# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1523849'
_audit_update_record             
;
2016-12-21 deposited with the CCDC.
2017-02-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C57 H48 Mo N8 O3 P2'
_chemical_formula_weight         1050.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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                   13.3538(6)
_cell_length_b                   13.5304(5)
_cell_length_c                   16.6261(7)
_cell_angle_alpha                71.257(4)
_cell_angle_beta                 88.524(4)
_cell_angle_gamma                62.823(4)
_cell_volume                     2504.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5516
_cell_measurement_theta_min      2.9159
_cell_measurement_theta_max      29.5943

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_F_000             1084
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.380
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91025
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_measurement_method       'ω scans'
_diffrn_ambient_temperature      120.00(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_reflns_number            23371
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.922
_diffrn_reflns_theta_max         29.660
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12615
_reflns_number_gt                9015
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+11.8675P] 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         12615
_refine_ls_number_parameters     688
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.1003
_refine_ls_wR_factor_ref         0.1972
_refine_ls_wR_factor_gt          0.1828
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_restrained_S_all      1.227
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1A Mo 0.18639(10) 0.51773(7) 0.83458(7) 0.0246(3) Uani 0.558(3) 1 d . . P A 1
O1A O 0.1577(10) 0.5018(11) 0.9367(9) 0.033(2) Uani 0.558(3) 1 d . . P A 1
C2A C 0.3554(10) 0.5012(10) 0.8385(8) 0.020(2) Uani 0.558(3) 1 d . . P A 1
N2A N 0.4399(7) 0.4981(7) 0.8406(6) 0.0280(19) Uani 0.558(3) 1 d . . P A 1
Mo1B Mo 0.24074(12) 0.51810(9) 0.80178(9) 0.0237(4) Uani 0.442(3) 1 d . . P A 2
O1B O 0.3717(11) 0.4996(11) 0.8127(7) 0.028(3) Uiso 0.442(3) 1 d . . P A 2
C2B C 0.1994(18) 0.503(2) 0.9288(18) 0.031(5) Uani 0.442(3) 1 d . . P A 2
N2B N 0.1766(12) 0.4897(11) 0.9978(10) 0.047(4) Uani 0.442(3) 1 d . . P A 2
P2 P -0.49761(11) 1.07246(11) 0.30688(8) 0.0171(3) Uani 1 1 d . . . . .
P1 P 0.80139(11) 0.14114(11) 0.84177(9) 0.0180(3) Uani 1 1 d . . . . .
C27 C 0.7217(5) 0.2534(5) 0.6661(4) 0.0295(12) Uani 1 1 d . . . . .
H27 H 0.7992 0.2268 0.6580 0.035 Uiso 1 1 calc R U . . .
N8 N 0.0330(6) 0.5333(5) 0.7892(5) 0.061(2) Uani 1 1 d . . . . .
C46 C -0.3783(4) 0.9301(4) 0.3631(3) 0.0199(10) Uani 1 1 d . . . . .
N5 N 0.2305(6) 0.5741(5) 0.6109(5) 0.059(2) Uani 1 1 d . . . . .
C49 C -0.1914(5) 0.7106(5) 0.4441(4) 0.0293(12) Uani 1 1 d . . . . .
H49 H -0.1270 0.6356 0.4714 0.035 Uiso 1 1 calc R U . . .
C52 C -0.4980(4) 1.1842(4) 0.3429(3) 0.0208(10) Uani 1 1 d . . . . .
C29 C 0.9919(4) 0.0890(5) 0.7594(4) 0.0261(11) Uani 1 1 d . . . . .
H29 H 0.9661 0.0479 0.7359 0.031 Uiso 1 1 calc R U . . .
C57 C -0.5802(5) 1.2381(5) 0.3885(3) 0.0261(11) Uani 1 1 d . . . . .
H57 H -0.6364 1.2137 0.4045 0.031 Uiso 1 1 calc R U . . .
C10 C 0.8258(4) -0.0097(4) 0.8825(3) 0.0188(10) Uani 1 1 d . . . . .
C28 C 0.9307(4) 0.1439(4) 0.8159(3) 0.0205(10) Uani 1 1 d . . . . .
C48 C -0.2777(5) 0.7197(5) 0.3922(4) 0.0281(12) Uani 1 1 d . . . . .
H48 H -0.2716 0.6512 0.3836 0.034 Uiso 1 1 calc R U . . .
C25 C 0.5236(5) 0.3585(5) 0.6081(4) 0.0276(12) Uani 1 1 d . . . . .
H25 H 0.4653 0.4032 0.5600 0.033 Uiso 1 1 calc R U . . .
C44 C -0.4462(5) 1.0692(5) 0.0653(4) 0.0287(12) Uani 1 1 d . . . . .
H44 H -0.4122 1.0118 0.0382 0.034 Uiso 1 1 calc R U . . .
C34 C -0.6268(4) 1.0637(4) 0.3264(3) 0.0180(10) Uani 1 1 d . . . . .
C40 C -0.4921(4) 1.1171(4) 0.1928(3) 0.0190(10) Uani 1 1 d . . . . .
C15 C 0.9358(4) -0.1043(5) 0.9033(4) 0.0247(11) Uani 1 1 d . . . . .
H15 H 0.9987 -0.0896 0.8921 0.030 Uiso 1 1 calc R U . . .
C51 C -0.2918(4) 0.9198(5) 0.4159(3) 0.0242(11) Uani 1 1 d . . . . .
H51 H -0.2967 0.9880 0.4242 0.029 Uiso 1 1 calc R U . . .
N7 N 0.0725(6) 0.5800(5) 0.5672(4) 0.0589(19) Uani 1 1 d . . . . .
C41 C -0.5445(5) 1.2385(5) 0.1429(4) 0.0253(11) Uani 1 1 d . . . . .
H41 H -0.5770 1.2962 0.1698 0.030 Uiso 1 1 calc R U . . .
C45 C -0.4427(4) 1.0325(5) 0.1536(3) 0.0218(10) Uani 1 1 d . . . . .
H45 H -0.4068 0.9505 0.1871 0.026 Uiso 1 1 calc R U . . .
C43 C -0.4986(5) 1.1881(5) 0.0161(3) 0.0281(12) Uani 1 1 d . . . . .
H43 H -0.5006 1.2120 -0.0444 0.034 Uiso 1 1 calc R U . . .
C19 C 0.6974(5) 0.3027(7) 1.0522(5) 0.0420(17) Uani 1 1 d . . . . .
H19 H 0.6803 0.3363 1.0961 0.050 Uiso 1 1 calc R U . . .
C14 C 0.9539(5) -0.2198(5) 0.9405(4) 0.0294(12) Uani 1 1 d . . . . .
H14 H 1.0288 -0.2845 0.9538 0.035 Uiso 1 1 calc R U . . .
C38 C -0.7313(4) 0.9758(5) 0.4143(4) 0.0261(11) Uani 1 1 d . . . . .
H38 H -0.7333 0.9167 0.4632 0.031 Uiso 1 1 calc R U . . .
C24 C 0.4948(5) 0.3345(5) 0.6900(4) 0.0280(12) Uani 1 1 d . . . . .
H24 H 0.4171 0.3629 0.6980 0.034 Uiso 1 1 calc R U . . .
C37 C -0.8296(5) 1.0594(5) 0.3586(4) 0.0290(12) Uani 1 1 d . . . . .
H37 H -0.8991 1.0577 0.3697 0.035 Uiso 1 1 calc R U . . .
C21 C 0.6875(5) 0.3269(5) 0.9020(4) 0.0331(14) Uani 1 1 d . . . . .
H21 H 0.6628 0.3769 0.8434 0.040 Uiso 1 1 calc R U . . .
N6 N 0.1676(6) 0.5909(5) 0.5438(5) 0.065(2) Uani 1 1 d . . . . .
C33 C 0.9713(4) 0.2021(4) 0.8519(4) 0.0235(11) Uani 1 1 d . . . . .
H33 H 0.9308 0.2388 0.8908 0.028 Uiso 1 1 calc R U . . .
C53 C -0.4115(5) 1.2175(5) 0.3218(3) 0.0267(12) Uani 1 1 d . . . . .
H53 H -0.3543 1.1796 0.2909 0.032 Uiso 1 1 calc R U . . .
C47 C -0.3728(4) 0.8293(4) 0.3529(3) 0.0217(10) Uani 1 1 d . . . . .
H47 H -0.4333 0.8355 0.3194 0.026 Uiso 1 1 calc R U . . .
C20 C 0.6586(6) 0.3748(6) 0.9676(5) 0.0449(18) Uani 1 1 d . . . . .
H20 H 0.6117 0.4577 0.9536 0.054 Uiso 1 1 calc R U . . .
C35 C -0.7262(4) 1.1483(4) 0.2693(3) 0.0238(11) Uani 1 1 d . . . . .
H35 H -0.7241 1.2064 0.2196 0.029 Uiso 1 1 calc R U . . .
C17 C 0.7901(5) 0.1311(5) 1.0102(4) 0.0269(12) Uani 1 1 d . . . . .
H17 H 0.8345 0.0476 1.0253 0.032 Uiso 1 1 calc R U . . .
C31 C 1.1295(5) 0.1536(5) 0.7726(4) 0.0326(13) Uani 1 1 d . . . . .
H31 H 1.1966 0.1581 0.7568 0.039 Uiso 1 1 calc R U . . .
C39 C -0.6290(4) 0.9775(5) 0.3993(3) 0.0246(11) Uani 1 1 d . . . . .
H39 H -0.5613 0.9206 0.4382 0.029 Uiso 1 1 calc R U . . .
C11 C 0.7328(4) -0.0306(5) 0.8991(4) 0.0252(11) Uani 1 1 d . . . . .
H11 H 0.6575 0.0334 0.8838 0.030 Uiso 1 1 calc R U . . .
N4 N 0.1788(6) 0.5490(4) 0.6805(5) 0.058(2) Uani 1 1 d . . . . .
C6 C -0.0917(8) 0.5330(7) 0.6870(7) 0.090(4) Uani 1 1 d . . . . .
H6 H -0.1093 0.5386 0.6302 0.108 Uiso 1 1 calc R U . . .
C54 C -0.4113(6) 1.3055(5) 0.3467(4) 0.0373(15) Uani 1 1 d . . . . .
H54 H -0.3531 1.3276 0.3340 0.045 Uiso 1 1 calc R U . . .
C5 C 0.0044(6) 0.5381(6) 0.7105(6) 0.065(3) Uani 1 1 d . . . . .
C32 C 1.0715(4) 0.2055(5) 0.8300(4) 0.0285(12) Uani 1 1 d . . . . .
H32 H 1.0998 0.2437 0.8547 0.034 Uiso 1 1 calc R U . . .
C13 C 0.8609(5) -0.2397(5) 0.9580(4) 0.0289(12) Uani 1 1 d . . . . .
H13 H 0.8727 -0.3185 0.9839 0.035 Uiso 1 1 calc R U . . .
C55 C -0.4967(6) 1.3610(5) 0.3902(4) 0.0386(15) Uani 1 1 d . . . . .
H55 H -0.4978 1.4229 0.4062 0.046 Uiso 1 1 calc R U . . .
C16 C 0.7535(4) 0.2040(5) 0.9243(4) 0.0238(11) Uani 1 1 d . . . . .
C23 C 0.5794(5) 0.2689(5) 0.7604(4) 0.0277(12) Uani 1 1 d . . . . .
H23 H 0.5600 0.2518 0.8167 0.033 Uiso 1 1 calc R U . . .
C12 C 0.7520(5) -0.1465(5) 0.9383(4) 0.0297(12) Uani 1 1 d . . . . .
H12 H 0.6895 -0.1615 0.9516 0.036 Uiso 1 1 calc R U . . .
C56 C -0.5801(5) 1.3279(5) 0.4108(4) 0.0343(14) Uani 1 1 d . . . . .
H56 H -0.6381 1.3672 0.4406 0.041 Uiso 1 1 calc R U . . .
C4 C 0.0812(7) 0.5549(6) 0.6518(5) 0.055(2) Uani 1 1 d . . . . .
C26 C 0.6367(5) 0.3179(5) 0.5953(4) 0.0335(13) Uani 1 1 d . . . . .
H26 H 0.6559 0.3341 0.5388 0.040 Uiso 1 1 calc R U . . .
C22 C 0.6934(4) 0.2279(4) 0.7483(3) 0.0218(10) Uani 1 1 d . . . . .
C7 C -0.1648(9) 0.5190(8) 0.7513(9) 0.107(5) Uani 1 1 d . . . . .
H7 H -0.2306 0.5135 0.7384 0.128 Uiso 1 1 calc R U . . .
C36 C -0.8284(4) 1.1467(5) 0.2860(4) 0.0280(12) Uani 1 1 d . . . . .
H36 H -0.8968 1.2045 0.2482 0.034 Uiso 1 1 calc R U . . .
C8 C -0.1349(8) 0.5140(7) 0.8305(8) 0.090(4) Uani 1 1 d . . . . .
H8 H -0.1821 0.5057 0.8731 0.108 Uiso 1 1 calc R U . . .
C9 C -0.0403(9) 0.5203(7) 0.8524(7) 0.083(3) Uani 1 1 d . . . . .
H9 H -0.0231 0.5160 0.9089 0.099 Uiso 1 1 calc R U . . .
N3 N 0.3152(4) 0.2391(4) 0.8386(3) 0.0329(11) Uani 1 1 d . . . . .
C3 C 0.2765(5) 0.3356(5) 0.8327(4) 0.0306(13) Uani 1 1 d . . . . .
O2 O 0.1282(4) 0.9453(4) 0.5839(3) 0.0362(10) Uani 1 1 d D . . . .
O3 O 0.0834(4) 0.8543(4) 0.4681(3) 0.0392(10) Uani 1 1 d D . . . .
C42 C -0.5487(5) 1.2735(5) 0.0548(3) 0.0273(12) Uani 1 1 d . . . . .
H42 H -0.5854 1.3553 0.0207 0.033 Uiso 1 1 calc R U . . .
N1 N 0.1097(4) 0.8067(4) 0.7480(3) 0.0311(11) Uani 1 1 d . . . . .
C1 C 0.1383(5) 0.7075(5) 0.7750(4) 0.0315(13) Uani 1 1 d . . . . .
C30 C 1.0907(5) 0.0950(5) 0.7379(4) 0.0327(13) Uani 1 1 d . . . . .
H30 H 1.1320 0.0585 0.6991 0.039 Uiso 1 1 calc R U . . .
C50 C -0.1993(5) 0.8102(5) 0.4558(4) 0.0294(12) Uani 1 1 d . . . . .
H50 H -0.1405 0.8033 0.4917 0.035 Uiso 1 1 calc R U . . .
C18 C 0.7612(5) 0.1816(6) 1.0732(4) 0.0393(16) Uani 1 1 d . . . . .
H18 H 0.7856 0.1322 1.1318 0.047 Uiso 1 1 calc R U . . .
H2WA H 0.057(3) 1.016(4) 0.566(4) 0.06(2) Uiso 1 1 d D . . . .
H2WB H 0.124(5) 0.907(5) 0.6424(18) 0.05(2) Uiso 1 1 d D . . . .
H3WB H 0.087(7) 0.778(3) 0.489(5) 0.07(3) Uiso 1 1 d D . . . .
H3WA H 0.108(10) 0.863(8) 0.518(4) 0.15(5) Uiso 1 1 d 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
Mo1A O1A 1.698(14) . ?
Mo1A N8 2.096(7) . ?
Mo1A C2A 2.165(12) . ?
Mo1A C3 2.205(5) . ?
Mo1A C1 2.209(6) . ?
Mo1A N4 2.455(8) . ?
C2A N2A 1.112(14) . ?
Mo1B O1B 1.655(13) . ?
Mo1B N4 2.038(6) . ?
Mo1B C2B 2.14(3) . ?
Mo1B C3 2.170(5) . ?
Mo1B C1 2.175(5) . ?
C2B N2B 1.16(3) . ?
P2 C52 1.794(5) . ?
P2 C34 1.797(5) . ?
P2 C46 1.799(5) . ?
P2 C40 1.807(5) . ?
P1 C28 1.782(5) . ?
P1 C16 1.796(5) . ?
P1 C10 1.802(5) . ?
P1 C22 1.808(5) . ?
C27 C22 1.386(8) . ?
C27 C26 1.392(8) . ?
C27 H27 0.9500 . ?
N8 C5 1.345(11) . ?
N8 C9 1.443(13) . ?
C46 C51 1.396(7) . ?
C46 C47 1.397(7) . ?
N5 N6 1.308(8) . ?
N5 N4 1.361(10) . ?
C49 C50 1.380(8) . ?
C49 C48 1.393(8) . ?
C49 H49 0.9500 . ?
C52 C57 1.375(7) . ?
C52 C53 1.419(7) . ?
C29 C30 1.389(7) . ?
C29 C28 1.399(7) . ?
C29 H29 0.9500 . ?
C57 C56 1.380(7) . ?
C57 H57 0.9500 . ?
C10 C15 1.392(7) . ?
C10 C11 1.397(7) . ?
C28 C33 1.407(7) . ?
C48 C47 1.392(7) . ?
C48 H48 0.9500 . ?
C25 C24 1.381(8) . ?
C25 C26 1.389(8) . ?
C25 H25 0.9500 . ?
C44 C43 1.379(8) . ?
C44 C45 1.385(7) . ?
C44 H44 0.9500 . ?
C34 C39 1.397(7) . ?
C34 C35 1.397(7) . ?
C40 C45 1.391(7) . ?
C40 C41 1.408(7) . ?
C15 C14 1.387(7) . ?
C15 H15 0.9500 . ?
C51 C50 1.379(7) . ?
C51 H51 0.9500 . ?
N7 C4 1.332(10) . ?
N7 N6 1.377(10) . ?
C41 C42 1.381(7) . ?
C41 H41 0.9500 . ?
C45 H45 0.9500 . ?
C43 C42 1.395(8) . ?
C43 H43 0.9500 . ?
C19 C20 1.375(10) . ?
C19 C18 1.380(9) . ?
C19 H19 0.9500 . ?
C14 C13 1.391(8) . ?
C14 H14 0.9500 . ?
C38 C37 1.376(8) . ?
C38 C39 1.393(7) . ?
C38 H38 0.9500 . ?
C24 C23 1.386(7) . ?
C24 H24 0.9500 . ?
C37 C36 1.397(8) . ?
C37 H37 0.9500 . ?
C21 C16 1.401(8) . ?
C21 C20 1.401(8) . ?
C21 H21 0.9500 . ?
C33 C32 1.394(7) . ?
C33 H33 0.9500 . ?
C53 C54 1.381(7) . ?
C53 H53 0.9500 . ?
C47 H47 0.9500 . ?
C20 H20 0.9500 . ?
C35 C36 1.395(7) . ?
C35 H35 0.9500 . ?
C17 C18 1.383(8) . ?
C17 C16 1.393(8) . ?
C17 H17 0.9500 . ?
C31 C32 1.377(8) . ?
C31 C30 1.385(8) . ?
C31 H31 0.9500 . ?
C39 H39 0.9500 . ?
C11 C12 1.391(7) . ?
C11 H11 0.9500 . ?
N4 C4 1.358(9) . ?
C6 C5 1.388(11) . ?
C6 C7 1.455(16) . ?
C6 H6 0.9500 . ?
C54 C55 1.384(9) . ?
C54 H54 0.9500 . ?
C5 C4 1.439(12) . ?
C32 H32 0.9500 . ?
C13 C12 1.377(8) . ?
C13 H13 0.9500 . ?
C55 C56 1.377(9) . ?
C55 H55 0.9500 . ?
C23 C22 1.395(7) . ?
C23 H23 0.9500 . ?
C12 H12 0.9500 . ?
C56 H56 0.9500 . ?
C26 H26 0.9500 . ?
C7 C8 1.359(16) . ?
C7 H7 0.9500 . ?
C36 H36 0.9500 . ?
C8 C9 1.370(13) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
N3 C3 1.134(7) . ?
O2 H2WA 0.95(2) . ?
O2 H2WB 0.958(19) . ?
O3 H3WB 0.95(2) . ?
O3 H3WA 0.96(2) . ?
C42 H42 0.9500 . ?
N1 C1 1.141(7) . ?
C30 H30 0.9500 . ?
C50 H50 0.9500 . ?
C18 H18 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1A Mo1A N8 94.7(5) . . ?
O1A Mo1A C2A 104.5(5) . . ?
N8 Mo1A C2A 160.7(4) . . ?
O1A Mo1A C3 104.9(5) . . ?
N8 Mo1A C3 89.6(2) . . ?
C2A Mo1A C3 83.4(3) . . ?
O1A Mo1A C1 104.3(4) . . ?
N8 Mo1A C1 96.0(2) . . ?
C2A Mo1A C1 81.7(3) . . ?
C3 Mo1A C1 149.7(2) . . ?
O1A Mo1A N4 165.5(4) . . ?
N8 Mo1A N4 70.9(3) . . ?
C2A Mo1A N4 90.0(4) . . ?
C3 Mo1A N4 77.1(2) . . ?
C1 Mo1A N4 76.7(2) . . ?
N2A C2A Mo1A 176.6(10) . . ?
O1B Mo1B N4 114.4(5) . . ?
O1B Mo1B C2B 101.8(7) . . ?
N4 Mo1B C2B 143.7(6) . . ?
O1B Mo1B C3 100.3(5) . . ?
N4 Mo1B C3 87.5(2) . . ?
C2B Mo1B C3 87.2(6) . . ?
O1B Mo1B C1 102.1(5) . . ?
N4 Mo1B C1 87.0(2) . . ?
C2B Mo1B C1 84.3(6) . . ?
C3 Mo1B C1 157.3(2) . . ?
N2B C2B Mo1B 177.0(17) . . ?
C52 P2 C34 109.2(2) . . ?
C52 P2 C46 110.8(2) . . ?
C34 P2 C46 108.9(2) . . ?
C52 P2 C40 107.6(2) . . ?
C34 P2 C40 109.3(2) . . ?
C46 P2 C40 111.0(2) . . ?
C28 P1 C16 108.9(2) . . ?
C28 P1 C10 109.9(2) . . ?
C16 P1 C10 108.2(2) . . ?
C28 P1 C22 110.2(3) . . ?
C16 P1 C22 108.8(2) . . ?
C10 P1 C22 110.9(2) . . ?
C22 C27 C26 120.1(5) . . ?
C22 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C5 N8 C9 117.4(8) . . ?
C5 N8 Mo1A 126.0(7) . . ?
C9 N8 Mo1A 115.9(6) . . ?
C51 C46 C47 120.1(5) . . ?
C51 C46 P2 120.9(4) . . ?
C47 C46 P2 119.0(4) . . ?
N6 N5 N4 107.3(7) . . ?
C50 C49 C48 120.1(5) . . ?
C50 C49 H49 119.9 . . ?
C48 C49 H49 119.9 . . ?
C57 C52 C53 120.3(5) . . ?
C57 C52 P2 121.6(4) . . ?
C53 C52 P2 118.0(4) . . ?
C30 C29 C28 119.5(5) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C52 C57 C56 119.3(5) . . ?
C52 C57 H57 120.3 . . ?
C56 C57 H57 120.3 . . ?
C15 C10 C11 120.1(5) . . ?
C15 C10 P1 120.9(4) . . ?
C11 C10 P1 118.8(4) . . ?
C29 C28 C33 119.6(5) . . ?
C29 C28 P1 120.3(4) . . ?
C33 C28 P1 120.1(4) . . ?
C47 C48 C49 120.0(5) . . ?
C47 C48 H48 120.0 . . ?
C49 C48 H48 120.0 . . ?
C24 C25 C26 120.8(5) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C43 C44 C45 120.7(5) . . ?
C43 C44 H44 119.6 . . ?
C45 C44 H44 119.6 . . ?
C39 C34 C35 120.7(5) . . ?
C39 C34 P2 120.7(4) . . ?
C35 C34 P2 118.6(4) . . ?
C45 C40 C41 120.1(5) . . ?
C45 C40 P2 120.5(4) . . ?
C41 C40 P2 119.3(4) . . ?
C14 C15 C10 120.4(5) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
C50 C51 C46 119.8(5) . . ?
C50 C51 H51 120.1 . . ?
C46 C51 H51 120.1 . . ?
C4 N7 N6 105.3(6) . . ?
C42 C41 C40 119.8(5) . . ?
C42 C41 H41 120.1 . . ?
C40 C41 H41 120.1 . . ?
C44 C45 C40 119.3(5) . . ?
C44 C45 H45 120.3 . . ?
C40 C45 H45 120.3 . . ?
C44 C43 C42 120.4(5) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C20 C19 C18 120.0(6) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C15 C14 C13 119.1(5) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C37 C38 C39 120.3(5) . . ?
C37 C38 H38 119.9 . . ?
C39 C38 H38 119.9 . . ?
C25 C24 C23 119.9(5) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C38 C37 C36 120.8(5) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C16 C21 C20 118.7(6) . . ?
C16 C21 H21 120.7 . . ?
C20 C21 H21 120.7 . . ?
N5 N6 N7 110.6(8) . . ?
C32 C33 C28 119.6(5) . . ?
C32 C33 H33 120.2 . . ?
C28 C33 H33 120.2 . . ?
C54 C53 C52 119.4(5) . . ?
C54 C53 H53 120.3 . . ?
C52 C53 H53 120.3 . . ?
C48 C47 C46 119.4(5) . . ?
C48 C47 H47 120.3 . . ?
C46 C47 H47 120.3 . . ?
C19 C20 C21 120.6(6) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C36 C35 C34 119.3(5) . . ?
C36 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
C18 C17 C16 119.1(6) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C32 C31 C30 120.4(5) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C38 C39 C34 119.3(5) . . ?
C38 C39 H39 120.3 . . ?
C34 C39 H39 120.3 . . ?
C12 C11 C10 119.1(5) . . ?
C12 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
C4 N4 N5 107.3(6) . . ?
C4 N4 Mo1B 129.3(7) . . ?
N5 N4 Mo1B 123.3(5) . . ?
C4 N4 Mo1A 109.0(6) . . ?
N5 N4 Mo1A 143.3(5) . . ?
C5 C6 C7 118.6(10) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
C53 C54 C55 119.3(6) . . ?
C53 C54 H54 120.3 . . ?
C55 C54 H54 120.3 . . ?
N8 C5 C6 123.8(10) . . ?
N8 C5 C4 112.7(7) . . ?
C6 C5 C4 123.4(10) . . ?
C31 C32 C33 120.2(5) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C12 C13 C14 120.8(5) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C56 C55 C54 120.9(5) . . ?
C56 C55 H55 119.5 . . ?
C54 C55 H55 119.5 . . ?
C17 C16 C21 120.5(5) . . ?
C17 C16 P1 119.5(4) . . ?
C21 C16 P1 119.7(4) . . ?
C24 C23 C22 119.9(5) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C13 C12 C11 120.5(5) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C55 C56 C57 120.7(6) . . ?
C55 C56 H56 119.7 . . ?
C57 C56 H56 119.7 . . ?
N7 C4 N4 109.5(8) . . ?
N7 C4 C5 130.0(7) . . ?
N4 C4 C5 120.5(7) . . ?
C25 C26 C27 119.3(6) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
C27 C22 C23 120.0(5) . . ?
C27 C22 P1 121.4(4) . . ?
C23 C22 P1 118.5(4) . . ?
C8 C7 C6 117.1(10) . . ?
C8 C7 H7 121.5 . . ?
C6 C7 H7 121.5 . . ?
C35 C36 C37 119.6(5) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C7 C8 C9 123.6(12) . . ?
C7 C8 H8 118.2 . . ?
C9 C8 H8 118.2 . . ?
C8 C9 N8 119.6(10) . . ?
C8 C9 H9 120.2 . . ?
N8 C9 H9 120.2 . . ?
N3 C3 Mo1B 164.3(6) . . ?
N3 C3 Mo1A 172.0(6) . . ?
H2WA O2 H2WB 104(4) . . ?
H3WB O3 H3WA 105(4) . . ?
C41 C42 C43 119.7(5) . . ?
C41 C42 H42 120.2 . . ?
C43 C42 H42 120.2 . . ?
N1 C1 Mo1B 160.2(6) . . ?
N1 C1 Mo1A 175.9(6) . . ?
C31 C30 C29 120.6(5) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C51 C50 C49 120.5(5) . . ?
C51 C50 H50 119.7 . . ?
C49 C50 H50 119.7 . . ?
C19 C18 C17 121.1(6) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C52 P2 C46 C51 -9.7(5) . . . . ?
C34 P2 C46 C51 -129.8(4) . . . . ?
C40 P2 C46 C51 109.8(4) . . . . ?
C52 P2 C46 C47 170.8(4) . . . . ?
C34 P2 C46 C47 50.7(5) . . . . ?
C40 P2 C46 C47 -69.8(5) . . . . ?
C34 P2 C52 C57 8.2(5) . . . . ?
C46 P2 C52 C57 -111.8(5) . . . . ?
C40 P2 C52 C57 126.7(4) . . . . ?
C34 P2 C52 C53 -170.8(4) . . . . ?
C46 P2 C52 C53 69.2(5) . . . . ?
C40 P2 C52 C53 -52.3(5) . . . . ?
C53 C52 C57 C56 2.4(8) . . . . ?
P2 C52 C57 C56 -176.6(4) . . . . ?
C28 P1 C10 C15 10.7(5) . . . . ?
C16 P1 C10 C15 -108.0(4) . . . . ?
C22 P1 C10 C15 132.7(4) . . . . ?
C28 P1 C10 C11 -174.1(4) . . . . ?
C16 P1 C10 C11 67.1(5) . . . . ?
C22 P1 C10 C11 -52.1(5) . . . . ?
C30 C29 C28 C33 -1.5(8) . . . . ?
C30 C29 C28 P1 178.1(4) . . . . ?
C16 P1 C28 C29 173.5(4) . . . . ?
C10 P1 C28 C29 55.3(5) . . . . ?
C22 P1 C28 C29 -67.2(5) . . . . ?
C16 P1 C28 C33 -6.9(5) . . . . ?
C10 P1 C28 C33 -125.2(4) . . . . ?
C22 P1 C28 C33 112.4(4) . . . . ?
C50 C49 C48 C47 -0.8(9) . . . . ?
C52 P2 C34 C39 -97.6(4) . . . . ?
C46 P2 C34 C39 23.5(5) . . . . ?
C40 P2 C34 C39 145.0(4) . . . . ?
C52 P2 C34 C35 79.4(4) . . . . ?
C46 P2 C34 C35 -159.5(4) . . . . ?
C40 P2 C34 C35 -38.0(5) . . . . ?
C52 P2 C40 C45 151.9(4) . . . . ?
C34 P2 C40 C45 -89.7(4) . . . . ?
C46 P2 C40 C45 30.5(5) . . . . ?
C52 P2 C40 C41 -32.0(5) . . . . ?
C34 P2 C40 C41 86.4(4) . . . . ?
C46 P2 C40 C41 -153.4(4) . . . . ?
C11 C10 C15 C14 0.1(8) . . . . ?
P1 C10 C15 C14 175.2(4) . . . . ?
C47 C46 C51 C50 1.9(8) . . . . ?
P2 C46 C51 C50 -177.7(4) . . . . ?
C45 C40 C41 C42 1.2(8) . . . . ?
P2 C40 C41 C42 -174.9(4) . . . . ?
C43 C44 C45 C40 -0.4(8) . . . . ?
C41 C40 C45 C44 -0.3(7) . . . . ?
P2 C40 C45 C44 175.8(4) . . . . ?
C45 C44 C43 C42 0.2(8) . . . . ?
C10 C15 C14 C13 -1.1(8) . . . . ?
C26 C25 C24 C23 -0.2(8) . . . . ?
C39 C38 C37 C36 0.4(8) . . . . ?
N4 N5 N6 N7 1.4(7) . . . . ?
C4 N7 N6 N5 -0.4(8) . . . . ?
C29 C28 C33 C32 0.7(8) . . . . ?
P1 C28 C33 C32 -178.9(4) . . . . ?
C57 C52 C53 C54 -0.8(8) . . . . ?
P2 C52 C53 C54 178.3(4) . . . . ?
C49 C48 C47 C46 2.7(8) . . . . ?
C51 C46 C47 C48 -3.2(8) . . . . ?
P2 C46 C47 C48 176.3(4) . . . . ?
C18 C19 C20 C21 -2.9(10) . . . . ?
C16 C21 C20 C19 2.1(9) . . . . ?
C39 C34 C35 C36 0.5(8) . . . . ?
P2 C34 C35 C36 -176.6(4) . . . . ?
C37 C38 C39 C34 -1.1(8) . . . . ?
C35 C34 C39 C38 0.6(8) . . . . ?
P2 C34 C39 C38 177.6(4) . . . . ?
C15 C10 C11 C12 1.5(8) . . . . ?
P1 C10 C11 C12 -173.8(4) . . . . ?
N6 N5 N4 C4 -1.7(7) . . . . ?
N6 N5 N4 Mo1B -178.9(4) . . . . ?
N6 N5 N4 Mo1A -172.6(5) . . . . ?
C52 C53 C54 C55 -1.2(9) . . . . ?
C9 N8 C5 C6 1.0(11) . . . . ?
Mo1A N8 C5 C6 171.3(6) . . . . ?
C9 N8 C5 C4 178.2(6) . . . . ?
Mo1A N8 C5 C4 -11.5(9) . . . . ?
C7 C6 C5 N8 -1.5(12) . . . . ?
C7 C6 C5 C4 -178.4(7) . . . . ?
C30 C31 C32 C33 -1.7(9) . . . . ?
C28 C33 C32 C31 0.9(8) . . . . ?
C15 C14 C13 C12 0.5(9) . . . . ?
C53 C54 C55 C56 1.5(9) . . . . ?
C18 C17 C16 C21 -0.4(8) . . . . ?
C18 C17 C16 P1 174.2(4) . . . . ?
C20 C21 C16 C17 -0.4(8) . . . . ?
C20 C21 C16 P1 -175.1(4) . . . . ?
C28 P1 C16 C17 -89.1(4) . . . . ?
C10 P1 C16 C17 30.2(5) . . . . ?
C22 P1 C16 C17 150.8(4) . . . . ?
C28 P1 C16 C21 85.6(5) . . . . ?
C10 P1 C16 C21 -155.0(4) . . . . ?
C22 P1 C16 C21 -34.5(5) . . . . ?
C25 C24 C23 C22 0.4(8) . . . . ?
C14 C13 C12 C11 1.1(9) . . . . ?
C10 C11 C12 C13 -2.1(9) . . . . ?
C54 C55 C56 C57 0.1(9) . . . . ?
C52 C57 C56 C55 -2.1(9) . . . . ?
N6 N7 C4 N4 -0.7(7) . . . . ?
N6 N7 C4 C5 177.6(7) . . . . ?
N5 N4 C4 N7 1.5(7) . . . . ?
Mo1B N4 C4 N7 178.4(4) . . . . ?
Mo1A N4 C4 N7 175.8(4) . . . . ?
N5 N4 C4 C5 -177.0(6) . . . . ?
Mo1B N4 C4 C5 -0.1(9) . . . . ?
Mo1A N4 C4 C5 -2.7(8) . . . . ?
N8 C5 C4 N7 -169.7(7) . . . . ?
C6 C5 C4 N7 7.5(13) . . . . ?
N8 C5 C4 N4 8.5(9) . . . . ?
C6 C5 C4 N4 -174.3(7) . . . . ?
C24 C25 C26 C27 -0.7(9) . . . . ?
C22 C27 C26 C25 1.4(9) . . . . ?
C26 C27 C22 C23 -1.2(8) . . . . ?
C26 C27 C22 P1 178.4(4) . . . . ?
C24 C23 C22 C27 0.3(8) . . . . ?
C24 C23 C22 P1 -179.3(4) . . . . ?
C28 P1 C22 C27 21.0(5) . . . . ?
C16 P1 C22 C27 140.3(4) . . . . ?
C10 P1 C22 C27 -100.8(5) . . . . ?
C28 P1 C22 C23 -159.4(4) . . . . ?
C16 P1 C22 C23 -40.1(5) . . . . ?
C10 P1 C22 C23 78.8(5) . . . . ?
C5 C6 C7 C8 1.3(13) . . . . ?
C34 C35 C36 C37 -1.1(8) . . . . ?
C38 C37 C36 C35 0.7(8) . . . . ?
C6 C7 C8 C9 -0.7(14) . . . . ?
C7 C8 C9 N8 0.3(13) . . . . ?
C5 N8 C9 C8 -0.3(10) . . . . ?
Mo1A N8 C9 C8 -171.7(6) . . . . ?
C40 C41 C42 C43 -1.4(8) . . . . ?
C44 C43 C42 C41 0.7(8) . . . . ?
C32 C31 C30 C29 0.9(9) . . . . ?
C28 C29 C30 C31 0.7(9) . . . . ?
C46 C51 C50 C49 0.0(8) . . . . ?
C48 C49 C50 C51 -0.6(9) . . . . ?
C20 C19 C18 C17 2.1(9) . . . . ?
C16 C17 C18 C19 -0.4(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C45 H45 N3 0.95 2.46 3.227(7) 137.3 2_566 y
C8 H8 N2B 0.95 2.17 2.88(2) 130.8 2_567 y
C9 H9 N2B 0.95 2.55 3.051(19) 112.9 2_567 y
C9 H9 O1A 0.95 2.38 2.894(17) 113.8 . y
O2 H2WA O3 0.95(2) 1.82(2) 2.776(6) 177(7) 2_576 y
O2 H2WB N1 0.958(19) 1.91(2) 2.850(7) 167(6) . y
O3 H3WB N5 0.95(2) 2.68(6) 3.394(7) 132(6) . y
O3 H3WB N7 0.95(2) 2.67(3) 3.614(7) 170(7) . y
O3 H3WB N6 0.95(2) 2.12(4) 3.013(7) 155(7) . y
O3 H3WA O2 0.96(2) 1.90(4) 2.800(6) 156(8) . y

_refine_diff_density_max         0.750
_refine_diff_density_min         -1.234
_refine_diff_density_rms         0.101


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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1523850'
_audit_update_record             
;
2016-12-21 deposited with the CCDC.
2017-02-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C57 H48 N8 O3.34 P2 W'
_chemical_formula_weight         1144.30

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

_space_group_crystal_system      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                   13.365(5)
_cell_length_b                   13.484(5)
_cell_length_c                   16.718(5)
_cell_angle_alpha                70.768(5)
_cell_angle_beta                 88.204(5)
_cell_angle_gamma                63.024(5)
_cell_volume                     2510.1(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    15979
_cell_measurement_theta_min      3.1880
_cell_measurement_theta_max      29.4530

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_F_000             1153
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.420
_shelx_estimated_absorpt_T_min   0.531
_shelx_estimated_absorpt_T_max   0.794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      125(3)
_diffrn_measurement_method       'ω scans'
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.3756
_diffrn_reflns_number            40286
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.918
_diffrn_reflns_theta_max         30.085
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             13585
_reflns_number_gt                11618
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+4.0956P] 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         13585
_refine_ls_number_parameters     676
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.0828
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_restrained_S_all      1.198
_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
P2 P 0.69888(7) 0.35763(7) 0.15859(6) 0.01653(18) Uani 1 1 d . . . . .
P1 P 0.99392(7) 0.43087(7) 0.69309(5) 0.01490(17) Uani 1 1 d . . . . .
N1 N 0.1847(3) 0.2578(3) 0.1586(2) 0.0300(7) Uani 1 1 d . . . . .
O1 O 0.3374(2) -0.0024(2) 0.05752(18) 0.0359(7) Uani 1 1 d . . . . .
C8 C 0.6470(4) -0.0193(4) 0.1531(3) 0.0433(11) Uani 1 1 d . . . . .
H8 H 0.6935 -0.0118 0.1098 0.052 Uiso 1 1 calc R U . . .
C2 C 0.1484(3) -0.0056(3) 0.1641(2) 0.0268(8) Uani 1 1 d . . . . .
N3 N 0.3928(3) -0.3065(3) 0.2494(2) 0.0257(7) Uani 1 1 d . . . . .
C57 C 0.7685(3) 0.5293(3) 0.1030(2) 0.0220(7) Uani 1 1 d . . . . .
H57 H 0.8432 0.4644 0.1187 0.026 Uiso 1 1 calc R U . . .
C14 C 0.6998(3) 0.6988(3) 0.5427(2) 0.0262(8) Uani 1 1 d . . . . .
H14 H 0.6416 0.7074 0.5056 0.031 Uiso 1 1 calc R U . . .
C30 C 1.0436(3) 0.2277(3) 0.9446(2) 0.0243(8) Uani 1 1 d . . . . .
H30 H 1.0782 0.1454 0.9785 0.029 Uiso 1 1 calc R U . . .
C12 C 0.7795(3) 0.7864(3) 0.6063(2) 0.0250(8) Uani 1 1 d . . . . .
H12 H 0.7757 0.8550 0.6135 0.030 Uiso 1 1 calc R U . . .
C32 C 0.9452(3) 0.4312(3) 0.9347(2) 0.0239(8) Uani 1 1 d . . . . .
H32 H 0.9121 0.4883 0.9618 0.029 Uiso 1 1 calc R U . . .
N7 N 0.4433(3) -0.0865(3) 0.4199(2) 0.0383(9) Uani 1 1 d . . . . .
C34 C 0.8077(3) 0.2700(3) 0.2501(2) 0.0184(7) Uani 1 1 d . . . . .
C28 C 0.9881(3) 0.3851(3) 0.8063(2) 0.0171(7) Uani 1 1 d . . . . .
C17 C 0.9064(3) 0.2873(3) 0.6770(2) 0.0254(8) Uani 1 1 d . . . . .
H17 H 0.8491 0.3252 0.7076 0.031 Uiso 1 1 calc R U . . .
C10 C 0.8769(3) 0.5746(3) 0.6365(2) 0.0171(7) Uani 1 1 d . . . . .
N2 N 0.0613(3) -0.0006(3) 0.1612(2) 0.0391(9) Uani 1 1 d . . . . .
C7 C 0.6785(4) -0.0298(4) 0.2343(3) 0.0480(13) Uani 1 1 d . . . . .
H7 H 0.7458 -0.0273 0.2473 0.058 Uiso 1 1 calc R U . . .
N6 N 0.3470(3) -0.0955(3) 0.4425(2) 0.0403(9) Uani 1 1 d . . . . .
N5 N 0.2829(3) -0.0751(3) 0.3736(2) 0.0351(8) Uani 1 1 d . . . . .
C52 C 0.6748(3) 0.5089(3) 0.1192(2) 0.0174(7) Uani 1 1 d . . . . .
C29 C 1.0395(3) 0.2634(3) 0.8558(2) 0.0221(7) Uani 1 1 d . . . . .
H29 H 1.0713 0.2057 0.8291 0.026 Uiso 1 1 calc R U . . .
C31 C 0.9975(3) 0.3116(3) 0.9832(2) 0.0249(8) Uani 1 1 d . . . . .
H31 H 1.0018 0.2868 1.0438 0.030 Uiso 1 1 calc R U . . .
C16 C 0.9924(3) 0.3202(3) 0.6568(2) 0.0193(7) Uani 1 1 d . . . . .
C46 C 0.7431(3) 0.2988(3) 0.0744(2) 0.0194(7) Uani 1 1 d . . . . .
C54 C 0.5502(3) 0.7196(3) 0.0584(2) 0.0258(8) Uani 1 1 d . . . . .
H54 H 0.4758 0.7849 0.0437 0.031 Uiso 1 1 calc R U . . .
C35 C 0.9219(3) 0.2231(3) 0.2379(2) 0.0237(8) Uani 1 1 d . . . . .
H35 H 0.9417 0.2359 0.1817 0.028 Uiso 1 1 calc R U . . .
C25 C 1.3286(3) 0.4388(3) 0.6411(2) 0.0266(8) Uani 1 1 d . . . . .
H25 H 1.3987 0.4390 0.6302 0.032 Uiso 1 1 calc R U . . .
C33 C 0.9408(3) 0.4687(3) 0.8462(2) 0.0195(7) Uani 1 1 d . . . . .
H33 H 0.9055 0.5513 0.8131 0.023 Uiso 1 1 calc R U . . .
C45 C 0.5303(3) 0.2942(3) 0.1517(2) 0.0232(8) Uani 1 1 d . . . . .
H45 H 0.5705 0.2584 0.1125 0.028 Uiso 1 1 calc R U . . .
C11 C 0.8713(3) 0.6759(3) 0.6474(2) 0.0205(7) Uani 1 1 d . . . . .
H11 H 0.9302 0.6686 0.6829 0.025 Uiso 1 1 calc R U . . .
C15 C 0.7900(3) 0.5867(3) 0.5838(2) 0.0208(7) Uani 1 1 d . . . . .
H15 H 0.7927 0.5189 0.5762 0.025 Uiso 1 1 calc R U . . .
C53 C 0.5657(3) 0.6050(3) 0.0965(2) 0.0228(8) Uani 1 1 d . . . . .
H53 H 0.5019 0.5915 0.1071 0.027 Uiso 1 1 calc R U . . .
C13 C 0.6932(3) 0.7976(3) 0.5546(2) 0.0270(8) Uani 1 1 d . . . . .
H13 H 0.6296 0.8734 0.5275 0.032 Uiso 1 1 calc R U . . .
C41 C 0.5089(3) 0.4076(3) 0.2430(2) 0.0229(8) Uani 1 1 d . . . . .
H41 H 0.5342 0.4496 0.2657 0.027 Uiso 1 1 calc R U . . .
C22 C 1.1238(3) 0.4381(3) 0.6739(2) 0.0167(7) Uani 1 1 d . . . . .
N4 N 0.3371(3) -0.0518(3) 0.3049(2) 0.0295(7) Uani 1 1 d . . . . .
C40 C 0.5701(3) 0.3531(3) 0.1859(2) 0.0188(7) Uani 1 1 d . . . . .
C20 C 1.0761(4) 0.1755(3) 0.5890(3) 0.0339(9) Uani 1 1 d . . . . .
H20 H 1.1342 0.1362 0.5594 0.041 Uiso 1 1 calc R U . . .
C49 C 0.7960(3) 0.2082(4) -0.0568(3) 0.0331(9) Uani 1 1 d . . . . .
H49 H 0.8133 0.1771 -0.1017 0.040 Uiso 1 1 calc R U . . .
C51 C 0.7067(3) 0.3761(3) -0.0109(2) 0.0223(7) Uani 1 1 d . . . . .
H51 H 0.6641 0.4596 -0.0242 0.027 Uiso 1 1 calc R U . . .
C27 C 1.2226(3) 0.3543(3) 0.7314(2) 0.0219(7) Uani 1 1 d . . . . .
H27 H 1.2198 0.2972 0.7818 0.026 Uiso 1 1 calc R U . . .
C37 C 0.9779(3) 0.1409(3) 0.3901(2) 0.0287(8) Uani 1 1 d . . . . .
H37 H 1.0359 0.0980 0.4379 0.034 Uiso 1 1 calc R U . . .
N8 N 0.4776(3) -0.0319(3) 0.1953(2) 0.0327(8) Uani 1 1 d . . . . .
C50 C 0.7337(3) 0.3295(4) -0.0756(3) 0.0306(9) Uani 1 1 d . . . . .
H50 H 0.7091 0.3814 -0.1336 0.037 Uiso 1 1 calc R U . . .
C48 C 0.8333(3) 0.1322(4) 0.0275(3) 0.0327(9) Uani 1 1 d . . . . .
H48 H 0.8774 0.0490 0.0401 0.039 Uiso 1 1 calc R U . . .
C44 C 0.4319(3) 0.2878(3) 0.1746(3) 0.0288(9) Uani 1 1 d . . . . .
H44 H 0.4047 0.2479 0.1510 0.035 Uiso 1 1 calc R U . . .
C47 C 0.8070(3) 0.1761(3) 0.0937(3) 0.0257(8) Uani 1 1 d . . . . .
H47 H 0.8322 0.1235 0.1515 0.031 Uiso 1 1 calc R U . . .
C26 C 1.3244(3) 0.3547(3) 0.7146(2) 0.0258(8) Uani 1 1 d . . . . .
H26 H 1.3917 0.2973 0.7534 0.031 Uiso 1 1 calc R U . . .
C56 C 0.7519(3) 0.6446(3) 0.0638(2) 0.0257(8) Uani 1 1 d . . . . .
H56 H 0.8152 0.6588 0.0521 0.031 Uiso 1 1 calc R U . . .
C23 C 1.1285(3) 0.5219(3) 0.6001(2) 0.0223(7) Uani 1 1 d . . . . .
H23 H 1.0616 0.5789 0.5608 0.027 Uiso 1 1 calc R U . . .
C24 C 1.2316(3) 0.5219(3) 0.5840(2) 0.0280(8) Uani 1 1 d . . . . .
H24 H 1.2350 0.5790 0.5338 0.034 Uiso 1 1 calc R U . . .
C39 C 0.7804(3) 0.2500(4) 0.3330(2) 0.0318(9) Uani 1 1 d . . . . .
H39 H 0.7032 0.2803 0.3420 0.038 Uiso 1 1 calc R U . . .
C21 C 1.0766(3) 0.2648(3) 0.6123(2) 0.0240(8) Uani 1 1 d . . . . .
H21 H 1.1340 0.2880 0.5979 0.029 Uiso 1 1 calc R U . . .
C55 C 0.6429(3) 0.7394(3) 0.0418(2) 0.0267(8) Uani 1 1 d . . . . .
H55 H 0.6319 0.8183 0.0151 0.032 Uiso 1 1 calc R U . . .
C38 C 0.8650(4) 0.1863(4) 0.4022(3) 0.0356(10) Uani 1 1 d . . . . .
H38 H 0.8457 0.1735 0.4586 0.043 Uiso 1 1 calc R U . . .
C1 C 0.2302(3) 0.1621(3) 0.1589(2) 0.0250(8) Uani 1 1 d . . . . .
C6 C 0.6105(4) -0.0440(4) 0.2968(3) 0.0446(12) Uani 1 1 d . . . . .
H6 H 0.6318 -0.0534 0.3535 0.054 Uiso 1 1 calc R U . . .
C18 C 0.9056(4) 0.1992(4) 0.6519(3) 0.0338(9) Uani 1 1 d . . . . .
H18 H 0.8469 0.1774 0.6641 0.041 Uiso 1 1 calc R U . . .
C43 C 0.3739(3) 0.3394(3) 0.2319(3) 0.0308(9) Uani 1 1 d . . . . .
H43 H 0.3073 0.3339 0.2482 0.037 Uiso 1 1 calc R U . . .
C5 C 0.5108(3) -0.0445(3) 0.2759(3) 0.0344(10) Uani 1 1 d . . . . .
C36 C 1.0059(3) 0.1581(3) 0.3081(2) 0.0266(8) Uani 1 1 d . . . . .
H36 H 1.0833 0.1251 0.2999 0.032 Uiso 1 1 calc R U . . .
C42 C 0.4118(3) 0.3993(3) 0.2659(3) 0.0289(9) Uani 1 1 d . . . . .
H42 H 0.3709 0.4348 0.3051 0.035 Uiso 1 1 calc R U . . .
C19 C 0.9913(4) 0.1435(4) 0.6087(2) 0.0371(10) Uani 1 1 d . . . . .
H19 H 0.9917 0.0821 0.5924 0.045 Uiso 1 1 calc R U . . .
C4 C 0.4330(3) -0.0599(3) 0.3357(3) 0.0326(9) Uani 1 1 d . . . . .
C3 C 0.3690(3) -0.2080(3) 0.2180(2) 0.0230(8) Uani 1 1 d . . . . .
C9 C 0.5478(4) -0.0198(3) 0.1353(3) 0.0365(10) Uani 1 1 d . . . . .
H9 H 0.5266 -0.0115 0.0788 0.044 Uiso 1 1 calc R U . . .
W1A W 0.31479(2) -0.01932(2) 0.16179(2) 0.01869(6) Uani 0.8838(9) 1 d . . P A 1
O3 O 0.4115(3) 0.6457(3) 0.5308(2) 0.0384(7) Uani 1 1 d D . . . .
W1B W 0.26019(15) -0.01857(11) 0.19545(11) 0.0246(6) Uani 0.1162(9) 1 d . . P A
2
O2 O 0.3759(3) 0.5514(3) 0.41417(19) 0.0363(7) Uani 1 1 d D . . . .
O10 O 0.6553(13) 0.0862(11) 0.3966(8) 0.094(7) Uani 0.344(12) 1 d . . . . .
H3B H 0.391(5) 0.632(4) 0.484(2) 0.08(2) Uiso 1 1 d D . . . .
H3A H 0.393(4) 0.725(2) 0.514(3) 0.067(17) Uiso 1 1 d D . . . .
H2A H 0.385(4) 0.592(4) 0.3589(17) 0.063(16) Uiso 1 1 d D . . . .
H2B H 0.444(4) 0.479(4) 0.435(4) 0.16(3) Uiso 1 1 d 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
P2 C40 1.790(3) . ?
P2 C46 1.794(3) . ?
P2 C52 1.797(3) . ?
P2 C34 1.800(4) . ?
P1 C16 1.794(4) . ?
P1 C22 1.795(3) . ?
P1 C10 1.798(3) . ?
P1 C28 1.799(3) . ?
N1 C1 1.148(5) . ?
O1 W1A 1.717(3) . ?
O1 W1B 2.481(4) . ?
C8 C9 1.371(6) . ?
C8 C7 1.377(7) . ?
C8 H8 0.9500 . ?
C2 N2 1.137(5) . ?
C2 W1B 1.513(4) . ?
C2 W1A 2.147(4) . ?
N3 C3 1.144(4) . ?
C57 C56 1.386(5) . ?
C57 C52 1.400(4) . ?
C57 H57 0.9500 . ?
C14 C13 1.375(5) . ?
C14 C15 1.387(5) . ?
C14 H14 0.9500 . ?
C30 C31 1.379(5) . ?
C30 C29 1.395(5) . ?
C30 H30 0.9500 . ?
C12 C11 1.385(5) . ?
C12 C13 1.385(5) . ?
C12 H12 0.9500 . ?
C32 C31 1.378(5) . ?
C32 C33 1.389(5) . ?
C32 H32 0.9500 . ?
N7 C4 1.327(5) . ?
N7 N6 1.376(5) . ?
C34 C39 1.393(5) . ?
C34 C35 1.400(5) . ?
C28 C33 1.392(5) . ?
C28 C29 1.404(5) . ?
C17 C18 1.389(5) . ?
C17 C16 1.403(5) . ?
C17 H17 0.9500 . ?
C10 C15 1.395(5) . ?
C10 C11 1.406(5) . ?
C7 C6 1.385(7) . ?
C7 H7 0.9500 . ?
N6 N5 1.332(5) . ?
N5 N4 1.364(5) . ?
C52 C53 1.395(5) . ?
C29 H29 0.9500 . ?
C31 H31 0.9500 . ?
C16 C21 1.390(5) . ?
C46 C47 1.398(5) . ?
C46 C51 1.401(5) . ?
C54 C53 1.381(5) . ?
C54 C55 1.384(5) . ?
C54 H54 0.9500 . ?
C35 C36 1.386(5) . ?
C35 H35 0.9500 . ?
C25 C24 1.379(5) . ?
C25 C26 1.391(5) . ?
C25 H25 0.9500 . ?
C33 H33 0.9500 . ?
C45 C44 1.391(5) . ?
C45 C40 1.394(5) . ?
C45 H45 0.9500 . ?
C11 H11 0.9500 . ?
C15 H15 0.9500 . ?
C53 H53 0.9500 . ?
C13 H13 0.9500 . ?
C41 C42 1.384(5) . ?
C41 C40 1.410(5) . ?
C41 H41 0.9500 . ?
C22 C23 1.394(5) . ?
C22 C27 1.398(5) . ?
N4 C4 1.340(5) . ?
N4 W1B 1.940(4) . ?
N4 W1A 2.289(3) . ?
C20 C19 1.381(6) . ?
C20 C21 1.385(5) . ?
C20 H20 0.9500 . ?
C49 C50 1.381(6) . ?
C49 C48 1.383(6) . ?
C49 H49 0.9500 . ?
C51 C50 1.383(5) . ?
C51 H51 0.9500 . ?
C27 C26 1.383(5) . ?
C27 H27 0.9500 . ?
C37 C36 1.381(5) . ?
C37 C38 1.386(5) . ?
C37 H37 0.9500 . ?
N8 C5 1.364(5) . ?
N8 C9 1.373(5) . ?
N8 W1A 2.182(3) . ?
C50 H50 0.9500 . ?
C48 C47 1.385(5) . ?
C48 H48 0.9500 . ?
C44 C43 1.381(5) . ?
C44 H44 0.9500 . ?
C47 H47 0.9500 . ?
C26 H26 0.9500 . ?
C56 C55 1.388(5) . ?
C56 H56 0.9500 . ?
C23 C24 1.396(5) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C39 C38 1.378(6) . ?
C39 H39 0.9500 . ?
C21 H21 0.9500 . ?
C55 H55 0.9500 . ?
C38 H38 0.9500 . ?
C1 W1B 2.149(4) . ?
C1 W1A 2.164(4) . ?
C6 C5 1.391(6) . ?
C6 H6 0.9500 . ?
C18 C19 1.387(6) . ?
C18 H18 0.9500 . ?
C43 C42 1.387(6) . ?
C43 H43 0.9500 . ?
C5 C4 1.456(6) . ?
C36 H36 0.9500 . ?
C42 H42 0.9500 . ?
C19 H19 0.9500 . ?
C3 W1A 2.162(4) . ?
C3 W1B 2.193(4) . ?
C9 H9 0.9500 . ?
O3 H3B 0.939(19) . ?
O3 H3A 0.927(19) . ?
O2 H2A 0.942(19) . ?
O2 H2B 0.95(2) . ?

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
C40 P2 C46 108.44(16) . . ?
C40 P2 C52 110.06(15) . . ?
C46 P2 C52 107.89(16) . . ?
C40 P2 C34 110.35(16) . . ?
C46 P2 C34 109.63(16) . . ?
C52 P2 C34 110.41(16) . . ?
C16 P1 C22 109.14(16) . . ?
C16 P1 C10 110.65(16) . . ?
C22 P1 C10 108.74(15) . . ?
C16 P1 C28 107.57(15) . . ?
C22 P1 C28 109.23(16) . . ?
C10 P1 C28 111.47(15) . . ?
C9 C8 C7 119.4(5) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
N2 C2 W1B 163.1(4) . . ?
N2 C2 W1A 175.8(4) . . ?
C56 C57 C52 119.6(3) . . ?
C56 C57 H57 120.2 . . ?
C52 C57 H57 120.2 . . ?
C13 C14 C15 121.0(4) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C31 C30 C29 120.1(3) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C11 C12 C13 120.4(3) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C31 C32 C33 120.3(3) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C4 N7 N6 104.1(3) . . ?
C39 C34 C35 119.2(3) . . ?
C39 C34 P2 121.2(3) . . ?
C35 C34 P2 119.6(3) . . ?
C33 C28 C29 119.7(3) . . ?
C33 C28 P1 120.8(3) . . ?
C29 C28 P1 119.4(3) . . ?
C18 C17 C16 119.7(4) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C15 C10 C11 119.5(3) . . ?
C15 C10 P1 121.0(3) . . ?
C11 C10 P1 119.4(3) . . ?
C8 C7 C6 119.0(4) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
N5 N6 N7 110.3(4) . . ?
N6 N5 N4 107.2(3) . . ?
C53 C52 C57 119.6(3) . . ?
C53 C52 P2 121.8(3) . . ?
C57 C52 P2 118.2(3) . . ?
C30 C29 C28 119.5(3) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C32 C31 C30 120.5(3) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C21 C16 C17 120.3(3) . . ?
C21 C16 P1 121.0(3) . . ?
C17 C16 P1 118.7(3) . . ?
C47 C46 C51 120.3(3) . . ?
C47 C46 P2 120.2(3) . . ?
C51 C46 P2 119.4(3) . . ?
C53 C54 C55 120.0(3) . . ?
C53 C54 H54 120.0 . . ?
C55 C54 H54 120.0 . . ?
C36 C35 C34 119.8(3) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C24 C25 C26 120.4(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C32 C33 C28 119.9(3) . . ?
C32 C33 H33 120.1 . . ?
C28 C33 H33 120.1 . . ?
C44 C45 C40 120.2(3) . . ?
C44 C45 H45 119.9 . . ?
C40 C45 H45 119.9 . . ?
C12 C11 C10 119.7(3) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C14 C15 C10 119.4(3) . . ?
C14 C15 H15 120.3 . . ?
C10 C15 H15 120.3 . . ?
C54 C53 C52 120.2(3) . . ?
C54 C53 H53 119.9 . . ?
C52 C53 H53 119.9 . . ?
C14 C13 C12 119.8(3) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C42 C41 C40 119.6(3) . . ?
C42 C41 H41 120.2 . . ?
C40 C41 H41 120.2 . . ?
C23 C22 C27 119.7(3) . . ?
C23 C22 P1 120.8(3) . . ?
C27 C22 P1 119.4(3) . . ?
C4 N4 N5 106.1(3) . . ?
C4 N4 W1B 138.5(3) . . ?
N5 N4 W1B 115.4(3) . . ?
C4 N4 W1A 115.8(3) . . ?
N5 N4 W1A 137.8(3) . . ?
C45 C40 C41 119.5(3) . . ?
C45 C40 P2 120.1(3) . . ?
C41 C40 P2 120.4(3) . . ?
C19 C20 C21 120.1(4) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C50 C49 C48 120.0(4) . . ?
C50 C49 H49 120.0 . . ?
C48 C49 H49 120.0 . . ?
C50 C51 C46 119.2(3) . . ?
C50 C51 H51 120.4 . . ?
C46 C51 H51 120.4 . . ?
C26 C27 C22 119.9(3) . . ?
C26 C27 H27 120.1 . . ?
C22 C27 H27 120.1 . . ?
C36 C37 C38 119.7(4) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
C5 N8 C9 117.0(4) . . ?
C5 N8 W1A 121.2(3) . . ?
C9 N8 W1A 121.7(3) . . ?
C49 C50 C51 120.7(4) . . ?
C49 C50 H50 119.7 . . ?
C51 C50 H50 119.7 . . ?
C49 C48 C47 120.7(4) . . ?
C49 C48 H48 119.7 . . ?
C47 C48 H48 119.7 . . ?
C43 C44 C45 119.8(4) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C48 C47 C46 119.2(4) . . ?
C48 C47 H47 120.4 . . ?
C46 C47 H47 120.4 . . ?
C27 C26 C25 120.2(3) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C57 C56 C55 120.1(3) . . ?
C57 C56 H56 119.9 . . ?
C55 C56 H56 119.9 . . ?
C22 C23 C24 120.0(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 119.9(3) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C38 C39 C34 120.3(4) . . ?
C38 C39 H39 119.9 . . ?
C34 C39 H39 119.9 . . ?
C20 C21 C16 119.5(4) . . ?
C20 C21 H21 120.2 . . ?
C16 C21 H21 120.2 . . ?
C54 C55 C56 120.4(3) . . ?
C54 C55 H55 119.8 . . ?
C56 C55 H55 119.8 . . ?
C39 C38 C37 120.4(4) . . ?
C39 C38 H38 119.8 . . ?
C37 C38 H38 119.8 . . ?
N1 C1 W1B 154.7(3) . . ?
N1 C1 W1A 178.9(4) . . ?
C7 C6 C5 119.6(5) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C19 C18 C17 119.2(4) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C44 C43 C42 120.7(3) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
N8 C5 C6 121.9(4) . . ?
N8 C5 C4 113.2(4) . . ?
C6 C5 C4 124.9(4) . . ?
C37 C36 C35 120.5(4) . . ?
C37 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C41 C42 C43 120.2(4) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C20 C19 C18 121.2(4) . . ?
C20 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
N7 C4 N4 112.2(4) . . ?
N7 C4 C5 129.8(4) . . ?
N4 C4 C5 117.9(4) . . ?
N3 C3 W1A 176.7(3) . . ?
N3 C3 W1B 152.7(3) . . ?
C8 C9 N8 123.1(4) . . ?
C8 C9 H9 118.5 . . ?
N8 C9 H9 118.5 . . ?
O1 W1A C2 103.87(15) . . ?
O1 W1A C3 102.03(13) . . ?
C2 W1A C3 83.29(13) . . ?
O1 W1A C1 102.85(13) . . ?
C2 W1A C1 84.68(13) . . ?
C3 W1A C1 154.32(14) . . ?
O1 W1A N8 91.97(14) . . ?
C2 W1A N8 163.99(14) . . ?
C3 W1A N8 95.83(12) . . ?
C1 W1A N8 89.60(12) . . ?
O1 W1A N4 163.58(13) . . ?
C2 W1A N4 92.48(13) . . ?
C3 W1A N4 78.17(12) . . ?
C1 W1A N4 79.78(12) . . ?
N8 W1A N4 71.75(13) . . ?
H3B O3 H3A 109(3) . . ?
C2 W1B N4 135.9(2) . . ?
C2 W1B C1 103.49(18) . . ?
N4 W1B C1 88.48(14) . . ?
C2 W1B C3 99.52(18) . . ?
N4 W1B C3 85.36(14) . . ?
C1 W1B C3 152.48(17) . . ?
C2 W1B O1 96.73(19) . . ?
N4 W1B O1 127.13(15) . . ?
C1 W1B O1 81.97(13) . . ?
C3 W1B O1 80.53(13) . . ?
H2A O2 H2B 106(4) . . ?

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
C40 P2 C34 C39 -25.9(4) . . . . ?
C46 P2 C34 C39 -145.3(3) . . . . ?
C52 P2 C34 C39 96.0(3) . . . . ?
C40 P2 C34 C35 155.5(3) . . . . ?
C46 P2 C34 C35 36.1(3) . . . . ?
C52 P2 C34 C35 -82.7(3) . . . . ?
C16 P1 C28 C33 -152.3(3) . . . . ?
C22 P1 C28 C33 89.3(3) . . . . ?
C10 P1 C28 C33 -30.9(3) . . . . ?
C16 P1 C28 C29 32.5(3) . . . . ?
C22 P1 C28 C29 -85.9(3) . . . . ?
C10 P1 C28 C29 154.0(3) . . . . ?
C16 P1 C10 C15 10.0(3) . . . . ?
C22 P1 C10 C15 129.9(3) . . . . ?
C28 P1 C10 C15 -109.6(3) . . . . ?
C16 P1 C10 C11 -171.7(3) . . . . ?
C22 P1 C10 C11 -51.8(3) . . . . ?
C28 P1 C10 C11 68.7(3) . . . . ?
C9 C8 C7 C6 1.8(7) . . . . ?
C4 N7 N6 N5 0.2(4) . . . . ?
N7 N6 N5 N4 -0.3(4) . . . . ?
C56 C57 C52 C53 -0.5(5) . . . . ?
C56 C57 C52 P2 172.9(3) . . . . ?
C40 P2 C52 C53 -13.3(3) . . . . ?
C46 P2 C52 C53 104.9(3) . . . . ?
C34 P2 C52 C53 -135.3(3) . . . . ?
C40 P2 C52 C57 173.5(3) . . . . ?
C46 P2 C52 C57 -68.4(3) . . . . ?
C34 P2 C52 C57 51.4(3) . . . . ?
C31 C30 C29 C28 0.0(5) . . . . ?
C33 C28 C29 C30 -0.7(5) . . . . ?
P1 C28 C29 C30 174.6(3) . . . . ?
C33 C32 C31 C30 -1.6(5) . . . . ?
C29 C30 C31 C32 1.2(5) . . . . ?
C18 C17 C16 C21 -0.2(5) . . . . ?
C18 C17 C16 P1 -178.0(3) . . . . ?
C22 P1 C16 C21 -7.0(3) . . . . ?
C10 P1 C16 C21 112.6(3) . . . . ?
C28 P1 C16 C21 -125.4(3) . . . . ?
C22 P1 C16 C17 170.8(3) . . . . ?
C10 P1 C16 C17 -69.6(3) . . . . ?
C28 P1 C16 C17 52.4(3) . . . . ?
C40 P2 C46 C47 -84.9(3) . . . . ?
C52 P2 C46 C47 155.9(3) . . . . ?
C34 P2 C46 C47 35.7(3) . . . . ?
C40 P2 C46 C51 91.0(3) . . . . ?
C52 P2 C46 C51 -28.2(3) . . . . ?
C34 P2 C46 C51 -148.5(3) . . . . ?
C39 C34 C35 C36 -0.2(5) . . . . ?
P2 C34 C35 C36 178.4(3) . . . . ?
C31 C32 C33 C28 0.8(5) . . . . ?
C29 C28 C33 C32 0.3(5) . . . . ?
P1 C28 C33 C32 -174.9(3) . . . . ?
C13 C12 C11 C10 0.1(5) . . . . ?
C15 C10 C11 C12 0.4(5) . . . . ?
P1 C10 C11 C12 -177.9(3) . . . . ?
C13 C14 C15 C10 -1.6(5) . . . . ?
C11 C10 C15 C14 0.3(5) . . . . ?
P1 C10 C15 C14 178.6(3) . . . . ?
C55 C54 C53 C52 0.9(6) . . . . ?
C57 C52 C53 C54 -0.3(5) . . . . ?
P2 C52 C53 C54 -173.5(3) . . . . ?
C15 C14 C13 C12 2.1(6) . . . . ?
C11 C12 C13 C14 -1.4(5) . . . . ?
C16 P1 C22 C23 95.4(3) . . . . ?
C10 P1 C22 C23 -25.4(3) . . . . ?
C28 P1 C22 C23 -147.2(3) . . . . ?
C16 P1 C22 C27 -81.0(3) . . . . ?
C10 P1 C22 C27 158.2(3) . . . . ?
C28 P1 C22 C27 36.4(3) . . . . ?
N6 N5 N4 C4 0.3(4) . . . . ?
N6 N5 N4 W1B -179.9(2) . . . . ?
N6 N5 N4 W1A 174.5(3) . . . . ?
C44 C45 C40 C41 -0.9(5) . . . . ?
C44 C45 C40 P2 178.2(3) . . . . ?
C42 C41 C40 C45 1.6(5) . . . . ?
C42 C41 C40 P2 -177.6(3) . . . . ?
C46 P2 C40 C45 8.8(3) . . . . ?
C52 P2 C40 C45 126.6(3) . . . . ?
C34 P2 C40 C45 -111.3(3) . . . . ?
C46 P2 C40 C41 -172.1(3) . . . . ?
C52 P2 C40 C41 -54.3(3) . . . . ?
C34 P2 C40 C41 67.8(3) . . . . ?
C47 C46 C51 C50 0.8(5) . . . . ?
P2 C46 C51 C50 -175.1(3) . . . . ?
C23 C22 C27 C26 -0.2(5) . . . . ?
P1 C22 C27 C26 176.2(3) . . . . ?
C48 C49 C50 C51 -0.8(6) . . . . ?
C46 C51 C50 C49 -0.2(5) . . . . ?
C50 C49 C48 C47 1.2(6) . . . . ?
C40 C45 C44 C43 -0.3(6) . . . . ?
C49 C48 C47 C46 -0.6(6) . . . . ?
C51 C46 C47 C48 -0.4(5) . . . . ?
P2 C46 C47 C48 175.4(3) . . . . ?
C22 C27 C26 C25 0.5(6) . . . . ?
C24 C25 C26 C27 -0.5(6) . . . . ?
C52 C57 C56 C55 0.7(6) . . . . ?
C27 C22 C23 C24 -0.1(5) . . . . ?
P1 C22 C23 C24 -176.5(3) . . . . ?
C26 C25 C24 C23 0.2(6) . . . . ?
C22 C23 C24 C25 0.1(6) . . . . ?
C35 C34 C39 C38 1.0(6) . . . . ?
P2 C34 C39 C38 -177.6(3) . . . . ?
C19 C20 C21 C16 1.2(6) . . . . ?
C17 C16 C21 C20 -1.0(5) . . . . ?
P1 C16 C21 C20 176.7(3) . . . . ?
C53 C54 C55 C56 -0.6(6) . . . . ?
C57 C56 C55 C54 -0.2(6) . . . . ?
C34 C39 C38 C37 -0.4(6) . . . . ?
C36 C37 C38 C39 -0.9(6) . . . . ?
C8 C7 C6 C5 -1.6(7) . . . . ?
C16 C17 C18 C19 1.3(6) . . . . ?
C45 C44 C43 C42 0.9(6) . . . . ?
C9 N8 C5 C6 0.7(5) . . . . ?
W1A N8 C5 C6 -175.3(3) . . . . ?
C9 N8 C5 C4 -178.4(3) . . . . ?
W1A N8 C5 C4 5.6(4) . . . . ?
C7 C6 C5 N8 0.3(6) . . . . ?
C7 C6 C5 C4 179.3(4) . . . . ?
C38 C37 C36 C35 1.7(6) . . . . ?
C34 C35 C36 C37 -1.1(6) . . . . ?
C40 C41 C42 C43 -1.0(6) . . . . ?
C44 C43 C42 C41 -0.3(6) . . . . ?
C21 C20 C19 C18 -0.1(6) . . . . ?
C17 C18 C19 C20 -1.2(6) . . . . ?
N6 N7 C4 N4 0.0(4) . . . . ?
N6 N7 C4 C5 -177.0(4) . . . . ?
N5 N4 C4 N7 -0.2(4) . . . . ?
W1B N4 C4 N7 -179.9(3) . . . . ?
W1A N4 C4 N7 -175.8(3) . . . . ?
N5 N4 C4 C5 177.2(3) . . . . ?
W1B N4 C4 C5 -2.5(6) . . . . ?
W1A N4 C4 C5 1.5(4) . . . . ?
N8 C5 C4 N7 172.3(4) . . . . ?
C6 C5 C4 N7 -6.7(7) . . . . ?
N8 C5 C4 N4 -4.5(5) . . . . ?
C6 C5 C4 N4 176.4(4) . . . . ?
C7 C8 C9 N8 -0.8(6) . . . . ?
C5 N8 C9 C8 -0.4(6) . . . . ?
W1A N8 C9 C8 175.5(3) . . . . ?
N2 C2 W1B N4 1.7(14) . . . . ?
N2 C2 W1B C1 -100.4(13) . . . . ?
N2 C2 W1B C3 94.8(13) . . . . ?
N2 C2 W1B O1 176.3(12) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C33 H33 N1 0.95 2.50 3.259(5) 136.7 2_666 y
C9 H9 O1 0.95 2.51 3.013(6) 113.4 . y
O3 H3B O2 0.939(19) 1.91(2) 2.808(5) 161(5) . y
O3 H3A N6 0.927(19) 2.11(2) 3.009(5) 164(4) 1_565 y
O3 H3A N5 0.927(19) 2.72(4) 3.454(4) 137(4) 1_565 y
O2 H2A N3 0.942(19) 1.92(2) 2.861(4) 173(4) 1_565 y
O2 H2B O3 0.95(2) 1.84(2) 2.772(4) 171(7) 2_666 y

_refine_diff_density_max         1.244
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.114

