemical_formula_sum            'C30 H32 B Bi Mo N6 O2'
_chemical_formula_weight         824.34

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   10.2310(3)
_cell_length_b                   14.2033(4)
_cell_length_c                   10.5668(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.271(3)
_cell_angle_gamma                90
_cell_volume                     1535.49(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(2)
_cell_measurement_reflns_used    5235
_cell_measurement_theta_min      3.8410
_cell_measurement_theta_max      28.0800

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_F_000             800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.492
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.048
_exptl_absorpt_coefficient_mu    6.168
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74450
_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(2)
_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            12168
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.457
_diffrn_reflns_theta_max         28.770
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.772
_diffrn_reflns_point_group_measured_fraction_full 0.965
_reflns_number_total             6154
_reflns_number_gt                5691
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.755
_reflns_Friedel_fraction_max     0.691
_reflns_Friedel_fraction_full    0.931

_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)+(0.0263P)²] 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 2243 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6154
_refine_ls_number_parameters     380
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0637
_refine_ls_wR_factor_gt          0.0609
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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
Bi Bi -0.07369(3) 0.37996(2) 0.35996(3) 0.02160(9) Uani 1 1 d . . . . .
Mo Mo 0.06889(7) 0.20718(5) 0.63131(7) 0.01522(18) Uani 1 1 d . . . . .
C4 C 0.0872(8) 0.3368(5) 0.2281(8) 0.0211(18) Uani 1 1 d . . . . .
N4 N 0.2434(6) 0.0761(4) 0.8182(7) 0.0212(17) Uani 1 1 d . . . . .
C28 C 0.2938(8) 0.3604(5) 0.7108(7) 0.023(2) Uani 1 1 d . . . . .
C27 C 0.4236(7) 0.3611(6) 0.7551(8) 0.024(2) Uani 1 1 d . . . . .
H27 H 0.473099 0.413790 0.776124 0.029 Uiso 1 1 calc R U . . .
N6 N 0.3614(7) 0.2150(4) 0.7247(7) 0.0192(16) Uani 1 1 d . . . . .
N2 N 0.3121(6) 0.0750(4) 0.5898(6) 0.0184(14) Uani 1 1 d . . . . .
C17 C 0.1952(7) 0.0659(5) 0.4171(7) 0.0197(18) Uani 1 1 d . . . . .
C19 C 0.3706(8) 0.0099(5) 0.5154(8) 0.0227(18) Uani 1 1 d . . . . .
C18 C 0.2987(8) 0.0032(6) 0.4051(8) 0.0237(19) Uani 1 1 d . . . . .
H18 H 0.316032 -0.035559 0.336309 0.028 Uiso 1 1 calc R U . . .
C23 C 0.1292(9) 0.0108(6) 0.9700(8) 0.031(2) Uani 1 1 d . . . . .
H23 H 0.105557 -0.024385 1.040541 0.037 Uiso 1 1 calc R U . . .
N3 N 0.1164(6) 0.1068(4) 0.8024(6) 0.0205(14) Uani 1 1 d . . . . .
N1 N 0.2023(6) 0.1090(4) 0.5296(6) 0.0194(14) Uani 1 1 d . . . . .
C26 C 0.4625(7) 0.2695(6) 0.7610(8) 0.0219(18) Uani 1 1 d . . . . .
O2 O -0.1076(5) 0.3383(4) 0.7974(6) 0.0318(15) Uani 1 1 d . . . . .
C22 C 0.0476(8) 0.0658(5) 0.8950(8) 0.0233(18) Uani 1 1 d . . . . .
C14 C -0.4221(10) 0.1930(7) 0.3861(11) 0.038(2) Uani 1 1 d . . . . .
H14 H -0.482357 0.182723 0.450252 0.046 Uiso 1 1 calc R U . . .
C16 C 0.0898(8) 0.0876(6) 0.3233(8) 0.0267(19) Uani 1 1 d . . . . .
H16A H 0.009297 0.098876 0.367108 0.040 Uiso 1 1 calc R U . . .
H16B H 0.079055 0.035252 0.266754 0.040 Uiso 1 1 calc R U . . .
H16C H 0.113252 0.142638 0.275826 0.040 Uiso 1 1 calc R U . . .
C24 C 0.2515(8) 0.0189(5) 0.9189(8) 0.029(2) Uani 1 1 d . . . . .
C8 C 0.1760(9) 0.2936(7) 0.0252(9) 0.038(2) Uani 1 1 d . . . . .
H8 H 0.162846 0.278444 -0.059487 0.046 Uiso 1 1 calc R U . . .
N5 N 0.2571(6) 0.2705(5) 0.6934(6) 0.0172(15) Uani 1 1 d . . . . .
C20 C 0.4949(8) -0.0388(6) 0.5528(10) 0.033(2) Uani 1 1 d . . . . .
H20A H 0.562081 0.007268 0.566858 0.050 Uiso 1 1 calc R U . . .
H20B H 0.521090 -0.080726 0.486384 0.050 Uiso 1 1 calc R U . . .
H20C H 0.481011 -0.073984 0.629107 0.050 Uiso 1 1 calc R U . . .
C3 C -0.0412(7) 0.2894(6) 0.7386(8) 0.0189(17) Uani 1 1 d . . . . .
O1 O -0.1844(6) 0.0866(4) 0.5787(7) 0.0383(16) Uani 1 1 d . . . . .
C21 C -0.0965(8) 0.0826(6) 0.9121(9) 0.035(2) Uani 1 1 d . . . . .
H21A H -0.116814 0.146698 0.891023 0.053 Uiso 1 1 calc R U . . .
H21B H -0.119735 0.070710 0.998573 0.053 Uiso 1 1 calc R U . . .
H21C H -0.144924 0.041053 0.857652 0.053 Uiso 1 1 calc R U . . .
C13 C -0.4367(10) 0.1486(7) 0.2718(12) 0.044(3) Uani 1 1 d . . . . .
H13 H -0.506601 0.108064 0.257878 0.053 Uiso 1 1 calc R U . . .
C15 C -0.3189(9) 0.2525(7) 0.4057(9) 0.034(2) Uani 1 1 d . . . . .
H15 H -0.309027 0.280566 0.484693 0.041 Uiso 1 1 calc R U . . .
C9 C 0.0710(8) 0.3175(6) 0.0999(9) 0.030(2) Uani 1 1 d . . . . .
H9 H -0.012033 0.320740 0.064038 0.036 Uiso 1 1 calc R U . . .
C1 C 0.0132(8) 0.2837(6) 0.5081(9) 0.0186(18) Uani 1 1 d . . . . .
C10 C -0.2287(8) 0.2725(6) 0.3125(9) 0.026(2) Uani 1 1 d . . . . .
C2 C -0.0908(8) 0.1299(5) 0.5963(8) 0.0222(18) Uani 1 1 d . . . . .
C25 C 0.3762(10) -0.0261(8) 0.9601(11) 0.050(3) Uani 1 1 d . . . . .
H25A H 0.407405 -0.066680 0.894147 0.075 Uiso 1 1 calc R U . . .
H25B H 0.361409 -0.062312 1.035331 0.075 Uiso 1 1 calc R U . . .
H25C H 0.440153 0.021772 0.977179 0.075 Uiso 1 1 calc R U . . .
B B 0.3500(9) 0.1078(7) 0.7230(9) 0.021(2) Uani 1 1 d . . . . .
C5 C 0.2145(8) 0.3344(6) 0.2788(8) 0.030(2) Uani 1 1 d . . . . .
H5 H 0.228481 0.347527 0.364054 0.036 Uiso 1 1 calc R U . . .
C30 C 0.2058(9) 0.4409(6) 0.6872(10) 0.033(2) Uani 1 1 d . . . . .
H30A H 0.159174 0.431137 0.609269 0.050 Uiso 1 1 calc R U . . .
H30B H 0.256398 0.497688 0.681458 0.050 Uiso 1 1 calc R U . . .
H30C H 0.144748 0.446316 0.755487 0.050 Uiso 1 1 calc R U . . .
C7 C 0.2996(9) 0.2921(7) 0.0755(10) 0.041(2) Uani 1 1 d . . . . .
H7 H 0.370596 0.277277 0.024641 0.049 Uiso 1 1 calc R U . . .
C29 C 0.5917(9) 0.2297(6) 0.8018(10) 0.032(2) Uani 1 1 d . . . . .
H29A H 0.579909 0.191454 0.875766 0.049 Uiso 1 1 calc R U . . .
H29B H 0.650877 0.280260 0.820955 0.049 Uiso 1 1 calc R U . . .
H29C H 0.627087 0.191977 0.734832 0.049 Uiso 1 1 calc R U . . .
C12 C -0.3464(10) 0.1647(8) 0.1776(11) 0.046(3) Uani 1 1 d . . . . .
H12 H -0.353762 0.133775 0.100311 0.055 Uiso 1 1 calc R U . . .
C6 C 0.3184(8) 0.3126(7) 0.2016(10) 0.040(2) Uani 1 1 d . . . . .
H6 H 0.402543 0.311619 0.235215 0.048 Uiso 1 1 calc R U . . .
C11 C -0.2461(11) 0.2264(7) 0.1984(11) 0.040(3) Uani 1 1 d . . . . .
H11 H -0.187269 0.237806 0.133343 0.047 Uiso 1 1 calc R U . . .
H99 H 0.443(7) 0.082(4) 0.752(7) 0.001(19) 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
Bi C4 2.247(8) . ?
Bi C10 2.255(9) . ?
Bi C1 2.258(8) . ?
Mo C1 1.787(8) . ?
Mo C3 1.983(8) . ?
Mo C2 2.001(8) . ?
Mo N5 2.221(6) . ?
Mo N1 2.231(6) . ?
Mo N3 2.351(6) . ?
C4 C9 1.391(12) . ?
C4 C5 1.406(11) . ?
N4 C24 1.341(10) . ?
N4 N3 1.380(9) . ?
N4 B 1.555(12) . ?
C28 N5 1.344(10) . ?
C28 C27 1.406(10) . ?
C28 C30 1.476(11) . ?
C27 C26 1.363(11) . ?
C27 H27 0.9300 . ?
N6 C26 1.346(10) . ?
N6 N5 1.366(9) . ?
N6 B 1.526(11) . ?
N2 C19 1.355(10) . ?
N2 N1 1.376(8) . ?
N2 B 1.531(12) . ?
C17 N1 1.339(10) . ?
C17 C18 1.389(11) . ?
C17 C16 1.494(11) . ?
C19 C18 1.378(12) . ?
C19 C20 1.498(11) . ?
C18 H18 0.9300 . ?
C23 C24 1.370(12) . ?
C23 C22 1.389(12) . ?
C23 H23 0.9300 . ?
N3 C22 1.342(10) . ?
C26 C29 1.499(12) . ?
O2 C3 1.154(9) . ?
C22 C21 1.505(11) . ?
C14 C15 1.368(14) . ?
C14 C13 1.370(15) . ?
C14 H14 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C24 C25 1.490(12) . ?
C8 C7 1.370(13) . ?
C8 C9 1.378(12) . ?
C8 H8 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
O1 C2 1.152(9) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C13 C12 1.381(15) . ?
C13 H13 0.9300 . ?
C15 C10 1.383(13) . ?
C15 H15 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.383(14) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
B H99 1.06(7) . ?
C5 C6 1.379(12) . ?
C5 H5 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C7 C6 1.376(13) . ?
C7 H7 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C12 C11 1.366(14) . ?
C12 H12 0.9300 . ?
C6 H6 0.9300 . ?
C11 H11 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
C4 Bi C10 101.2(3) . . ?
C4 Bi C1 88.7(3) . . ?
C10 Bi C1 91.1(3) . . ?
C1 Mo C3 83.0(4) . . ?
C1 Mo C2 86.7(4) . . ?
C3 Mo C2 87.9(3) . . ?
C1 Mo N5 104.0(3) . . ?
C3 Mo N5 95.0(3) . . ?
C2 Mo N5 169.2(3) . . ?
C1 Mo N1 102.9(3) . . ?
C3 Mo N1 173.9(3) . . ?
C2 Mo N1 94.0(3) . . ?
N5 Mo N1 82.1(2) . . ?
C1 Mo N3 173.2(3) . . ?
C3 Mo N3 91.9(3) . . ?
C2 Mo N3 88.6(3) . . ?
N5 Mo N3 80.9(2) . . ?
N1 Mo N3 82.3(2) . . ?
C9 C4 C5 118.2(8) . . ?
C9 C4 Bi 125.0(6) . . ?
C5 C4 Bi 116.7(6) . . ?
C24 N4 N3 110.0(7) . . ?
C24 N4 B 130.4(7) . . ?
N3 N4 B 119.5(6) . . ?
N5 C28 C27 108.4(7) . . ?
N5 C28 C30 122.9(8) . . ?
C27 C28 C30 128.7(8) . . ?
C26 C27 C28 106.5(7) . . ?
C26 C27 H27 126.8 . . ?
C28 C27 H27 126.8 . . ?
C26 N6 N5 109.6(6) . . ?
C26 N6 B 129.4(7) . . ?
N5 N6 B 120.8(6) . . ?
C19 N2 N1 109.5(6) . . ?
C19 N2 B 129.1(7) . . ?
N1 N2 B 121.3(6) . . ?
N1 C17 C18 109.6(7) . . ?
N1 C17 C16 122.1(7) . . ?
C18 C17 C16 128.3(7) . . ?
N2 C19 C18 107.6(7) . . ?
N2 C19 C20 122.5(8) . . ?
C18 C19 C20 129.8(8) . . ?
C19 C18 C17 106.4(7) . . ?
C19 C18 H18 126.8 . . ?
C17 C18 H18 126.8 . . ?
C24 C23 C22 106.0(7) . . ?
C24 C23 H23 127.0 . . ?
C22 C23 H23 127.0 . . ?
C22 N3 N4 105.7(6) . . ?
C22 N3 Mo 135.8(5) . . ?
N4 N3 Mo 118.4(5) . . ?
C17 N1 N2 106.9(6) . . ?
C17 N1 Mo 133.0(5) . . ?
N2 N1 Mo 119.8(5) . . ?
N6 C26 C27 108.2(7) . . ?
N6 C26 C29 122.7(7) . . ?
C27 C26 C29 129.1(7) . . ?
N3 C22 C23 110.2(7) . . ?
N3 C22 C21 122.4(7) . . ?
C23 C22 C21 127.4(7) . . ?
C15 C14 C13 119.9(10) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C24 C23 108.1(7) . . ?
N4 C24 C25 122.7(8) . . ?
C23 C24 C25 129.2(8) . . ?
C7 C8 C9 120.1(9) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C28 N5 N6 107.3(6) . . ?
C28 N5 Mo 131.8(5) . . ?
N6 N5 Mo 120.9(5) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 C3 Mo 177.6(7) . . ?
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 . . ?
C14 C13 C12 119.3(10) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C14 C15 C10 122.5(10) . . ?
C14 C15 H15 118.8 . . ?
C10 C15 H15 118.8 . . ?
C8 C9 C4 121.1(8) . . ?
C8 C9 H9 119.4 . . ?
C4 C9 H9 119.4 . . ?
Mo C1 Bi 175.3(5) . . ?
C15 C10 C11 116.1(9) . . ?
C15 C10 Bi 116.9(7) . . ?
C11 C10 Bi 127.0(7) . . ?
O1 C2 Mo 178.2(7) . . ?
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 . . ?
N6 B N2 109.5(7) . . ?
N6 B N4 109.6(7) . . ?
N2 B N4 109.4(7) . . ?
N6 B H99 106(4) . . ?
N2 B H99 112(4) . . ?
N4 B H99 110(4) . . ?
C6 C5 C4 119.7(8) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C8 C7 C6 119.8(9) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C11 C12 C13 119.6(11) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C7 C6 C5 121.1(9) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C12 C11 C10 122.5(11) . . ?
C12 C11 H11 118.7 . . ?
C10 C11 H11 118.7 . . ?

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
N5 C28 C27 C26 1.0(9) . . . . ?
C30 C28 C27 C26 -179.9(9) . . . . ?
N1 N2 C19 C18 1.0(8) . . . . ?
B N2 C19 C18 178.6(7) . . . . ?
N1 N2 C19 C20 178.4(7) . . . . ?
B N2 C19 C20 -4.1(12) . . . . ?
N2 C19 C18 C17 -0.5(9) . . . . ?
C20 C19 C18 C17 -177.6(8) . . . . ?
N1 C17 C18 C19 -0.3(9) . . . . ?
C16 C17 C18 C19 178.7(7) . . . . ?
C24 N4 N3 C22 -0.8(8) . . . . ?
B N4 N3 C22 178.0(7) . . . . ?
C24 N4 N3 Mo -179.2(5) . . . . ?
B N4 N3 Mo -0.4(9) . . . . ?
C18 C17 N1 N2 0.9(8) . . . . ?
C16 C17 N1 N2 -178.1(6) . . . . ?
C18 C17 N1 Mo -173.2(5) . . . . ?
C16 C17 N1 Mo 7.8(11) . . . . ?
C19 N2 N1 C17 -1.2(8) . . . . ?
B N2 N1 C17 -179.0(7) . . . . ?
C19 N2 N1 Mo 173.8(5) . . . . ?
B N2 N1 Mo -3.9(8) . . . . ?
N5 N6 C26 C27 0.8(9) . . . . ?
B N6 C26 C27 -175.3(8) . . . . ?
N5 N6 C26 C29 179.8(8) . . . . ?
B N6 C26 C29 3.6(14) . . . . ?
C28 C27 C26 N6 -1.1(9) . . . . ?
C28 C27 C26 C29 180.0(9) . . . . ?
N4 N3 C22 C23 0.8(8) . . . . ?
Mo N3 C22 C23 178.8(6) . . . . ?
N4 N3 C22 C21 179.0(7) . . . . ?
Mo N3 C22 C21 -3.0(12) . . . . ?
C24 C23 C22 N3 -0.5(9) . . . . ?
C24 C23 C22 C21 -178.6(8) . . . . ?
N3 N4 C24 C23 0.5(9) . . . . ?
B N4 C24 C23 -178.1(8) . . . . ?
N3 N4 C24 C25 179.7(8) . . . . ?
B N4 C24 C25 1.1(14) . . . . ?
C22 C23 C24 N4 0.0(9) . . . . ?
C22 C23 C24 C25 -179.1(9) . . . . ?
C27 C28 N5 N6 -0.5(9) . . . . ?
C30 C28 N5 N6 -179.6(8) . . . . ?
C27 C28 N5 Mo 178.1(6) . . . . ?
C30 C28 N5 Mo -1.0(12) . . . . ?
C26 N6 N5 C28 -0.2(9) . . . . ?
B N6 N5 C28 176.4(8) . . . . ?
C26 N6 N5 Mo -179.0(5) . . . . ?
B N6 N5 Mo -2.4(10) . . . . ?
C15 C14 C13 C12 0.0(16) . . . . ?
C13 C14 C15 C10 2.0(16) . . . . ?
C7 C8 C9 C4 -2.6(14) . . . . ?
C5 C4 C9 C8 2.1(12) . . . . ?
Bi C4 C9 C8 178.4(7) . . . . ?
C14 C15 C10 C11 -2.0(14) . . . . ?
C14 C15 C10 Bi 176.0(8) . . . . ?
C26 N6 B N2 -124.8(9) . . . . ?
N5 N6 B N2 59.4(10) . . . . ?
C26 N6 B N4 115.2(9) . . . . ?
N5 N6 B N4 -60.6(10) . . . . ?
C19 N2 B N6 127.3(8) . . . . ?
N1 N2 B N6 -55.5(9) . . . . ?
C19 N2 B N4 -112.6(8) . . . . ?
N1 N2 B N4 64.6(9) . . . . ?
C24 N4 B N6 -121.3(9) . . . . ?
N3 N4 B N6 60.2(9) . . . . ?
C24 N4 B N2 118.6(9) . . . . ?
N3 N4 B N2 -59.8(9) . . . . ?
C9 C4 C5 C6 -0.5(12) . . . . ?
Bi C4 C5 C6 -177.2(7) . . . . ?
C9 C8 C7 C6 1.4(15) . . . . ?
C14 C13 C12 C11 -1.7(17) . . . . ?
C8 C7 C6 C5 0.2(15) . . . . ?
C4 C5 C6 C7 -0.6(14) . . . . ?
C13 C12 C11 C10 1.6(17) . . . . ?
C15 C10 C11 C12 0.2(15) . . . . ?
Bi C10 C11 C12 -177.5(8) . . . . ?

_refine_diff_density_max         1.041
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.116

####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 1588343'
_audit_update_record             
;
2017-11-29 deposited with the CCDC.
2018-01-22 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         ?
_chemical_formula_sum            'C30 H32 As B Mo N6 O2'
_chemical_formula_weight         690.28

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'
As As 0.0499 2.0058 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   10.1096(2)
_cell_length_b                   31.7822(5)
_cell_length_c                   19.6195(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.640(2)
_cell_angle_gamma                90
_cell_volume                     6232.31(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    30442
_cell_measurement_theta_min      3.6590
_cell_measurement_theta_max      29.6150

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_F_000             2800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.109
_exptl_absorpt_coefficient_mu    1.511
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95535
_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            96971
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.275
_diffrn_reflns_theta_max         30.118
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             16083
_reflns_number_gt                12388
_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    ?
_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)+(0.0300P)²+8.3815P] 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         16083
_refine_ls_number_parameters     811
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.0937
_refine_ls_wR_factor_gt          0.0853
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.077
_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
B1 B -0.0956(3) 0.03288(11) 0.22532(18) 0.0261(7) Uani 1 1 d . . . . .
B2 B 0.9818(4) 0.34166(11) 0.3854(2) 0.0288(8) Uani 1 1 d . . . . .
C74 C 1.3413(4) 0.27038(10) 0.67550(17) 0.0345(7) Uani 1 1 d . . . . .
C75 C 1.2086(3) 0.26883(11) 0.64483(18) 0.0371(8) Uani 1 1 d . . . . .
H75 H 1.182626 0.282552 0.603100 0.045 Uiso 1 1 calc R U . . .
C76 C 1.3760(5) 0.24982(12) 0.7383(2) 0.0532(10) Uani 1 1 d . . . . .
H76 H 1.463746 0.250866 0.760783 0.064 Uiso 1 1 calc R U . . .
O4 O 1.5368(2) 0.29244(8) 0.41520(14) 0.0458(6) Uani 1 1 d . . . . .
O3 O 1.4680(3) 0.41752(8) 0.50806(16) 0.0561(8) Uani 1 1 d . . . . .
C77 C 1.1142(4) 0.24718(12) 0.6753(2) 0.0467(9) Uani 1 1 d . . . . .
H77 H 1.025538 0.246681 0.654143 0.056 Uiso 1 1 calc R U . . .
C78 C 1.1506(5) 0.22641(12) 0.7367(2) 0.0557(12) Uani 1 1 d . . . . .
H78 H 1.087319 0.211562 0.756857 0.067 Uiso 1 1 calc R U . . .
C79 C 1.2804(6) 0.22784(13) 0.7675(2) 0.0601(12) Uani 1 1 d . . . . .
H79 H 1.305363 0.213762 0.808972 0.072 Uiso 1 1 calc R U . . .
H100 H -0.199(3) 0.0348(10) 0.2001(16) 0.028(8) Uiso 1 1 d . . . . .
H101 H 0.878(3) 0.3423(10) 0.3592(17) 0.032(9) Uiso 1 1 d . . . . .
Mo1 Mo 0.21878(2) 0.03202(2) 0.30598(2) 0.01967(6) Uani 1 1 d . . . . .
Mo2 Mo 1.29436(2) 0.33662(2) 0.46923(2) 0.02358(7) Uani 1 1 d . . . . .
As1 As 0.41575(3) 0.05747(2) 0.47645(2) 0.02467(7) Uani 1 1 d . . . . .
As2 As 1.47493(3) 0.30502(2) 0.64023(2) 0.03686(9) Uani 1 1 d . . . . .
N4 N -0.0450(2) 0.07807(8) 0.24072(13) 0.0246(5) Uani 1 1 d . . . . .
C1 C 0.3049(3) 0.04740(9) 0.38926(15) 0.0232(6) Uani 1 1 d . . . . .
N6 N -0.0871(2) 0.00895(7) 0.29371(12) 0.0226(5) Uani 1 1 d . . . . .
N5 N 0.0344(2) 0.00366(7) 0.33480(12) 0.0228(5) Uani 1 1 d . . . . .
C3 C 0.3228(3) -0.02151(9) 0.32272(16) 0.0262(6) Uani 1 1 d . . . . .
N2 N -0.0086(2) 0.01061(8) 0.17824(13) 0.0251(5) Uani 1 1 d . . . . .
C50 C 1.3730(3) 0.31783(10) 0.55206(16) 0.0278(7) Uani 1 1 d . . . . .
O1 O 0.4600(2) 0.07590(7) 0.24962(13) 0.0407(6) Uani 1 1 d . . . . .
N12 N 0.9920(2) 0.36296(8) 0.45616(13) 0.0273(6) Uani 1 1 d . . . . .
C2 C 0.3726(3) 0.05980(10) 0.26892(16) 0.0273(6) Uani 1 1 d . . . . .
N11 N 1.1125(3) 0.36634(8) 0.49774(13) 0.0272(5) Uani 1 1 d . . . . .
N8 N 1.0265(2) 0.29544(8) 0.39605(13) 0.0259(5) Uani 1 1 d . . . . .
C25 C 0.2994(3) 0.09875(9) 0.51181(15) 0.0247(6) Uani 1 1 d . . . . .
N3 N 0.0826(2) 0.08548(7) 0.27369(13) 0.0238(5) Uani 1 1 d . . . . .
N1 N 0.1286(2) 0.00908(8) 0.19660(13) 0.0246(5) Uani 1 1 d . . . . .
C61 C 1.1589(3) 0.24402(9) 0.43527(16) 0.0285(7) Uani 1 1 d . . . . .
N7 N 1.1500(2) 0.28602(7) 0.43203(13) 0.0242(5) Uani 1 1 d . . . . .
N10 N 1.0759(3) 0.36420(8) 0.34172(13) 0.0273(5) Uani 1 1 d . . . . .
C15 C 0.0105(3) -0.01837(9) 0.39026(15) 0.0252(6) Uani 1 1 d . . . . .
C51 C 1.4052(3) 0.38836(11) 0.49270(19) 0.0349(8) Uani 1 1 d . . . . .
C19 C 0.5479(3) 0.09305(10) 0.44038(15) 0.0259(6) Uani 1 1 d . . . . .
N9 N 1.2120(3) 0.36375(8) 0.36178(13) 0.0279(6) Uani 1 1 d . . . . .
C54 C 1.0898(3) 0.38656(10) 0.55521(17) 0.0336(7) Uani 1 1 d . . . . .
C12 C 0.0985(3) 0.12750(9) 0.27803(16) 0.0280(7) Uani 1 1 d . . . . .
O2 O 0.3819(2) -0.05182(7) 0.33388(14) 0.0409(6) Uani 1 1 d . . . . .
C30 C 0.1664(3) 0.10466(9) 0.48255(17) 0.0281(7) Uani 1 1 d . . . . .
H30 H 0.133871 0.091988 0.440647 0.034 Uiso 1 1 calc R U . . .
C62 C 1.2824(3) 0.22209(10) 0.46891(19) 0.0365(8) Uani 1 1 d . . . . .
H62A H 1.351740 0.225100 0.440755 0.055 Uiso 1 1 calc R U . . .
H62B H 1.263506 0.192767 0.474185 0.055 Uiso 1 1 calc R U . . .
H62C H 1.311400 0.234311 0.513393 0.055 Uiso 1 1 calc R U . . .
C52 C 1.4482(3) 0.30877(10) 0.43380(17) 0.0305(7) Uani 1 1 d . . . . .
C16 C -0.1259(3) -0.02671(9) 0.38439(16) 0.0279(7) Uani 1 1 d . . . . .
H16 H -0.168956 -0.041331 0.415776 0.034 Uiso 1 1 calc R U . . .
C59 C 0.9594(3) 0.25949(10) 0.37713(17) 0.0306(7) Uani 1 1 d . . . . .
C56 C 0.8949(3) 0.38051(10) 0.48765(19) 0.0347(8) Uani 1 1 d . . . . .
C13 C 0.2260(3) 0.14773(10) 0.30864(19) 0.0354(8) Uani 1 1 d . . . . .
H13A H 0.257824 0.134998 0.352405 0.053 Uiso 1 1 calc R U . . .
H13B H 0.211305 0.177220 0.314971 0.053 Uiso 1 1 calc R U . . .
H13C H 0.291363 0.144053 0.278337 0.053 Uiso 1 1 calc R U . . .
C55 C 0.9551(4) 0.39590(10) 0.54994(18) 0.0378(8) Uani 1 1 d . . . . .
H55 H 0.913270 0.409941 0.582435 0.045 Uiso 1 1 calc R U . . .
C60 C 1.0410(3) 0.22640(10) 0.40142(18) 0.0342(8) Uani 1 1 d . . . . .
H60 H 1.021337 0.197891 0.396210 0.041 Uiso 1 1 calc R U . . .
C10 C -0.1084(3) 0.11502(10) 0.22550(17) 0.0327(7) Uani 1 1 d . . . . .
C29 C 0.0825(3) 0.12920(10) 0.51536(18) 0.0359(8) Uani 1 1 d . . . . .
H29 H -0.006471 0.132769 0.495800 0.043 Uiso 1 1 calc R U . . .
C17 C -0.1843(3) -0.00927(9) 0.32365(16) 0.0256(6) Uani 1 1 d . . . . .
C24 C 0.5376(3) 0.13611(10) 0.43262(19) 0.0385(8) Uani 1 1 d . . . . .
H24 H 0.466698 0.150314 0.447484 0.046 Uiso 1 1 calc R U . . .
C26 C 0.3464(3) 0.11830(10) 0.57417(17) 0.0326(7) Uani 1 1 d . . . . .
H26 H 0.434692 0.114404 0.594501 0.039 Uiso 1 1 calc R U . . .
C14 C 0.1188(3) -0.03086(11) 0.44652(17) 0.0352(8) Uani 1 1 d . . . . .
H14A H 0.178178 -0.050208 0.428833 0.053 Uiso 1 1 calc R U . . .
H14B H 0.080251 -0.044113 0.482884 0.053 Uiso 1 1 calc R U . . .
H14C H 0.167789 -0.006333 0.464156 0.053 Uiso 1 1 calc R U . . .
C20 C 0.6556(3) 0.07245(11) 0.41923(17) 0.0328(7) Uani 1 1 d . . . . .
H20 H 0.665047 0.043518 0.425160 0.039 Uiso 1 1 calc R U . . .
C18 C -0.3274(3) -0.00943(11) 0.29131(19) 0.0369(8) Uani 1 1 d . . . . .
H18A H -0.361465 0.018808 0.289381 0.055 Uiso 1 1 calc R U . . .
H18B H -0.378240 -0.026561 0.318253 0.055 Uiso 1 1 calc R U . . .
H18C H -0.334692 -0.020640 0.245463 0.055 Uiso 1 1 calc R U . . .
C64 C 1.2660(3) 0.38321(10) 0.31195(18) 0.0336(7) Uani 1 1 d . . . . .
C23 C 0.6314(4) 0.15825(12) 0.4030(2) 0.0473(10) Uani 1 1 d . . . . .
H23 H 0.623322 0.187259 0.397829 0.057 Uiso 1 1 calc R U . . .
C7 C -0.0435(3) -0.00820(10) 0.11651(17) 0.0329(7) Uani 1 1 d . . . . .
C58 C 0.8225(3) 0.25917(11) 0.3358(2) 0.0444(9) Uani 1 1 d . . . . .
H58A H 0.760396 0.272124 0.361847 0.067 Uiso 1 1 calc R U . . .
H58B H 0.795497 0.230657 0.325162 0.067 Uiso 1 1 calc R U . . .
H58C H 0.823591 0.274521 0.293711 0.067 Uiso 1 1 calc R U . . .
C28 C 0.1307(4) 0.14843(11) 0.57721(19) 0.0409(8) Uani 1 1 d . . . . .
H28 H 0.073771 0.164769 0.599383 0.049 Uiso 1 1 calc R U . . .
C8 C -0.1850(4) -0.01346(13) 0.0824(2) 0.0488(10) Uani 1 1 d . . . . .
H8A H -0.232990 -0.030277 0.111105 0.073 Uiso 1 1 calc R U . . .
H8B H -0.186077 -0.027144 0.038659 0.073 Uiso 1 1 calc R U . . .
H8C H -0.226646 0.013651 0.075396 0.073 Uiso 1 1 calc R U . . .
C5 C 0.1770(3) -0.00982(10) 0.14423(16) 0.0304(7) Uani 1 1 d . . . . .
C66 C 1.0463(4) 0.38450(10) 0.28065(17) 0.0345(7) Uani 1 1 d . . . . .
C6 C 0.0725(4) -0.02107(11) 0.09354(18) 0.0380(8) Uani 1 1 d . . . . .
H6 H 0.079226 -0.034616 0.052176 0.046 Uiso 1 1 calc R U . . .
C53 C 1.1978(4) 0.39550(12) 0.61368(18) 0.0434(9) Uani 1 1 d . . . . .
H53A H 1.230538 0.369508 0.634732 0.065 Uiso 1 1 calc R U . . .
H53B H 1.162862 0.412655 0.647115 0.065 Uiso 1 1 calc R U . . .
H53C H 1.269549 0.410104 0.596948 0.065 Uiso 1 1 calc R U . . .
C21 C 0.7497(3) 0.09508(12) 0.38912(19) 0.0416(9) Uani 1 1 d . . . . .
H21 H 0.821238 0.081160 0.374426 0.050 Uiso 1 1 calc R U . . .
C65 C 1.1653(4) 0.39658(10) 0.26055(18) 0.0385(8) Uani 1 1 d . . . . .
H65 H 1.176100 0.410882 0.220405 0.046 Uiso 1 1 calc R U . . .
C57 C 0.7520(3) 0.38161(13) 0.4552(2) 0.0494(10) Uani 1 1 d . . . . .
H57A H 0.745466 0.393368 0.409755 0.074 Uiso 1 1 calc R U . . .
H57B H 0.701894 0.398637 0.482665 0.074 Uiso 1 1 calc R U . . .
H57C H 0.716534 0.353542 0.452294 0.074 Uiso 1 1 calc R U . . .
C11 C -0.0201(3) 0.14685(10) 0.24827(18) 0.0347(8) Uani 1 1 d . . . . .
H11 H -0.036389 0.175622 0.244525 0.042 Uiso 1 1 calc R U . . .
C4 C 0.3242(4) -0.01588(13) 0.1454(2) 0.0458(9) Uani 1 1 d . . . . .
H4A H 0.368933 0.010725 0.152868 0.069 Uiso 1 1 calc R U . . .
H4B H 0.339999 -0.027363 0.102042 0.069 Uiso 1 1 calc R U . . .
H4C H 0.357949 -0.034900 0.181865 0.069 Uiso 1 1 calc R U . . .
C27 C 0.2623(4) 0.14356(11) 0.60624(18) 0.0384(8) Uani 1 1 d . . . . .
H27 H 0.294899 0.157180 0.647291 0.046 Uiso 1 1 calc R U . . .
C63 C 1.4145(4) 0.38798(13) 0.3156(2) 0.0525(10) Uani 1 1 d . . . . .
H63A H 1.448936 0.404602 0.355190 0.079 Uiso 1 1 calc R U . . .
H63B H 1.433797 0.401667 0.274629 0.079 Uiso 1 1 calc R U . . .
H63C H 1.455820 0.360712 0.319429 0.079 Uiso 1 1 calc R U . . .
C22 C 0.7372(4) 0.13761(13) 0.3811(2) 0.0447(9) Uani 1 1 d . . . . .
H22 H 0.799972 0.152647 0.360888 0.054 Uiso 1 1 calc R U . . .
C67 C 0.9077(4) 0.39139(13) 0.2450(2) 0.0523(10) Uani 1 1 d . . . . .
H67A H 0.864595 0.364713 0.234920 0.078 Uiso 1 1 calc R U . . .
H67B H 0.910350 0.406421 0.202737 0.078 Uiso 1 1 calc R U . . .
H67C H 0.858551 0.407485 0.274128 0.078 Uiso 1 1 calc R U . . .
C9 C -0.2508(3) 0.11818(12) 0.1927(2) 0.0465(10) Uani 1 1 d . . . . .
H9A H -0.262226 0.104042 0.148985 0.070 Uiso 1 1 calc R U . . .
H9B H -0.274887 0.147264 0.185962 0.070 Uiso 1 1 calc R U . . .
H9C H -0.307039 0.105273 0.222064 0.070 Uiso 1 1 calc R U . . .
C68 C 1.5944(4) 0.26351(16) 0.6076(2) 0.0557(12) Uani 1 1 d D U . . .
C69 C 1.6936(17) 0.2841(6) 0.5745(12) 0.050(3) Uani 0.58(3) 1 d . U P A 1
H69 H 1.693154 0.313308 0.570714 0.060 Uiso 0.58(3) 1 calc R U P A 1
C70 C 1.7924(15) 0.2603(7) 0.5475(8) 0.057(4) Uani 0.58(3) 1 d . U P A 1
H70 H 1.861880 0.273062 0.529020 0.068 Uiso 0.58(3) 1 calc R U P A 1
C71 C 1.7790(18) 0.2153(6) 0.5505(11) 0.069(5) Uani 0.58(3) 1 d . U P A 1
H71 H 1.839749 0.198115 0.532507 0.083 Uiso 0.58(3) 1 calc R U P A 1
C72 C 1.6815(18) 0.1984(5) 0.5783(11) 0.075(5) Uani 0.58(3) 1 d . U P A 1
H72 H 1.679349 0.169149 0.580540 0.090 Uiso 0.58(3) 1 calc R U P A 1
C73 C 1.579(2) 0.2206(5) 0.6055(10) 0.064(4) Uani 0.58(3) 1 d . U P A 1
H73 H 1.506492 0.207155 0.620503 0.077 Uiso 0.58(3) 1 calc R U P A 1
C70A C 1.660(2) 0.1859(9) 0.6089(18) 0.093(7) Uani 0.42(3) 1 d D U P A 2
H70A H 1.641343 0.158313 0.620129 0.112 Uiso 0.42(3) 1 calc R U P A 2
C69A C 1.589(3) 0.2211(6) 0.6278(14) 0.082(7) Uani 0.42(3) 1 d D U P A 2
C72A C 1.777(2) 0.2389(11) 0.5540(11) 0.069(6) Uani 0.42(3) 1 d D U P A 2
H72A H 1.838374 0.245267 0.524858 0.082 Uiso 0.42(3) 1 calc R U P A 2
C71A C 1.760(3) 0.1972(11) 0.5719(18) 0.101(11) Uani 0.42(3) 1 d D . P A 2
C73A C 1.705(3) 0.2715(10) 0.5782(18) 0.078(9) Uani 0.42(3) 1 d D . P A 2
H73A H 1.732442 0.299141 0.574019 0.093 Uiso 0.42(3) 1 calc R U P A 2
H69A H 1.525(13) 0.212(4) 0.654(7) 0.093 Uiso 0.42(3) 1 d . U P A 2
H71A H 1.831(13) 0.174(4) 0.559(6) 0.093 Uiso 0.42(3) 1 d . 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
B1 N6 1.533(4) . ?
B1 N4 1.540(4) . ?
B1 N2 1.540(4) . ?
B2 N12 1.534(4) . ?
B2 N8 1.542(4) . ?
B2 N10 1.548(4) . ?
C74 C75 1.386(5) . ?
C74 C76 1.393(5) . ?
C74 As2 1.948(4) . ?
C75 C77 1.383(5) . ?
C76 C79 1.384(6) . ?
O4 C52 1.142(4) . ?
O3 C51 1.138(4) . ?
C77 C78 1.373(6) . ?
C78 C79 1.361(6) . ?
Mo1 C1 1.800(3) . ?
Mo1 C3 2.001(3) . ?
Mo1 C2 2.017(3) . ?
Mo1 N3 2.218(2) . ?
Mo1 N5 2.219(2) . ?
Mo1 N1 2.320(2) . ?
Mo2 C50 1.800(3) . ?
Mo2 C52 2.003(3) . ?
Mo2 C51 2.004(3) . ?
Mo2 N11 2.212(2) . ?
Mo2 N7 2.220(2) . ?
Mo2 N9 2.314(3) . ?
As1 C1 1.926(3) . ?
As1 C25 1.957(3) . ?
As1 C19 1.962(3) . ?
As2 C50 1.919(3) . ?
As2 C68 1.960(4) . ?
N4 C10 1.350(4) . ?
N4 N3 1.374(3) . ?
N6 C17 1.349(3) . ?
N6 N5 1.374(3) . ?
N5 C15 1.346(4) . ?
C3 O2 1.138(4) . ?
N2 C7 1.349(4) . ?
N2 N1 1.380(3) . ?
O1 C2 1.134(4) . ?
N12 C56 1.356(4) . ?
N12 N11 1.365(4) . ?
N11 C54 1.347(4) . ?
N8 C59 1.352(4) . ?
N8 N7 1.371(3) . ?
C25 C26 1.391(4) . ?
C25 C30 1.394(4) . ?
N3 C12 1.347(4) . ?
N1 C5 1.345(4) . ?
C61 N7 1.339(4) . ?
C61 C60 1.391(4) . ?
C61 C62 1.495(4) . ?
N10 C66 1.354(4) . ?
N10 N9 1.374(3) . ?
C15 C16 1.392(4) . ?
C15 C14 1.487(4) . ?
C19 C24 1.379(4) . ?
C19 C20 1.387(4) . ?
N9 C64 1.340(4) . ?
C54 C55 1.383(5) . ?
C54 C53 1.487(5) . ?
C12 C11 1.395(4) . ?
C12 C13 1.484(4) . ?
C30 C29 1.380(4) . ?
C16 C17 1.365(4) . ?
C59 C60 1.377(5) . ?
C59 C58 1.496(5) . ?
C56 C55 1.371(5) . ?
C56 C57 1.489(5) . ?
C10 C11 1.379(5) . ?
C10 C9 1.489(5) . ?
C29 C28 1.381(5) . ?
C17 C18 1.490(4) . ?
C24 C23 1.378(5) . ?
C26 C27 1.387(5) . ?
C20 C21 1.393(5) . ?
C64 C65 1.387(5) . ?
C64 C63 1.500(5) . ?
C23 C22 1.377(5) . ?
C7 C6 1.381(5) . ?
C7 C8 1.494(5) . ?
C28 C27 1.376(5) . ?
C5 C6 1.385(5) . ?
C5 C4 1.497(5) . ?
C66 C65 1.376(5) . ?
C66 C67 1.486(5) . ?
C21 C22 1.365(5) . ?
C68 C73A 1.354(19) . ?
C68 C73 1.373(15) . ?
C68 C69A 1.409(18) . ?
C68 C69 1.432(17) . ?
C69 C70 1.418(18) . ?
C70 C71 1.440(18) . ?
C71 C72 1.31(3) . ?
C72 C73 1.43(2) . ?
C70A C71A 1.381(18) . ?
C70A C69A 1.410(18) . ?
C72A C71A 1.387(17) . ?
C72A C73A 1.390(17) . ?

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
N6 B1 N4 108.5(3) . . ?
N6 B1 N2 109.6(2) . . ?
N4 B1 N2 110.1(2) . . ?
N12 B2 N8 108.6(3) . . ?
N12 B2 N10 109.5(3) . . ?
N8 B2 N10 108.9(2) . . ?
C75 C74 C76 117.8(3) . . ?
C75 C74 As2 122.9(3) . . ?
C76 C74 As2 118.9(3) . . ?
C77 C75 C74 121.0(3) . . ?
C79 C76 C74 120.3(4) . . ?
C78 C77 C75 120.5(4) . . ?
C79 C78 C77 119.1(4) . . ?
C78 C79 C76 121.3(4) . . ?
C1 Mo1 C3 84.90(12) . . ?
C1 Mo1 C2 85.08(13) . . ?
C3 Mo1 C2 90.96(12) . . ?
C1 Mo1 N3 104.26(11) . . ?
C3 Mo1 N3 170.49(11) . . ?
C2 Mo1 N3 92.34(10) . . ?
C1 Mo1 N5 100.93(11) . . ?
C3 Mo1 N5 93.08(10) . . ?
C2 Mo1 N5 173.03(11) . . ?
N3 Mo1 N5 82.81(9) . . ?
C1 Mo1 N1 174.03(11) . . ?
C3 Mo1 N1 90.48(11) . . ?
C2 Mo1 N1 91.23(11) . . ?
N3 Mo1 N1 80.54(9) . . ?
N5 Mo1 N1 83.07(8) . . ?
C50 Mo2 C52 84.61(13) . . ?
C50 Mo2 C51 84.78(14) . . ?
C52 Mo2 C51 90.34(13) . . ?
C50 Mo2 N11 100.64(11) . . ?
C52 Mo2 N11 174.11(12) . . ?
C51 Mo2 N11 92.80(11) . . ?
C50 Mo2 N7 103.64(11) . . ?
C52 Mo2 N7 94.14(11) . . ?
C51 Mo2 N7 170.79(12) . . ?
N11 Mo2 N7 82.07(9) . . ?
C50 Mo2 N9 174.66(11) . . ?
C52 Mo2 N9 92.30(11) . . ?
C51 Mo2 N9 90.90(12) . . ?
N11 Mo2 N9 82.67(9) . . ?
N7 Mo2 N9 80.89(9) . . ?
C1 As1 C25 97.24(12) . . ?
C1 As1 C19 96.45(12) . . ?
C25 As1 C19 102.68(12) . . ?
C50 As2 C74 97.64(13) . . ?
C50 As2 C68 97.00(15) . . ?
C74 As2 C68 103.29(18) . . ?
C10 N4 N3 109.7(2) . . ?
C10 N4 B1 129.5(3) . . ?
N3 N4 B1 120.9(2) . . ?
Mo1 C1 As1 171.58(17) . . ?
C17 N6 N5 109.7(2) . . ?
C17 N6 B1 130.2(3) . . ?
N5 N6 B1 120.1(2) . . ?
C15 N5 N6 106.6(2) . . ?
C15 N5 Mo1 132.6(2) . . ?
N6 N5 Mo1 120.79(17) . . ?
O2 C3 Mo1 178.4(3) . . ?
C7 N2 N1 109.6(2) . . ?
C7 N2 B1 130.2(3) . . ?
N1 N2 B1 120.1(2) . . ?
Mo2 C50 As2 171.23(18) . . ?
C56 N12 N11 109.7(3) . . ?
C56 N12 B2 129.7(3) . . ?
N11 N12 B2 120.5(2) . . ?
O1 C2 Mo1 178.3(3) . . ?
C54 N11 N12 106.8(2) . . ?
C54 N11 Mo2 131.9(2) . . ?
N12 N11 Mo2 121.11(18) . . ?
C59 N8 N7 109.7(2) . . ?
C59 N8 B2 130.0(3) . . ?
N7 N8 B2 120.2(2) . . ?
C26 C25 C30 118.9(3) . . ?
C26 C25 As1 117.9(2) . . ?
C30 C25 As1 122.6(2) . . ?
C12 N3 N4 107.1(2) . . ?
C12 N3 Mo1 132.7(2) . . ?
N4 N3 Mo1 120.12(17) . . ?
C5 N1 N2 106.5(2) . . ?
C5 N1 Mo1 135.2(2) . . ?
N2 N1 Mo1 118.06(17) . . ?
N7 C61 C60 109.4(3) . . ?
N7 C61 C62 122.1(3) . . ?
C60 C61 C62 128.5(3) . . ?
C61 N7 N8 106.9(2) . . ?
C61 N7 Mo2 132.1(2) . . ?
N8 N7 Mo2 120.90(17) . . ?
C66 N10 N9 109.7(3) . . ?
C66 N10 B2 129.6(3) . . ?
N9 N10 B2 120.6(2) . . ?
N5 C15 C16 109.1(3) . . ?
N5 C15 C14 122.5(3) . . ?
C16 C15 C14 128.3(3) . . ?
O3 C51 Mo2 177.9(3) . . ?
C24 C19 C20 119.0(3) . . ?
C24 C19 As1 124.6(2) . . ?
C20 C19 As1 116.4(2) . . ?
C64 N9 N10 106.6(3) . . ?
C64 N9 Mo2 135.0(2) . . ?
N10 N9 Mo2 118.21(18) . . ?
N11 C54 C55 109.2(3) . . ?
N11 C54 C53 122.7(3) . . ?
C55 C54 C53 128.1(3) . . ?
N3 C12 C11 108.9(3) . . ?
N3 C12 C13 122.9(3) . . ?
C11 C12 C13 128.2(3) . . ?
C29 C30 C25 120.4(3) . . ?
O4 C52 Mo2 178.3(3) . . ?
C17 C16 C15 106.7(3) . . ?
N8 C59 C60 107.5(3) . . ?
N8 C59 C58 122.7(3) . . ?
C60 C59 C58 129.8(3) . . ?
N12 C56 C55 107.4(3) . . ?
N12 C56 C57 122.5(3) . . ?
C55 C56 C57 130.1(3) . . ?
C56 C55 C54 106.9(3) . . ?
C59 C60 C61 106.5(3) . . ?
N4 C10 C11 107.7(3) . . ?
N4 C10 C9 123.4(3) . . ?
C11 C10 C9 128.9(3) . . ?
C30 C29 C28 120.0(3) . . ?
N6 C17 C16 107.8(3) . . ?
N6 C17 C18 122.7(3) . . ?
C16 C17 C18 129.4(3) . . ?
C23 C24 C19 120.5(3) . . ?
C27 C26 C25 120.4(3) . . ?
C19 C20 C21 120.0(3) . . ?
N9 C64 C65 109.7(3) . . ?
N9 C64 C63 121.7(3) . . ?
C65 C64 C63 128.6(3) . . ?
C22 C23 C24 120.3(3) . . ?
N2 C7 C6 107.7(3) . . ?
N2 C7 C8 123.8(3) . . ?
C6 C7 C8 128.6(3) . . ?
C27 C28 C29 120.4(3) . . ?
N1 C5 C6 109.7(3) . . ?
N1 C5 C4 121.5(3) . . ?
C6 C5 C4 128.8(3) . . ?
N10 C66 C65 107.5(3) . . ?
N10 C66 C67 123.7(3) . . ?
C65 C66 C67 128.8(3) . . ?
C7 C6 C5 106.4(3) . . ?
C22 C21 C20 120.2(3) . . ?
C66 C65 C64 106.5(3) . . ?
C10 C11 C12 106.6(3) . . ?
C28 C27 C26 119.9(3) . . ?
C21 C22 C23 119.9(3) . . ?
C73A C68 C69A 111.8(17) . . ?
C73 C68 C69 121.8(11) . . ?
C73A C68 As2 126.9(13) . . ?
C73 C68 As2 127.1(9) . . ?
C69A C68 As2 119.8(12) . . ?
C69 C68 As2 110.3(8) . . ?
C70 C69 C68 120.4(15) . . ?
C69 C70 C71 116.1(15) . . ?
C72 C71 C70 120.4(13) . . ?
C71 C72 C73 126.0(13) . . ?
C68 C73 C72 114.5(15) . . ?
C71A C70A C69A 112(3) . . ?
C68 C69A C70A 130(3) . . ?
C71A C72A C73A 122(2) . . ?
C70A C71A C72A 120(2) . . ?
C68 C73A C72A 121(2) . . ?

_refine_diff_density_max         1.830
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_4b
_database_code_depnum_ccdc_archive 'CCDC 1588344'
_audit_update_record             
;
2017-11-29 deposited with the CCDC.
2018-01-22 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         ?
_chemical_formula_sum            'C30 H32 As B N6 O2 W'
_chemical_formula_weight         778.19

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'
As As 0.0499 2.0058 '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           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   10.0885(2)
_cell_length_b                   31.7494(5)
_cell_length_c                   19.6156(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.290(2)
_cell_angle_gamma                90
_cell_volume                     6200.54(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    59778
_cell_measurement_theta_min      3.9400
_cell_measurement_theta_max      29.5210

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_F_000             3056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.099
_exptl_absorpt_coefficient_mu    4.822
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.81527
_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            125360
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.222
_diffrn_reflns_theta_max         30.054
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             16450
_reflns_number_gt                13989
_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    ?
_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)+(0.0197P)²+26.6151P] 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         16450
_refine_ls_number_parameters     790
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0479
_refine_ls_wR_factor_ref         0.0909
_refine_ls_wR_factor_gt          0.0866
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_restrained_S_all      1.209
_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
C6 C 0.7477(6) 0.4049(2) 0.3886(3) 0.0457(15) Uani 1 1 d . . . . .
H114 H 0.818596 0.418823 0.373455 0.055 Uiso 1 1 calc R U . . .
C30 C 0.3211(6) 0.5161(2) 0.1459(3) 0.0465(15) Uani 1 1 d . . . . .
H13A H 0.355395 0.535456 0.182134 0.070 Uiso 1 1 calc R U . . .
H13B H 0.336461 0.527196 0.102356 0.070 Uiso 1 1 calc R U . . .
H13C H 0.366140 0.489519 0.154230 0.070 Uiso 1 1 calc R U . . .
C206 C 0.2703(11) 0.2716(2) 0.7695(4) 0.070(2) Uani 1 1 d . . . . .
H6 H 0.292388 0.285384 0.811658 0.083 Uiso 1 1 calc R U . . .
C207 C 0.1407(10) 0.2729(2) 0.7362(4) 0.064(2) Uani 1 1 d . . . . .
H7 H 0.075432 0.287242 0.755464 0.077 Uiso 1 1 calc R U . . .
C208 C 0.1080(8) 0.2528(2) 0.6745(4) 0.0581(19) Uani 1 1 d . . . . .
H8 H 0.019571 0.253210 0.651922 0.070 Uiso 1 1 calc R U . . .
C220 C -0.2455(6) 0.1183(2) 0.4569(4) 0.0515(17) Uani 1 1 d . . . . .
H26A H -0.280493 0.146418 0.452334 0.077 Uiso 1 1 calc R U . . .
H26B H -0.295092 0.102116 0.485624 0.077 Uiso 1 1 calc R U . . .
H26C H -0.253829 0.105423 0.412109 0.077 Uiso 1 1 calc R U . . .
C221 C -0.0892(7) 0.1085(2) 0.2450(3) 0.0517(17) Uani 1 1 d . . . . .
H27A H -0.140297 0.094027 0.275036 0.078 Uiso 1 1 calc R U . . .
H27B H -0.086285 0.091698 0.204545 0.078 Uiso 1 1 calc R U . . .
H27C H -0.130780 0.135069 0.231658 0.078 Uiso 1 1 calc R U . . .
C222 C 0.0493(6) 0.11564(17) 0.2816(3) 0.0342(12) Uani 1 1 d . . . . .
C223 C 0.1699(6) 0.10369(18) 0.2627(3) 0.0397(14) Uani 1 1 d . . . . .
H29 H 0.181395 0.089497 0.222636 0.048 Uiso 1 1 calc R U . . .
C224 C 0.2707(6) 0.11690(17) 0.3151(3) 0.0354(12) Uani 1 1 d . . . . .
C225 C 0.4196(7) 0.1122(2) 0.3195(4) 0.0524(17) Uani 1 1 d . . . . .
H31A H 0.460071 0.139615 0.319571 0.079 Uiso 1 1 calc R U . . .
H31B H 0.438633 0.096489 0.280425 0.079 Uiso 1 1 calc R U . . .
H31C H 0.455471 0.097659 0.361262 0.079 Uiso 1 1 calc R U . . .
B B -0.1017(6) 0.46801(19) 0.2238(3) 0.0266(12) Uani 1 1 d . . . . .
B2 B -0.0165(6) 0.15819(18) 0.3859(3) 0.0277(12) Uani 1 1 d . . . . .
H98 H -0.199(5) 0.4638(15) 0.197(3) 0.021(13) Uiso 1 1 d . . . . .
H99 H -0.116(5) 0.1598(17) 0.359(3) 0.030(14) Uiso 1 1 d . . . . .
C201 C 0.3770(5) 0.18344(17) 0.5552(3) 0.0296(11) Uani 1 1 d . . . . .
C202 C 0.4090(5) 0.11208(18) 0.4950(3) 0.0343(12) Uani 1 1 d . . . . .
C203 C 0.4494(5) 0.19098(17) 0.4350(3) 0.0315(11) Uani 1 1 d . . . . .
C204 C 0.3373(6) 0.23058(18) 0.6780(3) 0.0382(13) Uani 1 1 d . . . . .
C205 C 0.3700(9) 0.2505(2) 0.7423(3) 0.059(2) Uani 1 1 d . . . . .
H5 H 0.457285 0.249472 0.766305 0.071 Uiso 1 1 calc R U . . .
C209 C 0.2058(6) 0.2315(2) 0.6447(3) 0.0435(14) Uani 1 1 d . . . . .
H9 H 0.182171 0.217994 0.602438 0.052 Uiso 1 1 calc R U . . .
C216 C 0.2046(7) 0.1047(2) 0.6149(3) 0.0455(15) Uani 1 1 d . . . . .
H22A H 0.276570 0.090464 0.597847 0.068 Uiso 1 1 calc R U . . .
H22B H 0.170812 0.087222 0.648043 0.068 Uiso 1 1 calc R U . . .
H22C H 0.237330 0.130702 0.636407 0.068 Uiso 1 1 calc R U . . .
C217 C 0.0955(6) 0.11376(16) 0.5567(3) 0.0327(12) Uani 1 1 d . . . . .
C218 C -0.0402(6) 0.10440(18) 0.5512(3) 0.0387(13) Uani 1 1 d . . . . .
H24 H -0.081465 0.090450 0.583841 0.046 Uiso 1 1 calc R U . . .
C219 C -0.1019(6) 0.11955(17) 0.4888(3) 0.0349(12) Uani 1 1 d . . . . .
C226 C 0.2848(6) 0.27780(17) 0.4714(3) 0.0387(13) Uani 1 1 d . . . . .
H17A H 0.312446 0.265845 0.516451 0.058 Uiso 1 1 calc R U . . .
H17B H 0.266512 0.307257 0.475884 0.058 Uiso 1 1 calc R U . . .
H17C H 0.355182 0.274301 0.444307 0.058 Uiso 1 1 calc R U . . .
C227 C 0.1611(5) 0.25605(16) 0.4368(3) 0.0296(11) Uani 1 1 d . . . . .
C228 C 0.0427(6) 0.27335(17) 0.4032(3) 0.0356(12) Uani 1 1 d . . . . .
H19 H 0.022397 0.301882 0.398432 0.043 Uiso 1 1 calc R U . . .
C229 C -0.0395(5) 0.24035(16) 0.3781(3) 0.0316(12) Uani 1 1 d . . . . .
C230 C -0.1778(6) 0.24107(19) 0.3367(4) 0.0455(15) Uani 1 1 d . . . . .
H21A H -0.179007 0.224779 0.295410 0.068 Uiso 1 1 calc R U . . .
H21B H -0.202832 0.269612 0.324661 0.068 Uiso 1 1 calc R U . . .
H21C H -0.240272 0.229290 0.363583 0.068 Uiso 1 1 calc R U . . .
N201 N 0.1529(4) 0.21369(12) 0.4335(2) 0.0260(9) Uani 1 1 d . . . . .
N202 N 0.0278(4) 0.20443(13) 0.3973(2) 0.0268(9) Uani 1 1 d . . . . .
N203 N 0.1172(4) 0.13383(13) 0.4987(2) 0.0289(9) Uani 1 1 d . . . . .
N204 N -0.0053(4) 0.13715(13) 0.4571(2) 0.0289(9) Uani 1 1 d . . . . .
N205 N 0.2148(4) 0.13617(13) 0.3646(2) 0.0277(9) Uani 1 1 d . . . . .
N206 N 0.0784(4) 0.13553(13) 0.3434(2) 0.0280(9) Uani 1 1 d . . . . .
O3 O 0.5386(4) 0.20742(14) 0.4153(2) 0.0487(11) Uani 1 1 d . . . . .
O4 O 0.4732(4) 0.08284(14) 0.5105(3) 0.0575(13) Uani 1 1 d . . . . .
As2 As 0.47631(6) 0.19749(2) 0.64372(3) 0.04312(15) Uani 1 1 d . . . . .
W1 W 0.29817(2) 0.16356(2) 0.47118(2) 0.02526(5) Uani 1 1 d . . . . .
C1 C 0.3040(5) 0.45298(15) 0.3903(3) 0.0259(10) Uani 1 1 d . . . . .
C2 C 0.3686(5) 0.44103(16) 0.2694(3) 0.0282(11) Uani 1 1 d . . . . .
C3 C 0.3200(5) 0.52218(16) 0.3217(3) 0.0282(11) Uani 1 1 d . . . . .
C4 C 0.5481(5) 0.40705(17) 0.4411(3) 0.0304(11) Uani 1 1 d . . . . .
C5 C 0.6539(5) 0.42779(19) 0.4192(3) 0.0361(12) Uani 1 1 d . . . . .
H115 H 0.663006 0.456789 0.424774 0.043 Uiso 1 1 calc R U . . .
C7 C 0.7354(7) 0.3626(2) 0.3811(3) 0.0501(16) Uani 1 1 d . . . . .
H113 H 0.797843 0.347631 0.360548 0.060 Uiso 1 1 calc R U . . .
C8 C 0.6313(7) 0.3415(2) 0.4036(4) 0.0536(18) Uani 1 1 d . . . . .
H112 H 0.624035 0.312421 0.398699 0.064 Uiso 1 1 calc R U . . .
C9 C 0.5370(6) 0.36373(18) 0.4336(3) 0.0421(14) Uani 1 1 d . . . . .
H111 H 0.466476 0.349547 0.448699 0.051 Uiso 1 1 calc R U . . .
C10 C 0.2989(5) 0.40121(15) 0.5123(3) 0.0270(10) Uani 1 1 d . . . . .
C11 C 0.3467(6) 0.38184(18) 0.5755(3) 0.0375(13) Uani 1 1 d . . . . .
H105 H 0.435275 0.385792 0.596404 0.045 Uiso 1 1 calc R U . . .
C12 C 0.2621(7) 0.35684(19) 0.6067(3) 0.0434(15) Uani 1 1 d . . . . .
H106 H 0.294674 0.343230 0.647955 0.052 Uiso 1 1 calc R U . . .
C13 C 0.1291(7) 0.35189(19) 0.5770(3) 0.0448(15) Uani 1 1 d . . . . .
H107 H 0.072133 0.335639 0.599072 0.054 Uiso 1 1 calc R U . . .
C14 C 0.0814(6) 0.37067(18) 0.5157(3) 0.0393(13) Uani 1 1 d . . . . .
H108 H -0.007956 0.367066 0.495777 0.047 Uiso 1 1 calc R U . . .
C15 C 0.1661(5) 0.39532(16) 0.4825(3) 0.0308(11) Uani 1 1 d . . . . .
H109 H 0.133277 0.407843 0.440280 0.037 Uiso 1 1 calc R U . . .
C16 C 0.2247(6) 0.35343(17) 0.3088(3) 0.0385(13) Uani 1 1 d . . . . .
H12D H 0.288789 0.356138 0.277832 0.058 Uiso 1 1 calc R U . . .
H12E H 0.210074 0.324141 0.317218 0.058 Uiso 1 1 calc R U . . .
H12F H 0.258633 0.367176 0.351707 0.058 Uiso 1 1 calc R U . . .
C17 C 0.0953(6) 0.37340(15) 0.2774(3) 0.0319(12) Uani 1 1 d . . . . .
C18 C -0.0220(6) 0.35388(17) 0.2473(3) 0.0386(14) Uani 1 1 d . . . . .
H124 H -0.037046 0.325016 0.243481 0.046 Uiso 1 1 calc R U . . .
C19 C -0.1122(5) 0.38511(18) 0.2239(3) 0.0361(13) Uani 1 1 d . . . . .
C20 C -0.2550(6) 0.3819(2) 0.1890(4) 0.0516(17) Uani 1 1 d . . . . .
H12G H -0.312512 0.395128 0.217177 0.077 Uiso 1 1 calc R U . . .
H12H H -0.279317 0.352777 0.182457 0.077 Uiso 1 1 calc R U . . .
H12I H -0.264858 0.395744 0.144968 0.077 Uiso 1 1 calc R U . . .
C21 C 0.1192(6) 0.53088(18) 0.4460(3) 0.0363(12) Uani 1 1 d . . . . .
H21D H 0.163600 0.506068 0.466242 0.054 Uiso 1 1 calc R U . . .
H21E H 0.082054 0.546244 0.480574 0.054 Uiso 1 1 calc R U . . .
H21F H 0.182739 0.548300 0.427579 0.054 Uiso 1 1 calc R U . . .
C22 C 0.0096(5) 0.51851(16) 0.3895(3) 0.0279(11) Uani 1 1 d . . . . .
C23 C -0.1273(5) 0.52693(16) 0.3837(3) 0.0306(11) Uani 1 1 d . . . . .
H119 H -0.169382 0.541446 0.415419 0.037 Uiso 1 1 calc R U . . .
C24 C -0.1877(5) 0.50988(15) 0.3229(3) 0.0266(10) Uani 1 1 d . . . . .
C25 C -0.3319(5) 0.51007(19) 0.2903(3) 0.0379(13) Uani 1 1 d . . . . .
H11A H -0.339758 0.520935 0.244112 0.057 Uiso 1 1 calc R U . . .
H11B H -0.382146 0.527542 0.316815 0.057 Uiso 1 1 calc R U . . .
H11C H -0.366448 0.481862 0.288843 0.057 Uiso 1 1 calc R U . . .
C26 C -0.1899(6) 0.5137(2) 0.0801(3) 0.0498(16) Uani 1 1 d . . . . .
H12J H -0.231905 0.486524 0.073461 0.075 Uiso 1 1 calc R U . . .
H12K H -0.191248 0.527049 0.036107 0.075 Uiso 1 1 calc R U . . .
H12L H -0.237887 0.530763 0.108331 0.075 Uiso 1 1 calc R U . . .
C27 C -0.0478(6) 0.50851(17) 0.1150(3) 0.0325(12) Uani 1 1 d . . . . .
C28 C 0.0685(6) 0.52126(18) 0.0932(3) 0.0377(13) Uani 1 1 d . . . . .
H128 H 0.075634 0.534797 0.051948 0.045 Uiso 1 1 calc R U . . .
C29 C 0.1728(5) 0.51009(16) 0.1445(3) 0.0307(11) Uani 1 1 d . . . . .
N1 N 0.0794(4) 0.41549(12) 0.2730(2) 0.0253(9) Uani 1 1 d . . . . .
N2 N -0.0496(4) 0.42238(13) 0.2392(2) 0.0285(9) Uani 1 1 d . . . . .
N3 N 0.1243(4) 0.49163(13) 0.1967(2) 0.0254(9) Uani 1 1 d . . . . .
N4 N -0.0133(4) 0.49013(13) 0.1770(2) 0.0265(9) Uani 1 1 d . . . . .
N5 N 0.0313(4) 0.49658(12) 0.3334(2) 0.0225(8) Uani 1 1 d . . . . .
N6 N -0.0914(4) 0.49152(13) 0.2924(2) 0.0247(8) Uani 1 1 d . . . . .
O1 O 0.4575(4) 0.42496(13) 0.2499(2) 0.0414(10) Uani 1 1 d . . . . .
O2 O 0.3788(4) 0.55287(12) 0.3317(2) 0.0432(10) Uani 1 1 d . . . . .
As As 0.41593(5) 0.44267(2) 0.47726(3) 0.02798(11) Uani 1 1 d . . . . .
W W 0.21587(2) 0.46863(2) 0.30544(2) 0.02203(5) Uani 1 1 d . . . . .
C210 C 0.5861(19) 0.2459(5) 0.6175(10) 0.049(6) Uani 0.52(3) 1 d G . P A 1
C211 C 0.681(2) 0.2354(6) 0.5760(10) 0.070(5) Uani 0.52(3) 1 d G U P A 1
H211 H 0.687560 0.207764 0.561384 0.085 Uiso 0.52(3) 1 calc R U P A 1
C212 C 0.7646(16) 0.2663(7) 0.5564(9) 0.084(6) Uani 0.52(3) 1 d G U P A 1
H212 H 0.827810 0.259279 0.528659 0.100 Uiso 0.52(3) 1 calc R U P A 1
C213 C 0.7541(15) 0.3076(6) 0.5783(10) 0.085(6) Uani 0.52(3) 1 d G U P A 1
H213 H 0.810348 0.328265 0.565184 0.103 Uiso 0.52(3) 1 calc R U P A 1
C214 C 0.6596(15) 0.3181(5) 0.6198(12) 0.083(6) Uani 0.52(3) 1 d G U P A 1
H214 H 0.652635 0.345736 0.634436 0.100 Uiso 0.52(3) 1 calc R U P A 1
C215 C 0.5756(16) 0.2872(6) 0.6394(10) 0.062(5) Uani 0.52(3) 1 d G U P A 1
H215 H 0.512382 0.294222 0.667162 0.074 Uiso 0.52(3) 1 calc R U P A 1
C21A C 0.600(2) 0.2352(6) 0.6078(12) 0.053(7) Uani 0.48(3) 1 d G . P A 2
C21B C 0.701(2) 0.2172(6) 0.5769(12) 0.067(6) Uani 0.48(3) 1 d G U P A 2
H21W H 0.708561 0.188023 0.574877 0.080 Uiso 0.48(3) 1 calc R U P A 2
C21C C 0.7904(18) 0.2427(7) 0.5490(10) 0.082(7) Uani 0.48(3) 1 d G U P A 2
H21X H 0.857920 0.230641 0.528260 0.098 Uiso 0.48(3) 1 calc R U P A 2
C21D C 0.7789(16) 0.2863(7) 0.5520(11) 0.080(7) Uani 0.48(3) 1 d G U P A 2
H21Y H 0.838816 0.303353 0.533266 0.096 Uiso 0.48(3) 1 calc R U P A 2
C21E C 0.6780(17) 0.3043(6) 0.5829(14) 0.081(6) Uani 0.48(3) 1 d G U P A 2
H21Z H 0.670352 0.333447 0.584887 0.097 Uiso 0.48(3) 1 calc R U P A 2
C21F C 0.5885(18) 0.2788(6) 0.6108(13) 0.072(6) Uani 0.48(3) 1 d G U P A 2
H21H H 0.520991 0.290830 0.631504 0.087 Uiso 0.48(3) 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
C6 C7 1.356(9) . ?
C6 C5 1.402(8) . ?
C30 C29 1.504(8) . ?
C206 C207 1.365(12) . ?
C206 C205 1.387(11) . ?
C207 C208 1.359(11) . ?
C208 C209 1.399(9) . ?
C220 C219 1.482(8) . ?
C221 C222 1.482(8) . ?
C222 N206 1.356(7) . ?
C222 C223 1.381(8) . ?
C223 C224 1.388(8) . ?
C224 N205 1.346(7) . ?
C224 C225 1.498(8) . ?
B N6 1.527(7) . ?
B N4 1.548(7) . ?
B N2 1.554(7) . ?
B2 N204 1.535(7) . ?
B2 N202 1.540(7) . ?
B2 N206 1.545(7) . ?
C201 W1 1.823(5) . ?
C201 As2 1.912(5) . ?
C202 O4 1.145(7) . ?
C202 W1 1.992(6) . ?
C203 O3 1.159(6) . ?
C203 W1 1.985(5) . ?
C204 C209 1.382(9) . ?
C204 C205 1.401(8) . ?
C204 As2 1.956(6) . ?
C216 C217 1.480(8) . ?
C217 N203 1.352(6) . ?
C217 C218 1.389(8) . ?
C218 C219 1.368(8) . ?
C219 N204 1.359(6) . ?
C226 C227 1.491(8) . ?
C227 N201 1.348(6) . ?
C227 C228 1.381(8) . ?
C228 C229 1.377(8) . ?
C229 N202 1.350(6) . ?
C229 C230 1.497(8) . ?
N201 N202 1.376(6) . ?
N201 W1 2.209(4) . ?
N203 N204 1.371(6) . ?
N203 W1 2.199(4) . ?
N205 N206 1.372(6) . ?
N205 W1 2.296(4) . ?
As2 C21A 1.942(11) . ?
As2 C210 2.009(11) . ?
C1 W 1.826(5) . ?
C1 As 1.915(5) . ?
C2 O1 1.150(6) . ?
C2 W 1.999(5) . ?
C3 O2 1.141(6) . ?
C3 W 1.997(5) . ?
C4 C5 1.380(7) . ?
C4 C9 1.386(8) . ?
C4 As 1.967(5) . ?
C7 C8 1.377(9) . ?
C8 C9 1.389(8) . ?
C10 C15 1.386(7) . ?
C10 C11 1.397(7) . ?
C10 As 1.965(5) . ?
C11 C12 1.379(8) . ?
C12 C13 1.382(9) . ?
C13 C14 1.359(9) . ?
C14 C15 1.395(8) . ?
C16 C17 1.493(8) . ?
C17 N1 1.347(6) . ?
C17 C18 1.381(8) . ?
C18 C19 1.373(8) . ?
C19 N2 1.352(7) . ?
C19 C20 1.495(8) . ?
C21 C22 1.486(7) . ?
C22 N5 1.349(6) . ?
C22 C23 1.393(7) . ?
C23 C24 1.361(7) . ?
C24 N6 1.353(6) . ?
C24 C25 1.492(7) . ?
C26 C27 1.495(8) . ?
C27 N4 1.344(6) . ?
C27 C28 1.373(8) . ?
C28 C29 1.380(8) . ?
C29 N3 1.338(6) . ?
N1 N2 1.379(6) . ?
N1 W 2.205(4) . ?
N3 N4 1.380(5) . ?
N3 W 2.302(4) . ?
N5 N6 1.372(5) . ?
N5 W 2.210(4) . ?
C210 C211 1.3900 . ?
C210 C215 1.3900 . ?
C211 C212 1.3900 . ?
C212 C213 1.3900 . ?
C213 C214 1.3900 . ?
C214 C215 1.3900 . ?
C21A C21B 1.3900 . ?
C21A C21F 1.3900 . ?
C21B C21C 1.3900 . ?
C21C C21D 1.3900 . ?
C21D C21E 1.3900 . ?
C21E C21F 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
C7 C6 C5 120.3(6) . . ?
C207 C206 C205 121.9(7) . . ?
C208 C207 C206 119.2(7) . . ?
C207 C208 C209 120.8(8) . . ?
N206 C222 C223 107.1(5) . . ?
N206 C222 C221 123.8(5) . . ?
C223 C222 C221 129.1(5) . . ?
C222 C223 C224 106.9(5) . . ?
N205 C224 C223 109.2(5) . . ?
N205 C224 C225 122.4(5) . . ?
C223 C224 C225 128.4(5) . . ?
N6 B N4 109.7(4) . . ?
N6 B N2 108.2(4) . . ?
N4 B N2 109.2(4) . . ?
N204 B2 N202 107.8(4) . . ?
N204 B2 N206 109.1(4) . . ?
N202 B2 N206 109.4(4) . . ?
W1 C201 As2 171.8(3) . . ?
O4 C202 W1 178.2(6) . . ?
O3 C203 W1 178.4(5) . . ?
C209 C204 C205 118.9(6) . . ?
C209 C204 As2 122.4(4) . . ?
C205 C204 As2 118.3(5) . . ?
C206 C205 C204 119.0(7) . . ?
C204 C209 C208 120.1(6) . . ?
N203 C217 C218 109.1(5) . . ?
N203 C217 C216 122.6(5) . . ?
C218 C217 C216 128.3(5) . . ?
C219 C218 C217 107.1(5) . . ?
N204 C219 C218 107.4(5) . . ?
N204 C219 C220 122.8(5) . . ?
C218 C219 C220 129.8(5) . . ?
N201 C227 C228 109.4(5) . . ?
N201 C227 C226 121.6(5) . . ?
C228 C227 C226 129.0(5) . . ?
C229 C228 C227 107.0(5) . . ?
N202 C229 C228 107.2(5) . . ?
N202 C229 C230 123.2(5) . . ?
C228 C229 C230 129.6(5) . . ?
C227 N201 N202 106.4(4) . . ?
C227 N201 W1 132.1(4) . . ?
N202 N201 W1 121.5(3) . . ?
C229 N202 N201 110.0(4) . . ?
C229 N202 B2 130.0(4) . . ?
N201 N202 B2 120.0(4) . . ?
C217 N203 N204 106.6(4) . . ?
C217 N203 W1 131.5(4) . . ?
N204 N203 W1 121.7(3) . . ?
C219 N204 N203 109.8(4) . . ?
C219 N204 B2 130.0(5) . . ?
N203 N204 B2 120.1(4) . . ?
C224 N205 N206 106.9(4) . . ?
C224 N205 W1 134.0(4) . . ?
N206 N205 W1 118.9(3) . . ?
C222 N206 N205 109.8(4) . . ?
C222 N206 B2 129.5(5) . . ?
N205 N206 B2 120.5(4) . . ?
C201 As2 C21A 95.0(8) . . ?
C201 As2 C204 97.9(2) . . ?
C21A As2 C204 109.4(7) . . ?
C201 As2 C210 100.1(6) . . ?
C204 As2 C210 97.6(6) . . ?
C201 W1 C203 85.6(2) . . ?
C201 W1 C202 85.7(2) . . ?
C203 W1 C202 90.5(2) . . ?
C201 W1 N203 100.64(19) . . ?
C203 W1 N203 173.16(19) . . ?
C202 W1 N203 92.69(19) . . ?
C201 W1 N201 102.80(19) . . ?
C203 W1 N201 94.08(19) . . ?
C202 W1 N201 170.6(2) . . ?
N203 W1 N201 81.89(15) . . ?
C201 W1 N205 175.52(19) . . ?
C203 W1 N205 91.71(18) . . ?
C202 W1 N205 90.7(2) . . ?
N203 W1 N205 82.22(15) . . ?
N201 W1 N205 80.95(15) . . ?
W C1 As 171.5(3) . . ?
O1 C2 W 178.8(5) . . ?
O2 C3 W 179.2(5) . . ?
C5 C4 C9 119.6(5) . . ?
C5 C4 As 116.2(4) . . ?
C9 C4 As 124.1(4) . . ?
C4 C5 C6 119.6(6) . . ?
C6 C7 C8 120.5(6) . . ?
C7 C8 C9 120.0(6) . . ?
C4 C9 C8 120.0(6) . . ?
C15 C10 C11 119.1(5) . . ?
C15 C10 As 122.5(4) . . ?
C11 C10 As 117.7(4) . . ?
C12 C11 C10 119.8(6) . . ?
C11 C12 C13 120.4(6) . . ?
C14 C13 C12 120.3(6) . . ?
C13 C14 C15 120.2(6) . . ?
C10 C15 C14 120.2(5) . . ?
N1 C17 C18 109.5(5) . . ?
N1 C17 C16 122.3(5) . . ?
C18 C17 C16 128.2(5) . . ?
C19 C18 C17 107.1(5) . . ?
N2 C19 C18 107.3(5) . . ?
N2 C19 C20 122.8(5) . . ?
C18 C19 C20 129.9(5) . . ?
N5 C22 C23 108.8(4) . . ?
N5 C22 C21 123.1(5) . . ?
C23 C22 C21 128.2(5) . . ?
C24 C23 C22 107.0(4) . . ?
N6 C24 C23 107.9(4) . . ?
N6 C24 C25 122.1(5) . . ?
C23 C24 C25 130.0(5) . . ?
N4 C27 C28 107.5(5) . . ?
N4 C27 C26 123.5(5) . . ?
C28 C27 C26 129.1(5) . . ?
C27 C28 C29 106.7(5) . . ?
N3 C29 C28 109.9(5) . . ?
N3 C29 C30 121.8(5) . . ?
C28 C29 C30 128.3(5) . . ?
C17 N1 N2 106.3(4) . . ?
C17 N1 W 132.7(4) . . ?
N2 N1 W 120.9(3) . . ?
C19 N2 N1 109.8(4) . . ?
C19 N2 B 129.9(5) . . ?
N1 N2 B 120.3(4) . . ?
C29 N3 N4 106.1(4) . . ?
C29 N3 W 134.8(3) . . ?
N4 N3 W 118.9(3) . . ?
C27 N4 N3 109.9(4) . . ?
C27 N4 B 130.1(4) . . ?
N3 N4 B 120.0(4) . . ?
C22 N5 N6 106.8(4) . . ?
C22 N5 W 131.5(3) . . ?
N6 N5 W 121.6(3) . . ?
C24 N6 N5 109.5(4) . . ?
C24 N6 B 130.5(4) . . ?
N5 N6 B 120.0(4) . . ?
C1 As C10 97.2(2) . . ?
C1 As C4 96.5(2) . . ?
C10 As C4 102.8(2) . . ?
C1 W C3 85.4(2) . . ?
C1 W C2 85.0(2) . . ?
C3 W C2 90.8(2) . . ?
C1 W N1 104.16(19) . . ?
C3 W N1 170.14(18) . . ?
C2 W N1 92.48(17) . . ?
C1 W N5 100.90(18) . . ?
C3 W N5 93.49(17) . . ?
C2 W N5 172.93(18) . . ?
N1 W N5 82.37(14) . . ?
C1 W N3 174.27(18) . . ?
C3 W N3 90.03(18) . . ?
C2 W N3 91.63(18) . . ?
N1 W N3 80.59(15) . . ?
N5 W N3 82.77(14) . . ?
C211 C210 C215 120.0 . . ?
C211 C210 As2 115.2(9) . . ?
C215 C210 As2 124.8(9) . . ?
C212 C211 C210 120.0 . . ?
C211 C212 C213 120.0 . . ?
C214 C213 C212 120.0 . . ?
C215 C214 C213 120.0 . . ?
C214 C215 C210 120.0 . . ?
C21B C21A C21F 120.0 . . ?
C21B C21A As2 117.6(10) . . ?
C21F C21A As2 122.4(10) . . ?
C21C C21B C21A 120.0 . . ?
C21B C21C C21D 120.0 . . ?
C21E C21D C21C 120.0 . . ?
C21D C21E C21F 120.0 . . ?
C21E C21F C21A 120.0 . . ?

_refine_diff_density_max         2.573
_refine_diff_density_min         -1.706
_refine_diff_density_rms         0.140

