# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_phbmoco3
_database_code_depnum_ccdc_archive 'CCDC 1494716'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT241_phbmoco3            
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       C10S Check
RESPONSE: solvent
;
_vrf_PLAT910_phbmoco3            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          16 Note
RESPONSE: the mask of the beam-stopper is increased
;
# Added during the CSD deposition process: Tuesday 19 July 2016 09:44 AM
# end Validation Reply Form

_audit_creation_date             2016-06-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C27 H17 B Mo N3 O6 P6, C20 H40 Na O8, 2(C4 H8 O)'
_chemical_formula_sum            'C55 H73 B Mo N3 Na O16 P6'
_chemical_formula_weight         1347.72
_chemical_melting_point          ?
_chemical_oxdiff_formula         Mo1B1P6C40H40N3O3
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'
Mo Mo -1.6832 0.6857 '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'
Na Na 0.0362 0.0249 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.9566(4)
_cell_length_b                   29.5914(8)
_cell_length_c                   16.6475(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.824(3)
_cell_angle_gamma                90
_cell_volume                     6382.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10011
_cell_measurement_temperature    107(6)
_cell_measurement_theta_max      26.9080
_cell_measurement_theta_min      3.1220
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_preparation       '[MesMo(CO)] and PhB(OL)3Na in THF'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0988
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43016
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.808
_diffrn_ambient_temperature      107(6)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -20.00   13.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802  -99.0000   60.0000 33

#__ type_ start__ end____ width___ exp.time_
  2 omega   -3.00   45.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   57.0000  -90.0000 48

#__ type_ start__ end____ width___ exp.time_
  3 omega  -52.00   32.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  -38.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega    4.00   84.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   57.0000 -180.0000 80

#__ type_ start__ end____ width___ exp.time_
  5 omega  -52.00   30.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  -77.0000  120.0000 82
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_UB_11      0.0495903000
_diffrn_orient_matrix_UB_12      -0.0022122000
_diffrn_orient_matrix_UB_13      0.0181421000
_diffrn_orient_matrix_UB_21      -0.0227799000
_diffrn_orient_matrix_UB_22      -0.0005563000
_diffrn_orient_matrix_UB_23      0.0384980000
_diffrn_orient_matrix_UB_31      -0.0040683000
_diffrn_orient_matrix_UB_32      -0.0238576000
_diffrn_orient_matrix_UB_33      -0.0025985000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10703
_reflns_number_total             14875
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         14875
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0740
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0100P)²+27.4320P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1432
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14S(H14A,H14B), C23S(H23A,H23B), C25S(H25A,H25B), C22S(H22A,H22B), C26S(H26A,
 H26B), C18S(H18A,H18B), C27S(H27A,H27B), C24S(H24A,H24B), C15S(H15A,H15B),
 C13S(H13A,H13B), C17S(H17A,H17B), C28S(H28A,H28B), C20S(H20A,H20B), C21S(H21A,
 H21B), C19S(H19A,H19B), C16S(H16A,H16B), C12S(H12A,H12B), C8S(H8SA,H8SB),
 C9S(H9SA,H9SB), C4S(H4SA,H4SB), C7S(H7SA,H7SB), C1S(H1SA,H1SB), C11S(H11A,
 H11B), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C5S(H5SA,H5SB), C6S(H6SA,H6SB),
 C10S(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C5B(H5B), C4B(H4B), C3(H3), C3A(H3A), C6B(H6B), C6C(H6C), C3C(H3C), C7(H7),
 C3B(H3B), C6A(H6A), C4A(H4A), C5C(H5C), C4C(H4C), C4(H4), C6(H6), C5(H5),
 C5A(H5A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo01 Mo 0.62567(3) 0.63751(2) 0.20838(2) 0.01752(10) Uani 1 1 d . . . . .
P1A P 0.67940(9) 0.67846(4) 0.08697(7) 0.0186(3) Uani 1 1 d . . . . .
P1B P 0.44059(9) 0.65483(4) 0.17902(7) 0.0177(3) Uani 1 1 d . . . . .
P2B P 0.31306(10) 0.61125(4) 0.18305(8) 0.0222(3) Uani 1 1 d . . . . .
P1C P 0.61837(10) 0.70917(4) 0.28365(7) 0.0198(3) Uani 1 1 d . . . . .
P2A P 0.81536(9) 0.68267(4) 0.01999(8) 0.0219(3) Uani 1 1 d . . . . .
P2C P 0.62666(10) 0.72440(4) 0.40675(8) 0.0235(3) Uani 1 1 d . . . . .
Na00 Na 0.55127(16) 0.38744(7) 0.25003(12) 0.0307(5) Uani 1 1 d . . . . .
O1C O 0.5768(2) 0.77696(10) 0.17433(18) 0.0193(7) Uani 1 1 d . . . . .
O1B O 0.4017(2) 0.74738(10) 0.16404(18) 0.0178(7) Uani 1 1 d . . . . .
O1A O 0.5186(2) 0.73463(10) 0.05466(18) 0.0162(7) Uani 1 1 d . . . . .
O5S O 0.5909(2) 0.31343(11) 0.34354(19) 0.0221(7) Uani 1 1 d . . . . .
O10S O 0.6398(3) 0.31153(11) 0.1807(2) 0.0250(8) Uani 1 1 d . . . . .
O6S O 0.5552(3) 0.39581(11) 0.4121(2) 0.0280(8) Uani 1 1 d . . . . .
O8S O 0.4865(3) 0.45691(11) 0.1556(2) 0.0263(8) Uani 1 1 d . . . . .
O7S O 0.4660(3) 0.46388(11) 0.32104(19) 0.0261(8) Uani 1 1 d . . . . .
O3 O 0.6160(3) 0.54647(11) 0.1120(2) 0.0326(9) Uani 1 1 d . . . . .
N1C N 0.5814(3) 0.79542(12) 0.3094(2) 0.0165(8) Uani 1 1 d . . . . .
O9S O 0.5518(3) 0.37883(11) 0.0875(2) 0.0283(8) Uani 1 1 d . . . . .
N1A N 0.6665(3) 0.74301(12) -0.0211(2) 0.0163(8) Uani 1 1 d . . . . .
N1B N 0.2647(3) 0.69935(12) 0.1639(2) 0.0167(8) Uani 1 1 d . . . . .
O3S O 0.7034(3) 0.43024(13) 0.2618(2) 0.0375(9) Uani 1 1 d . . . . .
O4S O 0.3817(3) 0.36221(14) 0.2517(2) 0.0396(10) Uani 1 1 d . . . . .
O2 O 0.5764(4) 0.58919(13) 0.3706(2) 0.0466(11) Uani 1 1 d . . . . .
O1 O 0.8590(3) 0.61800(15) 0.2480(3) 0.0507(12) Uani 1 1 d . . . . .
C1B C 0.3723(3) 0.70417(15) 0.1671(2) 0.0166(9) Uani 1 1 d . . . . .
C1C C 0.5877(3) 0.76211(16) 0.2505(3) 0.0184(10) Uani 1 1 d . . . . .
C1A C 0.6152(3) 0.72158(15) 0.0401(3) 0.0171(9) Uani 1 1 d . . . . .
C2B C 0.2256(4) 0.65573(16) 0.1724(3) 0.0208(10) Uani 1 1 d . . . . .
C10 C 0.6194(4) 0.57973(16) 0.1474(3) 0.0231(11) Uani 1 1 d . . . . .
C2C C 0.5997(3) 0.78119(17) 0.3887(3) 0.0212(10) Uani 1 1 d . . . . .
O1S O 0.4282(4) 0.96861(15) 0.3862(3) 0.0593(13) Uani 1 1 d . . . . .
C2A C 0.7666(4) 0.72761(16) -0.0370(3) 0.0198(10) Uani 1 1 d . . . . .
C5B C 0.0962(4) 0.73142(17) 0.1583(3) 0.0235(11) Uani 1 1 d . . . . .
H5B H 0.0533 0.7565 0.1538 0.028 Uiso 1 1 calc R . . . .
C9 C 0.5911(4) 0.60666(16) 0.3105(3) 0.0265(11) Uani 1 1 d . . . . .
C4B C 0.0532(4) 0.68726(17) 0.1667(3) 0.0256(11) Uani 1 1 d . . . . .
H4B H -0.0180 0.6834 0.1678 0.031 Uiso 1 1 calc R . . . .
C3 C 0.5165(4) 0.85239(16) 0.0746(3) 0.0237(11) Uani 1 1 d . . . . .
H3 H 0.5786 0.8520 0.1033 0.028 Uiso 1 1 calc R . . . .
C2 C 0.4541(4) 0.81396(15) 0.0765(3) 0.0186(10) Uani 1 1 d . . . . .
C8 C 0.7734(4) 0.62559(18) 0.2345(3) 0.0300(12) Uani 1 1 d . . . . .
C3A C 0.8218(4) 0.75124(17) -0.0962(3) 0.0249(11) Uani 1 1 d . . . . .
H3A H 0.8885 0.7420 -0.1079 0.030 Uiso 1 1 calc R . . . .
C6B C 0.2002(3) 0.73632(16) 0.1570(3) 0.0183(10) Uani 1 1 d . . . . .
H6B H 0.2285 0.7650 0.1515 0.022 Uiso 1 1 calc R . . . .
C6C C 0.5565(4) 0.83982(16) 0.2925(3) 0.0221(10) Uani 1 1 d . . . . .
H6C H 0.5436 0.8485 0.2397 0.026 Uiso 1 1 calc R . . . .
C3C C 0.5953(4) 0.81461(18) 0.4490(3) 0.0277(12) Uani 1 1 d . . . . .
H3C H 0.6089 0.8064 0.5020 0.033 Uiso 1 1 calc R . . . .
C7 C 0.3619(4) 0.81676(17) 0.0315(3) 0.0233(11) Uani 1 1 d . . . . .
H7 H 0.3172 0.7922 0.0308 0.028 Uiso 1 1 calc R . . . .
C3B C 0.1162(4) 0.65119(16) 0.1729(3) 0.0225(11) Uani 1 1 d . . . . .
H3B H 0.0874 0.6225 0.1776 0.027 Uiso 1 1 calc R . . . .
C14S C 0.2097(4) 0.38084(18) 0.2723(3) 0.0333(13) Uani 1 1 d . . . . .
H14A H 0.2046 0.4103 0.2471 0.040 Uiso 1 1 calc R . . . .
H14B H 0.1532 0.3771 0.3093 0.040 Uiso 1 1 calc R . . . .
C23S C 0.6239(4) 0.27145(16) 0.2252(3) 0.0255(11) Uani 1 1 d . . . . .
H23A H 0.6638 0.2469 0.2028 0.031 Uiso 1 1 calc R . . . .
H23B H 0.5515 0.2631 0.2232 0.031 Uiso 1 1 calc R . . . .
C6A C 0.6228(4) 0.77822(16) -0.0654(3) 0.0223(11) Uani 1 1 d . . . . .
H6A H 0.5548 0.7868 -0.0566 0.027 Uiso 1 1 calc R . . . .
C25S C 0.6154(4) 0.32119(17) 0.4258(3) 0.0316(12) Uani 1 1 d . . . . .
H25A H 0.6863 0.3314 0.4312 0.038 Uiso 1 1 calc R . . . .
H25B H 0.6083 0.2933 0.4559 0.038 Uiso 1 1 calc R . . . .
C22S C 0.6142(4) 0.30466(17) 0.0982(3) 0.0309(12) Uani 1 1 d . . . . .
H22A H 0.5439 0.2937 0.0928 0.037 Uiso 1 1 calc R . . . .
H22B H 0.6600 0.2823 0.0753 0.037 Uiso 1 1 calc R . . . .
C4A C 0.7812(4) 0.78680(17) -0.1365(3) 0.0267(12) Uani 1 1 d . . . . .
H4A H 0.8203 0.8024 -0.1739 0.032 Uiso 1 1 calc R . . . .
C26S C 0.5450(4) 0.35579(17) 0.4578(3) 0.0320(13) Uani 1 1 d . . . . .
H26A H 0.4744 0.3450 0.4547 0.038 Uiso 1 1 calc R . . . .
H26B H 0.5621 0.3618 0.5137 0.038 Uiso 1 1 calc R . . . .
C18S C 0.4183(4) 0.48817(17) 0.1910(3) 0.0297(12) Uani 1 1 d . . . . .
H18A H 0.3514 0.4742 0.1990 0.036 Uiso 1 1 calc R . . . .
H18B H 0.4090 0.5142 0.1562 0.036 Uiso 1 1 calc R . . . .
C27S C 0.5057(5) 0.43314(17) 0.4490(3) 0.0330(13) Uani 1 1 d . . . . .
H27A H 0.5375 0.4392 0.5010 0.040 Uiso 1 1 calc R . . . .
H27B H 0.4333 0.4263 0.4571 0.040 Uiso 1 1 calc R . . . .
C24S C 0.6574(4) 0.28014(17) 0.3103(3) 0.0284(12) Uani 1 1 d . . . . .
H24A H 0.6537 0.2524 0.3413 0.034 Uiso 1 1 calc R . . . .
H24B H 0.7282 0.2908 0.3118 0.034 Uiso 1 1 calc R . . . .
C15S C 0.2109(4) 0.34300(18) 0.2098(3) 0.0323(13) Uani 1 1 d . . . . .
H15A H 0.1816 0.3154 0.2311 0.039 Uiso 1 1 calc R . . . .
H15B H 0.1727 0.3516 0.1616 0.039 Uiso 1 1 calc R . . . .
B1 B 0.4889(4) 0.76771(17) 0.1191(3) 0.0163(11) Uani 1 1 d . . . . .
C5C C 0.5506(4) 0.87057(17) 0.3517(3) 0.0268(11) Uani 1 1 d . . . . .
H5C H 0.5324 0.9002 0.3396 0.032 Uiso 1 1 calc R . . . .
C4C C 0.5720(4) 0.85810(18) 0.4320(3) 0.0304(12) Uani 1 1 d . . . . .
H4C H 0.5701 0.8796 0.4728 0.036 Uiso 1 1 calc R . . . .
C13S C 0.3130(4) 0.37445(19) 0.3141(3) 0.0359(14) Uani 1 1 d . . . . .
H13A H 0.3353 0.4022 0.3400 0.043 Uiso 1 1 calc R . . . .
H13B H 0.3094 0.3507 0.3542 0.043 Uiso 1 1 calc R . . . .
C4 C 0.4904(4) 0.89089(17) 0.0321(3) 0.0299(12) Uani 1 1 d . . . . .
H4 H 0.5341 0.9158 0.0327 0.036 Uiso 1 1 calc R . . . .
C17S C 0.4641(4) 0.50246(16) 0.2700(3) 0.0288(12) Uani 1 1 d . . . . .
H17A H 0.5335 0.5138 0.2627 0.035 Uiso 1 1 calc R . . . .
H17B H 0.4228 0.5262 0.2935 0.035 Uiso 1 1 calc R . . . .
C6 C 0.3354(4) 0.85506(17) -0.0118(3) 0.0323(13) Uani 1 1 d . . . . .
H6 H 0.2741 0.8557 -0.0416 0.039 Uiso 1 1 calc R . . . .
C28S C 0.5155(5) 0.47356(17) 0.3959(3) 0.0331(13) Uani 1 1 d . . . . .
H28A H 0.4835 0.4996 0.4207 0.040 Uiso 1 1 calc R . . . .
H28B H 0.5878 0.4804 0.3876 0.040 Uiso 1 1 calc R . . . .
C20S C 0.5421(4) 0.41824(18) 0.0406(3) 0.0336(13) Uani 1 1 d . . . . .
H20A H 0.5255 0.4105 -0.0147 0.040 Uiso 1 1 calc R . . . .
H20B H 0.6063 0.4351 0.0417 0.040 Uiso 1 1 calc R . . . .
C21S C 0.6252(4) 0.34831(18) 0.0552(3) 0.0326(13) Uani 1 1 d . . . . .
H21A H 0.6945 0.3601 0.0627 0.039 Uiso 1 1 calc R . . . .
H21B H 0.6124 0.3441 -0.0019 0.039 Uiso 1 1 calc R . . . .
C19S C 0.4571(4) 0.44590(18) 0.0759(3) 0.0333(13) Uani 1 1 d . . . . .
H19A H 0.4464 0.4732 0.0447 0.040 Uiso 1 1 calc R . . . .
H19B H 0.3932 0.4288 0.0755 0.040 Uiso 1 1 calc R . . . .
C16S C 0.3253(4) 0.33711(18) 0.1925(3) 0.0295(12) Uani 1 1 d . . . . .
H16A H 0.3441 0.3054 0.1952 0.035 Uiso 1 1 calc R . . . .
H16B H 0.3406 0.3483 0.1392 0.035 Uiso 1 1 calc R . . . .
C5 C 0.3988(5) 0.89209(18) -0.0112(3) 0.0364(14) Uani 1 1 d . . . . .
H5 H 0.3803 0.9179 -0.0398 0.044 Uiso 1 1 calc R . . . .
C5A C 0.6789(4) 0.79997(17) -0.1212(3) 0.0275(12) Uani 1 1 d . . . . .
H5A H 0.6496 0.8239 -0.1498 0.033 Uiso 1 1 calc R . . . .
C12S C 0.7447(5) 0.45711(19) 0.1983(4) 0.0393(14) Uani 1 1 d . . . . .
H12A H 0.6899 0.4730 0.1697 0.047 Uiso 1 1 calc R . . . .
H12B H 0.7814 0.4383 0.1605 0.047 Uiso 1 1 calc R . . . .
C8S C 0.7654(5) 0.4253(2) 0.5858(4) 0.0523(17) Uani 1 1 d . . . . .
H8SA H 0.7894 0.4034 0.5470 0.063 Uiso 1 1 calc R . . . .
H8SB H 0.7120 0.4114 0.6177 0.063 Uiso 1 1 calc R . . . .
C9S C 0.7795(5) 0.4295(2) 0.3245(4) 0.0525(18) Uani 1 1 d . . . . .
H9SA H 0.8288 0.4054 0.3159 0.063 Uiso 1 1 calc R . . . .
H9SB H 0.7475 0.4251 0.3762 0.063 Uiso 1 1 calc R . . . .
O2S O 0.7268(5) 0.4633(2) 0.5467(4) 0.112(3) Uani 1 1 d . . . . .
C4S C 0.3597(5) 0.9493(2) 0.4398(5) 0.063(2) Uani 1 1 d . . . . .
H4SA H 0.3936 0.9256 0.4704 0.075 Uiso 1 1 calc R . . . .
H4SB H 0.3013 0.9364 0.4110 0.075 Uiso 1 1 calc R . . . .
C7S C 0.8530(5) 0.4405(3) 0.6387(4) 0.0581(19) Uani 1 1 d . . . . .
H7SA H 0.9142 0.4224 0.6299 0.070 Uiso 1 1 calc R . . . .
H7SB H 0.8348 0.4388 0.6949 0.070 Uiso 1 1 calc R . . . .
C1S C 0.3976(6) 1.0145(2) 0.3765(5) 0.066(2) Uani 1 1 d . . . . .
H1SA H 0.3439 1.0172 0.3356 0.080 Uiso 1 1 calc R . . . .
H1SB H 0.4558 1.0332 0.3616 0.080 Uiso 1 1 calc R . . . .
C11S C 0.8179(7) 0.4904(3) 0.2388(5) 0.079(3) Uani 1 1 d . . . . .
H11A H 0.8836 0.4910 0.2116 0.095 Uiso 1 1 calc R . . . .
H11B H 0.7888 0.5206 0.2380 0.095 Uiso 1 1 calc R . . . .
C2S C 0.3584(7) 1.0279(3) 0.4561(6) 0.088(3) Uani 1 1 d . . . . .
H2SA H 0.4125 1.0423 0.4878 0.105 Uiso 1 1 calc R . . . .
H2SB H 0.3013 1.0489 0.4500 0.105 Uiso 1 1 calc R . . . .
C3S C 0.3242(6) 0.9862(3) 0.4950(5) 0.082(3) Uani 1 1 d . . . . .
H3SA H 0.2497 0.9857 0.5001 0.098 Uiso 1 1 calc R . . . .
H3SB H 0.3556 0.9830 0.5480 0.098 Uiso 1 1 calc R . . . .
C5S C 0.7735(7) 0.5020(3) 0.5782(8) 0.106(4) Uani 1 1 d . . . . .
H5SA H 0.7300 0.5155 0.6185 0.128 Uiso 1 1 calc R . . . .
H5SB H 0.7846 0.5240 0.5360 0.128 Uiso 1 1 calc R . . . .
C6S C 0.8697(8) 0.4886(3) 0.6132(7) 0.102(3) Uani 1 1 d . . . . .
H6SA H 0.8873 0.5074 0.6591 0.122 Uiso 1 1 calc R . . . .
H6SB H 0.9246 0.4905 0.5744 0.122 Uiso 1 1 calc R . . . .
C10S C 0.8312(8) 0.4744(4) 0.3210(6) 0.122(5) Uani 1 1 d . . . . .
H10A H 0.7998 0.4953 0.3583 0.147 Uiso 1 1 calc R . . . .
H10B H 0.9039 0.4716 0.3347 0.147 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo01 P1A 2.4655(12) . ?
Mo01 P1B 2.4937(13) . ?
Mo01 P1C 2.4657(13) . ?
Mo01 C10 1.990(5) . ?
Mo01 C9 1.987(5) . ?
Mo01 C8 1.988(6) . ?
P1A P2A 2.1020(16) . ?
P1A C1A 1.706(5) . ?
P1B P2B 2.0977(17) . ?
P1B C1B 1.718(5) . ?
P2B C2B 1.744(5) . ?
P1C P2C 2.0994(18) . ?
P1C C1C 1.706(5) . ?
P2A C2A 1.746(5) . ?
P2C C2C 1.742(5) . ?
Na00 O5S 2.731(4) . ?
Na00 O10S 2.781(4) . ?
Na00 O6S 2.709(4) . ?
Na00 O8S 2.714(4) . ?
Na00 O7S 2.788(4) . ?
Na00 O9S 2.719(4) . ?
Na00 O3S 2.349(4) . ?
Na00 O4S 2.320(4) . ?
O1C C1C 1.348(5) . ?
O1C B1 1.479(6) . ?
O1B C1B 1.336(5) . ?
O1B B1 1.491(5) . ?
O1A C1A 1.335(5) . ?
O1A B1 1.506(5) . ?
O5S C25S 1.420(6) . ?
O5S C24S 1.426(6) . ?
O10S C23S 1.416(6) . ?
O10S C22S 1.423(6) . ?
O6S C26S 1.415(6) . ?
O6S C27S 1.422(6) . ?
O8S C18S 1.414(6) . ?
O8S C19S 1.413(6) . ?
O7S C17S 1.423(6) . ?
O7S C28S 1.423(6) . ?
O3 C10 1.147(6) . ?
N1C C1C 1.393(6) . ?
N1C C2C 1.403(6) . ?
N1C C6C 1.381(6) . ?
O9S C20S 1.408(6) . ?
O9S C21S 1.422(6) . ?
N1A C1A 1.378(5) . ?
N1A C2A 1.403(6) . ?
N1A C6A 1.393(6) . ?
N1B C1B 1.401(6) . ?
N1B C2B 1.395(6) . ?
N1B C6B 1.380(6) . ?
O3S C12S 1.433(6) . ?
O3S C9S 1.424(7) . ?
O4S C13S 1.425(6) . ?
O4S C16S 1.426(6) . ?
O2 C9 1.144(6) . ?
O1 C8 1.151(6) . ?
C2B C3B 1.424(6) . ?
C2C C3C 1.410(6) . ?
O1S C4S 1.390(8) . ?
O1S C1S 1.423(8) . ?
C2A C3A 1.412(6) . ?
C5B H5B 0.9300 . ?
C5B C4B 1.428(7) . ?
C5B C6B 1.357(6) . ?
C4B H4B 0.9300 . ?
C4B C3B 1.346(7) . ?
C3 H3 0.9300 . ?
C3 C2 1.396(6) . ?
C3 C4 1.380(7) . ?
C2 C7 1.403(7) . ?
C2 B1 1.603(7) . ?
C3A H3A 0.9300 . ?
C3A C4A 1.350(7) . ?
C6B H6B 0.9300 . ?
C6C H6C 0.9300 . ?
C6C C5C 1.343(7) . ?
C3C H3C 0.9300 . ?
C3C C4C 1.351(7) . ?
C7 H7 0.9300 . ?
C7 C6 1.384(7) . ?
C3B H3B 0.9300 . ?
C14S H14A 0.9700 . ?
C14S H14B 0.9700 . ?
C14S C15S 1.529(7) . ?
C14S C13S 1.512(8) . ?
C23S H23A 0.9700 . ?
C23S H23B 0.9700 . ?
C23S C24S 1.498(7) . ?
C6A H6A 0.9300 . ?
C6A C5A 1.351(6) . ?
C25S H25A 0.9700 . ?
C25S H25B 0.9700 . ?
C25S C26S 1.476(7) . ?
C22S H22A 0.9700 . ?
C22S H22B 0.9700 . ?
C22S C21S 1.484(7) . ?
C4A H4A 0.9300 . ?
C4A C5A 1.409(7) . ?
C26S H26A 0.9700 . ?
C26S H26B 0.9700 . ?
C18S H18A 0.9700 . ?
C18S H18B 0.9700 . ?
C18S C17S 1.496(7) . ?
C27S H27A 0.9700 . ?
C27S H27B 0.9700 . ?
C27S C28S 1.494(7) . ?
C24S H24A 0.9700 . ?
C24S H24B 0.9700 . ?
C15S H15A 0.9700 . ?
C15S H15B 0.9700 . ?
C15S C16S 1.525(7) . ?
C5C H5C 0.9300 . ?
C5C C4C 1.411(7) . ?
C4C H4C 0.9300 . ?
C13S H13A 0.9700 . ?
C13S H13B 0.9700 . ?
C4 H4 0.9300 . ?
C4 C5 1.379(8) . ?
C17S H17A 0.9700 . ?
C17S H17B 0.9700 . ?
C6 H6 0.9300 . ?
C6 C5 1.370(8) . ?
C28S H28A 0.9700 . ?
C28S H28B 0.9700 . ?
C20S H20A 0.9700 . ?
C20S H20B 0.9700 . ?
C20S C19S 1.500(7) . ?
C21S H21A 0.9700 . ?
C21S H21B 0.9700 . ?
C19S H19A 0.9700 . ?
C19S H19B 0.9700 . ?
C16S H16A 0.9700 . ?
C16S H16B 0.9700 . ?
C5 H5 0.9300 . ?
C5A H5A 0.9300 . ?
C12S H12A 0.9700 . ?
C12S H12B 0.9700 . ?
C12S C11S 1.518(9) . ?
C8S H8SA 0.9700 . ?
C8S H8SB 0.9700 . ?
C8S O2S 1.388(8) . ?
C8S C7S 1.496(9) . ?
C9S H9SA 0.9700 . ?
C9S H9SB 0.9700 . ?
C9S C10S 1.490(11) . ?
O2S C5S 1.395(10) . ?
C4S H4SA 0.9700 . ?
C4S H4SB 0.9700 . ?
C4S C3S 1.502(10) . ?
C7S H7SA 0.9700 . ?
C7S H7SB 0.9700 . ?
C7S C6S 1.500(11) . ?
C1S H1SA 0.9700 . ?
C1S H1SB 0.9700 . ?
C1S C2S 1.480(11) . ?
C11S H11A 0.9700 . ?
C11S H11B 0.9700 . ?
C11S C10S 1.456(11) . ?
C2S H2SA 0.9700 . ?
C2S H2SB 0.9700 . ?
C2S C3S 1.467(11) . ?
C3S H3SA 0.9700 . ?
C3S H3SB 0.9700 . ?
C5S H5SA 0.9700 . ?
C5S H5SB 0.9700 . ?
C5S C6S 1.425(12) . ?
C6S H6SA 0.9700 . ?
C6S H6SB 0.9700 . ?
C10S H10A 0.9700 . ?
C10S H10B 0.9700 . ?

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
P1A Mo01 P1B 91.17(4) . . ?
P1A Mo01 P1C 90.42(4) . . ?
P1C Mo01 P1B 83.06(4) . . ?
C10 Mo01 P1A 90.78(13) . . ?
C10 Mo01 P1B 92.56(15) . . ?
C10 Mo01 P1C 175.47(15) . . ?
C9 Mo01 P1A 175.73(16) . . ?
C9 Mo01 P1B 91.98(16) . . ?
C9 Mo01 P1C 87.10(14) . . ?
C9 Mo01 C10 91.96(19) . . ?
C9 Mo01 C8 87.6(2) . . ?
C8 Mo01 P1A 89.11(15) . . ?
C8 Mo01 P1B 177.92(16) . . ?
C8 Mo01 P1C 94.89(16) . . ?
C8 Mo01 C10 89.5(2) . . ?
P2A P1A Mo01 135.45(7) . . ?
C1A P1A Mo01 126.95(15) . . ?
C1A P1A P2A 96.87(15) . . ?
P2B P1B Mo01 128.54(7) . . ?
C1B P1B Mo01 133.63(16) . . ?
C1B P1B P2B 96.97(16) . . ?
C2B P2B P1B 92.52(16) . . ?
P2C P1C Mo01 132.75(7) . . ?
C1C P1C Mo01 129.49(16) . . ?
C1C P1C P2C 97.29(16) . . ?
C2A P2A P1A 91.95(16) . . ?
C2C P2C P1C 91.81(16) . . ?
O5S Na00 O10S 60.91(10) . . ?
O5S Na00 O7S 118.77(12) . . ?
O10S Na00 O7S 178.93(14) . . ?
O6S Na00 O5S 60.33(10) . . ?
O6S Na00 O10S 119.04(12) . . ?
O6S Na00 O8S 120.59(12) . . ?
O6S Na00 O7S 60.36(11) . . ?
O6S Na00 O9S 178.76(14) . . ?
O8S Na00 O5S 172.57(13) . . ?
O8S Na00 O10S 119.83(12) . . ?
O8S Na00 O7S 60.64(10) . . ?
O8S Na00 O9S 59.97(11) . . ?
O9S Na00 O5S 119.28(12) . . ?
O9S Na00 O10S 60.26(11) . . ?
O9S Na00 O7S 120.33(12) . . ?
O3S Na00 O5S 103.53(14) . . ?
O3S Na00 O10S 96.86(14) . . ?
O3S Na00 O6S 82.15(14) . . ?
O3S Na00 O8S 83.82(13) . . ?
O3S Na00 O7S 82.20(13) . . ?
O3S Na00 O9S 96.88(14) . . ?
O4S Na00 O5S 84.58(14) . . ?
O4S Na00 O10S 98.12(14) . . ?
O4S Na00 O6S 91.27(14) . . ?
O4S Na00 O8S 88.02(15) . . ?
O4S Na00 O7S 82.82(13) . . ?
O4S Na00 O9S 89.85(14) . . ?
O4S Na00 O3S 164.99(17) . . ?
C1C O1C B1 126.4(3) . . ?
C1B O1B B1 128.6(3) . . ?
C1A O1A B1 124.6(4) . . ?
C25S O5S Na00 117.2(3) . . ?
C25S O5S C24S 111.0(4) . . ?
C24S O5S Na00 116.2(3) . . ?
C23S O10S Na00 113.3(3) . . ?
C23S O10S C22S 110.6(4) . . ?
C22S O10S Na00 115.1(3) . . ?
C26S O6S Na00 117.3(3) . . ?
C26S O6S C27S 111.8(4) . . ?
C27S O6S Na00 119.9(3) . . ?
C18S O8S Na00 116.4(3) . . ?
C19S O8S Na00 116.5(3) . . ?
C19S O8S C18S 112.4(4) . . ?
C17S O7S Na00 113.6(3) . . ?
C28S O7S Na00 111.0(3) . . ?
C28S O7S C17S 111.4(4) . . ?
C1C N1C C2C 116.0(4) . . ?
C6C N1C C1C 123.1(4) . . ?
C6C N1C C2C 120.8(4) . . ?
C20S O9S Na00 118.2(3) . . ?
C20S O9S C21S 111.8(4) . . ?
C21S O9S Na00 116.5(3) . . ?
C1A N1A C2A 116.6(4) . . ?
C1A N1A C6A 122.6(4) . . ?
C6A N1A C2A 120.9(4) . . ?
C2B N1B C1B 117.0(4) . . ?
C6B N1B C1B 121.5(4) . . ?
C6B N1B C2B 121.4(4) . . ?
C12S O3S Na00 124.0(3) . . ?
C9S O3S Na00 128.6(4) . . ?
C9S O3S C12S 106.7(4) . . ?
C13S O4S Na00 121.9(3) . . ?
C13S O4S C16S 108.4(4) . . ?
C16S O4S Na00 129.4(3) . . ?
O1B C1B P1B 132.2(3) . . ?
O1B C1B N1B 112.4(4) . . ?
N1B C1B P1B 115.4(3) . . ?
O1C C1C P1C 128.6(3) . . ?
O1C C1C N1C 115.1(4) . . ?
N1C C1C P1C 116.0(3) . . ?
O1A C1A P1A 125.8(3) . . ?
O1A C1A N1A 117.7(4) . . ?
N1A C1A P1A 116.4(3) . . ?
N1B C2B P2B 118.2(3) . . ?
N1B C2B C3B 116.8(4) . . ?
C3B C2B P2B 125.0(4) . . ?
O3 C10 Mo01 179.8(5) . . ?
N1C C2C P2C 118.8(3) . . ?
N1C C2C C3C 116.8(4) . . ?
C3C C2C P2C 124.3(4) . . ?
C4S O1S C1S 106.5(5) . . ?
N1A C2A P2A 118.2(3) . . ?
N1A C2A C3A 116.7(4) . . ?
C3A C2A P2A 125.0(4) . . ?
C4B C5B H5B 120.4 . . ?
C6B C5B H5B 120.4 . . ?
C6B C5B C4B 119.2(4) . . ?
O2 C9 Mo01 176.5(5) . . ?
C5B C4B H4B 120.1 . . ?
C3B C4B C5B 119.8(4) . . ?
C3B C4B H4B 120.1 . . ?
C2 C3 H3 118.5 . . ?
C4 C3 H3 118.5 . . ?
C4 C3 C2 123.1(5) . . ?
C3 C2 C7 115.4(4) . . ?
C3 C2 B1 123.1(4) . . ?
C7 C2 B1 121.2(4) . . ?
O1 C8 Mo01 178.3(5) . . ?
C2A C3A H3A 118.8 . . ?
C4A C3A C2A 122.4(5) . . ?
C4A C3A H3A 118.8 . . ?
N1B C6B H6B 119.5 . . ?
C5B C6B N1B 121.0(4) . . ?
C5B C6B H6B 119.5 . . ?
N1C C6C H6C 119.6 . . ?
C5C C6C N1C 120.7(5) . . ?
C5C C6C H6C 119.6 . . ?
C2C C3C H3C 119.0 . . ?
C4C C3C C2C 122.0(5) . . ?
C4C C3C H3C 119.0 . . ?
C2 C7 H7 119.0 . . ?
C6 C7 C2 122.0(5) . . ?
C6 C7 H7 119.0 . . ?
C2B C3B H3B 119.1 . . ?
C4B C3B C2B 121.8(4) . . ?
C4B C3B H3B 119.1 . . ?
H14A C14S H14B 109.3 . . ?
C15S C14S H14A 111.4 . . ?
C15S C14S H14B 111.4 . . ?
C13S C14S H14A 111.4 . . ?
C13S C14S H14B 111.4 . . ?
C13S C14S C15S 101.8(4) . . ?
O10S C23S H23A 110.1 . . ?
O10S C23S H23B 110.1 . . ?
O10S C23S C24S 108.0(4) . . ?
H23A C23S H23B 108.4 . . ?
C24S C23S H23A 110.1 . . ?
C24S C23S H23B 110.1 . . ?
N1A C6A H6A 119.9 . . ?
C5A C6A N1A 120.1(4) . . ?
C5A C6A H6A 119.9 . . ?
O5S C25S H25A 109.8 . . ?
O5S C25S H25B 109.8 . . ?
O5S C25S C26S 109.3(4) . . ?
H25A C25S H25B 108.3 . . ?
C26S C25S H25A 109.8 . . ?
C26S C25S H25B 109.8 . . ?
O10S C22S H22A 110.0 . . ?
O10S C22S H22B 110.0 . . ?
O10S C22S C21S 108.6(4) . . ?
H22A C22S H22B 108.4 . . ?
C21S C22S H22A 110.0 . . ?
C21S C22S H22B 110.0 . . ?
C3A C4A H4A 120.4 . . ?
C3A C4A C5A 119.1(4) . . ?
C5A C4A H4A 120.4 . . ?
O6S C26S C25S 108.9(4) . . ?
O6S C26S H26A 109.9 . . ?
O6S C26S H26B 109.9 . . ?
C25S C26S H26A 109.9 . . ?
C25S C26S H26B 109.9 . . ?
H26A C26S H26B 108.3 . . ?
O8S C18S H18A 110.1 . . ?
O8S C18S H18B 110.1 . . ?
O8S C18S C17S 108.0(4) . . ?
H18A C18S H18B 108.4 . . ?
C17S C18S H18A 110.1 . . ?
C17S C18S H18B 110.1 . . ?
O6S C27S H27A 109.9 . . ?
O6S C27S H27B 109.9 . . ?
O6S C27S C28S 108.9(4) . . ?
H27A C27S H27B 108.3 . . ?
C28S C27S H27A 109.9 . . ?
C28S C27S H27B 109.9 . . ?
O5S C24S C23S 108.5(4) . . ?
O5S C24S H24A 110.0 . . ?
O5S C24S H24B 110.0 . . ?
C23S C24S H24A 110.0 . . ?
C23S C24S H24B 110.0 . . ?
H24A C24S H24B 108.4 . . ?
C14S C15S H15A 111.1 . . ?
C14S C15S H15B 111.1 . . ?
H15A C15S H15B 109.1 . . ?
C16S C15S C14S 103.4(4) . . ?
C16S C15S H15A 111.1 . . ?
C16S C15S H15B 111.1 . . ?
O1C B1 O1B 110.2(4) . . ?
O1C B1 O1A 111.1(4) . . ?
O1C B1 C2 109.0(4) . . ?
O1B B1 O1A 107.4(4) . . ?
O1B B1 C2 110.9(4) . . ?
O1A B1 C2 108.2(4) . . ?
C6C C5C H5C 119.8 . . ?
C6C C5C C4C 120.3(5) . . ?
C4C C5C H5C 119.8 . . ?
C3C C4C C5C 119.2(5) . . ?
C3C C4C H4C 120.4 . . ?
C5C C4C H4C 120.4 . . ?
O4S C13S C14S 104.8(4) . . ?
O4S C13S H13A 110.8 . . ?
O4S C13S H13B 110.8 . . ?
C14S C13S H13A 110.8 . . ?
C14S C13S H13B 110.8 . . ?
H13A C13S H13B 108.9 . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.5(5) . . ?
C5 C4 H4 120.3 . . ?
O7S C17S C18S 107.5(4) . . ?
O7S C17S H17A 110.2 . . ?
O7S C17S H17B 110.2 . . ?
C18S C17S H17A 110.2 . . ?
C18S C17S H17B 110.2 . . ?
H17A C17S H17B 108.5 . . ?
C7 C6 H6 119.8 . . ?
C5 C6 C7 120.4(5) . . ?
C5 C6 H6 119.8 . . ?
O7S C28S C27S 108.4(4) . . ?
O7S C28S H28A 110.0 . . ?
O7S C28S H28B 110.0 . . ?
C27S C28S H28A 110.0 . . ?
C27S C28S H28B 110.0 . . ?
H28A C28S H28B 108.4 . . ?
O9S C20S H20A 110.3 . . ?
O9S C20S H20B 110.3 . . ?
O9S C20S C19S 107.2(4) . . ?
H20A C20S H20B 108.5 . . ?
C19S C20S H20A 110.3 . . ?
C19S C20S H20B 110.3 . . ?
O9S C21S C22S 107.6(4) . . ?
O9S C21S H21A 110.2 . . ?
O9S C21S H21B 110.2 . . ?
C22S C21S H21A 110.2 . . ?
C22S C21S H21B 110.2 . . ?
H21A C21S H21B 108.5 . . ?
O8S C19S C20S 107.7(4) . . ?
O8S C19S H19A 110.2 . . ?
O8S C19S H19B 110.2 . . ?
C20S C19S H19A 110.2 . . ?
C20S C19S H19B 110.2 . . ?
H19A C19S H19B 108.5 . . ?
O4S C16S C15S 107.5(4) . . ?
O4S C16S H16A 110.2 . . ?
O4S C16S H16B 110.2 . . ?
C15S C16S H16A 110.2 . . ?
C15S C16S H16B 110.2 . . ?
H16A C16S H16B 108.5 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.7(5) . . ?
C6 C5 H5 120.2 . . ?
C6A C5A C4A 120.7(5) . . ?
C6A C5A H5A 119.7 . . ?
C4A C5A H5A 119.7 . . ?
O3S C12S H12A 110.6 . . ?
O3S C12S H12B 110.6 . . ?
O3S C12S C11S 105.6(5) . . ?
H12A C12S H12B 108.7 . . ?
C11S C12S H12A 110.6 . . ?
C11S C12S H12B 110.6 . . ?
H8SA C8S H8SB 108.5 . . ?
O2S C8S H8SA 110.2 . . ?
O2S C8S H8SB 110.2 . . ?
O2S C8S C7S 107.4(6) . . ?
C7S C8S H8SA 110.2 . . ?
C7S C8S H8SB 110.2 . . ?
O3S C9S H9SA 110.7 . . ?
O3S C9S H9SB 110.7 . . ?
O3S C9S C10S 105.4(6) . . ?
H9SA C9S H9SB 108.8 . . ?
C10S C9S H9SA 110.7 . . ?
C10S C9S H9SB 110.7 . . ?
C8S O2S C5S 109.6(7) . . ?
O1S C4S H4SA 110.2 . . ?
O1S C4S H4SB 110.2 . . ?
O1S C4S C3S 107.4(6) . . ?
H4SA C4S H4SB 108.5 . . ?
C3S C4S H4SA 110.2 . . ?
C3S C4S H4SB 110.2 . . ?
C8S C7S H7SA 111.1 . . ?
C8S C7S H7SB 111.1 . . ?
C8S C7S C6S 103.3(7) . . ?
H7SA C7S H7SB 109.1 . . ?
C6S C7S H7SA 111.1 . . ?
C6S C7S H7SB 111.1 . . ?
O1S C1S H1SA 110.8 . . ?
O1S C1S H1SB 110.8 . . ?
O1S C1S C2S 104.7(6) . . ?
H1SA C1S H1SB 108.9 . . ?
C2S C1S H1SA 110.8 . . ?
C2S C1S H1SB 110.8 . . ?
C12S C11S H11A 110.6 . . ?
C12S C11S H11B 110.6 . . ?
H11A C11S H11B 108.7 . . ?
C10S C11S C12S 105.8(6) . . ?
C10S C11S H11A 110.6 . . ?
C10S C11S H11B 110.6 . . ?
C1S C2S H2SA 110.5 . . ?
C1S C2S H2SB 110.5 . . ?
H2SA C2S H2SB 108.7 . . ?
C3S C2S C1S 106.2(6) . . ?
C3S C2S H2SA 110.5 . . ?
C3S C2S H2SB 110.5 . . ?
C4S C3S H3SA 110.9 . . ?
C4S C3S H3SB 110.9 . . ?
C2S C3S C4S 104.1(6) . . ?
C2S C3S H3SA 110.9 . . ?
C2S C3S H3SB 110.9 . . ?
H3SA C3S H3SB 109.0 . . ?
O2S C5S H5SA 110.2 . . ?
O2S C5S H5SB 110.2 . . ?
O2S C5S C6S 107.3(7) . . ?
H5SA C5S H5SB 108.5 . . ?
C6S C5S H5SA 110.2 . . ?
C6S C5S H5SB 110.2 . . ?
C7S C6S H6SA 110.9 . . ?
C7S C6S H6SB 110.9 . . ?
C5S C6S C7S 104.5(7) . . ?
C5S C6S H6SA 110.9 . . ?
C5S C6S H6SB 110.9 . . ?
H6SA C6S H6SB 108.9 . . ?
C9S C10S H10A 110.5 . . ?
C9S C10S H10B 110.5 . . ?
C11S C10S C9S 106.2(7) . . ?
C11S C10S H10A 110.5 . . ?
C11S C10S H10B 110.5 . . ?
H10A C10S H10B 108.7 . . ?

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
Mo01 P1A C1A O1A -11.5(5) . . . . ?
Mo01 P1A C1A N1A 172.1(2) . . . . ?
Mo01 P1B C1B O1B 6.2(5) . . . . ?
Mo01 P1B C1B N1B -170.0(2) . . . . ?
Mo01 P1C C1C O1C -11.5(5) . . . . ?
Mo01 P1C C1C N1C 174.4(2) . . . . ?
P1A P2A C2A N1A -0.6(3) . . . . ?
P1A P2A C2A C3A 176.6(4) . . . . ?
P1B P2B C2B N1B 1.4(3) . . . . ?
P1B P2B C2B C3B -177.6(4) . . . . ?
P2B P1B C1B O1B 175.9(4) . . . . ?
P2B P1B C1B N1B -0.3(3) . . . . ?
P2B C2B C3B C4B 178.1(4) . . . . ?
P1C P2C C2C N1C 1.5(3) . . . . ?
P1C P2C C2C C3C -178.2(4) . . . . ?
P2A P1A C1A O1A 177.1(4) . . . . ?
P2A P1A C1A N1A 0.7(4) . . . . ?
P2A C2A C3A C4A -177.7(4) . . . . ?
P2C P1C C1C O1C 175.6(4) . . . . ?
P2C P1C C1C N1C 1.6(3) . . . . ?
P2C C2C C3C C4C -178.6(4) . . . . ?
Na00 O5S C25S C26S 43.1(5) . . . . ?
Na00 O5S C24S C23S -46.0(5) . . . . ?
Na00 O10S C23S C24S -52.0(4) . . . . ?
Na00 O10S C22S C21S 46.1(5) . . . . ?
Na00 O6S C26S C25S 47.5(5) . . . . ?
Na00 O6S C27S C28S -34.4(6) . . . . ?
Na00 O8S C18S C17S 50.0(5) . . . . ?
Na00 O8S C19S C20S -50.2(5) . . . . ?
Na00 O7S C17S C18S 49.4(5) . . . . ?
Na00 O7S C28S C27S -57.7(5) . . . . ?
Na00 O9S C20S C19S -45.2(5) . . . . ?
Na00 O9S C21S C22S 51.2(5) . . . . ?
Na00 O3S C12S C11S 160.9(4) . . . . ?
Na00 O3S C9S C10S -156.3(6) . . . . ?
Na00 O4S C13S C14S 142.6(4) . . . . ?
Na00 O4S C16S C15S -161.4(4) . . . . ?
O5S C25S C26S O6S -58.4(6) . . . . ?
O10S C23S C24S O5S 65.1(5) . . . . ?
O10S C22S C21S O9S -63.5(6) . . . . ?
O6S C27S C28S O7S 61.0(6) . . . . ?
O8S C18S C17S O7S -65.6(5) . . . . ?
N1C C2C C3C C4C 1.7(7) . . . . ?
N1C C6C C5C C4C 1.3(7) . . . . ?
O9S C20S C19S O8S 61.1(6) . . . . ?
N1A C2A C3A C4A -0.4(7) . . . . ?
N1A C6A C5A C4A 1.3(7) . . . . ?
N1B C2B C3B C4B -1.0(7) . . . . ?
O3S C12S C11S C10S 11.9(9) . . . . ?
O3S C9S C10S C11S -25.2(10) . . . . ?
C1B O1B B1 O1C -102.3(5) . . . . ?
C1B O1B B1 O1A 18.9(6) . . . . ?
C1B O1B B1 C2 136.9(4) . . . . ?
C1B N1B C2B P2B -2.0(5) . . . . ?
C1B N1B C2B C3B 177.2(4) . . . . ?
C1B N1B C6B C5B -176.4(4) . . . . ?
C1C O1C B1 O1B 11.8(6) . . . . ?
C1C O1C B1 O1A -107.0(4) . . . . ?
C1C O1C B1 C2 133.7(4) . . . . ?
C1C N1C C2C P2C -0.7(5) . . . . ?
C1C N1C C2C C3C 179.0(4) . . . . ?
C1C N1C C6C C5C 179.5(4) . . . . ?
C1A O1A B1 O1C -11.3(6) . . . . ?
C1A O1A B1 O1B -131.8(4) . . . . ?
C1A O1A B1 C2 108.4(5) . . . . ?
C1A N1A C2A P2A 1.2(5) . . . . ?
C1A N1A C2A C3A -176.3(4) . . . . ?
C1A N1A C6A C5A 175.8(4) . . . . ?
C2B N1B C1B P1B 1.4(5) . . . . ?
C2B N1B C1B O1B -175.5(3) . . . . ?
C2B N1B C6B C5B -0.1(6) . . . . ?
C2C N1C C1C P1C -0.8(5) . . . . ?
C2C N1C C1C O1C -175.7(4) . . . . ?
C2C N1C C6C C5C 0.9(7) . . . . ?
C2C C3C C4C C5C 0.5(8) . . . . ?
O1S C4S C3S C2S 12.9(10) . . . . ?
O1S C1S C2S C3S -25.4(9) . . . . ?
C2A N1A C1A P1A -1.2(5) . . . . ?
C2A N1A C1A O1A -177.9(4) . . . . ?
C2A N1A C6A C5A -4.2(7) . . . . ?
C2A C3A C4A C5A -2.3(8) . . . . ?
C5B C4B C3B C2B 0.8(7) . . . . ?
C4B C5B C6B N1B -0.2(7) . . . . ?
C3 C2 C7 C6 0.3(7) . . . . ?
C3 C2 B1 O1C 17.3(6) . . . . ?
C3 C2 B1 O1B 138.8(4) . . . . ?
C3 C2 B1 O1A -103.7(5) . . . . ?
C3 C4 C5 C6 -0.3(8) . . . . ?
C2 C3 C4 C5 -0.3(8) . . . . ?
C2 C7 C6 C5 -0.9(8) . . . . ?
C3A C4A C5A C6A 1.9(8) . . . . ?
C6B N1B C1B P1B 177.9(3) . . . . ?
C6B N1B C1B O1B 0.9(5) . . . . ?
C6B N1B C2B P2B -178.5(3) . . . . ?
C6B N1B C2B C3B 0.7(6) . . . . ?
C6B C5B C4B C3B -0.2(7) . . . . ?
C6C N1C C1C P1C -179.4(3) . . . . ?
C6C N1C C1C O1C 5.7(6) . . . . ?
C6C N1C C2C P2C 177.9(3) . . . . ?
C6C N1C C2C C3C -2.4(6) . . . . ?
C6C C5C C4C C3C -2.0(8) . . . . ?
C7 C2 B1 O1C -169.1(4) . . . . ?
C7 C2 B1 O1B -47.6(6) . . . . ?
C7 C2 B1 O1A 69.9(5) . . . . ?
C7 C6 C5 C4 0.9(8) . . . . ?
C14S C15S C16S O4S 11.1(6) . . . . ?
C23S O10S C22S C21S 176.1(4) . . . . ?
C6A N1A C1A P1A 178.9(3) . . . . ?
C6A N1A C1A O1A 2.2(6) . . . . ?
C6A N1A C2A P2A -178.9(3) . . . . ?
C6A N1A C2A C3A 3.7(6) . . . . ?
C25S O5S C24S C23S 176.7(4) . . . . ?
C22S O10S C23S C24S 177.0(4) . . . . ?
C26S O6S C27S C28S -177.6(5) . . . . ?
C18S O8S C19S C20S 171.8(4) . . . . ?
C27S O6S C26S C25S -168.3(4) . . . . ?
C24S O5S C25S C26S 180.0(4) . . . . ?
C15S C14S C13S O4S 37.9(5) . . . . ?
B1 O1C C1C P1C 74.7(6) . . . . ?
B1 O1C C1C N1C -111.2(5) . . . . ?
B1 O1B C1B P1B 44.8(7) . . . . ?
B1 O1B C1B N1B -138.9(4) . . . . ?
B1 O1A C1A P1A 86.2(5) . . . . ?
B1 O1A C1A N1A -97.4(5) . . . . ?
B1 C2 C7 C6 -173.8(4) . . . . ?
C13S O4S C16S C15S 13.1(6) . . . . ?
C13S C14S C15S C16S -29.1(5) . . . . ?
C4 C3 C2 C7 0.3(7) . . . . ?
C4 C3 C2 B1 174.3(4) . . . . ?
C17S O7S C28S C27S 174.6(4) . . . . ?
C28S O7S C17S C18S 175.7(4) . . . . ?
C20S O9S C21S C22S -168.6(5) . . . . ?
C21S O9S C20S C19S 175.3(4) . . . . ?
C19S O8S C18S C17S -172.0(4) . . . . ?
C16S O4S C13S C14S -32.4(6) . . . . ?
C12S O3S C9S C10S 33.2(7) . . . . ?
C12S C11S C10S C9S 7.9(11) . . . . ?
C8S O2S C5S C6S 23.4(12) . . . . ?
C8S C7S C6S C5S 23.1(10) . . . . ?
C9S O3S C12S C11S -28.1(7) . . . . ?
O2S C8S C7S C6S -9.7(8) . . . . ?
O2S C5S C6S C7S -28.7(12) . . . . ?
C4S O1S C1S C2S 34.2(8) . . . . ?
C7S C8S O2S C5S -7.8(10) . . . . ?
C1S O1S C4S C3S -29.6(9) . . . . ?
C1S C2S C3S C4S 7.8(10) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'nylon tip'
_olex2_submission_original_sample_id RS7041
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_rs3104
_database_code_depnum_ccdc_archive 'CCDC 1494722'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_audit_creation_date             2016-07-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H17 Mo N3 O6 P6 Ti, C4 H8 O1'
_chemical_formula_sum            'C30 H25 Mo N3 O7 P6 Ti'
_chemical_formula_weight         869.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mo1 Ti1 P6 O6 N6 C50 H50'
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'
Mo Mo -1.6832 0.6857 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   11.0367(3)
_cell_length_b                   19.6039(7)
_cell_length_c                   15.6787(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.440(3)
_cell_angle_gamma                90
_cell_volume                     3386.17(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6202
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.3140
_cell_measurement_theta_min      3.1050
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_preparation       'From saturated THF solution at RT'
_exptl_crystal_recrystallization_method 'From saturated THF solution at RT'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.1100
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25661
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.781
_diffrn_ambient_temperature      100
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -102.00  -61.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303 -179.0000  120.0000 41

#__ type_ start__ end____ width___ exp.time_
  2 omega  -97.00  -61.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303 -179.0000   30.0000 36

#__ type_ start__ end____ width___ exp.time_
  3 omega -101.00  -61.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303 -179.0000 -150.0000 40

#__ type_ start__ end____ width___ exp.time_
  4 omega  -35.00   97.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990    0.0000    0.0000 132

#__ type_ start__ end____ width___ exp.time_
  5 omega  -96.00  -27.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303  -77.0000  120.0000 69
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_UB_11      0.0168847000
_diffrn_orient_matrix_UB_12      0.0189386000
_diffrn_orient_matrix_UB_13      -0.0359462000
_diffrn_orient_matrix_UB_21      -0.0409474000
_diffrn_orient_matrix_UB_22      0.0262765000
_diffrn_orient_matrix_UB_23      0.0101571000
_diffrn_orient_matrix_UB_31      0.0467754000
_diffrn_orient_matrix_UB_32      0.0161299000
_diffrn_orient_matrix_UB_33      0.0256171000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6988
_reflns_number_total             10325
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.469
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         10325
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0563
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0246P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0926
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C27-O7 \\sim O8-C34 \\sim O8-C31 \\sim C27-C28
 with sigma of 0.02
 C30-O7 \\sim C30-C29 \\sim C29-C28 \\sim C32-C31 \\sim C32-C33 \\sim C33-C34
 with sigma of 0.002
 O8-C34 \\sim O7-C30 \\sim O8-C31 \\sim O7-C27
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C27) = Uanis(C31)
Uanis(C28) = Uanis(C32)
Uanis(C29) = Uanis(C33)
Uanis(C30) = Uanis(C34)
Uanis(O7) = Uanis(O8)
4. Rigid body (RIGU) restrains
 C28, C27, C29, O7, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C33, C34, O8, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=
 Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(O8)=1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(O7)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C16(H16), C9(H9), C11(H11), C6(H6), C18(H18), C20(H20), C12(H12),
 C21(H21), C15(H15), C22(H22), C19(H19), C4(H4), C5(H5), C10(H10), C17(H17),
 C1A(H1A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.29505(2) 0.47091(2) 0.75907(2) 0.01323(7) Uani 1 1 d . . . . .
Ti1 Ti -0.09518(5) 0.57992(3) 0.76737(4) 0.01401(13) Uani 1 1 d . . . . .
P5 P 0.27626(7) 0.59581(5) 0.77067(6) 0.01537(19) Uani 1 1 d . . . . .
P1 P 0.14289(7) 0.43861(5) 0.86295(6) 0.01583(19) Uani 1 1 d . . . . .
P3 P 0.13626(7) 0.45484(4) 0.64129(6) 0.01591(19) Uani 1 1 d . . . . .
P2 P 0.13326(8) 0.34484(5) 0.92760(6) 0.0200(2) Uani 1 1 d . . . . .
P4 P 0.12990(8) 0.38401(5) 0.54029(6) 0.0215(2) Uani 1 1 d . . . . .
P6 P 0.41312(8) 0.67033(5) 0.77393(6) 0.0190(2) Uani 1 1 d . . . . .
O2 O -0.07417(18) 0.51668(11) 0.68350(15) 0.0197(5) Uani 1 1 d . . . . .
O1 O -0.05281(19) 0.52554(12) 0.86249(14) 0.0194(5) Uani 1 1 d . . . . .
O3 O 0.03815(18) 0.63582(11) 0.76013(14) 0.0177(5) Uani 1 1 d . . . . .
N1 N -0.0664(2) 0.42399(14) 0.93539(16) 0.0148(6) Uani 1 1 d . . . . .
N2 N -0.0872(2) 0.44119(14) 0.57009(17) 0.0152(6) Uani 1 1 d . . . . .
N3 N 0.1830(2) 0.72023(13) 0.76287(17) 0.0141(6) Uani 1 1 d . . . . .
O6 O 0.3417(2) 0.31434(13) 0.74071(17) 0.0280(6) Uani 1 1 d . . . . .
O4 O 0.4968(2) 0.49050(13) 0.62843(17) 0.0305(6) Uani 1 1 d . . . . .
C2 C -0.0124(3) 0.36205(17) 0.9604(2) 0.0175(7) Uani 1 1 d . . . . .
O5 O 0.5051(2) 0.47561(15) 0.90339(17) 0.0358(7) Uani 1 1 d . . . . .
C14 C 0.3069(3) 0.73673(17) 0.7672(2) 0.0167(7) Uani 1 1 d . . . . .
C3 C -0.0805(3) 0.31690(18) 1.0083(2) 0.0220(8) Uani 1 1 d . . . . .
H3 H -0.0446 0.2753 1.0279 0.026 Uiso 1 1 calc R . . . .
C16 C 0.2498(3) 0.85611(18) 0.7575(2) 0.0240(8) Uani 1 1 d . . . . .
H16 H 0.2719 0.9029 0.7549 0.029 Uiso 1 1 calc R . . . .
C26 C 0.3233(3) 0.37183(18) 0.7476(2) 0.0167(7) Uani 1 1 d . . . . .
C9 C -0.0974(3) 0.35899(18) 0.4569(2) 0.0238(8) Uani 1 1 d . . . . .
H9 H -0.0586 0.3282 0.4205 0.029 Uiso 1 1 calc R . . . .
C11 C -0.2773(3) 0.41449(18) 0.4991(2) 0.0242(8) Uani 1 1 d . . . . .
H11 H -0.3626 0.4210 0.4921 0.029 Uiso 1 1 calc R . . . .
C7 C -0.0171(3) 0.47475(17) 0.6338(2) 0.0160(7) Uani 1 1 d . . . . .
C6 C -0.1847(3) 0.43935(18) 0.9560(2) 0.0184(7) Uani 1 1 d . . . . .
H6 H -0.2203 0.4816 0.9385 0.022 Uiso 1 1 calc R . . . .
C1 C -0.0002(3) 0.46712(17) 0.8856(2) 0.0154(7) Uani 1 1 d . . . . .
C18 C 0.0953(3) 0.77082(17) 0.7574(2) 0.0188(8) Uani 1 1 d . . . . .
H18 H 0.0120 0.7584 0.7553 0.023 Uiso 1 1 calc R . . . .
C25 C 0.4259(3) 0.47441(18) 0.8515(2) 0.0198(7) Uani 1 1 d . . . . .
C20 C -0.2247(3) 0.67048(18) 0.7201(2) 0.0245(8) Uani 1 1 d . . . . .
H20 H -0.1970 0.7038 0.6818 0.029 Uiso 1 1 calc R . . . .
C12 C -0.2115(3) 0.45111(18) 0.5589(2) 0.0189(7) Uani 1 1 d . . . . .
H12 H -0.2506 0.4835 0.5931 0.023 Uiso 1 1 calc R . . . .
C21 C -0.2850(3) 0.60966(19) 0.6975(2) 0.0237(8) Uani 1 1 d . . . . .
H21 H -0.3062 0.5947 0.6410 0.028 Uiso 1 1 calc R . . . .
C8 C -0.0269(3) 0.39534(17) 0.5195(2) 0.0181(7) Uani 1 1 d . . . . .
C15 C 0.3364(3) 0.80710(18) 0.7637(2) 0.0221(8) Uani 1 1 d . . . . .
H15 H 0.4194 0.8202 0.7657 0.027 Uiso 1 1 calc R . . . .
C28 C -0.6078(5) 0.2451(3) 1.0468(3) 0.0242(12) Uani 0.843(6) 1 d D U P A 1
H28A H -0.6937 0.2403 1.0256 0.029 Uiso 0.843(6) 1 calc R . P A 1
H28B H -0.6045 0.2590 1.1076 0.029 Uiso 0.843(6) 1 calc R . P A 1
C22 C -0.3088(3) 0.57457(19) 0.7727(2) 0.0228(8) Uani 1 1 d . . . . .
H22 H -0.3482 0.5316 0.7759 0.027 Uiso 1 1 calc R . . . .
C19 C -0.2125(3) 0.67331(18) 0.8100(2) 0.0224(8) Uani 1 1 d . . . . .
H19 H -0.1757 0.7091 0.8431 0.027 Uiso 1 1 calc R . . . .
C24 C 0.4209(3) 0.48489(18) 0.6752(2) 0.0205(8) Uani 1 1 d . . . . .
C27 C -0.5388(5) 0.1804(3) 1.0351(2) 0.0292(13) Uani 0.843(6) 1 d D U P A 1
H27A H -0.4650 0.1791 1.0742 0.035 Uiso 0.843(6) 1 calc R . P A 1
H27B H -0.5898 0.1403 1.0467 0.035 Uiso 0.843(6) 1 calc R . P A 1
C4 C -0.2640(3) 0.61414(19) 0.8420(2) 0.0232(8) Uani 1 1 d . . . . .
H4 H -0.2680 0.6027 0.9006 0.028 Uiso 1 1 calc R . . . .
C13 C 0.1549(3) 0.65139(17) 0.7644(2) 0.0150(7) Uani 1 1 d . . . . .
C5 C -0.2486(3) 0.39459(18) 1.0007(2) 0.0205(8) Uani 1 1 d . . . . .
H5 H -0.3290 0.4055 1.0144 0.025 Uiso 1 1 calc R . . . .
C10 C -0.2205(3) 0.36704(19) 0.4475(2) 0.0250(8) Uani 1 1 d . . . . .
H10 H -0.2671 0.3408 0.4065 0.030 Uiso 1 1 calc R . . . .
C17 C 0.1258(3) 0.83684(18) 0.7549(2) 0.0209(8) Uani 1 1 d . . . . .
H17 H 0.0643 0.8708 0.7515 0.025 Uiso 1 1 calc R . . . .
C29 C -0.5424(6) 0.2948(3) 0.9942(3) 0.0294(14) Uani 0.843(6) 1 d D U P A 1
H29A H -0.5985 0.3306 0.9711 0.035 Uiso 0.843(6) 1 calc R . P A 1
H29B H -0.4753 0.3168 1.0288 0.035 Uiso 0.843(6) 1 calc R . P A 1
C1A C -0.1966(3) 0.33140(19) 1.0273(2) 0.0227(8) Uani 1 1 d . . . . .
H1A H -0.2422 0.2996 1.0580 0.027 Uiso 1 1 calc R . . . .
C30 C -0.4942(7) 0.2541(2) 0.9236(4) 0.0395(13) Uani 0.843(6) 1 d D U P A 1
H30A H -0.5406 0.2644 0.8691 0.047 Uiso 0.843(6) 1 calc R . P A 1
H30B H -0.4079 0.2657 0.9171 0.047 Uiso 0.843(6) 1 calc R . P A 1
O7 O -0.5058(3) 0.18048(18) 0.94468(19) 0.0382(10) Uani 0.843(6) 1 d D U P A 1
C31 C -0.548(2) 0.1779(14) 1.010(2) 0.0292(13) Uani 0.157(6) 1 d D U P A 2
H31A H -0.5248 0.1558 1.0656 0.035 Uiso 0.157(6) 1 calc R . P A 2
H31B H -0.5922 0.1449 0.9720 0.035 Uiso 0.157(6) 1 calc R . P A 2
C32 C -0.619(3) 0.2416(14) 1.0211(19) 0.0242(12) Uani 0.157(6) 1 d D U P A 2
H32A H -0.6221 0.2526 1.0826 0.029 Uiso 0.157(6) 1 calc R . P A 2
H32B H -0.7026 0.2360 0.9962 0.029 Uiso 0.157(6) 1 calc R . P A 2
C33 C -0.556(4) 0.2971(17) 0.976(2) 0.0294(14) Uani 0.157(6) 1 d D U P A 2
H33A H -0.6125 0.3328 0.9536 0.035 Uiso 0.157(6) 1 calc R . P A 2
H33B H -0.4892 0.3180 1.0124 0.035 Uiso 0.157(6) 1 calc R . P A 2
C34 C -0.511(4) 0.2526(16) 0.9081(19) 0.0395(13) Uani 0.157(6) 1 d D U P A 2
H34A H -0.5769 0.2283 0.8751 0.047 Uiso 0.157(6) 1 calc R . P A 2
H34B H -0.4586 0.2771 0.8692 0.047 Uiso 0.157(6) 1 calc R . P A 2
O8 O -0.4414(17) 0.2078(10) 0.9700(11) 0.0382(10) Uani 0.157(6) 1 d 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
Mo1 P5 2.4651(9) . ?
Mo1 P1 2.4903(9) . ?
Mo1 P3 2.4885(9) . ?
Mo1 C26 1.977(3) . ?
Mo1 C25 1.984(3) . ?
Mo1 C24 1.988(3) . ?
Ti1 O2 1.832(2) . ?
Ti1 O1 1.870(2) . ?
Ti1 O3 1.844(2) . ?
Ti1 C20 2.370(3) . ?
Ti1 C21 2.378(3) . ?
Ti1 C22 2.366(3) . ?
Ti1 C19 2.362(3) . ?
Ti1 C4 2.356(3) . ?
P5 P6 2.0998(12) . ?
P5 C13 1.725(3) . ?
P1 P2 2.1048(13) . ?
P1 C1 1.732(3) . ?
P3 P4 2.1041(13) . ?
P3 C7 1.734(3) . ?
P2 C2 1.750(3) . ?
P4 C8 1.755(3) . ?
P6 C14 1.751(3) . ?
O2 C7 1.319(4) . ?
O1 C1 1.324(4) . ?
O3 C13 1.322(3) . ?
N1 C2 1.398(4) . ?
N1 C6 1.396(4) . ?
N1 C1 1.388(4) . ?
N2 C7 1.392(4) . ?
N2 C12 1.387(4) . ?
N2 C8 1.394(4) . ?
N3 C14 1.403(4) . ?
N3 C18 1.385(4) . ?
N3 C13 1.385(4) . ?
O6 C26 1.152(4) . ?
O4 C24 1.151(4) . ?
C2 C3 1.407(5) . ?
O5 C25 1.158(4) . ?
C14 C15 1.420(5) . ?
C3 H3 0.9500 . ?
C3 C1A 1.363(5) . ?
C16 H16 0.9500 . ?
C16 C15 1.355(5) . ?
C16 C17 1.418(5) . ?
C9 H9 0.9500 . ?
C9 C8 1.409(5) . ?
C9 C10 1.367(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.356(5) . ?
C11 C10 1.405(5) . ?
C6 H6 0.9500 . ?
C6 C5 1.348(5) . ?
C18 H18 0.9500 . ?
C18 C17 1.338(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.401(5) . ?
C20 C19 1.409(5) . ?
C12 H12 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.402(5) . ?
C15 H15 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C27 1.497(5) . ?
C28 C29 1.490(3) . ?
C22 H22 0.9500 . ?
C22 C4 1.401(5) . ?
C19 H19 0.9500 . ?
C19 C4 1.398(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 O7 1.484(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C5 C1A 1.418(5) . ?
C10 H10 0.9500 . ?
C17 H17 0.9500 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.488(3) . ?
C1A H1A 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 O7 1.487(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.488(3) . ?
C31 O8 1.488(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.488(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.488(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 O8 1.488(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P5 Mo1 P1 98.12(3) . . ?
P5 Mo1 P3 97.00(3) . . ?
P3 Mo1 P1 88.89(3) . . ?
C26 Mo1 P5 175.57(9) . . ?
C26 Mo1 P1 85.74(10) . . ?
C26 Mo1 P3 85.20(9) . . ?
C26 Mo1 C25 89.33(14) . . ?
C26 Mo1 C24 87.43(14) . . ?
C25 Mo1 P5 88.43(11) . . ?
C25 Mo1 P1 91.21(10) . . ?
C25 Mo1 P3 174.50(11) . . ?
C25 Mo1 C24 88.35(13) . . ?
C24 Mo1 P5 88.68(10) . . ?
C24 Mo1 P1 173.17(10) . . ?
C24 Mo1 P3 90.90(10) . . ?
O2 Ti1 O1 98.64(11) . . ?
O2 Ti1 O3 102.84(10) . . ?
O2 Ti1 C20 112.48(12) . . ?
O2 Ti1 C21 88.93(11) . . ?
O2 Ti1 C22 99.46(11) . . ?
O2 Ti1 C19 145.38(11) . . ?
O2 Ti1 C4 133.38(12) . . ?
O1 Ti1 C20 142.55(12) . . ?
O1 Ti1 C21 132.73(12) . . ?
O1 Ti1 C22 98.56(11) . . ?
O1 Ti1 C19 109.34(12) . . ?
O1 Ti1 C4 86.20(11) . . ?
O3 Ti1 O1 103.04(10) . . ?
O3 Ti1 C20 90.23(11) . . ?
O3 Ti1 C21 120.69(12) . . ?
O3 Ti1 C22 146.00(12) . . ?
O3 Ti1 C19 90.55(11) . . ?
O3 Ti1 C4 121.28(12) . . ?
C20 Ti1 C21 34.32(12) . . ?
C22 Ti1 C20 57.37(12) . . ?
C22 Ti1 C21 34.38(12) . . ?
C19 Ti1 C20 34.65(12) . . ?
C19 Ti1 C21 57.15(12) . . ?
C19 Ti1 C22 57.34(12) . . ?
C4 Ti1 C20 57.45(13) . . ?
C4 Ti1 C21 57.15(13) . . ?
C4 Ti1 C22 34.51(12) . . ?
C4 Ti1 C19 34.47(12) . . ?
P6 P5 Mo1 129.00(4) . . ?
C13 P5 Mo1 133.77(12) . . ?
C13 P5 P6 96.71(12) . . ?
P2 P1 Mo1 126.34(5) . . ?
C1 P1 Mo1 135.30(12) . . ?
C1 P1 P2 96.32(12) . . ?
P4 P3 Mo1 129.22(5) . . ?
C7 P3 Mo1 131.53(12) . . ?
C7 P3 P4 96.26(12) . . ?
C2 P2 P1 92.70(12) . . ?
C8 P4 P3 92.53(12) . . ?
C14 P6 P5 92.15(11) . . ?
C7 O2 Ti1 158.7(2) . . ?
C1 O1 Ti1 142.7(2) . . ?
C13 O3 Ti1 156.0(2) . . ?
C2 N1 C6 120.7(3) . . ?
C1 N1 C2 117.2(3) . . ?
C1 N1 C6 122.0(3) . . ?
C7 N2 C8 116.7(3) . . ?
C12 N2 C7 121.9(3) . . ?
C12 N2 C8 121.4(3) . . ?
C18 N3 C14 120.9(3) . . ?
C18 N3 C13 122.9(3) . . ?
C13 N3 C14 116.2(3) . . ?
N1 C2 P2 118.0(2) . . ?
N1 C2 C3 117.6(3) . . ?
C3 C2 P2 124.4(3) . . ?
N3 C14 P6 118.6(2) . . ?
N3 C14 C15 116.6(3) . . ?
C15 C14 P6 124.8(3) . . ?
C2 C3 H3 119.2 . . ?
C1A C3 C2 121.7(3) . . ?
C1A C3 H3 119.2 . . ?
C15 C16 H16 120.4 . . ?
C15 C16 C17 119.3(3) . . ?
C17 C16 H16 120.4 . . ?
O6 C26 Mo1 178.9(3) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?
C10 C9 C8 121.4(3) . . ?
C12 C11 H11 119.7 . . ?
C12 C11 C10 120.7(3) . . ?
C10 C11 H11 119.7 . . ?
O2 C7 P3 126.8(2) . . ?
O2 C7 N2 117.0(3) . . ?
N2 C7 P3 116.2(2) . . ?
N1 C6 H6 119.8 . . ?
C5 C6 N1 120.4(3) . . ?
C5 C6 H6 119.8 . . ?
O1 C1 P1 127.8(2) . . ?
O1 C1 N1 116.3(3) . . ?
N1 C1 P1 115.8(2) . . ?
N3 C18 H18 119.4 . . ?
C17 C18 N3 121.2(3) . . ?
C17 C18 H18 119.4 . . ?
O5 C25 Mo1 177.6(3) . . ?
Ti1 C20 H20 120.1 . . ?
C21 C20 Ti1 73.14(19) . . ?
C21 C20 H20 126.2 . . ?
C21 C20 C19 107.6(3) . . ?
C19 C20 Ti1 72.36(19) . . ?
C19 C20 H20 126.2 . . ?
N2 C12 H12 120.1 . . ?
C11 C12 N2 119.8(3) . . ?
C11 C12 H12 120.1 . . ?
Ti1 C21 H21 121.0 . . ?
C20 C21 Ti1 72.54(18) . . ?
C20 C21 H21 125.8 . . ?
C22 C21 Ti1 72.36(19) . . ?
C22 C21 C20 108.4(3) . . ?
C22 C21 H21 125.8 . . ?
N2 C8 P4 118.4(2) . . ?
N2 C8 C9 117.3(3) . . ?
C9 C8 P4 124.2(3) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 C14 121.9(3) . . ?
C16 C15 H15 119.0 . . ?
H28A C28 H28B 109.2 . . ?
C27 C28 H28A 111.2 . . ?
C27 C28 H28B 111.2 . . ?
C29 C28 H28A 111.2 . . ?
C29 C28 H28B 111.2 . . ?
C29 C28 C27 102.6(5) . . ?
Ti1 C22 H22 120.1 . . ?
C21 C22 Ti1 73.25(19) . . ?
C21 C22 H22 126.1 . . ?
C4 C22 Ti1 72.36(18) . . ?
C4 C22 C21 107.8(3) . . ?
C4 C22 H22 126.1 . . ?
Ti1 C19 H19 120.3 . . ?
C20 C19 Ti1 73.0(2) . . ?
C20 C19 H19 126.0 . . ?
C4 C19 Ti1 72.54(19) . . ?
C4 C19 C20 108.0(3) . . ?
C4 C19 H19 126.0 . . ?
O4 C24 Mo1 176.8(3) . . ?
C28 C27 H27A 110.6 . . ?
C28 C27 H27B 110.6 . . ?
H27A C27 H27B 108.7 . . ?
O7 C27 C28 105.8(4) . . ?
O7 C27 H27A 110.6 . . ?
O7 C27 H27B 110.6 . . ?
Ti1 C4 H4 119.8 . . ?
C22 C4 Ti1 73.13(19) . . ?
C22 C4 H4 125.9 . . ?
C19 C4 Ti1 72.98(19) . . ?
C19 C4 C22 108.3(3) . . ?
C19 C4 H4 125.9 . . ?
O3 C13 P5 127.5(3) . . ?
O3 C13 N3 116.3(3) . . ?
N3 C13 P5 116.3(2) . . ?
C6 C5 H5 119.8 . . ?
C6 C5 C1A 120.4(3) . . ?
C1A C5 H5 119.8 . . ?
C9 C10 C11 119.3(3) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 120.1(3) . . ?
C18 C17 H17 120.0 . . ?
C28 C29 H29A 110.6 . . ?
C28 C29 H29B 110.6 . . ?
H29A C29 H29B 108.8 . . ?
C30 C29 C28 105.6(5) . . ?
C30 C29 H29A 110.6 . . ?
C30 C29 H29B 110.6 . . ?
C3 C1A C5 119.1(3) . . ?
C3 C1A H1A 120.4 . . ?
C5 C1A H1A 120.4 . . ?
C29 C30 H30A 110.0 . . ?
C29 C30 H30B 110.0 . . ?
H30A C30 H30B 108.4 . . ?
O7 C30 C29 108.4(5) . . ?
O7 C30 H30A 110.0 . . ?
O7 C30 H30B 110.0 . . ?
C27 O7 C30 104.0(4) . . ?
H31A C31 H31B 109.7 . . ?
C32 C31 H31A 112.0 . . ?
C32 C31 H31B 112.0 . . ?
O8 C31 H31A 112.0 . . ?
O8 C31 H31B 112.0 . . ?
O8 C31 C32 99(2) . . ?
C31 C32 H32A 110.2 . . ?
C31 C32 H32B 110.2 . . ?
C31 C32 C33 107(3) . . ?
H32A C32 H32B 108.5 . . ?
C33 C32 H32A 110.2 . . ?
C33 C32 H32B 110.2 . . ?
C32 C33 H33A 112.7 . . ?
C32 C33 H33B 112.7 . . ?
H33A C33 H33B 110.1 . . ?
C34 C33 C32 95(3) . . ?
C34 C33 H33A 112.7 . . ?
C34 C33 H33B 112.6 . . ?
C33 C34 H34A 113.0 . . ?
C33 C34 H34B 113.0 . . ?
H34A C34 H34B 110.4 . . ?
O8 C34 C33 93(2) . . ?
O8 C34 H34A 113.0 . . ?
O8 C34 H34B 113.0 . . ?
C31 O8 C34 97(2) . . ?

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
Mo1 P5 C13 O3 7.9(4) . . . . ?
Mo1 P5 C13 N3 -171.50(16) . . . . ?
Mo1 P1 C1 O1 -16.5(4) . . . . ?
Mo1 P1 C1 N1 164.94(16) . . . . ?
Mo1 P3 C7 O2 16.5(4) . . . . ?
Mo1 P3 C7 N2 -161.35(18) . . . . ?
Ti1 O2 C7 P3 6.1(8) . . . . ?
Ti1 O2 C7 N2 -176.1(5) . . . . ?
Ti1 O1 C1 P1 54.3(5) . . . . ?
Ti1 O1 C1 N1 -127.2(3) . . . . ?
Ti1 O3 C13 P5 13.4(7) . . . . ?
Ti1 O3 C13 N3 -167.2(4) . . . . ?
Ti1 C20 C21 C22 63.9(2) . . . . ?
Ti1 C20 C19 C4 -64.6(2) . . . . ?
Ti1 C21 C22 C4 64.6(2) . . . . ?
Ti1 C22 C4 C19 65.0(2) . . . . ?
Ti1 C19 C4 C22 -65.1(2) . . . . ?
P5 P6 C14 N3 0.2(3) . . . . ?
P5 P6 C14 C15 -178.1(3) . . . . ?
P1 P2 C2 N1 0.4(2) . . . . ?
P1 P2 C2 C3 178.5(3) . . . . ?
P3 P4 C8 N2 -0.1(3) . . . . ?
P3 P4 C8 C9 -177.5(3) . . . . ?
P2 P1 C1 O1 179.8(3) . . . . ?
P2 P1 C1 N1 1.3(2) . . . . ?
P2 C2 C3 C1A -175.7(3) . . . . ?
P4 P3 C7 O2 177.7(3) . . . . ?
P4 P3 C7 N2 -0.1(3) . . . . ?
P6 P5 C13 O3 179.9(3) . . . . ?
P6 P5 C13 N3 0.5(2) . . . . ?
P6 C14 C15 C16 179.2(3) . . . . ?
O2 Ti1 O1 C1 14.1(3) . . . . ?
O2 Ti1 O3 C13 -63.8(5) . . . . ?
O1 Ti1 O2 C7 -68.9(6) . . . . ?
O1 Ti1 O3 C13 38.4(5) . . . . ?
O3 Ti1 O2 C7 36.7(6) . . . . ?
O3 Ti1 O1 C1 -91.3(3) . . . . ?
N1 C2 C3 C1A 2.4(5) . . . . ?
N1 C6 C5 C1A 0.0(5) . . . . ?
N3 C14 C15 C16 0.8(5) . . . . ?
N3 C18 C17 C16 0.4(5) . . . . ?
C2 N1 C6 C5 0.2(5) . . . . ?
C2 N1 C1 P1 -1.3(4) . . . . ?
C2 N1 C1 O1 -180.0(3) . . . . ?
C2 C3 C1A C5 -2.2(5) . . . . ?
C14 N3 C18 C17 0.9(5) . . . . ?
C14 N3 C13 P5 -0.4(4) . . . . ?
C14 N3 C13 O3 -179.9(3) . . . . ?
C7 N2 C12 C11 -176.4(3) . . . . ?
C7 N2 C8 P4 0.1(4) . . . . ?
C7 N2 C8 C9 177.6(3) . . . . ?
C6 N1 C2 P2 176.9(2) . . . . ?
C6 N1 C2 C3 -1.3(4) . . . . ?
C6 N1 C1 P1 -177.7(2) . . . . ?
C6 N1 C1 O1 3.6(4) . . . . ?
C6 C5 C1A C3 1.0(5) . . . . ?
C1 N1 C2 P2 0.5(4) . . . . ?
C1 N1 C2 C3 -177.8(3) . . . . ?
C1 N1 C6 C5 176.4(3) . . . . ?
C18 N3 C14 P6 -179.9(2) . . . . ?
C18 N3 C14 C15 -1.4(4) . . . . ?
C18 N3 C13 P5 179.6(2) . . . . ?
C18 N3 C13 O3 0.1(4) . . . . ?
C20 Ti1 O2 C7 132.3(6) . . . . ?
C20 Ti1 O1 C1 160.7(3) . . . . ?
C20 Ti1 O3 C13 -176.9(5) . . . . ?
C20 C21 C22 Ti1 -64.1(2) . . . . ?
C20 C21 C22 C4 0.6(4) . . . . ?
C20 C19 C4 Ti1 64.9(2) . . . . ?
C20 C19 C4 C22 -0.3(4) . . . . ?
C12 N2 C7 P3 178.1(2) . . . . ?
C12 N2 C7 O2 0.1(5) . . . . ?
C12 N2 C8 P4 -178.0(2) . . . . ?
C12 N2 C8 C9 -0.5(5) . . . . ?
C12 C11 C10 C9 -1.3(5) . . . . ?
C21 Ti1 O2 C7 157.9(6) . . . . ?
C21 Ti1 O1 C1 110.7(3) . . . . ?
C21 Ti1 O3 C13 -160.3(5) . . . . ?
C21 C20 C19 Ti1 65.2(2) . . . . ?
C21 C20 C19 C4 0.6(4) . . . . ?
C21 C22 C4 Ti1 -65.2(2) . . . . ?
C21 C22 C4 C19 -0.2(4) . . . . ?
C8 N2 C7 P3 0.1(4) . . . . ?
C8 N2 C7 O2 -178.0(3) . . . . ?
C8 N2 C12 C11 1.6(5) . . . . ?
C8 C9 C10 C11 2.5(5) . . . . ?
C15 C16 C17 C18 -1.0(5) . . . . ?
C28 C27 O7 C30 29.8(6) . . . . ?
C28 C29 C30 O7 -12.6(6) . . . . ?
C22 Ti1 O2 C7 -169.2(6) . . . . ?
C22 Ti1 O1 C1 115.2(3) . . . . ?
C22 Ti1 O3 C13 166.5(5) . . . . ?
C19 Ti1 O2 C7 147.0(6) . . . . ?
C19 Ti1 O1 C1 173.5(3) . . . . ?
C19 Ti1 O3 C13 148.4(5) . . . . ?
C19 C20 C21 Ti1 -64.7(2) . . . . ?
C19 C20 C21 C22 -0.7(4) . . . . ?
C27 C28 C29 C30 30.3(6) . . . . ?
C4 Ti1 O2 C7 -161.9(6) . . . . ?
C4 Ti1 O1 C1 147.5(3) . . . . ?
C4 Ti1 O3 C13 131.9(5) . . . . ?
C13 N3 C14 P6 0.1(4) . . . . ?
C13 N3 C14 C15 178.6(3) . . . . ?
C13 N3 C18 C17 -179.1(3) . . . . ?
C10 C9 C8 P4 175.8(3) . . . . ?
C10 C9 C8 N2 -1.6(5) . . . . ?
C10 C11 C12 N2 -0.8(5) . . . . ?
C17 C16 C15 C14 0.4(6) . . . . ?
C29 C28 C27 O7 -37.6(5) . . . . ?
C29 C30 O7 C27 -10.6(6) . . . . ?
C31 C32 C33 C34 32(3) . . . . ?
C32 C31 O8 C34 -45(3) . . . . ?
C32 C33 C34 O8 -59(3) . . . . ?
C33 C34 O8 C31 67(3) . . . . ?
O8 C31 C32 C33 8(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2014-03-05
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_rs4082b
_database_code_depnum_ccdc_archive 'CCDC 1495146'
_audit_update_record             
;
2016-07-21 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_audit_creation_date             2016-07-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.25(C84 H127.75 Mo4 N12 O16 P12), 0.87(C H2 Cl2), 0.5(C0.98 H2 Cl2)'
_chemical_formula_sum            'C22.36 H35.49 Cl2.75 Mo N3 O4 P3'
_chemical_formula_weight         696.76
_chemical_absolute_configuration ?
_chemical_melting_point          471
_chemical_oxdiff_formula         P3N3Mo1O6C50H50
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'

_cell_length_a                   59.1004(11)
_cell_length_b                   34.6994(6)
_cell_length_c                   12.38327(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     25394.9(8)
_cell_formula_units_Z            32
_cell_measurement_reflns_used    13414
_cell_measurement_temperature    106.05(13)
_cell_measurement_theta_max      31.7750
_cell_measurement_theta_min      3.3410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             11406
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       78
_diffrn_reflns_limit_h_min       -67
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            32415
_diffrn_reflns_point_group_measured_fraction_full 0.789
_diffrn_reflns_point_group_measured_fraction_max 0.762
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.963
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      106.05(13)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -80.00  -33.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  127.0000  -43.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega  -31.00   41.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865   57.0000  -60.0000 144

#__ type_ start__ end____ width___ exp.time_
  3 omega  -43.00   51.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -19.0000  -30.0000 188

#__ type_ start__ end____ width___ exp.time_
  4 omega -103.00  -70.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865 -179.0000   90.0000 66
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_UB_11      0.0019117000
_diffrn_orient_matrix_UB_12      0.0200754000
_diffrn_orient_matrix_UB_13      0.0054380000
_diffrn_orient_matrix_UB_21      -0.0118295000
_diffrn_orient_matrix_UB_22      0.0033614000
_diffrn_orient_matrix_UB_23      -0.0025006000
_diffrn_orient_matrix_UB_31      -0.0007084000
_diffrn_orient_matrix_UB_32      -0.0017793000
_diffrn_orient_matrix_UB_33      0.0569757000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.460
_reflns_Friedel_fraction_full    0.558
_reflns_Friedel_fraction_max     0.503
_reflns_number_gt                11466
_reflns_number_total             12027
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 
;
 Flack x determined using 3237 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         12027
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0471
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0494P)²+185.0356P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1093
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl6S) = Uanis(Cl5S)
Uanis(Cl7S) = Uanis(Cl8S)
Uanis(Cl1) = Uanis(C0AA) = Uanis(Cl3)
3. Others
 Sof(H3SC)=Sof(H3SD)=Sof(Cl6S)=Sof(Cl7S)=1-FVAR(1)
 Sof(Cl8S)=Sof(Cl5S)=Sof(H3SA)=Sof(H3SB)=FVAR(1)
 Sof(Cl4S)=Sof(Cl3S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=FVAR(2)
 Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C13A(H13A), C10A(H10A), C7A(H7A), C7(H7), C16A(H16A), C13(H13),
 C16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB), C3S(H3SC,H3SD), C2S(H2SA,H2SB), C0AA(H0AA,H0AB)
4.c Aromatic/amide H refined with riding coordinates:
 C5A(H5A), C5(H5), C4A(H4A), C6(H6), C6A(H6A), C4(H4), C3A(H3A), C3(H3)
4.d Idealised Me refined as rotating group:
 C17A(H17A,H17B,H17C), C9(H9A,H9B,H9C), C11A(H11A,H11B,H11C), C11(H11D,H11E,
 H11F), C8A(H8AA,H8AB,H8AC), C15A(H15A,H15B,H15C), C12(H12A,H12B,H12C),
 C12A(H12D,H12E,H12F), C18A(H18A,H18B,H18C), C14A(H14A,H14B,H14C), C8(H8A,H8B,
 H8C), C9A(H9AA,H9AB,H9AC), C17(H17D,H17E,H17F), C18(H18D,H18E,H18F), C15(H15D,
 H15E,H15F), C14(H14D,H14E,H14F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.51079(2) 0.60738(2) 0.33071(4) 0.01376(10) Uani 1 1 d . . . . .
Mo2 Mo 0.56072(2) 0.48278(2) 0.04242(4) 0.01395(10) Uani 1 1 d . . . . .
P2A P 0.53611(2) 0.54139(4) 0.04489(13) 0.0161(3) Uani 1 1 d . . . . .
P1A P 0.52128(3) 0.58045(4) 0.15334(12) 0.0146(3) Uani 1 1 d . . . . .
P3A P 0.49677(2) 0.65858(4) 0.20144(12) 0.0148(3) Uani 1 1 d . . . . .
P2 P 0.52308(2) 0.43592(4) 0.32940(13) 0.0166(3) Uani 1 1 d . . . . .
P1 P 0.54530(3) 0.46261(5) 0.22015(13) 0.0191(3) Uani 1 1 d . . . . .
P3 P 0.59085(3) 0.50592(5) 0.17300(13) 0.0197(3) Uani 1 1 d . . . . .
C5A C 0.51139(12) 0.6109(2) -0.2397(6) 0.0287(16) Uani 1 1 d . . . . .
H5A H 0.5063 0.6259 -0.2969 0.034 Uiso 1 1 calc R . . . .
C5 C 0.56413(15) 0.4789(2) 0.6147(6) 0.0342(17) Uani 1 1 d . . . . .
H5 H 0.5730 0.4878 0.6714 0.041 Uiso 1 1 calc R . . . .
C1A C 0.51077(9) 0.60984(16) 0.0534(5) 0.0146(11) Uani 1 1 d . . . . .
O1A O 0.49904(7) 0.64259(11) 0.0712(4) 0.0175(8) Uani 1 1 d . . . . .
C1 C 0.56262(11) 0.48022(18) 0.3204(6) 0.0245(14) Uani 1 1 d . . . . .
N1A N 0.51503(8) 0.60035(14) -0.0527(4) 0.0152(10) Uani 1 1 d . . . . .
N3A N 0.51264(8) 0.69904(14) 0.1833(4) 0.0177(10) Uani 1 1 d . . . . .
N3 N 0.59866(8) 0.55177(14) 0.1774(4) 0.0197(10) Uani 1 1 d . . . . .
N2 N 0.61513(10) 0.48153(15) 0.1904(5) 0.0290(13) Uani 1 1 d . . . . .
O1 O 0.58169(9) 0.50064(16) 0.3033(4) 0.0377(13) Uani 1 1 d . . . . .
O19 O 0.55541(8) 0.65292(14) 0.3779(5) 0.0332(12) Uani 1 1 d . . . . .
C4A C 0.52366(12) 0.5770(2) -0.2622(5) 0.0292(15) Uani 1 1 d . . . . .
H4A H 0.5264 0.5695 -0.3331 0.035 Uiso 1 1 calc R . . . .
C10 C 0.59260(10) 0.57849(17) 0.0882(6) 0.0232(13) Uani 1 1 d . . . . .
H10 H 0.5807 0.5653 0.0470 0.028 Uiso 1 1 calc R . . . .
C2 C 0.53782(10) 0.45073(16) 0.4433(5) 0.0185(12) Uani 1 1 d . . . . .
C6 C 0.57028(13) 0.4857(2) 0.5122(5) 0.0274(15) Uani 1 1 d . . . . .
H6 H 0.5835 0.4995 0.4987 0.033 Uiso 1 1 calc R . . . .
C6A C 0.50686(11) 0.62210(19) -0.1390(5) 0.0209(12) Uani 1 1 d . . . . .
H6A H 0.4983 0.6442 -0.1265 0.025 Uiso 1 1 calc R . . . .
N1 N 0.55745(9) 0.47264(16) 0.4261(4) 0.0221(11) Uani 1 1 d . . . . .
O28 O 0.49125(10) 0.65217(14) 0.5288(4) 0.0348(12) Uani 1 1 d . . . . .
C20 C 0.57610(11) 0.4337(2) 0.0129(6) 0.0258(14) Uani 1 1 d . . . . .
C17A C 0.45021(11) 0.6761(2) 0.0206(6) 0.0337(17) Uani 1 1 d . . . . .
H17A H 0.4581 0.6524 0.0063 0.051 Uiso 0.96(9) 1 calc GR . P A 1
H17B H 0.4495 0.6912 -0.0443 0.051 Uiso 0.96(9) 1 calc GR . P A 1
H17C H 0.4352 0.6704 0.0448 0.051 Uiso 0.96(9) 1 calc GR . P A 1
C13A C 0.45481(10) 0.66217(18) 0.2881(5) 0.0234(12) Uani 1 1 d . . . . .
H13A H 0.4625 0.6409 0.3249 0.028 Uiso 1 1 calc R . . . .
N2A N 0.47030(8) 0.67460(14) 0.2013(4) 0.0185(10) Uani 1 1 d . . . . .
O2 O 0.58820(8) 0.51548(16) -0.1525(4) 0.0347(12) Uani 1 1 d . . . . .
O35 O 0.53382(10) 0.54480(15) 0.4760(4) 0.0375(13) Uani 1 1 d . . . . .
C9 C 0.63260(11) 0.5885(2) 0.2483(7) 0.0319(16) Uani 1 1 d . . . . .
H9A H 0.6415 0.5755 0.1948 0.048 Uiso 1 1 calc GR . . . .
H9B H 0.6414 0.5919 0.3127 0.048 Uiso 1 1 calc GR . . . .
H9C H 0.6281 0.6133 0.2211 0.048 Uiso 1 1 calc GR . . . .
C37 C 0.52530(11) 0.56710(18) 0.4229(5) 0.0206(12) Uani 1 1 d . . . . .
C10A C 0.50742(11) 0.73299(17) 0.2514(6) 0.0233(13) Uani 1 1 d . . . . .
H10A H 0.4917 0.7297 0.2742 0.028 Uiso 1 1 calc R . . . .
C2A C 0.52746(10) 0.56662(17) -0.0693(5) 0.0174(11) Uani 1 1 d . . . . .
C7A C 0.53322(11) 0.69586(19) 0.1165(6) 0.0247(13) Uani 1 1 d . . . . .
H7A H 0.5361 0.6682 0.1077 0.030 Uiso 1 1 calc R . . . .
O3 O 0.58386(9) 0.40493(15) -0.0164(5) 0.0417(14) Uani 1 1 d . . . . .
C44 C 0.53907(11) 0.63646(18) 0.3541(5) 0.0231(13) Uani 1 1 d . . . . .
C11A C 0.50804(13) 0.7707(2) 0.1886(7) 0.0357(17) Uani 1 1 d . . . . .
H11A H 0.5233 0.7761 0.1669 0.054 Uiso 1 1 calc GR . . . .
H11B H 0.5026 0.7912 0.2335 0.054 Uiso 1 1 calc GR . . . .
H11C H 0.4986 0.7685 0.1257 0.054 Uiso 1 1 calc GR . . . .
C19 C 0.57791(10) 0.50382(18) -0.0810(5) 0.0204(12) Uani 1 1 d . . . . .
C7 C 0.61160(10) 0.56460(19) 0.2744(6) 0.0248(14) Uani 1 1 d . . . . .
H7 H 0.6172 0.5410 0.3089 0.030 Uiso 1 1 calc R . . . .
C11 C 0.58203(12) 0.61605(19) 0.1267(7) 0.0317(16) Uani 1 1 d . . . . .
H11D H 0.5696 0.6105 0.1740 0.048 Uiso 1 1 calc GR . . . .
H11E H 0.5767 0.6304 0.0656 0.048 Uiso 1 1 calc GR . . . .
H11F H 0.5932 0.6309 0.1647 0.048 Uiso 1 1 calc GR . . . .
C8A C 0.53004(13) 0.7118(2) 0.0040(6) 0.0341(16) Uani 1 1 d . . . . .
H8AA H 0.5163 0.7018 -0.0263 0.051 Uiso 1 1 calc GR . . . .
H8AB H 0.5426 0.7043 -0.0404 0.051 Uiso 1 1 calc GR . . . .
H8AC H 0.5292 0.7394 0.0072 0.051 Uiso 1 1 calc GR . . . .
C56 C 0.49847(11) 0.63550(17) 0.4555(5) 0.0208(12) Uani 1 1 d . . . . .
C16A C 0.46293(10) 0.69902(19) 0.1094(6) 0.0255(14) Uani 1 1 d . . . . .
H16A H 0.4768 0.7086 0.0755 0.031 Uiso 1 1 calc R . . . .
C13 C 0.63334(11) 0.4902(2) 0.1152(9) 0.045(2) Uani 1 1 d . . . . .
H13 H 0.6303 0.5163 0.0885 0.054 Uiso 1 1 calc R . . . .
C4 C 0.54416(14) 0.4582(2) 0.6364(5) 0.0344(17) Uani 1 1 d . . . . .
H4 H 0.5396 0.4538 0.7072 0.041 Uiso 1 1 calc R . . . .
C16 C 0.6148(3) 0.4465(2) 0.2615(8) 0.076(4) Uani 1 1 d . . . . .
H16 H 0.5987 0.4438 0.2789 0.092 Uiso 1 1 calc R . . . .
C3A C 0.53145(10) 0.55549(18) -0.1778(5) 0.0222(12) Uani 1 1 d . . . . .
H3A H 0.5395 0.5330 -0.1918 0.027 Uiso 1 1 calc R . . . .
C15A C 0.45087(13) 0.6927(2) 0.3743(6) 0.0333(16) Uani 1 1 d . . . . .
H15A H 0.4650 0.7047 0.3924 0.050 Uiso 1 1 calc GR . . . .
H15B H 0.4446 0.6808 0.4375 0.050 Uiso 1 1 calc GR . . . .
H15C H 0.4406 0.7118 0.3473 0.050 Uiso 1 1 calc GR . . . .
C3 C 0.53149(12) 0.44452(18) 0.5517(5) 0.0261(13) Uani 1 1 d . . . . .
H3 H 0.5183 0.4308 0.5663 0.031 Uiso 1 1 calc R . . . .
C12 C 0.61170(12) 0.5865(2) 0.0070(6) 0.0336(16) Uani 1 1 d . . . . .
H12A H 0.6238 0.5997 0.0428 0.050 Uiso 1 1 calc GR . . . .
H12B H 0.6060 0.6022 -0.0508 0.050 Uiso 1 1 calc GR . . . .
H12C H 0.6172 0.5625 -0.0217 0.050 Uiso 1 1 calc GR . . . .
C12A C 0.52110(13) 0.7358(2) 0.3551(6) 0.0327(16) Uani 1 1 d . . . . .
H12D H 0.5204 0.7117 0.3930 0.049 Uiso 1 1 calc GR . . . .
H12E H 0.5150 0.7559 0.3998 0.049 Uiso 1 1 calc GR . . . .
H12F H 0.5366 0.7415 0.3380 0.049 Uiso 1 1 calc GR . . . .
C18A C 0.44942(13) 0.7351(2) 0.1437(7) 0.0369(18) Uani 1 1 d . . . . .
H18A H 0.4470 0.7513 0.0820 0.055 Uiso 1 1 calc GR . . . .
H18B H 0.4578 0.7490 0.1975 0.055 Uiso 1 1 calc GR . . . .
H18C H 0.4351 0.7273 0.1729 0.055 Uiso 1 1 calc GR . . . .
C14A C 0.43241(11) 0.6456(2) 0.2489(6) 0.0337(16) Uani 1 1 d . . . . .
H14A H 0.4235 0.6657 0.2169 0.051 Uiso 1 1 calc GR . . . .
H14B H 0.4243 0.6347 0.3089 0.051 Uiso 1 1 calc GR . . . .
H14C H 0.4353 0.6259 0.1962 0.051 Uiso 1 1 calc GR . . . .
C8 C 0.59680(13) 0.5843(2) 0.3579(6) 0.0360(17) Uani 1 1 d . . . . .
H8A H 0.5937 0.6103 0.3353 0.054 Uiso 1 1 calc GR . . . .
H8B H 0.6045 0.5847 0.4262 0.054 Uiso 1 1 calc GR . . . .
H8C H 0.5828 0.5705 0.3650 0.054 Uiso 1 1 calc GR . . . .
Cl4S Cl 0.43111(7) 0.34999(13) 0.8275(3) 0.0747(14) Uani 0.742(7) 1 d . . P B 1
Cl3S Cl 0.42849(6) 0.37312(13) 0.6056(3) 0.0680(13) Uani 0.742(7) 1 d . . P B 1
Cl8S Cl 0.64772(10) 0.47955(16) 0.6709(5) 0.1016(17) Uani 0.777(6) 1 d . . P C
-2
Cl5S Cl 0.62411(8) 0.54969(15) 0.6195(4) 0.0823(13) Uani 0.777(6) 1 d . . P C
-2
C21 C 0.53693(11) 0.46065(18) -0.0530(5) 0.0215(13) Uani 1 1 d . . . . .
O4 O 0.52377(9) 0.44700(17) -0.1088(4) 0.0368(13) Uani 1 1 d . . . . .
C9A C 0.55483(11) 0.7129(2) 0.1665(7) 0.0323(16) Uani 1 1 d . . . . .
H9AA H 0.5534 0.7404 0.1712 0.048 Uiso 1 1 calc GR . . . .
H9AB H 0.5676 0.7066 0.1220 0.048 Uiso 1 1 calc GR . . . .
H9AC H 0.5570 0.7024 0.2375 0.048 Uiso 1 1 calc GR . . . .
C3S C 0.63774(18) 0.5211(4) 0.7170(9) 0.073(5) Uani 0.98(4) 1 d . . . . .
H3SA H 0.6502 0.5357 0.7475 0.088 Uiso 0.777(6) 1 calc R . P C -2
H3SB H 0.6271 0.5158 0.7749 0.088 Uiso 0.777(6) 1 calc R . P C -2
H3SC H 0.6266 0.5331 0.7639 0.088 Uiso 0.223(6) 1 calc R . P C 2
H3SD H 0.6529 0.5270 0.7417 0.088 Uiso 0.223(6) 1 calc R . P C 2
C2S C 0.4187(2) 0.3865(6) 0.7306(13) 0.086(7) Uani 0.742(7) 1 d . . P B 1
H2SA H 0.4023 0.3858 0.7327 0.103 Uiso 0.742(7) 1 calc R . P B 1
H2SB H 0.4238 0.4123 0.7486 0.103 Uiso 0.742(7) 1 calc R . P B 1
C17 C 0.6255(2) 0.4557(3) 0.3730(8) 0.074(4) Uani 1 1 d . . . . .
H17D H 0.6413 0.4614 0.3639 0.110 Uiso 1 1 calc GR . . . .
H17E H 0.6239 0.4338 0.4198 0.110 Uiso 1 1 calc GR . . . .
H17F H 0.6180 0.4775 0.4045 0.110 Uiso 1 1 calc GR . . . .
C18 C 0.6200(3) 0.4118(3) 0.2210(11) 0.097(5) Uani 1 1 d . . . . .
H18D H 0.6140 0.4095 0.1492 0.146 Uiso 1 1 calc GR . . . .
H18E H 0.6136 0.3921 0.2659 0.146 Uiso 1 1 calc GR . . . .
H18F H 0.6361 0.4088 0.2189 0.146 Uiso 1 1 calc GR . . . .
C15 C 0.63501(14) 0.4652(3) 0.0167(7) 0.056(3) Uani 1 1 d . . . . .
H15D H 0.6400 0.4399 0.0372 0.085 Uiso 1 1 calc GR . . . .
H15E H 0.6457 0.4763 -0.0330 0.085 Uiso 1 1 calc GR . . . .
H15F H 0.6204 0.4635 -0.0172 0.085 Uiso 1 1 calc GR . . . .
C14 C 0.65645(14) 0.4924(3) 0.1737(13) 0.087(5) Uani 1 1 d . . . . .
H14D H 0.6551 0.5086 0.2364 0.130 Uiso 1 1 calc GR . . . .
H14E H 0.6676 0.5031 0.1257 0.130 Uiso 1 1 calc GR . . . .
H14F H 0.6610 0.4670 0.1954 0.130 Uiso 1 1 calc GR . . . .
Cl6S Cl 0.6337(3) 0.5321(5) 0.5836(15) 0.0823(13) Uani 0.223(6) 1 d . . P C 2
Cl7S Cl 0.6324(4) 0.4630(6) 0.6976(17) 0.1016(17) Uani 0.223(6) 1 d . . P C 2
Cl3 Cl 0.57327(7) 0.32004(11) 0.7093(4) 0.1017(9) Uani 1 1 d . . . . .
Cl1 Cl 0.59003(7) 0.37835(11) 0.5657(4) 0.1017(9) Uani 1 1 d . . . . .
C0AA C 0.5733(3) 0.3674(4) 0.6761(13) 0.1017(9) Uani 1 1 d . . . . .
H0AA H 0.5785 0.3822 0.7377 0.122 Uiso 1 1 calc R . . . .
H0AB H 0.5578 0.3753 0.6609 0.122 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 P1A 2.4663(16) . ?
Mo1 P3A 2.5310(15) . ?
Mo1 P2 2.5033(15) 2_665 ?
Mo1 C37 1.998(6) . ?
Mo1 C44 1.974(6) . ?
Mo1 C56 1.967(6) . ?
Mo2 P2A 2.5005(15) . ?
Mo2 P1 2.4828(16) . ?
Mo2 P3 2.5361(16) . ?
Mo2 C20 1.965(7) . ?
Mo2 C19 1.975(6) . ?
Mo2 C21 1.990(6) . ?
P2A P1A 2.100(2) . ?
P2A C2A 1.740(6) . ?
P1A C1A 1.720(6) . ?
P3A O1A 1.711(5) . ?
P3A N3A 1.703(5) . ?
P3A N2A 1.660(5) . ?
P2 Mo1 2.5031(15) 2_665 ?
P2 P1 2.100(2) . ?
P2 C2 1.735(6) . ?
P1 C1 1.721(7) . ?
P3 N3 1.657(5) . ?
P3 N2 1.680(6) . ?
P3 O1 1.712(5) . ?
C5A H5A 0.9300 . ?
C5A C4A 1.408(10) . ?
C5A C6A 1.333(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.342(10) . ?
C5 C4 1.407(11) . ?
C1A O1A 1.349(7) . ?
C1A N1A 1.378(8) . ?
C1 O1 1.348(7) . ?
C1 N1 1.371(9) . ?
N1A C6A 1.395(8) . ?
N1A C2A 1.397(8) . ?
N3A C10A 1.481(8) . ?
N3A C7A 1.475(8) . ?
N3 C10 1.486(8) . ?
N3 C7 1.493(8) . ?
N2 C13 1.456(11) . ?
N2 C16 1.500(10) . ?
O19 C44 1.160(8) . ?
C4A H4A 0.9300 . ?
C4A C3A 1.365(9) . ?
C10 H10 0.9800 . ?
C10 C11 1.522(9) . ?
C10 C12 1.537(9) . ?
C2 N1 1.403(8) . ?
C2 C3 1.411(9) . ?
C6 H6 0.9300 . ?
C6 N1 1.384(8) . ?
C6A H6A 0.9300 . ?
O28 C56 1.158(8) . ?
C20 O3 1.157(8) . ?
C17A H17A 0.9600 . ?
C17A H17B 0.9600 . ?
C17A H17C 0.9600 . ?
C17A C16A 1.552(10) . ?
C13A H13A 0.9800 . ?
C13A N2A 1.476(8) . ?
C13A C15A 1.522(9) . ?
C13A C14A 1.523(9) . ?
N2A C16A 1.485(8) . ?
O2 C19 1.148(8) . ?
O35 C37 1.133(8) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 C7 1.528(9) . ?
C10A H10A 0.9800 . ?
C10A C11A 1.523(9) . ?
C10A C12A 1.521(10) . ?
C2A C3A 1.418(9) . ?
C7A H7A 0.9800 . ?
C7A C8A 1.510(10) . ?
C7A C9A 1.538(9) . ?
C11A H11A 0.9600 . ?
C11A H11B 0.9600 . ?
C11A H11C 0.9600 . ?
C7 H7 0.9800 . ?
C7 C8 1.517(10) . ?
C11 H11D 0.9600 . ?
C11 H11E 0.9600 . ?
C11 H11F 0.9600 . ?
C8A H8AA 0.9600 . ?
C8A H8AB 0.9600 . ?
C8A H8AC 0.9600 . ?
C16A H16A 0.9800 . ?
C16A C18A 1.544(9) . ?
C13 H13 0.9800 . ?
C13 C15 1.500(13) . ?
C13 C14 1.548(12) . ?
C4 H4 0.9300 . ?
C4 C3 1.372(9) . ?
C16 H16 0.9800 . ?
C16 C17 1.553(13) . ?
C16 C18 1.341(15) . ?
C3A H3A 0.9300 . ?
C15A H15A 0.9600 . ?
C15A H15B 0.9600 . ?
C15A H15C 0.9600 . ?
C3 H3 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C12A H12D 0.9600 . ?
C12A H12E 0.9600 . ?
C12A H12F 0.9600 . ?
C18A H18A 0.9600 . ?
C18A H18B 0.9600 . ?
C18A H18C 0.9600 . ?
C14A H14A 0.9600 . ?
C14A H14B 0.9600 . ?
C14A H14C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
Cl4S C2S 1.89(2) . ?
Cl3S C2S 1.715(14) . ?
Cl8S C3S 1.659(14) . ?
Cl8S Cl6S 2.276(17) . ?
Cl8S Cl7S 1.12(2) . ?
Cl5S C3S 1.758(13) . ?
Cl5S Cl6S 0.943(19) . ?
C21 O4 1.143(8) . ?
C9A H9AA 0.9600 . ?
C9A H9AB 0.9600 . ?
C9A H9AC 0.9600 . ?
C3S H3SA 0.9700 . ?
C3S H3SB 0.9700 . ?
C3S H3SC 0.9700 . ?
C3S H3SD 0.9700 . ?
C3S Cl6S 1.71(2) . ?
C3S Cl7S 2.06(2) . ?
C2S H2SA 0.9700 . ?
C2S H2SB 0.9700 . ?
C17 H17D 0.9600 . ?
C17 H17E 0.9600 . ?
C17 H17F 0.9600 . ?
C18 H18D 0.9600 . ?
C18 H18E 0.9600 . ?
C18 H18F 0.9600 . ?
C15 H15D 0.9600 . ?
C15 H15E 0.9600 . ?
C15 H15F 0.9600 . ?
C14 H14D 0.9600 . ?
C14 H14E 0.9600 . ?
C14 H14F 0.9600 . ?
Cl3 C0AA 1.693(15) . ?
Cl1 C0AA 1.731(16) . ?
C0AA H0AA 0.9700 . ?
C0AA H0AB 0.9700 . ?

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
P1A Mo1 P3A 77.59(5) . . ?
P1A Mo1 P2 88.16(5) . 2_665 ?
P2 Mo1 P3A 98.94(5) 2_665 . ?
C37 Mo1 P1A 97.82(18) . . ?
C37 Mo1 P3A 173.21(19) . . ?
C37 Mo1 P2 85.82(19) . 2_665 ?
C44 Mo1 P1A 96.41(19) . . ?
C44 Mo1 P3A 90.66(19) . . ?
C44 Mo1 P2 170.1(2) . 2_665 ?
C44 Mo1 C37 84.8(3) . . ?
C56 Mo1 P1A 168.70(18) . . ?
C56 Mo1 P3A 91.58(18) . . ?
C56 Mo1 P2 90.39(19) . 2_665 ?
C56 Mo1 C37 93.2(2) . . ?
C56 Mo1 C44 86.8(3) . . ?
P2A Mo2 P3 98.23(5) . . ?
P1 Mo2 P2A 90.28(6) . . ?
P1 Mo2 P3 77.39(5) . . ?
C20 Mo2 P2A 167.5(2) . . ?
C20 Mo2 P1 95.2(2) . . ?
C20 Mo2 P3 93.9(2) . . ?
C20 Mo2 C19 86.5(3) . . ?
C20 Mo2 C21 83.2(3) . . ?
C19 Mo2 P2A 90.47(18) . . ?
C19 Mo2 P1 168.20(18) . . ?
C19 Mo2 P3 90.85(18) . . ?
C19 Mo2 C21 92.7(2) . . ?
C21 Mo2 P2A 84.85(19) . . ?
C21 Mo2 P1 99.12(19) . . ?
C21 Mo2 P3 175.31(19) . . ?
P1A P2A Mo2 140.86(8) . . ?
C2A P2A Mo2 124.8(2) . . ?
C2A P2A P1A 94.2(2) . . ?
P2A P1A Mo1 156.82(8) . . ?
C1A P1A Mo1 109.0(2) . . ?
C1A P1A P2A 94.2(2) . . ?
O1A P3A Mo1 110.05(15) . . ?
N3A P3A Mo1 118.77(18) . . ?
N3A P3A O1A 95.7(2) . . ?
N2A P3A Mo1 122.97(19) . . ?
N2A P3A O1A 100.5(2) . . ?
N2A P3A N3A 104.1(2) . . ?
P1 P2 Mo1 140.24(8) . 2_665 ?
C2 P2 Mo1 125.0(2) . 2_665 ?
C2 P2 P1 94.5(2) . . ?
P2 P1 Mo2 157.62(9) . . ?
C1 P1 Mo2 108.7(2) . . ?
C1 P1 P2 93.7(2) . . ?
N3 P3 Mo2 121.3(2) . . ?
N3 P3 N2 104.0(3) . . ?
N3 P3 O1 99.2(3) . . ?
N2 P3 Mo2 121.5(2) . . ?
N2 P3 O1 95.4(3) . . ?
O1 P3 Mo2 110.19(17) . . ?
C4A C5A H5A 118.9 . . ?
C6A C5A H5A 118.9 . . ?
C6A C5A C4A 122.2(7) . . ?
C6 C5 H5 120.1 . . ?
C6 C5 C4 119.9(7) . . ?
C4 C5 H5 120.1 . . ?
O1A C1A P1A 124.6(5) . . ?
O1A C1A N1A 116.8(5) . . ?
N1A C1A P1A 118.6(4) . . ?
C1A O1A P3A 117.8(4) . . ?
O1 C1 P1 124.8(5) . . ?
O1 C1 N1 115.9(6) . . ?
N1 C1 P1 119.2(5) . . ?
C1A N1A C6A 122.6(5) . . ?
C1A N1A C2A 115.9(5) . . ?
C6A N1A C2A 121.5(5) . . ?
C10A N3A P3A 117.7(4) . . ?
C7A N3A P3A 117.8(4) . . ?
C7A N3A C10A 123.4(5) . . ?
C10 N3 P3 120.5(4) . . ?
C10 N3 C7 122.4(5) . . ?
C7 N3 P3 117.1(4) . . ?
C13 N2 P3 116.4(5) . . ?
C13 N2 C16 123.6(8) . . ?
C16 N2 P3 118.2(7) . . ?
C1 O1 P3 117.9(4) . . ?
C5A C4A H4A 120.7 . . ?
C3A C4A C5A 118.6(6) . . ?
C3A C4A H4A 120.7 . . ?
N3 C10 H10 105.6 . . ?
N3 C10 C11 113.6(6) . . ?
N3 C10 C12 115.0(5) . . ?
C11 C10 H10 105.6 . . ?
C11 C10 C12 110.6(6) . . ?
C12 C10 H10 105.6 . . ?
N1 C2 P2 116.9(5) . . ?
N1 C2 C3 116.5(6) . . ?
C3 C2 P2 126.5(5) . . ?
C5 C6 H6 119.3 . . ?
C5 C6 N1 121.5(7) . . ?
N1 C6 H6 119.3 . . ?
C5A C6A N1A 119.3(6) . . ?
C5A C6A H6A 120.4 . . ?
N1A C6A H6A 120.4 . . ?
C1 N1 C2 115.6(5) . . ?
C1 N1 C6 123.4(6) . . ?
C6 N1 C2 120.9(6) . . ?
O3 C20 Mo2 171.8(6) . . ?
H17A C17A H17B 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
C16A C17A H17A 109.5 . . ?
C16A C17A H17B 109.5 . . ?
C16A C17A H17C 109.5 . . ?
N2A C13A H13A 105.6 . . ?
N2A C13A C15A 113.7(5) . . ?
N2A C13A C14A 114.7(6) . . ?
C15A C13A H13A 105.6 . . ?
C15A C13A C14A 110.7(6) . . ?
C14A C13A H13A 105.6 . . ?
C13A N2A P3A 119.1(4) . . ?
C13A N2A C16A 122.9(5) . . ?
C16A N2A P3A 117.9(4) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
O35 C37 Mo1 178.6(6) . . ?
N3A C10A H10A 105.7 . . ?
N3A C10A C11A 112.8(6) . . ?
N3A C10A C12A 114.9(5) . . ?
C11A C10A H10A 105.7 . . ?
C12A C10A H10A 105.7 . . ?
C12A C10A C11A 111.4(6) . . ?
N1A C2A P2A 117.2(4) . . ?
N1A C2A C3A 117.0(5) . . ?
C3A C2A P2A 125.8(5) . . ?
N3A C7A H7A 106.1 . . ?
N3A C7A C8A 112.8(6) . . ?
N3A C7A C9A 115.5(6) . . ?
C8A C7A H7A 106.1 . . ?
C8A C7A C9A 109.5(6) . . ?
C9A C7A H7A 106.1 . . ?
O19 C44 Mo1 173.8(6) . . ?
C10A C11A H11A 109.5 . . ?
C10A C11A H11B 109.5 . . ?
C10A C11A H11C 109.5 . . ?
H11A C11A H11B 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
O2 C19 Mo2 178.7(6) . . ?
N3 C7 C9 114.1(6) . . ?
N3 C7 H7 105.9 . . ?
N3 C7 C8 112.8(5) . . ?
C9 C7 H7 105.9 . . ?
C8 C7 C9 111.5(6) . . ?
C8 C7 H7 105.9 . . ?
C10 C11 H11D 109.5 . . ?
C10 C11 H11E 109.5 . . ?
C10 C11 H11F 109.5 . . ?
H11D C11 H11E 109.5 . . ?
H11D C11 H11F 109.5 . . ?
H11E C11 H11F 109.5 . . ?
C7A C8A H8AA 109.5 . . ?
C7A C8A H8AB 109.5 . . ?
C7A C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
O28 C56 Mo1 179.8(7) . . ?
C17A C16A H16A 106.0 . . ?
N2A C16A C17A 113.1(5) . . ?
N2A C16A H16A 106.0 . . ?
N2A C16A C18A 113.8(6) . . ?
C18A C16A C17A 111.1(6) . . ?
C18A C16A H16A 106.0 . . ?
N2 C13 H13 105.8 . . ?
N2 C13 C15 116.7(7) . . ?
N2 C13 C14 111.3(9) . . ?
C15 C13 H13 105.8 . . ?
C15 C13 C14 110.6(7) . . ?
C14 C13 H13 105.8 . . ?
C5 C4 H4 120.4 . . ?
C3 C4 C5 119.2(6) . . ?
C3 C4 H4 120.4 . . ?
N2 C16 H16 102.7 . . ?
N2 C16 C17 110.5(8) . . ?
C17 C16 H16 102.7 . . ?
C18 C16 N2 120.4(10) . . ?
C18 C16 H16 102.7 . . ?
C18 C16 C17 115.0(9) . . ?
C4A C3A C2A 121.4(6) . . ?
C4A C3A H3A 119.3 . . ?
C2A C3A H3A 119.3 . . ?
C13A C15A H15A 109.5 . . ?
C13A C15A H15B 109.5 . . ?
C13A C15A H15C 109.5 . . ?
H15A C15A H15B 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 122.0(6) . . ?
C4 C3 H3 119.0 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10A C12A H12D 109.5 . . ?
C10A C12A H12E 109.5 . . ?
C10A C12A H12F 109.5 . . ?
H12D C12A H12E 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C16A C18A H18A 109.5 . . ?
C16A C18A H18B 109.5 . . ?
C16A C18A H18C 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
C13A C14A H14A 109.5 . . ?
C13A C14A H14B 109.5 . . ?
C13A C14A H14C 109.5 . . ?
H14A C14A H14B 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3S Cl8S Cl6S 48.5(7) . . ?
Cl7S Cl8S C3S 93.3(12) . . ?
Cl7S Cl8S Cl6S 104.9(11) . . ?
Cl6S Cl5S C3S 71.6(11) . . ?
O4 C21 Mo2 177.7(6) . . ?
C7A C9A H9AA 109.5 . . ?
C7A C9A H9AB 109.5 . . ?
C7A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
Cl8S C3S Cl5S 114.6(7) . . ?
Cl8S C3S H3SA 108.6 . . ?
Cl8S C3S H3SB 108.6 . . ?
Cl8S C3S H3SC 145.0 . . ?
Cl8S C3S H3SD 88.0 . . ?
Cl8S C3S Cl6S 84.9(9) . . ?
Cl8S C3S Cl7S 33.0(7) . . ?
Cl5S C3S H3SA 108.6 . . ?
Cl5S C3S H3SB 108.6 . . ?
Cl5S C3S H3SC 81.9 . . ?
Cl5S C3S H3SD 121.3 . . ?
Cl5S C3S Cl7S 113.8(8) . . ?
H3SA C3S H3SB 107.6 . . ?
H3SA C3S H3SC 93.2 . . ?
H3SA C3S H3SD 20.7 . . ?
H3SB C3S H3SC 37.0 . . ?
H3SB C3S H3SD 113.9 . . ?
H3SC C3S H3SD 110.2 . . ?
Cl6S C3S Cl5S 31.5(7) . . ?
Cl6S C3S H3SA 111.5 . . ?
Cl6S C3S H3SB 131.6 . . ?
Cl6S C3S H3SC 112.8 . . ?
Cl6S C3S H3SD 112.8 . . ?
Cl6S C3S Cl7S 94.8(10) . . ?
Cl7S C3S H3SA 132.4 . . ?
Cl7S C3S H3SB 78.5 . . ?
Cl7S C3S H3SC 112.8 . . ?
Cl7S C3S H3SD 112.8 . . ?
Cl4S C2S H2SA 110.7 . . ?
Cl4S C2S H2SB 110.7 . . ?
Cl3S C2S Cl4S 105.2(9) . . ?
Cl3S C2S H2SA 110.7 . . ?
Cl3S C2S H2SB 110.7 . . ?
H2SA C2S H2SB 108.8 . . ?
C16 C17 H17D 109.5 . . ?
C16 C17 H17E 109.5 . . ?
C16 C17 H17F 109.5 . . ?
H17D C17 H17E 109.5 . . ?
H17D C17 H17F 109.5 . . ?
H17E C17 H17F 109.5 . . ?
C16 C18 H18D 109.5 . . ?
C16 C18 H18E 109.5 . . ?
C16 C18 H18F 109.5 . . ?
H18D C18 H18E 109.5 . . ?
H18D C18 H18F 109.5 . . ?
H18E C18 H18F 109.5 . . ?
C13 C15 H15D 109.5 . . ?
C13 C15 H15E 109.5 . . ?
C13 C15 H15F 109.5 . . ?
H15D C15 H15E 109.5 . . ?
H15D C15 H15F 109.5 . . ?
H15E C15 H15F 109.5 . . ?
C13 C14 H14D 109.5 . . ?
C13 C14 H14E 109.5 . . ?
C13 C14 H14F 109.5 . . ?
H14D C14 H14E 109.5 . . ?
H14D C14 H14F 109.5 . . ?
H14E C14 H14F 109.5 . . ?
Cl5S Cl6S Cl8S 120.9(14) . . ?
Cl5S Cl6S C3S 76.9(13) . . ?
C3S Cl6S Cl8S 46.5(6) . . ?
Cl8S Cl7S C3S 53.7(10) . . ?
Cl3 C0AA Cl1 113.9(10) . . ?
Cl3 C0AA H0AA 108.8 . . ?
Cl3 C0AA H0AB 108.8 . . ?
Cl1 C0AA H0AA 108.8 . . ?
Cl1 C0AA H0AB 108.8 . . ?
H0AA C0AA H0AB 107.7 . . ?

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
Mo1 P1A C1A O1A 1.0(5) . . . . ?
Mo1 P1A C1A N1A 179.0(4) . . . . ?
Mo1 P3A O1A C1A -10.5(4) . . . . ?
Mo1 P3A N3A C10A -93.1(4) . . . . ?
Mo1 P3A N3A C7A 75.7(5) . . . . ?
Mo1 P3A N2A C13A 7.6(5) . . . . ?
Mo1 P3A N2A C16A -168.7(4) . . . . ?
Mo1 P2 C2 N1 175.2(3) 2_665 . . . ?
Mo1 P2 C2 C3 -8.0(7) 2_665 . . . ?
Mo2 P2A C2A N1A -175.6(3) . . . . ?
Mo2 P2A C2A C3A 6.0(6) . . . . ?
Mo2 P1 C1 O1 -1.7(7) . . . . ?
Mo2 P1 C1 N1 -180.0(5) . . . . ?
Mo2 P3 N3 C10 -15.3(5) . . . . ?
Mo2 P3 N3 C7 164.0(4) . . . . ?
Mo2 P3 N2 C13 85.8(6) . . . . ?
Mo2 P3 N2 C16 -79.4(6) . . . . ?
Mo2 P3 O1 C1 10.5(6) . . . . ?
P2A P1A C1A O1A -178.9(4) . . . . ?
P2A P1A C1A N1A -0.9(4) . . . . ?
P2A C2A C3A C4A 179.0(5) . . . . ?
P1A P2A C2A N1A 0.0(4) . . . . ?
P1A P2A C2A C3A -178.4(5) . . . . ?
P1A C1A O1A P3A 6.6(6) . . . . ?
P1A C1A N1A C6A 178.9(4) . . . . ?
P1A C1A N1A C2A 1.1(7) . . . . ?
P3A N3A C10A C11A -138.2(5) . . . . ?
P3A N3A C10A C12A 92.7(6) . . . . ?
P3A N3A C7A C8A 102.3(6) . . . . ?
P3A N3A C7A C9A -130.7(5) . . . . ?
P3A N2A C16A C17A 97.1(6) . . . . ?
P3A N2A C16A C18A -134.8(5) . . . . ?
P2 P1 C1 O1 178.2(6) . . . . ?
P2 P1 C1 N1 0.0(6) . . . . ?
P2 C2 N1 C1 0.7(7) . . . . ?
P2 C2 N1 C6 -180.0(5) . . . . ?
P2 C2 C3 C4 -178.6(6) . . . . ?
P1 P2 C2 N1 -0.6(5) . . . . ?
P1 P2 C2 C3 176.2(5) . . . . ?
P1 C1 O1 P3 -6.1(9) . . . . ?
P1 C1 N1 C2 -0.4(8) . . . . ?
P1 C1 N1 C6 -179.7(5) . . . . ?
P3 N3 C10 C11 130.7(5) . . . . ?
P3 N3 C10 C12 -100.5(6) . . . . ?
P3 N3 C7 C9 133.1(5) . . . . ?
P3 N3 C7 C8 -98.3(6) . . . . ?
P3 N2 C13 C15 -93.1(8) . . . . ?
P3 N2 C13 C14 138.8(6) . . . . ?
P3 N2 C16 C17 -103.6(10) . . . . ?
P3 N2 C16 C18 118.4(13) . . . . ?
C5A C4A C3A C2A -0.2(10) . . . . ?
C5 C6 N1 C1 177.4(7) . . . . ?
C5 C6 N1 C2 -1.9(10) . . . . ?
C5 C4 C3 C2 -0.3(11) . . . . ?
C1A N1A C6A C5A -179.0(6) . . . . ?
C1A N1A C2A P2A -0.6(7) . . . . ?
C1A N1A C2A C3A 178.0(5) . . . . ?
O1A P3A N3A C10A 150.2(4) . . . . ?
O1A P3A N3A C7A -41.0(5) . . . . ?
O1A P3A N2A C13A 129.9(5) . . . . ?
O1A P3A N2A C16A -46.3(5) . . . . ?
O1A C1A N1A C6A -3.0(8) . . . . ?
O1A C1A N1A C2A 179.2(5) . . . . ?
N1A C1A O1A P3A -171.3(4) . . . . ?
N1A C2A C3A C4A 0.6(9) . . . . ?
N3A P3A O1A C1A 112.9(4) . . . . ?
N3A P3A N2A C13A -131.4(5) . . . . ?
N3A P3A N2A C16A 52.4(5) . . . . ?
N3 P3 N2 C13 -55.5(6) . . . . ?
N3 P3 N2 C16 139.3(6) . . . . ?
N3 P3 O1 C1 138.9(5) . . . . ?
N2 P3 N3 C10 126.1(5) . . . . ?
N2 P3 N3 C7 -54.6(5) . . . . ?
N2 P3 O1 C1 -116.0(6) . . . . ?
O1 P3 N3 C10 -135.9(5) . . . . ?
O1 P3 N3 C7 43.5(5) . . . . ?
O1 P3 N2 C13 -156.5(6) . . . . ?
O1 P3 N2 C16 38.3(6) . . . . ?
O1 C1 N1 C2 -178.8(6) . . . . ?
O1 C1 N1 C6 1.9(10) . . . . ?
C4A C5A C6A N1A 1.9(11) . . . . ?
C10 N3 C7 C9 -47.6(8) . . . . ?
C10 N3 C7 C8 81.0(7) . . . . ?
C6 C5 C4 C3 1.4(12) . . . . ?
C6A C5A C4A C3A -1.1(11) . . . . ?
C6A N1A C2A P2A -178.4(4) . . . . ?
C6A N1A C2A C3A 0.1(8) . . . . ?
N1 C1 O1 P3 172.2(5) . . . . ?
N1 C2 C3 C4 -1.8(9) . . . . ?
C13A N2A C16A C17A -79.0(7) . . . . ?
C13A N2A C16A C18A 49.1(8) . . . . ?
N2A P3A O1A C1A -141.6(4) . . . . ?
N2A P3A N3A C10A 47.9(5) . . . . ?
N2A P3A N3A C7A -143.3(5) . . . . ?
C10A N3A C7A C8A -89.6(7) . . . . ?
C10A N3A C7A C9A 37.4(9) . . . . ?
C2A N1A C6A C5A -1.4(9) . . . . ?
C7A N3A C10A C11A 53.7(8) . . . . ?
C7A N3A C10A C12A -75.4(8) . . . . ?
C7 N3 C10 C11 -48.6(7) . . . . ?
C7 N3 C10 C12 80.3(7) . . . . ?
C13 N2 C16 C17 92.3(11) . . . . ?
C13 N2 C16 C18 -45.6(17) . . . . ?
C4 C5 C6 N1 -0.4(12) . . . . ?
C16 N2 C13 C15 71.2(10) . . . . ?
C16 N2 C13 C14 -56.9(10) . . . . ?
C15A C13A N2A P3A 103.1(6) . . . . ?
C15A C13A N2A C16A -80.8(7) . . . . ?
C3 C2 N1 C1 -176.5(6) . . . . ?
C3 C2 N1 C6 2.9(9) . . . . ?
C14A C13A N2A P3A -128.1(5) . . . . ?
C14A C13A N2A C16A 48.0(8) . . . . ?
Cl8S C3S Cl6S Cl5S 161.1(12) . . . . ?
Cl5S C3S Cl6S Cl8S -161.1(12) . . . . ?
C3S Cl5S Cl6S Cl8S 15.9(10) . . . . ?
Cl6S Cl8S C3S Cl5S 10.7(7) . . . . ?
Cl6S Cl8S C3S Cl7S 107.0(13) . . . . ?
Cl6S Cl8S Cl7S C3S -47.9(7) . . . . ?
Cl6S Cl5S C3S Cl8S -20.7(13) . . . . ?
Cl6S Cl5S C3S Cl7S -57.1(15) . . . . ?
Cl7S Cl8S C3S Cl5S -96.3(13) . . . . ?
Cl7S Cl8S C3S Cl6S -107.0(13) . . . . ?
Cl7S C3S Cl6S Cl8S -31.5(6) . . . . ?
Cl7S C3S Cl6S Cl5S 129.6(12) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_mw26
_database_code_depnum_ccdc_archive 'CCDC 1495123'
_audit_update_record             
;
2016-07-21 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_audit_creation_date             2016-07-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;

_chemical_name_common            ?
_chemical_name_systematic        
'tris([1,3,4]azadiphospholo[1,2-a]pyridin-3-yl) phosphate'
_chemical_formula_moiety         'C18 H12 N3 O4 P7'
_chemical_formula_sum            'C18 H12 N3 O4 P7'
_chemical_formula_weight         551.10
_chemical_melting_point          413
_chemical_oxdiff_formula         'P7 C50 H50 N2 O4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6804(3)
_cell_length_b                   11.7969(5)
_cell_length_c                   12.7633(5)
_cell_angle_alpha                112.956(4)
_cell_angle_beta                 104.532(3)
_cell_angle_gamma                93.858(3)
_cell_volume                     1144.80(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5229
_cell_measurement_temperature    105(1)
_cell_measurement_theta_max      29.4860
_cell_measurement_theta_min      3.1420
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12458
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.825
_diffrn_ambient_temperature      105(1)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -23.00    8.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   60.0000 31

#__ type_ start__ end____ width___ exp.time_
  2 omega  -19.00    8.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
  3 omega  -24.00   15.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000  -90.0000 39

#__ type_ start__ end____ width___ exp.time_
  4 omega   -3.00   94.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   38.0000   90.0000 97

#__ type_ start__ end____ width___ exp.time_
  5 omega   42.00   90.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  179.0000  -30.0000 48

#__ type_ start__ end____ width___ exp.time_
  6 omega    2.00   91.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000 -180.0000 89

#__ type_ start__ end____ width___ exp.time_
  7 omega  -46.00   48.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  -38.0000  -90.0000 94

#__ type_ start__ end____ width___ exp.time_
  8 omega  -98.00  -32.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  179.0000    0.0000 66

#__ type_ start__ end____ width___ exp.time_
  9 omega    1.00   91.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000  -60.0000 90
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_UB_11      0.0813507000
_diffrn_orient_matrix_UB_12      0.0284600000
_diffrn_orient_matrix_UB_13      0.0348217000
_diffrn_orient_matrix_UB_21      0.0042603000
_diffrn_orient_matrix_UB_22      -0.0456469000
_diffrn_orient_matrix_UB_23      0.0233982000
_diffrn_orient_matrix_UB_31      0.0272550000
_diffrn_orient_matrix_UB_32      -0.0390092000
_diffrn_orient_matrix_UB_33      -0.0474045000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4093
_reflns_number_total             4678
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4678
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0589
_refine_ls_restrained_S_all      1.179
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0265P)²+1.6761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1129
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O00E)
3. Others
 Sof(O0)=Sof(O00E)=Sof(O00K)=Sof(O00N)=Sof(P0)=1-FVAR(1)
 Sof(P1)=Sof(O3)=Sof(O2)=Sof(O4)=Sof(O1)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C15(H15), C4(H4), C10(H10), C9(H9), C17(H17),
 C11(H11), C3(H3), C18(H18), C16(H16)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P7 P 0.72437(11) 0.15271(9) 0.01943(8) 0.0266(2) Uani 1 1 d . . . . .
P6 P 0.51834(12) 0.23545(9) 0.03161(8) 0.0268(2) Uani 1 1 d . . . . .
P3 P 0.13138(12) 0.19534(9) 0.55036(8) 0.0312(2) Uani 1 1 d . . . . .
P4 P 0.46189(12) 0.56763(11) 0.21078(9) 0.0394(3) Uani 1 1 d . . . . .
P5 P 0.37682(13) 0.73533(10) 0.22396(10) 0.0430(3) Uani 1 1 d . . . . .
P2 P 0.26440(15) 0.18632(13) 0.43121(10) 0.0497(3) Uani 1 1 d . . . . .
P1 P 0.30548(19) 0.31534(16) 0.24511(16) 0.0182(4) Uani 0.652(3) 1 d . . P A 2
O3 O 0.231(11) 0.356(8) 0.135(7) 0.0331(7) Uani 0.652(3) 1 d . . P A 2
N2 N 0.1384(3) 0.5406(2) 0.1571(2) 0.0185(5) Uani 1 1 d . . . . .
N3 N 0.5954(3) 0.1232(2) 0.1799(2) 0.0222(6) Uani 1 1 d . . . . .
N1 N 0.0151(3) 0.3065(3) 0.4061(2) 0.0230(6) Uani 1 1 d . . . . .
O2 O 0.1398(5) 0.2747(4) 0.2619(4) 0.0214(10) Uani 0.652(3) 1 d . . P A 2
C14 C 0.7189(4) 0.0978(3) 0.1274(3) 0.0199(7) Uani 1 1 d . . . . .
C7 C 0.2711(4) 0.4841(3) 0.1679(3) 0.0229(7) Uani 1 1 d . . . . .
C12 C 0.1744(4) 0.6672(3) 0.1810(3) 0.0240(7) Uani 1 1 d . . . . .
C5 C -0.2101(4) 0.4094(3) 0.4037(3) 0.0224(7) Uani 1 1 d . . . . .
H5 H -0.2771 0.4549 0.3736 0.027 Uiso 1 1 calc R . . . .
C6 C -0.0864(4) 0.3736(3) 0.3613(3) 0.0207(7) Uani 1 1 d . . . . .
H6 H -0.0686 0.3939 0.3013 0.025 Uiso 1 1 calc R . . . .
O4 O 0.3429(4) 0.1834(3) 0.1711(3) 0.0211(8) Uani 0.652(3) 1 d . . P A 2
C2 C -0.0056(4) 0.2768(3) 0.4980(3) 0.0225(7) Uani 1 1 d . . . . .
C8 C -0.0204(4) 0.4800(3) 0.1245(3) 0.0204(7) Uani 1 1 d . . . . .
H8 H -0.0419 0.3954 0.1080 0.025 Uiso 1 1 calc R . . . .
O1 O 0.4311(4) 0.4002(3) 0.3515(3) 0.0233(8) Uani 0.652(3) 1 d . . P A 2
C15 C 0.8308(4) 0.0310(3) 0.1677(3) 0.0273(8) Uani 1 1 d . . . . .
H15 H 0.9150 0.0125 0.1346 0.033 Uiso 1 1 calc R . . . .
C4 C -0.2387(4) 0.3781(3) 0.4942(3) 0.0265(7) Uani 1 1 d . . . . .
H4 H -0.3261 0.4009 0.5223 0.032 Uiso 1 1 calc R . . . .
C10 C -0.1127(4) 0.6705(3) 0.1391(3) 0.0299(8) Uani 1 1 d . . . . .
H10 H -0.1977 0.7139 0.1335 0.036 Uiso 1 1 calc R . . . .
C9 C -0.1435(4) 0.5434(3) 0.1168(3) 0.0263(7) Uani 1 1 d . . . . .
H9 H -0.2493 0.5027 0.0966 0.032 Uiso 1 1 calc R . . . .
C17 C 0.6892(4) 0.0181(3) 0.3020(3) 0.0256(7) Uani 1 1 d . . . . .
H17 H 0.6791 -0.0087 0.3599 0.031 Uiso 1 1 calc R . . . .
C11 C 0.0418(5) 0.7293(3) 0.1689(3) 0.0295(8) Uani 1 1 d . . . . .
H11 H 0.0611 0.8129 0.1819 0.035 Uiso 1 1 calc R . . . .
C3 C -0.1383(4) 0.3147(3) 0.5397(3) 0.0250(7) Uani 1 1 d . . . . .
H3 H -0.1570 0.2955 0.6000 0.030 Uiso 1 1 calc R . . . .
C18 C 0.5805(4) 0.0801(3) 0.2654(3) 0.0307(8) Uani 1 1 d . . . . .
H18 H 0.4943 0.0947 0.2968 0.037 Uiso 1 1 calc R . . . .
C16 C 0.8188(4) -0.0070(3) 0.2540(3) 0.0252(7) Uani 1 1 d . . . . .
H16 H 0.8953 -0.0491 0.2806 0.030 Uiso 1 1 calc R . . . .
C13 C 0.4923(5) 0.1890(4) 0.1386(3) 0.0378(10) Uani 1 1 d . . . . .
C1 C 0.1422(5) 0.2638(4) 0.3668(3) 0.0374(10) Uani 1 1 d . . . . .
O0 O 0.1915(10) 0.3351(7) 0.2990(7) 0.0181(17) Uani 0.348(3) 1 d . . P A -2
O00E O 0.23(2) 0.357(14) 0.135(13) 0.0331(7) Uani 0.348(3) 1 d . . P A -2
O00K O 0.4236(8) 0.2674(6) 0.2316(6) 0.0194(15) Uani 0.348(3) 1 d . . P A -2
O00N O 0.1455(7) 0.1290(5) 0.1077(5) 0.0214(15) Uani 0.348(3) 1 d . . P A -2
P0 P 0.2341(4) 0.2537(3) 0.1806(3) 0.0164(8) Uani 0.348(3) 1 d . . 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
P7 P6 2.1050(12) . ?
P7 C14 1.746(3) . ?
P6 C13 1.715(3) . ?
P3 P2 2.1045(13) . ?
P3 C2 1.743(3) . ?
P4 P5 2.1181(16) . ?
P4 C7 1.708(4) . ?
P5 C12 1.737(4) . ?
P2 C1 1.708(4) . ?
P1 O3 1.66(10) . ?
P1 O2 1.577(4) . ?
P1 O4 1.580(4) . ?
P1 O1 1.444(4) . ?
P1 O0 1.325(8) . ?
P1 O00E 1.66(19) . ?
P1 P0 0.899(3) . ?
O3 C7 1.39(9) . ?
O3 P0 1.53(10) . ?
N2 C7 1.374(4) . ?
N2 C12 1.398(4) . ?
N2 C8 1.390(4) . ?
N3 C14 1.391(4) . ?
N3 C18 1.401(4) . ?
N3 C13 1.362(4) . ?
N1 C6 1.387(4) . ?
N1 C2 1.397(4) . ?
N1 C1 1.371(4) . ?
O2 C1 1.389(5) . ?
O2 O0 0.721(6) . ?
O2 P0 1.436(5) . ?
C14 C15 1.413(4) . ?
C7 O00E 1.38(16) . ?
C12 C11 1.414(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.342(4) . ?
C5 C4 1.413(4) . ?
C6 H6 0.9300 . ?
O4 C13 1.462(5) . ?
O4 O00K 1.052(7) . ?
O4 P0 1.296(4) . ?
C2 C3 1.414(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.350(4) . ?
O1 O00K 1.694(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.364(5) . ?
C4 H4 0.9300 . ?
C4 C3 1.352(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.406(5) . ?
C10 C11 1.355(5) . ?
C9 H9 0.9300 . ?
C17 H17 0.9300 . ?
C17 C18 1.334(5) . ?
C17 C16 1.407(4) . ?
C11 H11 0.9300 . ?
C3 H3 0.9300 . ?
C18 H18 0.9300 . ?
C16 H16 0.9300 . ?
C13 O00K 1.480(6) . ?
C1 O0 1.530(8) . ?
O0 P0 1.594(8) . ?
O00E P0 1.5(2) . ?
O00K P0 1.581(7) . ?
O00N P0 1.429(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 P7 P6 94.28(11) . . ?
C13 P6 P7 92.64(12) . . ?
C2 P3 P2 94.08(11) . . ?
C7 P4 P5 93.06(12) . . ?
C12 P5 P4 94.01(12) . . ?
C1 P2 P3 93.06(12) . . ?
O3 P1 O00E 0(7) . . ?
O2 P1 O3 98(3) . . ?
O2 P1 O4 100.8(3) . . ?
O2 P1 O00E 98(6) . . ?
O4 P1 O3 99(3) . . ?
O4 P1 O00E 100(5) . . ?
O1 P1 O3 121(3) . . ?
O1 P1 O2 116.7(2) . . ?
O1 P1 O4 117.5(2) . . ?
O1 P1 O00E 120(5) . . ?
O0 P1 O3 101(3) . . ?
O0 P1 O2 27.0(3) . . ?
O0 P1 O4 126.0(4) . . ?
O0 P1 O1 93.1(4) . . ?
O0 P1 O00E 101(6) . . ?
P0 P1 O3 66(3) . . ?
P0 P1 O2 64.2(2) . . ?
P0 P1 O4 55.1(2) . . ?
P0 P1 O1 171.8(2) . . ?
P0 P1 O0 89.5(4) . . ?
P0 P1 O00E 67(5) . . ?
C7 O3 P1 113(4) . . ?
C7 O3 P0 145(6) . . ?
P0 O3 P1 32(2) . . ?
C7 N2 C12 114.5(3) . . ?
C7 N2 C8 124.3(3) . . ?
C8 N2 C12 121.2(3) . . ?
C14 N3 C18 120.9(3) . . ?
C13 N3 C14 114.4(3) . . ?
C13 N3 C18 124.6(3) . . ?
C6 N1 C2 121.4(3) . . ?
C1 N1 C6 124.7(3) . . ?
C1 N1 C2 113.9(3) . . ?
C1 O2 P1 118.6(3) . . ?
C1 O2 P0 139.9(4) . . ?
O0 O2 P1 56.6(8) . . ?
O0 O2 C1 86.9(8) . . ?
O0 O2 P0 88.9(9) . . ?
P0 O2 P1 34.30(15) . . ?
N3 C14 P7 117.4(2) . . ?
N3 C14 C15 116.9(3) . . ?
C15 C14 P7 125.6(2) . . ?
O3 C7 P4 126(4) . . ?
N2 C7 P4 120.7(2) . . ?
N2 C7 O3 113(4) . . ?
N2 C7 O00E 113(7) . . ?
O00E C7 P4 126(7) . . ?
O00E C7 O3 0(10) . . ?
N2 C12 P5 117.7(2) . . ?
N2 C12 C11 116.8(3) . . ?
C11 C12 P5 125.5(3) . . ?
C6 C5 H5 120.0 . . ?
C6 C5 C4 120.0(3) . . ?
C4 C5 H5 120.0 . . ?
N1 C6 H6 119.7 . . ?
C5 C6 N1 120.5(3) . . ?
C5 C6 H6 119.7 . . ?
C13 O4 P1 114.5(3) . . ?
O00K O4 P1 50.6(4) . . ?
O00K O4 C13 70.0(4) . . ?
O00K O4 P0 84.0(4) . . ?
P0 O4 P1 34.66(17) . . ?
P0 O4 C13 133.1(3) . . ?
N1 C2 P3 117.8(2) . . ?
N1 C2 C3 116.5(3) . . ?
C3 C2 P3 125.7(2) . . ?
N2 C8 H8 119.9 . . ?
C9 C8 N2 120.2(3) . . ?
C9 C8 H8 119.9 . . ?
P1 O1 O00K 45.0(2) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 C14 121.8(3) . . ?
C16 C15 H15 119.1 . . ?
C5 C4 H4 120.2 . . ?
C3 C4 C5 119.6(3) . . ?
C3 C4 H4 120.2 . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C11 C10 C9 119.5(3) . . ?
C8 C9 C10 120.4(3) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C18 C17 H17 119.6 . . ?
C18 C17 C16 120.7(3) . . ?
C16 C17 H17 119.6 . . ?
C12 C11 H11 119.1 . . ?
C10 C11 C12 121.9(3) . . ?
C10 C11 H11 119.1 . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.8(3) . . ?
C4 C3 H3 119.1 . . ?
N3 C18 H18 119.8 . . ?
C17 C18 N3 120.4(3) . . ?
C17 C18 H18 119.8 . . ?
C15 C16 C17 119.1(3) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
N3 C13 P6 121.2(2) . . ?
N3 C13 O4 111.8(3) . . ?
N3 C13 O00K 111.3(3) . . ?
O4 C13 P6 125.0(3) . . ?
O4 C13 O00K 41.9(3) . . ?
O00K C13 P6 120.1(3) . . ?
N1 C1 P2 121.1(2) . . ?
N1 C1 O2 111.7(3) . . ?
N1 C1 O0 110.2(4) . . ?
O2 C1 P2 126.4(3) . . ?
O2 C1 O0 28.1(3) . . ?
O0 C1 P2 124.9(4) . . ?
P1 O0 C1 126.6(6) . . ?
P1 O0 P0 34.3(2) . . ?
O2 O0 P1 96.3(9) . . ?
O2 O0 C1 65.0(8) . . ?
O2 O0 P0 64.2(8) . . ?
C1 O0 P0 116.3(5) . . ?
C7 O00E P1 114(8) . . ?
C7 O00E P0 145(10) . . ?
P0 O00E P1 32(4) . . ?
O4 O00K O1 139.6(5) . . ?
O4 O00K C13 68.1(4) . . ?
O4 O00K P0 54.6(4) . . ?
C13 O00K O1 152.2(5) . . ?
C13 O00K P0 111.5(5) . . ?
P0 O00K O1 91.0(3) . . ?
P1 P0 O3 81(2) . . ?
P1 P0 O2 81.5(3) . . ?
P1 P0 O4 90.2(3) . . ?
P1 P0 O0 56.2(4) . . ?
P1 P0 O00E 81(5) . . ?
P1 P0 O00K 50.3(3) . . ?
P1 P0 O00N 156.0(4) . . ?
O3 P0 O0 95(3) . . ?
O3 P0 O00E 0(8) . . ?
O3 P0 O00K 99(3) . . ?
O2 P0 O3 110(4) . . ?
O2 P0 O0 26.9(2) . . ?
O2 P0 O00E 110(7) . . ?
O2 P0 O00K 118.2(4) . . ?
O4 P0 O3 121(4) . . ?
O4 P0 O2 125.8(3) . . ?
O4 P0 O0 127.1(4) . . ?
O4 P0 O00E 121(7) . . ?
O4 P0 O00K 41.4(3) . . ?
O4 P0 O00N 74.9(3) . . ?
O00E P0 O0 95(6) . . ?
O00E P0 O00K 99(6) . . ?
O00K P0 O0 100.8(4) . . ?
O00N P0 O3 122(2) . . ?
O00N P0 O2 92.0(4) . . ?
O00N P0 O0 118.9(4) . . ?
O00N P0 O00E 123(5) . . ?
O00N P0 O00K 116.1(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
P7 P6 C13 N3 0.4(4) . . . . ?
P7 P6 C13 O4 -162.2(4) . . . . ?
P7 P6 C13 O00K 147.8(4) . . . . ?
P7 C14 C15 C16 179.1(3) . . . . ?
P6 P7 C14 N3 0.1(2) . . . . ?
P6 P7 C14 C15 -178.9(3) . . . . ?
P6 C13 O00K O4 110.3(4) . . . . ?
P6 C13 O00K O1 -65.4(11) . . . . ?
P6 C13 O00K P0 76.3(5) . . . . ?
P3 P2 C1 N1 1.6(4) . . . . ?
P3 P2 C1 O2 -167.8(4) . . . . ?
P3 P2 C1 O0 157.4(5) . . . . ?
P3 C2 C3 C4 179.8(3) . . . . ?
P4 P5 C12 N2 1.1(2) . . . . ?
P4 P5 C12 C11 -179.5(3) . . . . ?
P4 C7 O00E P1 64(14) . . . . ?
P4 C7 O00E P0 73(25) . . . . ?
P5 P4 C7 O3 176(5) . . . . ?
P5 P4 C7 N2 -0.6(2) . . . . ?
P5 P4 C7 O00E 176(9) . . . . ?
P5 C12 C11 C10 -177.5(3) . . . . ?
P2 P3 C2 N1 -0.3(3) . . . . ?
P2 P3 C2 C3 178.9(3) . . . . ?
P2 C1 O0 P1 24.6(10) . . . . ?
P2 C1 O0 O2 103.4(9) . . . . ?
P2 C1 O0 P0 63.2(7) . . . . ?
P1 O3 C7 P4 64(7) . . . . ?
P1 O3 C7 N2 -119(5) . . . . ?
P1 O3 C7 O00E -10(100) . . . . ?
P1 O3 P0 O2 77.5(13) . . . . ?
P1 O3 P0 O4 -84.9(17) . . . . ?
P1 O3 P0 O0 54.7(9) . . . . ?
P1 O3 P0 O00E 16(100) . . . . ?
P1 O3 P0 O00K -47.2(10) . . . . ?
P1 O3 P0 O00N -176.3(18) . . . . ?
P1 O2 C1 P2 -48.4(6) . . . . ?
P1 O2 C1 N1 141.3(3) . . . . ?
P1 O2 C1 O0 48.9(7) . . . . ?
P1 O2 O0 C1 -127.6(4) . . . . ?
P1 O2 O0 P0 12.5(5) . . . . ?
P1 O2 P0 O3 -77(3) . . . . ?
P1 O2 P0 O4 84.1(5) . . . . ?
P1 O2 P0 O0 -18.6(8) . . . . ?
P1 O2 P0 O00E -77(5) . . . . ?
P1 O2 P0 O00K 35.5(4) . . . . ?
P1 O2 P0 O00N 156.8(4) . . . . ?
P1 O4 C13 P6 -73.2(4) . . . . ?
P1 O4 C13 N3 122.7(3) . . . . ?
P1 O4 C13 O00K 24.7(4) . . . . ?
P1 O4 O00K O1 26.3(5) . . . . ?
P1 O4 O00K C13 -150.6(4) . . . . ?
P1 O4 O00K P0 -10.2(3) . . . . ?
P1 O4 P0 O3 80(3) . . . . ?
P1 O4 P0 O2 -79.6(5) . . . . ?
P1 O4 P0 O0 -46.0(5) . . . . ?
P1 O4 P0 O00E 80(5) . . . . ?
P1 O4 P0 O00K 13.9(4) . . . . ?
P1 O4 P0 O00N -161.0(3) . . . . ?
P1 O1 O00K O4 -32.1(7) . . . . ?
P1 O1 O00K C13 141.8(11) . . . . ?
P1 O1 O00K P0 -3.02(13) . . . . ?
P1 O0 P0 O3 -76(3) . . . . ?
P1 O0 P0 O2 157.6(10) . . . . ?
P1 O0 P0 O4 60.0(5) . . . . ?
P1 O0 P0 O00E -76(6) . . . . ?
P1 O0 P0 O00K 24.3(4) . . . . ?
P1 O0 P0 O00N 152.5(4) . . . . ?
P1 O00E P0 O3 -164(100) . . . . ?
P1 O00E P0 O2 77(2) . . . . ?
P1 O00E P0 O4 -85(3) . . . . ?
P1 O00E P0 O0 54.7(15) . . . . ?
P1 O00E P0 O00K -47.1(19) . . . . ?
P1 O00E P0 O00N -176(3) . . . . ?
O3 P1 O2 C1 -163(3) . . . . ?
O3 P1 O2 O0 -99(3) . . . . ?
O3 P1 O2 P0 59(3) . . . . ?
O3 P1 O4 C13 79(3) . . . . ?
O3 P1 O4 O00K 110(3) . . . . ?
O3 P1 O4 P0 -52(3) . . . . ?
O3 P1 O1 O00K -107(4) . . . . ?
O3 P1 O0 O2 86(3) . . . . ?
O3 P1 O0 C1 149(3) . . . . ?
O3 P1 O0 P0 66(3) . . . . ?
O3 P1 O00E C7 -178(100) . . . . ?
O3 P1 O00E P0 12(100) . . . . ?
O3 P1 P0 O2 -112(4) . . . . ?
O3 P1 P0 O4 122(4) . . . . ?
O3 P1 P0 O0 -102(4) . . . . ?
O3 P1 P0 O00E 0(11) . . . . ?
O3 P1 P0 O00K 110(4) . . . . ?
O3 P1 P0 O00N 172(4) . . . . ?
O3 C7 O00E P1 170(100) . . . . ?
O3 C7 O00E P0 179(100) . . . . ?
N2 C7 O00E P1 -119(9) . . . . ?
N2 C7 O00E P0 -110(21) . . . . ?
N2 C12 C11 C10 1.9(5) . . . . ?
N2 C8 C9 C10 1.3(4) . . . . ?
N3 C14 C15 C16 0.1(5) . . . . ?
N3 C13 O00K O4 -99.3(5) . . . . ?
N3 C13 O00K O1 85.0(10) . . . . ?
N3 C13 O00K P0 -133.3(4) . . . . ?
N1 C2 C3 C4 -1.0(5) . . . . ?
N1 C1 O0 P1 -177.3(6) . . . . ?
N1 C1 O0 O2 -98.5(8) . . . . ?
N1 C1 O0 P0 -138.7(5) . . . . ?
O2 P1 O3 C7 113(6) . . . . ?
O2 P1 O3 P0 -57.4(17) . . . . ?
O2 P1 O4 C13 179.1(3) . . . . ?
O2 P1 O4 O00K -150.4(5) . . . . ?
O2 P1 O4 P0 47.7(3) . . . . ?
O2 P1 O1 O00K 135.0(4) . . . . ?
O2 P1 O0 C1 63.5(8) . . . . ?
O2 P1 O0 P0 -20.2(9) . . . . ?
O2 P1 O00E C7 113(11) . . . . ?
O2 P1 O00E P0 -57(3) . . . . ?
O2 P1 P0 O3 112(4) . . . . ?
O2 P1 P0 O4 -126.3(3) . . . . ?
O2 P1 P0 O0 10.0(4) . . . . ?
O2 P1 P0 O00E 112(7) . . . . ?
O2 P1 P0 O00K -138.2(3) . . . . ?
O2 P1 P0 O00N -75.6(8) . . . . ?
O2 C1 O0 P1 -78.8(9) . . . . ?
O2 C1 O0 P0 -40.1(6) . . . . ?
O2 O0 P0 P1 -157.6(10) . . . . ?
O2 O0 P0 O3 126(3) . . . . ?
O2 O0 P0 O4 -97.6(9) . . . . ?
O2 O0 P0 O00E 126(6) . . . . ?
O2 O0 P0 O00K -133.3(8) . . . . ?
O2 O0 P0 O00N -5.2(10) . . . . ?
C14 N3 C18 C17 2.9(5) . . . . ?
C14 N3 C13 P6 -0.4(5) . . . . ?
C14 N3 C13 O4 164.3(3) . . . . ?
C14 N3 C13 O00K -150.5(4) . . . . ?
C14 C15 C16 C17 1.6(5) . . . . ?
C7 O3 P0 P1 -16(12) . . . . ?
C7 O3 P0 O2 62(13) . . . . ?
C7 O3 P0 O4 -101(12) . . . . ?
C7 O3 P0 O0 39(12) . . . . ?
C7 O3 P0 O00E 0(100) . . . . ?
C7 O3 P0 O00K -63(12) . . . . ?
C7 O3 P0 O00N 168(10) . . . . ?
C7 N2 C12 P5 -1.7(3) . . . . ?
C7 N2 C12 C11 178.8(3) . . . . ?
C7 N2 C8 C9 179.6(3) . . . . ?
C7 O00E P0 P1 -16(22) . . . . ?
C7 O00E P0 O3 -180(100) . . . . ?
C7 O00E P0 O2 62(24) . . . . ?
C7 O00E P0 O4 -100(23) . . . . ?
C7 O00E P0 O0 39(23) . . . . ?
C7 O00E P0 O00K -63(23) . . . . ?
C7 O00E P0 O00N 168(19) . . . . ?
C12 N2 C7 P4 1.4(4) . . . . ?
C12 N2 C7 O3 -175(4) . . . . ?
C12 N2 C7 O00E -176(8) . . . . ?
C12 N2 C8 C9 -0.8(4) . . . . ?
C5 C4 C3 C2 -0.9(5) . . . . ?
C6 N1 C2 P3 -178.5(2) . . . . ?
C6 N1 C2 C3 2.2(5) . . . . ?
C6 N1 C1 P2 177.8(3) . . . . ?
C6 N1 C1 O2 -11.4(6) . . . . ?
C6 N1 C1 O0 18.7(6) . . . . ?
C6 C5 C4 C3 1.7(5) . . . . ?
O4 P1 O3 C7 -145(5) . . . . ?
O4 P1 O3 P0 45(2) . . . . ?
O4 P1 O2 C1 95.9(4) . . . . ?
O4 P1 O2 O0 160.2(9) . . . . ?
O4 P1 O2 P0 -42.3(2) . . . . ?
O4 P1 O1 O00K 15.0(3) . . . . ?
O4 P1 O0 O2 -24.3(11) . . . . ?
O4 P1 O0 C1 39.2(9) . . . . ?
O4 P1 O0 P0 -44.5(4) . . . . ?
O4 P1 O00E C7 -145(10) . . . . ?
O4 P1 O00E P0 45(4) . . . . ?
O4 P1 P0 O3 -122(4) . . . . ?
O4 P1 P0 O2 126.3(3) . . . . ?
O4 P1 P0 O0 136.3(4) . . . . ?
O4 P1 P0 O00E -122(7) . . . . ?
O4 P1 P0 O00K -12.0(3) . . . . ?
O4 P1 P0 O00N 50.7(8) . . . . ?
O4 C13 O00K O1 -175.7(12) . . . . ?
O4 C13 O00K P0 -34.0(3) . . . . ?
O4 O00K P0 P1 161.7(5) . . . . ?
O4 O00K P0 O3 -128(3) . . . . ?
O4 O00K P0 O2 113.4(4) . . . . ?
O4 O00K P0 O0 135.3(4) . . . . ?
O4 O00K P0 O00E -128(6) . . . . ?
O4 O00K P0 O00N 5.4(5) . . . . ?
C2 N1 C6 C5 -1.5(5) . . . . ?
C2 N1 C1 P2 -2.0(5) . . . . ?
C2 N1 C1 O2 168.8(3) . . . . ?
C2 N1 C1 O0 -161.1(4) . . . . ?
C8 N2 C7 P4 -179.0(2) . . . . ?
C8 N2 C7 O3 4(4) . . . . ?
C8 N2 C7 O00E 4(8) . . . . ?
C8 N2 C12 P5 178.7(2) . . . . ?
C8 N2 C12 C11 -0.7(4) . . . . ?
O1 P1 O3 C7 -15(8) . . . . ?
O1 P1 O3 P0 175.1(6) . . . . ?
O1 P1 O2 C1 -32.7(5) . . . . ?
O1 P1 O2 O0 31.6(10) . . . . ?
O1 P1 O2 P0 -170.9(3) . . . . ?
O1 P1 O4 C13 -52.9(3) . . . . ?
O1 P1 O4 O00K -22.4(5) . . . . ?
O1 P1 O4 P0 175.7(3) . . . . ?
O1 P1 O0 O2 -152.0(8) . . . . ?
O1 P1 O0 C1 -88.5(7) . . . . ?
O1 P1 O0 P0 -172.2(2) . . . . ?
O1 P1 O00E C7 -15(15) . . . . ?
O1 P1 O00E P0 175.1(10) . . . . ?
O1 O00K P0 P1 4.5(2) . . . . ?
O1 O00K P0 O3 75(3) . . . . ?
O1 O00K P0 O2 -43.9(5) . . . . ?
O1 O00K P0 O4 -157.3(5) . . . . ?
O1 O00K P0 O0 -22.0(4) . . . . ?
O1 O00K P0 O00E 75(6) . . . . ?
O1 O00K P0 O00N -151.9(4) . . . . ?
C4 C5 C6 N1 -0.5(5) . . . . ?
C9 C10 C11 C12 -1.4(5) . . . . ?
C11 C10 C9 C8 -0.2(5) . . . . ?
C18 N3 C14 P7 178.6(3) . . . . ?
C18 N3 C14 C15 -2.3(5) . . . . ?
C18 N3 C13 P6 -178.8(3) . . . . ?
C18 N3 C13 O4 -14.0(5) . . . . ?
C18 N3 C13 O00K 31.2(6) . . . . ?
C18 C17 C16 C15 -1.0(5) . . . . ?
C16 C17 C18 N3 -1.2(6) . . . . ?
C13 N3 C14 P7 0.2(4) . . . . ?
C13 N3 C14 C15 179.3(3) . . . . ?
C13 N3 C18 C17 -178.8(4) . . . . ?
C13 O4 O00K O1 176.9(8) . . . . ?
C13 O4 O00K P0 140.3(3) . . . . ?
C13 O4 P0 P1 -69.2(5) . . . . ?
C13 O4 P0 O3 11(3) . . . . ?
C13 O4 P0 O2 -148.8(4) . . . . ?
C13 O4 P0 O0 -115.2(5) . . . . ?
C13 O4 P0 O00E 11(5) . . . . ?
C13 O4 P0 O00K -55.2(5) . . . . ?
C13 O4 P0 O00N 129.8(5) . . . . ?
C13 O00K P0 P1 -158.7(6) . . . . ?
C13 O00K P0 O3 -88(3) . . . . ?
C13 O00K P0 O2 152.9(4) . . . . ?
C13 O00K P0 O4 39.5(4) . . . . ?
C13 O00K P0 O0 174.8(4) . . . . ?
C13 O00K P0 O00E -88(6) . . . . ?
C13 O00K P0 O00N 45.0(5) . . . . ?
C1 N1 C6 C5 178.7(3) . . . . ?
C1 N1 C2 P3 1.3(4) . . . . ?
C1 N1 C2 C3 -178.0(3) . . . . ?
C1 O2 O0 P1 127.6(4) . . . . ?
C1 O2 O0 P0 140.1(3) . . . . ?
C1 O2 P0 P1 -65.1(7) . . . . ?
C1 O2 P0 O3 -143(3) . . . . ?
C1 O2 P0 O4 18.9(10) . . . . ?
C1 O2 P0 O0 -83.8(10) . . . . ?
C1 O2 P0 O00E -142(5) . . . . ?
C1 O2 P0 O00K -29.6(9) . . . . ?
C1 O2 P0 O00N 91.7(7) . . . . ?
C1 O0 P0 P1 -117.2(6) . . . . ?
C1 O0 P0 O3 167(3) . . . . ?
C1 O0 P0 O2 40.5(6) . . . . ?
C1 O0 P0 O4 -57.2(8) . . . . ?
C1 O0 P0 O00E 167(6) . . . . ?
C1 O0 P0 O00K -92.8(6) . . . . ?
C1 O0 P0 O00N 35.3(8) . . . . ?
O0 P1 O3 C7 86(6) . . . . ?
O0 P1 O3 P0 -84.6(16) . . . . ?
O0 P1 O2 C1 -64.3(9) . . . . ?
O0 P1 O2 P0 157.5(10) . . . . ?
O0 P1 O4 C13 -169.9(5) . . . . ?
O0 P1 O4 O00K -139.4(6) . . . . ?
O0 P1 O4 P0 58.7(5) . . . . ?
O0 P1 O1 O00K 148.8(4) . . . . ?
O0 P1 O00E C7 86(11) . . . . ?
O0 P1 O00E P0 -85(3) . . . . ?
O0 P1 P0 O3 102(4) . . . . ?
O0 P1 P0 O2 -10.0(4) . . . . ?
O0 P1 P0 O4 -136.3(4) . . . . ?
O0 P1 P0 O00E 102(7) . . . . ?
O0 P1 P0 O00K -148.2(4) . . . . ?
O0 P1 P0 O00N -85.6(9) . . . . ?
O0 O2 C1 P2 -97.3(9) . . . . ?
O0 O2 C1 N1 92.5(9) . . . . ?
O0 O2 P0 P1 18.6(8) . . . . ?
O0 O2 P0 O3 -59(3) . . . . ?
O0 O2 P0 O4 102.7(9) . . . . ?
O0 O2 P0 O00E -59(5) . . . . ?
O0 O2 P0 O00K 54.2(9) . . . . ?
O0 O2 P0 O00N 175.5(9) . . . . ?
O00E P1 O3 C7 2(100) . . . . ?
O00E P1 O3 P0 -168(100) . . . . ?
O00E P1 O2 C1 -163(5) . . . . ?
O00E P1 O2 O0 -98(5) . . . . ?
O00E P1 O2 P0 59(5) . . . . ?
O00E P1 O4 C13 79(6) . . . . ?
O00E P1 O4 O00K 110(6) . . . . ?
O00E P1 O4 P0 -52(6) . . . . ?
O00E P1 O1 O00K -107(7) . . . . ?
O00E P1 O0 O2 86(5) . . . . ?
O00E P1 O0 C1 150(5) . . . . ?
O00E P1 O0 P0 66(5) . . . . ?
O00E P1 P0 O3 0(11) . . . . ?
O00E P1 P0 O2 -112(7) . . . . ?
O00E P1 P0 O4 122(7) . . . . ?
O00E P1 P0 O0 -102(7) . . . . ?
O00E P1 P0 O00K 110(7) . . . . ?
O00E P1 P0 O00N 172(7) . . . . ?
O00K O4 C13 P6 -97.9(5) . . . . ?
O00K O4 C13 N3 98.1(5) . . . . ?
O00K O4 P0 P1 -13.9(4) . . . . ?
O00K O4 P0 O3 66(3) . . . . ?
O00K O4 P0 O2 -93.6(6) . . . . ?
O00K O4 P0 O0 -60.0(6) . . . . ?
O00K O4 P0 O00E 66(5) . . . . ?
O00K O4 P0 O00N -175.0(5) . . . . ?
P0 P1 O3 C7 170(7) . . . . ?
P0 P1 O2 C1 138.2(5) . . . . ?
P0 P1 O2 O0 -157.5(10) . . . . ?
P0 P1 O4 C13 131.4(4) . . . . ?
P0 P1 O4 O00K 161.9(5) . . . . ?
P0 P1 O0 O2 20.2(9) . . . . ?
P0 P1 O0 C1 83.6(7) . . . . ?
P0 P1 O00E C7 170(14) . . . . ?
P0 O3 C7 P4 73(13) . . . . ?
P0 O3 C7 N2 -110(11) . . . . ?
P0 O3 C7 O00E -1(100) . . . . ?
P0 O2 C1 P2 -12.8(9) . . . . ?
P0 O2 C1 N1 177.0(6) . . . . ?
P0 O2 C1 O0 84.5(10) . . . . ?
P0 O2 O0 P1 -12.5(5) . . . . ?
P0 O2 O0 C1 -140.1(3) . . . . ?
P0 O4 C13 P6 -37.5(7) . . . . ?
P0 O4 C13 N3 158.5(4) . . . . ?
P0 O4 C13 O00K 60.4(6) . . . . ?
P0 O4 O00K O1 36.6(8) . . . . ?
P0 O4 O00K C13 -140.3(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_chemical_properties_physical    ', Moisture-sensitive'
####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1494723'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_audit_creation_date             2016-07-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C36 H24 N6 O6 P12 Ti, 2(C12 H30 Na O6), 2(C H2 Cl2)'
_chemical_formula_sum            'C62 H88 Cl4 N6 Na2 O18 P12 Ti'
_chemical_formula_weight         1812.70
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.9086(7)
_cell_length_b                   24.9553(13)
_cell_length_c                   13.7959(7)
_cell_angle_alpha                90
_cell_angle_beta                 108.1170(10)
_cell_angle_gamma                90
_cell_volume                     4223.9(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8622
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.50
_shelx_estimated_absorpt_T_max   0.934
_shelx_estimated_absorpt_T_min   0.911
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            50291
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.086
_diffrn_reflns_theta_min         1.632
_diffrn_ambient_temperature      99.55
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Apex2'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5616
_reflns_number_total             8349
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0374
_refine_ls_restrained_S_all      0.906
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0278P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0710
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C28(H28A,H28B), C29(H29A,H29B), C21(H21A,
 H21B), C20(H20A,H20B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C17(H17), C11(H11), C9(H9), C4(H4), C15(H15), C18(H18), C3(H3),
 C16(H16), C12(H12), C5(H5), C10(H10)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C26(H26A,H26B,H26C), C23(H23A,H23B,
 H23C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 1.0000 0.5000 0.5000 0.01070(14) Uani 1 2 d S T P . .
P2 P 0.63280(5) 0.60192(2) 0.22654(5) 0.01792(16) Uani 1 1 d . . . . .
P3 P 0.85326(5) 0.53339(2) 0.69888(5) 0.01878(16) Uani 1 1 d . . . . .
P1 P 0.73446(5) 0.56942(2) 0.36588(5) 0.01520(15) Uani 1 1 d . . . . .
P4 P 0.71147(6) 0.51799(2) 0.74139(5) 0.02197(17) Uani 1 1 d . . . . .
P5 P 0.84007(5) 0.40205(2) 0.28672(5) 0.01997(16) Uani 1 1 d . . . . .
P6 P 0.81097(6) 0.31975(2) 0.25012(5) 0.02438(17) Uani 1 1 d . . . . .
O3 O 1.00817(12) 0.42566(5) 0.45998(11) 0.0130(4) Uani 1 1 d . . . . .
O1 O 0.91994(12) 0.51810(5) 0.35893(11) 0.0114(3) Uani 1 1 d . . . . .
O2 O 0.86335(12) 0.48479(5) 0.52401(11) 0.0126(4) Uani 1 1 d . . . . .
N1 N 0.80623(15) 0.54875(6) 0.20705(14) 0.0117(4) Uani 1 1 d . . . . .
O8 O 0.13732(14) 0.79513(6) 0.06102(13) 0.0268(4) Uani 1 1 d . . . . .
O9 O 0.19870(14) 0.78174(6) 0.26801(13) 0.0249(4) Uani 1 1 d . . . . .
O6 O -0.07801(13) 0.73518(6) 0.10340(12) 0.0208(4) Uani 1 1 d . . . . .
N3 N 0.97518(15) 0.33681(6) 0.42244(14) 0.0131(4) Uani 1 1 d . . . . .
N2 N 0.70789(15) 0.47101(6) 0.56597(14) 0.0115(4) Uani 1 1 d . . . . .
O7 O 0.04604(14) 0.67341(6) 0.27009(12) 0.0221(4) Uani 1 1 d . . . . .
C6 C 0.87372(19) 0.52743(8) 0.15559(18) 0.0153(5) Uani 1 1 d . . . . .
H6 H 0.9348 0.5062 0.1913 0.018 Uiso 1 1 calc R . . . .
C13 C 0.94797(19) 0.39056(8) 0.39690(17) 0.0130(5) Uani 1 1 d . . . . .
C17 C 1.0801(2) 0.27055(9) 0.53372(19) 0.0233(6) Uani 1 1 d . . . . .
H17 H 1.1361 0.2613 0.5945 0.028 Uiso 1 1 calc R . . . .
C8 C 0.65048(19) 0.47901(8) 0.63551(17) 0.0148(5) Uani 1 1 d . . . . .
C11 C 0.56258(19) 0.42065(8) 0.45620(19) 0.0189(6) Uani 1 1 d . . . . .
H11 H 0.5321 0.4010 0.3949 0.023 Uiso 1 1 calc R . . . .
C1 C 0.82896(18) 0.54280(8) 0.31214(17) 0.0118(5) Uani 1 1 d . . . . .
C9 C 0.5456(2) 0.45554(8) 0.61132(19) 0.0197(6) Uani 1 1 d . . . . .
H9 H 0.5048 0.4598 0.6575 0.024 Uiso 1 1 calc R . . . .
C4 C 0.7622(2) 0.56871(9) 0.00132(19) 0.0229(6) Uani 1 1 d . . . . .
H4 H 0.7487 0.5761 -0.0691 0.028 Uiso 1 1 calc R . . . .
C15 C 0.9411(2) 0.24368(9) 0.3828(2) 0.0259(7) Uani 1 1 d . . . . .
H15 H 0.9018 0.2162 0.3388 0.031 Uiso 1 1 calc R . . . .
C18 C 1.0578(2) 0.32251(8) 0.50981(18) 0.0174(6) Uani 1 1 d . . . . .
H18 H 1.0991 0.3496 0.5533 0.021 Uiso 1 1 calc R . . . .
C2 C 0.71359(19) 0.57882(8) 0.15586(18) 0.0150(5) Uani 1 1 d . . . . .
C3 C 0.6957(2) 0.58845(8) 0.05117(18) 0.0201(6) Uani 1 1 d . . . . .
H3 H 0.6348 0.6095 0.0146 0.024 Uiso 1 1 calc R . . . .
C16 C 1.0204(2) 0.22958(9) 0.4686(2) 0.0295(7) Uani 1 1 d . . . . .
H16 H 1.0360 0.1929 0.4852 0.035 Uiso 1 1 calc R . . . .
C12 C 0.66284(19) 0.44178(8) 0.47683(17) 0.0152(5) Uani 1 1 d . . . . .
H12 H 0.7031 0.4368 0.4304 0.018 Uiso 1 1 calc R . . . .
C24 C -0.0663(2) 0.66305(9) 0.21932(19) 0.0244(6) Uani 1 1 d . . . . .
H24A H -0.1004 0.6469 0.2675 0.029 Uiso 1 1 calc R . . . .
H24B H -0.0740 0.6376 0.1625 0.029 Uiso 1 1 calc R . . . .
C5 C 0.8526(2) 0.53678(8) 0.05518(18) 0.0207(6) Uani 1 1 d . . . . .
H5 H 0.8986 0.5219 0.0202 0.025 Uiso 1 1 calc R . . . .
C7 C 0.81040(18) 0.49476(8) 0.58830(17) 0.0121(5) Uani 1 1 d . . . . .
C10 C 0.5019(2) 0.42733(8) 0.52490(19) 0.0209(6) Uani 1 1 d . . . . .
H10 H 0.4312 0.4121 0.5103 0.025 Uiso 1 1 calc R . . . .
C27 C 0.1397(2) 0.78439(10) -0.03925(19) 0.0324(7) Uani 1 1 d . . . . .
H27A H 0.1564 0.8175 -0.0697 0.049 Uiso 1 1 calc GR . . . .
H27B H 0.0686 0.7708 -0.0807 0.049 Uiso 1 1 calc GR . . . .
H27C H 0.1959 0.7575 -0.0366 0.049 Uiso 1 1 calc GR . . . .
C25 C -0.1214(2) 0.71466(9) 0.17915(19) 0.0259(6) Uani 1 1 d . . . . .
H25A H -0.2008 0.7088 0.1491 0.031 Uiso 1 1 calc R . . . .
H25B H -0.1096 0.7408 0.2355 0.031 Uiso 1 1 calc R . . . .
C28 C 0.2353(2) 0.81857(9) 0.12397(19) 0.0285(7) Uani 1 1 d . . . . .
H28A H 0.2503 0.8522 0.0927 0.034 Uiso 1 1 calc R . . . .
H28B H 0.2971 0.7937 0.1312 0.034 Uiso 1 1 calc R . . . .
C30 C 0.1880(2) 0.78794(10) 0.36645(19) 0.0347(7) Uani 1 1 d . . . . .
H30A H 0.2586 0.7979 0.4148 0.052 Uiso 1 1 calc GR . . . .
H30B H 0.1633 0.7541 0.3879 0.052 Uiso 1 1 calc GR . . . .
H30C H 0.1346 0.8161 0.3647 0.052 Uiso 1 1 calc GR . . . .
C29 C 0.2236(2) 0.82993(9) 0.22563(19) 0.0296(7) Uani 1 1 d . . . . .
H29A H 0.2923 0.8452 0.2712 0.035 Uiso 1 1 calc R . . . .
H29B H 0.1646 0.8564 0.2188 0.035 Uiso 1 1 calc R . . . .
C26 C -0.1176(2) 0.78798(9) 0.07259(19) 0.0287(7) Uani 1 1 d . . . . .
H26A H -0.1973 0.7873 0.0450 0.043 Uiso 1 1 calc GR . . . .
H26B H -0.0871 0.8008 0.0200 0.043 Uiso 1 1 calc GR . . . .
H26C H -0.0954 0.8121 0.1316 0.043 Uiso 1 1 calc GR . . . .
C23 C 0.1014(2) 0.62645(9) 0.3202(2) 0.0350(7) Uani 1 1 d . . . . .
H23A H 0.0657 0.6133 0.3687 0.052 Uiso 1 1 calc GR . . . .
H23B H 0.1775 0.6353 0.3567 0.052 Uiso 1 1 calc GR . . . .
H23C H 0.0988 0.5986 0.2693 0.052 Uiso 1 1 calc GR . . . .
O4 O 0.09271(15) 0.64450(7) 0.03474(14) 0.0366(5) Uani 1 1 d . . . . .
O5 O 0.28248(15) 0.67725(7) 0.17260(14) 0.0361(5) Uani 1 1 d . . . . .
C21 C 0.2770(2) 0.62624(9) 0.1288(2) 0.0345(7) Uani 1 1 d . . . . .
H21A H 0.2616 0.5992 0.1750 0.041 Uiso 1 1 calc R . . . .
H21B H 0.3482 0.6174 0.1198 0.041 Uiso 1 1 calc R . . . .
C20 C 0.1915(2) 0.62414(11) 0.0295(2) 0.0406(8) Uani 1 1 d . . . . .
H20A H 0.2151 0.6451 -0.0208 0.049 Uiso 1 1 calc R . . . .
H20B H 0.1810 0.5865 0.0057 0.049 Uiso 1 1 calc R . . . .
C19 C 0.0053(2) 0.63903(11) -0.0578(2) 0.0385(8) Uani 1 1 d . . . . .
H19A H 0.0203 0.6608 -0.1111 0.058 Uiso 1 1 calc GR . . . .
H19B H -0.0626 0.6512 -0.0473 0.058 Uiso 1 1 calc GR . . . .
H19C H -0.0019 0.6013 -0.0789 0.058 Uiso 1 1 calc GR . . . .
C22 C 0.3723(2) 0.68309(11) 0.2623(2) 0.0363(7) Uani 1 1 d . . . . .
H22A H 0.3671 0.6565 0.3128 0.055 Uiso 1 1 calc GR . . . .
H22B H 0.3717 0.7192 0.2902 0.055 Uiso 1 1 calc GR . . . .
H22C H 0.4402 0.6777 0.2460 0.055 Uiso 1 1 calc GR . . . .
C14 C 0.91420(19) 0.29784(8) 0.35571(18) 0.0180(6) Uani 1 1 d . . . . .
Na1 Na 0.11101(8) 0.71688(3) 0.14902(7) 0.0198(2) Uani 1 1 d . . . . .
Cl2 Cl 0.60791(6) 0.44958(3) 0.04169(5) 0.03343(18) Uani 1 1 d . . . . .
Cl1 Cl 0.53175(6) 0.39021(3) 0.18655(5) 0.03604(19) Uani 1 1 d . . . . .
C31 C 0.5638(2) 0.45433(9) 0.14963(19) 0.0294(7) Uani 1 1 d . . . . .
H31A H 0.4986 0.4776 0.1341 0.035 Uiso 1 1 calc R . . . .
H31B H 0.6218 0.4708 0.2065 0.035 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O3 1.9479(13) 3_766 ?
Ti1 O3 1.9479(13) . ?
Ti1 O1 1.9516(14) 3_766 ?
Ti1 O1 1.9516(14) . ?
Ti1 O2 1.9310(15) . ?
Ti1 O2 1.9310(15) 3_766 ?
P2 P1 2.1228(9) . ?
P2 C2 1.733(2) . ?
P3 P4 2.1235(10) . ?
P3 C7 1.743(2) . ?
P1 C1 1.744(2) . ?
P4 C8 1.728(2) . ?
P5 P6 2.1206(8) . ?
P5 C13 1.737(2) . ?
P6 C14 1.729(2) . ?
O3 C13 1.307(2) . ?
O1 C1 1.305(2) . ?
O2 C7 1.301(2) . ?
N1 C6 1.390(3) . ?
N1 C1 1.395(3) . ?
N1 C2 1.402(3) . ?
O8 C27 1.419(3) . ?
O8 C28 1.419(3) . ?
O8 Na1 2.3789(17) . ?
O9 C30 1.416(3) . ?
O9 C29 1.417(3) . ?
O9 Na1 2.3325(18) . ?
O6 C25 1.425(3) . ?
O6 C26 1.429(3) . ?
O6 Na1 2.3671(18) . ?
N3 C13 1.404(2) . ?
N3 C18 1.385(3) . ?
N3 C14 1.401(3) . ?
N2 C8 1.397(3) . ?
N2 C12 1.392(3) . ?
N2 C7 1.394(3) . ?
O7 C24 1.425(3) . ?
O7 C23 1.433(3) . ?
O7 Na1 2.3539(18) . ?
C6 H6 0.9500 . ?
C6 C5 1.346(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.347(3) . ?
C17 C16 1.420(3) . ?
C8 C9 1.416(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.343(3) . ?
C11 C10 1.415(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.348(3) . ?
C4 H4 0.9500 . ?
C4 C3 1.350(3) . ?
C4 C5 1.417(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.349(3) . ?
C15 C14 1.416(3) . ?
C18 H18 0.9500 . ?
C2 C3 1.410(3) . ?
C3 H3 0.9500 . ?
C16 H16 0.9500 . ?
C12 H12 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.492(3) . ?
C5 H5 0.9500 . ?
C10 H10 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.484(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
O4 C20 1.395(3) . ?
O4 C19 1.424(3) . ?
O4 Na1 2.3605(19) . ?
O5 C21 1.402(3) . ?
O5 C22 1.416(3) . ?
O5 Na1 2.3528(19) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C20 1.469(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
Cl2 C31 1.756(3) . ?
Cl1 C31 1.767(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ti1 O3 180.00(9) 3_766 . ?
O3 Ti1 O1 89.79(6) . . ?
O3 Ti1 O1 90.21(6) . 3_766 ?
O3 Ti1 O1 90.21(6) 3_766 . ?
O3 Ti1 O1 89.79(6) 3_766 3_766 ?
O1 Ti1 O1 180.0 3_766 . ?
O2 Ti1 O3 90.33(6) 3_766 . ?
O2 Ti1 O3 90.32(6) . 3_766 ?
O2 Ti1 O3 89.68(6) . . ?
O2 Ti1 O3 89.67(6) 3_766 3_766 ?
O2 Ti1 O1 90.69(6) . 3_766 ?
O2 Ti1 O1 89.31(6) . . ?
O2 Ti1 O1 89.31(6) 3_766 3_766 ?
O2 Ti1 O1 90.69(6) 3_766 . ?
O2 Ti1 O2 180.0 . 3_766 ?
C2 P2 P1 94.11(8) . . ?
C7 P3 P4 94.32(8) . . ?
C1 P1 P2 94.46(8) . . ?
C8 P4 P3 94.22(8) . . ?
C13 P5 P6 94.75(7) . . ?
C14 P6 P5 94.16(7) . . ?
C13 O3 Ti1 138.91(14) . . ?
C1 O1 Ti1 135.92(14) . . ?
C7 O2 Ti1 141.36(14) . . ?
C6 N1 C1 121.84(19) . . ?
C6 N1 C2 121.30(19) . . ?
C1 N1 C2 116.83(19) . . ?
C27 O8 C28 112.9(2) . . ?
C27 O8 Na1 113.11(13) . . ?
C28 O8 Na1 105.52(13) . . ?
C30 O9 C29 113.91(18) . . ?
C30 O9 Na1 125.46(14) . . ?
C29 O9 Na1 114.91(14) . . ?
C25 O6 C26 111.34(18) . . ?
C25 O6 Na1 110.08(14) . . ?
C26 O6 Na1 120.02(14) . . ?
C18 N3 C13 121.97(18) . . ?
C18 N3 C14 121.09(18) . . ?
C14 N3 C13 116.93(19) . . ?
C12 N2 C8 121.09(19) . . ?
C12 N2 C7 121.68(19) . . ?
C7 N2 C8 117.21(18) . . ?
C24 O7 C23 111.56(18) . . ?
C24 O7 Na1 105.53(13) . . ?
C23 O7 Na1 118.99(15) . . ?
N1 C6 H6 120.0 . . ?
C5 C6 N1 120.1(2) . . ?
C5 C6 H6 120.0 . . ?
O3 C13 P5 128.40(15) . . ?
O3 C13 N3 115.01(19) . . ?
N3 C13 P5 116.59(16) . . ?
C18 C17 H17 119.8 . . ?
C18 C17 C16 120.4(2) . . ?
C16 C17 H17 119.8 . . ?
N2 C8 P4 117.49(17) . . ?
N2 C8 C9 116.8(2) . . ?
C9 C8 P4 125.66(19) . . ?
C12 C11 H11 119.7 . . ?
C12 C11 C10 120.6(2) . . ?
C10 C11 H11 119.7 . . ?
O1 C1 P1 127.61(17) . . ?
O1 C1 N1 115.50(19) . . ?
N1 C1 P1 116.89(16) . . ?
C8 C9 H9 119.0 . . ?
C10 C9 C8 122.1(2) . . ?
C10 C9 H9 119.0 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.3(2) . . ?
C5 C4 H4 120.4 . . ?
C16 C15 H15 118.8 . . ?
C16 C15 C14 122.5(2) . . ?
C14 C15 H15 118.8 . . ?
N3 C18 H18 119.7 . . ?
C17 C18 N3 120.6(2) . . ?
C17 C18 H18 119.7 . . ?
N1 C2 P2 117.57(17) . . ?
N1 C2 C3 116.7(2) . . ?
C3 C2 P2 125.71(18) . . ?
C4 C3 C2 122.1(2) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C17 C16 H16 120.6 . . ?
C15 C16 C17 118.8(2) . . ?
C15 C16 H16 120.6 . . ?
N2 C12 H12 119.9 . . ?
C11 C12 N2 120.2(2) . . ?
C11 C12 H12 119.9 . . ?
O7 C24 H24A 110.0 . . ?
O7 C24 H24B 110.0 . . ?
O7 C24 C25 108.69(19) . . ?
H24A C24 H24B 108.3 . . ?
C25 C24 H24A 110.0 . . ?
C25 C24 H24B 110.0 . . ?
C6 C5 C4 120.5(2) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
O2 C7 P3 127.68(17) . . ?
O2 C7 N2 115.59(19) . . ?
N2 C7 P3 116.72(17) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 C11 119.1(2) . . ?
C9 C10 H10 120.4 . . ?
O8 C27 H27A 109.5 . . ?
O8 C27 H27B 109.5 . . ?
O8 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O6 C25 C24 109.4(2) . . ?
O6 C25 H25A 109.8 . . ?
O6 C25 H25B 109.8 . . ?
C24 C25 H25A 109.8 . . ?
C24 C25 H25B 109.8 . . ?
H25A C25 H25B 108.2 . . ?
O8 C28 H28A 109.9 . . ?
O8 C28 H28B 109.9 . . ?
O8 C28 C29 108.9(2) . . ?
H28A C28 H28B 108.3 . . ?
C29 C28 H28A 109.9 . . ?
C29 C28 H28B 109.9 . . ?
O9 C30 H30A 109.5 . . ?
O9 C30 H30B 109.5 . . ?
O9 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O9 C29 C28 109.30(19) . . ?
O9 C29 H29A 109.8 . . ?
O9 C29 H29B 109.8 . . ?
C28 C29 H29A 109.8 . . ?
C28 C29 H29B 109.8 . . ?
H29A C29 H29B 108.3 . . ?
O6 C26 H26A 109.5 . . ?
O6 C26 H26B 109.5 . . ?
O6 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O7 C23 H23A 109.5 . . ?
O7 C23 H23B 109.5 . . ?
O7 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 O4 C19 113.6(2) . . ?
C20 O4 Na1 114.20(15) . . ?
C19 O4 Na1 124.02(15) . . ?
C21 O5 C22 112.85(19) . . ?
C21 O5 Na1 113.78(16) . . ?
C22 O5 Na1 123.83(15) . . ?
O5 C21 H21A 109.5 . . ?
O5 C21 H21B 109.5 . . ?
O5 C21 C20 110.9(2) . . ?
H21A C21 H21B 108.0 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
O4 C20 C21 111.9(2) . . ?
O4 C20 H20A 109.2 . . ?
O4 C20 H20B 109.2 . . ?
C21 C20 H20A 109.2 . . ?
C21 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
O4 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O5 C22 H22A 109.5 . . ?
O5 C22 H22B 109.5 . . ?
O5 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C14 P6 117.55(16) . . ?
N3 C14 C15 116.6(2) . . ?
C15 C14 P6 125.83(18) . . ?
O9 Na1 O8 71.00(6) . . ?
O9 Na1 O6 106.72(6) . . ?
O9 Na1 O7 91.29(6) . . ?
O9 Na1 O4 157.96(8) . . ?
O9 Na1 O5 87.97(7) . . ?
O6 Na1 O8 90.28(6) . . ?
O7 Na1 O8 151.56(7) . . ?
O7 Na1 O6 73.28(6) . . ?
O7 Na1 O4 97.91(7) . . ?
O4 Na1 O8 106.73(7) . . ?
O4 Na1 O6 95.12(7) . . ?
O5 Na1 O8 97.94(7) . . ?
O5 Na1 O6 164.91(7) . . ?
O5 Na1 O7 103.63(7) . . ?
O5 Na1 O4 70.44(6) . . ?
Cl2 C31 Cl1 110.48(13) . . ?
Cl2 C31 H31A 109.6 . . ?
Cl2 C31 H31B 109.6 . . ?
Cl1 C31 H31A 109.6 . . ?
Cl1 C31 H31B 109.6 . . ?
H31A C31 H31B 108.1 . . ?

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
Ti1 O3 C13 P5 22.2(3) . . . . ?
Ti1 O3 C13 N3 -157.91(15) . . . . ?
Ti1 O1 C1 P1 -2.5(3) . . . . ?
Ti1 O1 C1 N1 176.87(12) . . . . ?
Ti1 O2 C7 P3 -0.2(3) . . . . ?
Ti1 O2 C7 N2 -179.35(14) . . . . ?
P2 P1 C1 O1 176.61(17) . . . . ?
P2 P1 C1 N1 -2.71(15) . . . . ?
P2 C2 C3 C4 -179.59(18) . . . . ?
P3 P4 C8 N2 0.56(16) . . . . ?
P3 P4 C8 C9 -177.55(18) . . . . ?
P1 P2 C2 N1 1.55(16) . . . . ?
P1 P2 C2 C3 -177.13(18) . . . . ?
P4 P3 C7 O2 -177.34(18) . . . . ?
P4 P3 C7 N2 1.84(16) . . . . ?
P4 C8 C9 C10 177.29(18) . . . . ?
P5 P6 C14 N3 0.17(18) . . . . ?
P5 P6 C14 C15 178.3(2) . . . . ?
P6 P5 C13 O3 179.0(2) . . . . ?
P6 P5 C13 N3 -0.90(18) . . . . ?
N1 C6 C5 C4 0.5(3) . . . . ?
N1 C2 C3 C4 1.7(3) . . . . ?
O8 C28 C29 O9 57.7(3) . . . . ?
N2 C8 C9 C10 -0.8(3) . . . . ?
O7 C24 C25 O6 64.6(2) . . . . ?
C6 N1 C1 P1 -177.62(15) . . . . ?
C6 N1 C1 O1 3.0(3) . . . . ?
C6 N1 C2 P2 178.17(15) . . . . ?
C6 N1 C2 C3 -3.0(3) . . . . ?
C13 N3 C18 C17 178.2(2) . . . . ?
C13 N3 C14 P6 -0.8(3) . . . . ?
C13 N3 C14 C15 -179.1(2) . . . . ?
C8 N2 C12 C11 0.0(3) . . . . ?
C8 N2 C7 P3 -1.8(2) . . . . ?
C8 N2 C7 O2 177.45(17) . . . . ?
C8 C9 C10 C11 0.3(3) . . . . ?
C1 N1 C6 C5 -175.99(19) . . . . ?
C1 N1 C2 P2 -3.8(2) . . . . ?
C1 N1 C2 C3 175.02(18) . . . . ?
C18 N3 C13 P5 -178.32(17) . . . . ?
C18 N3 C13 O3 1.8(3) . . . . ?
C18 N3 C14 P6 178.68(17) . . . . ?
C18 N3 C14 C15 0.4(3) . . . . ?
C18 C17 C16 C15 -0.1(4) . . . . ?
C2 N1 C6 C5 2.0(3) . . . . ?
C2 N1 C1 P1 4.3(2) . . . . ?
C2 N1 C1 O1 -175.07(17) . . . . ?
C3 C4 C5 C6 -1.8(3) . . . . ?
C16 C17 C18 N3 1.1(4) . . . . ?
C16 C15 C14 P6 -177.5(2) . . . . ?
C16 C15 C14 N3 0.6(4) . . . . ?
C12 N2 C8 P4 -177.60(15) . . . . ?
C12 N2 C8 C9 0.7(3) . . . . ?
C12 N2 C7 P3 176.39(15) . . . . ?
C12 N2 C7 O2 -4.3(3) . . . . ?
C12 C11 C10 C9 0.4(3) . . . . ?
C5 C4 C3 C2 0.6(3) . . . . ?
C7 N2 C8 P4 0.6(2) . . . . ?
C7 N2 C8 C9 178.91(18) . . . . ?
C7 N2 C12 C11 -178.14(19) . . . . ?
C10 C11 C12 N2 -0.6(3) . . . . ?
C27 O8 C28 C29 178.12(19) . . . . ?
C30 O9 C29 C28 178.8(2) . . . . ?
C26 O6 C25 C24 -172.2(2) . . . . ?
C23 O7 C24 C25 173.7(2) . . . . ?
O5 C21 C20 O4 -49.6(3) . . . . ?
C19 O4 C20 C21 -175.0(2) . . . . ?
C22 O5 C21 C20 -172.8(2) . . . . ?
C14 N3 C13 P5 1.2(3) . . . . ?
C14 N3 C13 O3 -178.68(19) . . . . ?
C14 N3 C18 C17 -1.3(3) . . . . ?
C14 C15 C16 C17 -0.8(4) . . . . ?
Na1 O8 C28 C29 -57.9(2) . . . . ?
Na1 O9 C29 C28 -26.3(3) . . . . ?
Na1 O6 C25 C24 -36.5(2) . . . . ?
Na1 O7 C24 C25 -55.8(2) . . . . ?
Na1 O4 C20 C21 35.0(3) . . . . ?
Na1 O5 C21 C20 39.5(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_4270
_database_code_depnum_ccdc_archive 'CCDC 1494721'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT340_exp_4270            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01989 Ang.
RESPONSE: large disorder around the soidum ion
;
# Added during the CSD deposition process: Tuesday 19 July 2016 09:44 AM
# end Validation Reply Form

_audit_creation_date             2016-07-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H17 B N3 O3 P6, C12.46 H27.9 Na O4.4'
_chemical_formula_sum            'C36.46 H44.90 B N3 Na O7.40 P6'
_chemical_formula_weight         863.20
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         Na1O9B1P6C50H50N3
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'
Na Na 0.0362 0.0249 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   33.7644(14)
_cell_length_b                   12.0728(6)
_cell_length_c                   11.6209(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4737.1(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8830
_cell_measurement_temperature    106(9)
_cell_measurement_theta_max      22.7310
_cell_measurement_theta_min      3.3650
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1799
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1077
_diffrn_reflns_av_unetI/netI     0.0965
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34644
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.945
_diffrn_ambient_temperature      106(9)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -88.00   26.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802  -19.0000 -180.0000 114

#__ type_ start__ end____ width___ exp.time_
  2 omega   52.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  179.0000  120.0000 30

#__ type_ start__ end____ width___ exp.time_
  3 omega   -3.00   38.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   57.0000   30.0000 41

#__ type_ start__ end____ width___ exp.time_
  4 omega  -50.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  -57.0000 -120.0000 90

#__ type_ start__ end____ width___ exp.time_
  5 omega  -94.00  -68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802  179.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega  -87.00    3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802  -57.0000  120.0000 90
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_UB_11      -0.0091756000
_diffrn_orient_matrix_UB_12      0.0287251000
_diffrn_orient_matrix_UB_13      -0.0460957000
_diffrn_orient_matrix_UB_21      -0.0124859000
_diffrn_orient_matrix_UB_22      -0.0462516000
_diffrn_orient_matrix_UB_23      -0.0100537000
_diffrn_orient_matrix_UB_31      -0.0141776000
_diffrn_orient_matrix_UB_32      0.0221320000
_diffrn_orient_matrix_UB_33      0.0387099000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                7128
_reflns_number_total             9513
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 
;
 Flack x determined using 1897 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         9513
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.1122
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1630P)²+6.5040P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2802
_refine_ls_wR_factor_ref         0.3057
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O00X) = Uanis(Na07) = Uanis(O00L) = Uanis(O00W) = Uanis(O013) =
Uanis(O00K) = Uanis(C3) = Uanis(C01I) = Uanis(C01C) = Uanis(C01D) = Uanis(C01G)
= Uanis(C01A) = Uanis(C19) = Uanis(C019) = Uanis(C6) = Uanis(C14) = Uanis(C01H)
Uanis(O2) = Uanis(C6AA) = Uanis(C5) = Uanis(C8) = Uanis(C5AA) = Uanis(O3) =
Uanis(C11) = Uanis(C12) = Uanis(C15) = Uanis(C16)
Uanis(C7AA) = Uanis(C10) = Uanis(C4) = Uanis(O1)
3. Rigid body (RIGU) restrains
 O2, C6AA, C5, C8, C5AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C11, C12, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O00L)=Sof(O00W)=Sof(O013)=Sof(C019)=Sof(H01A)=Sof(H01B)=Sof(C01A)=
 Sof(H01C)=Sof(H01D)=Sof(H01E)=Sof(C01H)=Sof(H01M)=Sof(H01N)=Sof(C01I)=
 Sof(H01O)=Sof(H01P)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C19)=Sof(H19A)=Sof(H19B)=FVAR(1)
 Sof(O00K)=Sof(O00X)=Sof(C01C)=Sof(H01F)=Sof(H01G)=Sof(H01H)=Sof(C01D)=
 Sof(H01I)=Sof(H01J)=Sof(C01G)=Sof(H01K)=Sof(H01L)=Sof(H3AD)=Sof(H3AE)=
 Sof(H3AF)=FVAR(2)
 Fixed Sof: H3AA(0.33333) H3AB(0.33333) H3AC(0.33333) O2(0.5) C6AA(0.5)
 H6AA(0.5) H6AB(0.5) C5(0.5) H5A(0.5) H5B(0.5) C8(0.5) H8A(0.5) H8B(0.5)
 C5AA(0.5) H5AA(0.5) H5AB(0.5) O3(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5)
 H12A(0.5) H12B(0.5) C15(0.5) H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5)
 O1(0.33333) C7AA(0.25) H7AA(0.25) H7AB(0.25) H7AC(0.25) C4(0.25) H4A(0.25)
 H4B(0.25) C10(0.25) H10A(0.25) H10B(0.25)
5.a Free rotating group:
 O2(C6AA,C5,C8,C5AA), O3(C11,C12,C15,C16,O1,C7AA)
5.b Secondary CH2 refined with riding coordinates:
 C019(H01A,H01B), C01D(H01I,H01J), C01G(H01K,H01L), C01H(H01M,H01N), C01I(H01O,
 H01P), C3(H3A,H3B), C14(H14A,H14B), C19(H19A,H19B), C6AA(H6AA,H6AB), C5(H5A,
 H5B), C8(H8A,H8B), C5AA(H5AA,H5AB), C11(H11A,H11B), C12(H12A,H12B), C15(H15A,
 H15B), C16(H16A,H16B), C4(H4A,H4B), C10(H10A,H10B)
5.c Me refined with riding coordinates:
 C3AA(H3AD,H3AE,H3AF)
5.d Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00I(H00I), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00U(H00U), C00Z(H00Z), C010(H010), C011(H011), C012(H012), C014(H014),
 C016(H016), C2AA(H2AA), C0(H0), C4AA(H4AA), C2(H2)
5.e Idealised Me refined with everything fixed:
 C7AA(H7AA,H7AB,H7AC)
5.f Idealised Me refined as rotating group:
 C01A(H01C,H01D,H01E), C01C(H01F,H01G,H01H), C6(H6A,H6B,H6C), C3AA(H3AA,H3AB,
 H3AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P001 P 0.29695(8) 0.1095(3) 0.5191(3) 0.0424(7) Uani 1 1 d . . . . .
P002 P 0.41877(9) -0.1546(2) 0.6950(3) 0.0454(7) Uani 1 1 d . . . . .
P003 P 0.28869(10) 0.1090(3) 0.3383(3) 0.0481(8) Uani 1 1 d . . . . .
P004 P 0.46381(10) -0.2435(3) 0.7837(3) 0.0569(9) Uani 1 1 d . . . . .
Na07 Na 0.62609(14) 0.4515(4) 0.6833(4) 0.0519(9) Uani 1 1 d . . . . .
O08 O 0.4030(2) 0.0567(6) 0.7755(6) 0.0389(17) Uani 1 1 d . . . . .
O00A O 0.37139(19) 0.0447(6) 0.5953(5) 0.0316(14) Uani 1 1 d . . . . .
N00B N 0.3618(3) 0.0482(7) 0.4033(7) 0.0336(18) Uani 1 1 d . . . . .
N00C N 0.4515(2) -0.0408(7) 0.8661(7) 0.0349(19) Uani 1 1 d . . . . .
C00E C 0.3457(3) 0.0653(8) 0.5101(8) 0.032(2) Uani 1 1 d . . . . .
C00G C 0.4232(3) -0.0391(8) 0.7815(9) 0.035(2) Uani 1 1 d . . . . .
C00H C 0.3121(3) -0.0917(9) 0.7331(10) 0.044(3) Uani 1 1 d . . . . .
H00H H 0.3202 -0.1169 0.6612 0.053 Uiso 1 1 calc R . . . .
C00I C 0.4850(3) 0.0434(10) 1.0245(11) 0.047(3) Uani 1 1 d . . . . .
H00I H 0.4890 0.1039 1.0728 0.057 Uiso 1 1 calc R . . . .
C00J C 0.3297(3) 0.0019(9) 0.7799(9) 0.039(2) Uani 1 1 d . . . . .
O00K O 0.6779(4) 0.5395(11) 0.5786(11) 0.0519(9) Uani 0.634(12) 1 d . . P A 1
O00L O 0.5793(4) 0.3380(12) 0.7707(12) 0.0519(9) Uani 0.601(9) 1 d . . P A .
C00N C 0.2827(3) -0.1482(11) 0.7919(11) 0.052(3) Uani 1 1 d . . . . .
H00N H 0.2713 -0.2101 0.7578 0.062 Uiso 1 1 calc R . . . .
C00O C 0.4579(3) 0.0501(10) 0.9382(9) 0.043(3) Uani 1 1 d . . . . .
H00O H 0.4436 0.1151 0.9272 0.052 Uiso 1 1 calc R . . . .
C00P C 0.4013(3) 0.0178(10) 0.3885(11) 0.047(3) Uani 1 1 d . . . . .
H00P H 0.4175 0.0065 0.4521 0.056 Uiso 1 1 calc R . . . .
C00Q C 0.5068(3) -0.0527(11) 1.0412(10) 0.048(3) Uani 1 1 d . . . . .
H00Q H 0.5252 -0.0573 1.1007 0.058 Uiso 1 1 calc R . . . .
C00S C 0.4737(3) -0.1363(9) 0.8786(10) 0.044(3) Uani 1 1 d . . . . .
C00U C 0.5010(3) -0.1381(11) 0.9708(9) 0.046(3) Uani 1 1 d . . . . .
H00U H 0.5156 -0.2023 0.9828 0.055 Uiso 1 1 calc R . . . .
C00V C 0.3364(3) 0.0672(9) 0.3108(8) 0.040(2) Uani 1 1 d . . . . .
O00W O 0.6139(4) 0.6121(12) 0.7919(12) 0.0519(9) Uani 0.601(9) 1 d . . P A .
O00X O 0.6405(4) 0.3485(11) 0.5137(11) 0.0519(9) Uani 0.634(12) 1 d . . P A 1
C00Z C 0.4159(4) 0.0048(14) 0.2807(13) 0.069(4) Uani 1 1 d . . . . .
H00Z H 0.4424 -0.0133 0.2702 0.083 Uiso 1 1 calc R . . . .
C010 C 0.3534(4) 0.0504(12) 0.1988(11) 0.063(4) Uani 1 1 d . . . . .
H010 H 0.3377 0.0620 0.1341 0.075 Uiso 1 1 calc R . . . .
C011 C 0.2700(5) -0.1165(14) 0.8974(12) 0.069(4) Uani 1 1 d . . . . .
H011 H 0.2501 -0.1549 0.9355 0.083 Uiso 1 1 calc R . . . .
C012 C 0.3162(5) 0.0346(15) 0.8868(10) 0.078(5) Uani 1 1 d . . . . .
H012 H 0.3265 0.0983 0.9204 0.093 Uiso 1 1 calc R . . . .
O013 O 0.5792(4) 0.5648(12) 0.5880(12) 0.0519(9) Uani 0.601(9) 1 d . . P A .
C014 C 0.3910(6) 0.0187(15) 0.1849(12) 0.083(5) Uani 1 1 d . . . . .
H014 H 0.4008 0.0057 0.1113 0.100 Uiso 1 1 calc R . . . .
C016 C 0.2875(5) -0.0267(16) 0.9452(12) 0.081(5) Uani 1 1 d . . . . .
H016 H 0.2802 -0.0052 1.0191 0.097 Uiso 1 1 calc R . . . .
C019 C 0.5837(6) 0.6729(18) 0.7560(17) 0.0519(9) Uani 0.601(9) 1 d . . P . .
H01A H 0.5926 0.7491 0.7500 0.062 Uiso 0.601(9) 1 calc R . P A .
H01B H 0.5633 0.6706 0.8146 0.062 Uiso 0.601(9) 1 calc R . P . .
C01A C 0.6330(7) 0.6431(18) 0.8911(17) 0.0519(9) Uani 0.601(9) 1 d . . P . .
H01C H 0.6138 0.6550 0.9509 0.078 Uiso 0.601(9) 1 calc GR . P A .
H01D H 0.6474 0.7104 0.8777 0.078 Uiso 0.601(9) 1 calc GR . P . .
H01E H 0.6510 0.5858 0.9140 0.078 Uiso 0.601(9) 1 calc GR . P . .
C01C C 0.6891(6) 0.6587(16) 0.5900(16) 0.0519(9) Uani 0.634(12) 1 d . . P A 1
H01F H 0.6726 0.7028 0.5407 0.078 Uiso 0.634(12) 1 calc GR . P A 1
H01G H 0.7163 0.6681 0.5682 0.078 Uiso 0.634(12) 1 calc GR . P A 1
H01H H 0.6856 0.6819 0.6683 0.078 Uiso 0.634(12) 1 calc GR . P A 1
C01D C 0.6796(6) 0.3823(17) 0.4723(16) 0.0519(9) Uani 0.634(12) 1 d . . P A 1
H01I H 0.6839 0.3515 0.3962 0.062 Uiso 0.634(12) 1 calc R . P A 1
H01J H 0.6997 0.3523 0.5231 0.062 Uiso 0.634(12) 1 calc R . P A 1
C01G C 0.6839(6) 0.5033(17) 0.4670(16) 0.0519(9) Uani 0.634(12) 1 d . . P A 1
H01K H 0.7101 0.5236 0.4403 0.062 Uiso 0.634(12) 1 calc R . P A 1
H01L H 0.6644 0.5352 0.4154 0.062 Uiso 0.634(12) 1 calc R . P A 1
C01H C 0.5429(6) 0.3257(18) 0.9250(18) 0.0519(9) Uani 0.601(9) 1 d . . P A 1
H01M H 0.5407 0.2956 1.0021 0.062 Uiso 0.601(9) 1 calc R . P A 1
H01N H 0.5309 0.3987 0.9249 0.062 Uiso 0.601(9) 1 calc R . P A 1
C01I C 0.5660(7) 0.6418(18) 0.6474(17) 0.0519(9) Uani 0.601(9) 1 d . . P A .
H01O H 0.5384 0.6247 0.6630 0.062 Uiso 0.601(9) 1 calc R . P . .
H01P H 0.5661 0.7074 0.5992 0.062 Uiso 0.601(9) 1 calc R . P . .
O0AA O 0.3545(2) 0.1909(6) 0.7314(6) 0.0350(15) Uani 1 1 d . . . . .
B2 B 0.3653(4) 0.0729(11) 0.7178(10) 0.040(3) Uani 1 1 d . . . . .
C3 C 0.5841(6) 0.3348(18) 0.8940(17) 0.0519(9) Uani 0.601(9) 1 d . . P A 1
H3A H 0.5993 0.2710 0.9188 0.062 Uiso 0.601(9) 1 calc R . P A 1
H3B H 0.5960 0.4020 0.9236 0.062 Uiso 0.601(9) 1 calc R . P A 1
C6 C 0.5599(7) 0.5304(19) 0.4883(16) 0.0519(9) Uani 0.601(9) 1 d . . P . .
H6A H 0.5764 0.4791 0.4473 0.078 Uiso 0.601(9) 1 calc GR . P A .
H6B H 0.5546 0.5935 0.4405 0.078 Uiso 0.601(9) 1 calc GR . P . .
H6C H 0.5354 0.4949 0.5084 0.078 Uiso 0.601(9) 1 calc GR . P . .
C14 C 0.5231(7) 0.2586(19) 0.8495(17) 0.0519(9) Uani 0.601(9) 1 d . . P A 1
H14A H 0.4949 0.2742 0.8483 0.062 Uiso 0.601(9) 1 calc R . P A 1
H14B H 0.5274 0.1808 0.8660 0.062 Uiso 0.601(9) 1 calc R . P A 1
C0AA C 0.3788(3) 0.2726(8) 0.7015(8) 0.035(2) Uani 1 1 d . . . . .
P0 P 0.42987(9) 0.2749(3) 0.6908(3) 0.0570(9) Uani 1 1 d . . . . .
P1 P 0.43298(14) 0.4472(4) 0.6574(4) 0.0763(12) Uani 1 1 d . . . . .
C1AA C 0.3823(4) 0.4647(9) 0.6622(10) 0.053(3) Uani 1 1 d . . . . .
N00E N 0.3598(3) 0.3709(7) 0.6853(7) 0.045(2) Uani 1 1 d . . . . .
C2AA C 0.3172(4) 0.3786(11) 0.6886(11) 0.059(3) Uani 1 1 d . . . . .
H2AA H 0.3023 0.3153 0.7027 0.070 Uiso 1 1 calc R . . . .
C0 C 0.2991(5) 0.4739(14) 0.6718(14) 0.080(5) Uani 1 1 d . . . . .
H0 H 0.2716 0.4771 0.6715 0.096 Uiso 1 1 calc R . . . .
C4AA C 0.3218(8) 0.5724(15) 0.6541(16) 0.101(7) Uani 1 1 d . . . . .
H4AA H 0.3091 0.6402 0.6452 0.121 Uiso 1 1 calc R . . . .
C2 C 0.3614(8) 0.5665(12) 0.6504(13) 0.090(6) Uani 1 1 d . . . . .
H2 H 0.3758 0.6314 0.6398 0.109 Uiso 1 1 calc R . . . .
C19 C 0.5438(6) 0.2949(19) 0.7363(18) 0.0519(9) Uani 0.601(9) 1 d . . P A 1
H19A H 0.5477 0.2321 0.6856 0.062 Uiso 0.601(9) 1 calc R . P A 1
H19B H 0.5282 0.3503 0.6964 0.062 Uiso 0.601(9) 1 calc R . P A 1
C3AA C 0.6322(6) 0.2465(19) 0.495(2) 0.121(9) Uani 1 1 d . . . . .
H3AD H 0.6062 0.2307 0.5247 0.181 Uiso 0.634(12) 1 calc R . P A 1
H3AE H 0.6328 0.2321 0.4141 0.181 Uiso 0.634(12) 1 calc R . P A 1
H3AF H 0.6512 0.2004 0.5335 0.181 Uiso 0.634(12) 1 calc R . P A 1
H3AA H 0.6367 0.2692 0.4172 0.181 Uiso 0.3333 1 calc GR . P A -1
H3AB H 0.6231 0.1712 0.4964 0.181 Uiso 0.3333 1 calc GR . P A -1
H3AC H 0.6564 0.2523 0.5380 0.181 Uiso 0.3333 1 calc GR . P A -1
O2 O 0.6735(6) 0.3435(18) 0.778(2) 0.093(3) Uani 0.5 1 d . U P A -2
C6AA C 0.6611(5) 0.262(2) 0.862(3) 0.093(3) Uani 0.5 1 d G U P A -2
H6AA H 0.6431 0.2094 0.8272 0.112 Uiso 0.5 1 calc R . P A -2
H6AB H 0.6477 0.2982 0.9257 0.112 Uiso 0.5 1 calc R . P A -2
C5 C 0.6988(7) 0.2041(19) 0.904(3) 0.093(3) Uani 0.5 1 d G U P A -2
H5A H 0.7056 0.1419 0.8550 0.112 Uiso 0.5 1 calc R . P A -2
H5B H 0.6961 0.1787 0.9827 0.112 Uiso 0.5 1 calc R . P A -2
C8 C 0.7295(6) 0.298(2) 0.894(3) 0.093(3) Uani 0.5 1 d G U P A -2
H8A H 0.7284 0.3471 0.9600 0.112 Uiso 0.5 1 calc R . P A -2
H8B H 0.7562 0.2687 0.8866 0.112 Uiso 0.5 1 calc R . P A -2
C5AA C 0.7161(6) 0.356(2) 0.784(2) 0.093(3) Uani 0.5 1 d G U P A -2
H5AA H 0.7231 0.4340 0.7859 0.112 Uiso 0.5 1 calc R . P A -2
H5AB H 0.7285 0.3227 0.7169 0.112 Uiso 0.5 1 calc R . P A -2
O3 O 0.6714(5) 0.3522(13) 0.7968(15) 0.093(3) Uani 0.5 1 d . U P A 2
C11 C 0.7083(6) 0.4101(14) 0.814(2) 0.093(3) Uani 0.5 1 d G U P A 2
H11A H 0.7059 0.4632 0.8759 0.112 Uiso 0.5 1 calc R . P A 2
H11B H 0.7158 0.4494 0.7441 0.112 Uiso 0.5 1 calc R . P A 2
C12 C 0.7394(5) 0.3216(18) 0.843(2) 0.093(3) Uani 0.5 1 d G U P A 2
H12A H 0.7400 0.3065 0.9253 0.112 Uiso 0.5 1 calc R . P A 2
H12B H 0.7656 0.3433 0.8178 0.112 Uiso 0.5 1 calc R . P A 2
C15 C 0.7238(5) 0.2214(16) 0.775(2) 0.093(3) Uani 0.5 1 d G U P A 2
H15A H 0.7316 0.2253 0.6948 0.112 Uiso 0.5 1 calc R . P A 2
H15B H 0.7330 0.1521 0.8077 0.112 Uiso 0.5 1 calc R . P A 2
C16 C 0.6789(5) 0.2347(13) 0.7892(19) 0.093(3) Uani 0.5 1 d G U P A 2
H16A H 0.6651 0.2033 0.7236 0.112 Uiso 0.5 1 calc R . P A 2
H16B H 0.6699 0.1975 0.8584 0.112 Uiso 0.5 1 calc R . P A 2
O1 O 0.6029(8) 0.316(3) 0.546(2) 0.099(9) Uani 0.3333 1 d G . P A -1
C7AA C 0.5271(5) 0.362(4) 0.839(4) 0.099(9) Uani 0.25 1 d G . P A -1
H7AA H 0.5283 0.3466 0.9199 0.149 Uiso 0.25 1 calc . . P B -1
H7AB H 0.5083 0.3134 0.8031 0.149 Uiso 0.25 1 calc . . P C -1
H7AC H 0.5192 0.4375 0.8271 0.149 Uiso 0.25 1 calc . . P D -1
C4 C 0.584(3) 0.236(7) 0.597(7) 0.099(9) Uani 0.25 1 d . . P A -1
H4A H 0.6039 0.1864 0.6290 0.119 Uiso 0.25 1 calc R . P A -1
H4B H 0.5702 0.1947 0.5378 0.119 Uiso 0.25 1 calc R . P A -1
C10 C 0.557(3) 0.260(6) 0.684(6) 0.099(9) Uani 0.25 1 d . . P A -1
H10A H 0.5486 0.1924 0.7226 0.119 Uiso 0.25 1 calc R . P A -1
H10B H 0.5338 0.2966 0.6530 0.119 Uiso 0.25 1 calc R . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P001 P003 2.120(4) . ?
P001 C00E 1.734(10) . ?
P002 P004 2.127(4) . ?
P002 C00G 1.725(11) . ?
P003 C00V 1.720(12) . ?
P004 C00S 1.733(13) . ?
Na07 O00K 2.381(14) . ?
Na07 O00L 2.324(16) . ?
Na07 O00W 2.349(14) . ?
Na07 O00X 2.381(13) . ?
Na07 O013 2.368(15) . ?
Na07 O2 2.341(15) . ?
Na07 O3 2.349(15) . ?
Na07 O1 2.41(2) . ?
O08 C00G 1.343(13) . ?
O08 B2 1.453(14) . ?
O00A C00E 1.340(11) . ?
O00A B2 1.478(13) . ?
N00B C00E 1.370(13) . ?
N00B C00P 1.395(14) . ?
N00B C00V 1.392(13) . ?
N00C C00G 1.371(12) . ?
N00C C00O 1.398(14) . ?
N00C C00S 1.383(14) . ?
C00H H00H 0.9300 . ?
C00H C00J 1.387(15) . ?
C00H C00N 1.385(16) . ?
C00I H00I 0.9300 . ?
C00I C00O 1.361(16) . ?
C00I C00Q 1.388(17) . ?
C00J C012 1.380(17) . ?
C00J B2 1.643(16) . ?
O00K C01C 1.49(2) . ?
O00K C01G 1.38(2) . ?
O00L C3 1.44(2) . ?
O00L C19 1.37(2) . ?
O00L C7AA 1.95(2) . ?
O00L C10 1.57(7) . ?
C00N H00N 0.9300 . ?
C00N C011 1.354(19) . ?
C00O H00O 0.9300 . ?
C00P H00P 0.9300 . ?
C00P C00Z 1.355(18) . ?
C00Q H00Q 0.9300 . ?
C00Q C00U 1.332(17) . ?
C00S C00U 1.413(15) . ?
C00U H00U 0.9300 . ?
C00V C010 1.436(16) . ?
O00W C019 1.32(2) . ?
O00W C01A 1.37(2) . ?
O00X C01D 1.46(2) . ?
O00X C3AA 1.28(2) . ?
O00X O1 1.38(3) . ?
C00Z H00Z 0.9300 . ?
C00Z C014 1.41(2) . ?
C010 H010 0.9300 . ?
C010 C014 1.34(2) . ?
C011 H011 0.9300 . ?
C011 C016 1.36(2) . ?
C012 H012 0.9300 . ?
C012 C016 1.395(19) . ?
O013 C01I 1.24(2) . ?
O013 C6 1.39(2) . ?
C014 H014 0.9300 . ?
C016 H016 0.9300 . ?
C019 H01A 0.9700 . ?
C019 H01B 0.9700 . ?
C019 C01I 1.45(3) . ?
C01A H01C 0.9600 . ?
C01A H01D 0.9600 . ?
C01A H01E 0.9600 . ?
C01C H01F 0.9600 . ?
C01C H01G 0.9600 . ?
C01C H01H 0.9600 . ?
C01D H01I 0.9700 . ?
C01D H01J 0.9700 . ?
C01D C01G 1.47(3) . ?
C01G H01K 0.9700 . ?
C01G H01L 0.9700 . ?
C01H H01M 0.9700 . ?
C01H H01N 0.9700 . ?
C01H C3 1.44(3) . ?
C01H C14 1.37(3) . ?
C01H C7AA 1.22(5) . ?
C01I H01O 0.9700 . ?
C01I H01P 0.9700 . ?
O0AA B2 1.480(15) . ?
O0AA C0AA 1.330(12) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C19 1.55(3) . ?
C14 C7AA 1.26(6) . ?
C0AA P0 1.730(11) . ?
C0AA N00E 1.362(13) . ?
P0 P1 2.118(5) . ?
P1 C1AA 1.725(16) . ?
C1AA N00E 1.391(15) . ?
C1AA C2 1.42(2) . ?
N00E C2AA 1.441(17) . ?
C2AA H2AA 0.9300 . ?
C2AA C0 1.318(19) . ?
C0 H0 0.9300 . ?
C0 C4AA 1.43(3) . ?
C4AA H4AA 0.9300 . ?
C4AA C2 1.34(3) . ?
C2 H2 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C7AA 1.55(4) . ?
C19 C10 0.86(8) . ?
C3AA H3AD 0.9600 . ?
C3AA H3AE 0.9600 . ?
C3AA H3AF 0.9600 . ?
C3AA H3AA 0.9600 . ?
C3AA H3AB 0.9600 . ?
C3AA H3AC 0.9600 . ?
C3AA O1 1.43(3) . ?
O2 C6AA 1.4427 . ?
O2 C5AA 1.4463 . ?
O2 C11 1.48(3) . ?
O2 C16 1.33(3) . ?
C6AA H6AA 0.9700 . ?
C6AA H6AB 0.9700 . ?
C6AA C5 1.5349 . ?
C6AA O3 1.37(3) . ?
C6AA C16 1.09(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C8 1.5390 . ?
C5 C15 1.73(4) . ?
C5 C16 1.54(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C5AA 1.5340 . ?
C8 C11 1.80(3) . ?
C8 C12 0.74(4) . ?
C8 C15 1.67(4) . ?
C5AA H5AA 0.9700 . ?
C5AA H5AB 0.9700 . ?
C5AA O3 1.52(3) . ?
C5AA C11 0.78(4) . ?
C5AA C12 1.13(3) . ?
C5AA C15 1.65(3) . ?
C5AA C16 1.93(3) . ?
O3 C11 1.4429 . ?
O3 C16 1.4428 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.5364 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C15 1.5395 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.5346 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
O1 C4 1.30(9) . ?
C7AA H7AA 0.9600 . ?
C7AA H7AB 0.9600 . ?
C7AA H7AC 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C10 1.40(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?

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
C00E P001 P003 93.7(3) . . ?
C00G P002 P004 93.7(4) . . ?
C00V P003 P001 93.6(3) . . ?
C00S P004 P002 94.0(4) . . ?
O00K Na07 O00X 70.1(5) . . ?
O00K Na07 O1 101.7(9) . . ?
O00L Na07 O00K 170.2(5) . . ?
O00L Na07 O00W 97.6(5) . . ?
O00L Na07 O00X 101.1(5) . . ?
O00L Na07 O013 95.2(5) . . ?
O00L Na07 O2 86.0(7) . . ?
O00L Na07 O3 84.1(6) . . ?
O00L Na07 O1 70.7(9) . . ?
O00W Na07 O00K 92.0(5) . . ?
O00W Na07 O00X 155.7(5) . . ?
O00W Na07 O013 70.0(5) . . ?
O00W Na07 O1 149.0(7) . . ?
O00X Na07 O1 33.4(8) . . ?
O013 Na07 O00K 89.7(5) . . ?
O013 Na07 O00X 92.9(5) . . ?
O013 Na07 O1 82.2(7) . . ?
O2 Na07 O00W 109.1(8) . . ?
O2 Na07 O013 178.5(7) . . ?
O2 Na07 O3 6.1(9) . . ?
O3 Na07 O00W 103.5(6) . . ?
O3 Na07 O013 173.3(6) . . ?
C00G O08 B2 125.7(8) . . ?
C00E O00A B2 125.4(8) . . ?
C00E N00B C00P 122.0(9) . . ?
C00E N00B C00V 115.6(8) . . ?
C00V N00B C00P 122.4(9) . . ?
C00G N00C C00O 121.7(9) . . ?
C00G N00C C00S 117.8(9) . . ?
C00S N00C C00O 120.5(9) . . ?
O00A C00E P001 128.8(7) . . ?
O00A C00E N00B 112.7(8) . . ?
N00B C00E P001 118.5(7) . . ?
O08 C00G P002 128.5(7) . . ?
O08 C00G N00C 113.8(9) . . ?
N00C C00G P002 117.7(8) . . ?
C00J C00H H00H 119.5 . . ?
C00N C00H H00H 119.5 . . ?
C00N C00H C00J 120.9(11) . . ?
C00O C00I H00I 119.7 . . ?
C00O C00I C00Q 120.6(11) . . ?
C00Q C00I H00I 119.7 . . ?
C00H C00J B2 124.4(10) . . ?
C012 C00J C00H 116.4(11) . . ?
C012 C00J B2 119.1(10) . . ?
C01C O00K Na07 124.9(10) . . ?
C01G O00K Na07 116.5(12) . . ?
C01G O00K C01C 110.5(15) . . ?
C3 O00L Na07 112.0(12) . . ?
C3 O00L C7AA 72.6(16) . . ?
C3 O00L C10 132(3) . . ?
C19 O00L Na07 133.9(12) . . ?
C19 O00L C3 112.2(17) . . ?
C19 O00L C7AA 51.9(16) . . ?
C19 O00L C10 33(3) . . ?
C7AA O00L Na07 134.7(18) . . ?
C10 O00L Na07 114(3) . . ?
C10 O00L C7AA 85(4) . . ?
C00H C00N H00N 118.8 . . ?
C011 C00N C00H 122.4(13) . . ?
C011 C00N H00N 118.8 . . ?
N00C C00O H00O 120.0 . . ?
C00I C00O N00C 120.0(11) . . ?
C00I C00O H00O 120.0 . . ?
N00B C00P H00P 120.2 . . ?
C00Z C00P N00B 119.5(12) . . ?
C00Z C00P H00P 120.2 . . ?
C00I C00Q H00Q 120.6 . . ?
C00U C00Q C00I 118.9(10) . . ?
C00U C00Q H00Q 120.6 . . ?
N00C C00S P004 116.8(8) . . ?
N00C C00S C00U 116.5(11) . . ?
C00U C00S P004 126.6(9) . . ?
C00Q C00U C00S 123.4(11) . . ?
C00Q C00U H00U 118.3 . . ?
C00S C00U H00U 118.3 . . ?
N00B C00V P003 118.7(7) . . ?
N00B C00V C010 115.6(10) . . ?
C010 C00V P003 125.7(9) . . ?
C019 O00W Na07 115.1(12) . . ?
C019 O00W C01A 118.3(16) . . ?
C01A O00W Na07 126.5(12) . . ?
C01D O00X Na07 108.1(10) . . ?
C3AA O00X Na07 126.5(13) . . ?
C3AA O00X C01D 114.3(15) . . ?
C3AA O00X O1 64.7(17) . . ?
O1 O00X Na07 74.5(12) . . ?
O1 O00X C01D 176.8(15) . . ?
C00P C00Z H00Z 120.0 . . ?
C00P C00Z C014 120.1(13) . . ?
C014 C00Z H00Z 120.0 . . ?
C00V C010 H010 119.1 . . ?
C014 C010 C00V 121.9(12) . . ?
C014 C010 H010 119.1 . . ?
C00N C011 H011 121.3 . . ?
C00N C011 C016 117.3(12) . . ?
C016 C011 H011 121.3 . . ?
C00J C012 H012 119.5 . . ?
C00J C012 C016 121.0(13) . . ?
C016 C012 H012 119.5 . . ?
C01I O013 Na07 114.4(13) . . ?
C01I O013 C6 121.2(17) . . ?
C6 O013 Na07 122.0(12) . . ?
C00Z C014 H014 119.8 . . ?
C010 C014 C00Z 120.4(12) . . ?
C010 C014 H014 119.8 . . ?
C011 C016 C012 121.8(13) . . ?
C011 C016 H016 119.1 . . ?
C012 C016 H016 119.1 . . ?
O00W C019 H01A 108.1 . . ?
O00W C019 H01B 108.1 . . ?
O00W C019 C01I 116.7(17) . . ?
H01A C019 H01B 107.3 . . ?
C01I C019 H01A 108.1 . . ?
C01I C019 H01B 108.1 . . ?
O00W C01A H01C 109.5 . . ?
O00W C01A H01D 109.5 . . ?
O00W C01A H01E 109.5 . . ?
H01C C01A H01D 109.5 . . ?
H01C C01A H01E 109.5 . . ?
H01D C01A H01E 109.5 . . ?
O00K C01C H01F 109.5 . . ?
O00K C01C H01G 109.5 . . ?
O00K C01C H01H 109.5 . . ?
H01F C01C H01G 109.5 . . ?
H01F C01C H01H 109.5 . . ?
H01G C01C H01H 109.5 . . ?
O00X C01D H01I 109.1 . . ?
O00X C01D H01J 109.1 . . ?
O00X C01D C01G 112.3(16) . . ?
H01I C01D H01J 107.9 . . ?
C01G C01D H01I 109.1 . . ?
C01G C01D H01J 109.1 . . ?
O00K C01G C01D 105.1(16) . . ?
O00K C01G H01K 110.7 . . ?
O00K C01G H01L 110.7 . . ?
C01D C01G H01K 110.7 . . ?
C01D C01G H01L 110.7 . . ?
H01K C01G H01L 108.8 . . ?
H01M C01H H01N 108.1 . . ?
C3 C01H H01M 109.5 . . ?
C3 C01H H01N 109.5 . . ?
C14 C01H H01M 109.5 . . ?
C14 C01H H01N 109.5 . . ?
C14 C01H C3 110.9(18) . . ?
C7AA C01H H01M 149.6 . . ?
C7AA C01H H01N 59.3 . . ?
C7AA C01H C3 101(2) . . ?
C7AA C01H C14 58(3) . . ?
O013 C01I C019 122.1(19) . . ?
O013 C01I H01O 106.8 . . ?
O013 C01I H01P 106.8 . . ?
C019 C01I H01O 106.8 . . ?
C019 C01I H01P 106.8 . . ?
H01O C01I H01P 106.6 . . ?
C0AA O0AA B2 122.2(8) . . ?
O08 B2 O00A 106.9(9) . . ?
O08 B2 C00J 111.7(9) . . ?
O08 B2 O0AA 107.3(9) . . ?
O00A B2 C00J 113.8(9) . . ?
O00A B2 O0AA 111.0(9) . . ?
O0AA B2 C00J 105.9(9) . . ?
O00L C3 H3A 112.1 . . ?
O00L C3 H3B 112.1 . . ?
C01H C3 O00L 98.3(16) . . ?
C01H C3 H3A 112.1 . . ?
C01H C3 H3B 112.1 . . ?
H3A C3 H3B 109.8 . . ?
O013 C6 H6A 109.5 . . ?
O013 C6 H6B 109.5 . . ?
O013 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C01H C14 H14A 112.0 . . ?
C01H C14 H14B 112.0 . . ?
C01H C14 C19 99.0(18) . . ?
H14A C14 H14B 109.7 . . ?
C19 C14 H14A 112.0 . . ?
C19 C14 H14B 112.0 . . ?
C7AA C14 C01H 55(2) . . ?
C7AA C14 H14A 85.0 . . ?
C7AA C14 H14B 164.1 . . ?
C7AA C14 C19 66(2) . . ?
O0AA C0AA P0 130.3(8) . . ?
O0AA C0AA N00E 113.0(9) . . ?
N00E C0AA P0 116.5(8) . . ?
C0AA P0 P1 94.5(4) . . ?
C1AA P1 P0 93.7(4) . . ?
N00E C1AA P1 116.7(9) . . ?
N00E C1AA C2 116.8(15) . . ?
C2 C1AA P1 126.4(13) . . ?
C0AA N00E C1AA 118.6(11) . . ?
C0AA N00E C2AA 121.6(10) . . ?
C1AA N00E C2AA 119.9(11) . . ?
N00E C2AA H2AA 119.5 . . ?
C0 C2AA N00E 121.1(15) . . ?
C0 C2AA H2AA 119.5 . . ?
C2AA C0 H0 120.1 . . ?
C2AA C0 C4AA 119.9(17) . . ?
C4AA C0 H0 120.1 . . ?
C0 C4AA H4AA 120.1 . . ?
C2 C4AA C0 119.7(15) . . ?
C2 C4AA H4AA 120.1 . . ?
C1AA C2 H2 118.8 . . ?
C4AA C2 C1AA 122.4(17) . . ?
C4AA C2 H2 118.8 . . ?
O00L C19 C14 104.7(16) . . ?
O00L C19 H19A 110.8 . . ?
O00L C19 H19B 110.8 . . ?
O00L C19 C7AA 84.0(17) . . ?
C14 C19 H19A 110.8 . . ?
C14 C19 H19B 110.8 . . ?
H19A C19 H19B 108.9 . . ?
C7AA C19 C14 48(2) . . ?
C7AA C19 H19A 158.0 . . ?
C7AA C19 H19B 79.0 . . ?
C10 C19 O00L 87(6) . . ?
C10 C19 C14 133(6) . . ?
C10 C19 H19A 28.2 . . ?
C10 C19 H19B 106.5 . . ?
C10 C19 C7AA 170(7) . . ?
O00X C3AA H3AD 109.5 . . ?
O00X C3AA H3AE 109.5 . . ?
O00X C3AA H3AF 109.5 . . ?
O00X C3AA H3AA 81.3 . . ?
O00X C3AA H3AB 168.2 . . ?
O00X C3AA H3AC 70.0 . . ?
O00X C3AA O1 61.0(16) . . ?
H3AD C3AA H3AE 109.5 . . ?
H3AD C3AA H3AF 109.5 . . ?
H3AD C3AA H3AA 122.5 . . ?
H3AD C3AA H3AB 61.0 . . ?
H3AD C3AA H3AC 127.6 . . ?
H3AE C3AA H3AF 109.5 . . ?
H3AE C3AA H3AA 28.2 . . ?
H3AE C3AA H3AB 81.3 . . ?
H3AE C3AA H3AC 120.1 . . ?
H3AF C3AA H3AA 119.7 . . ?
H3AF C3AA H3AB 70.0 . . ?
H3AF C3AA H3AC 39.7 . . ?
H3AA C3AA H3AB 109.5 . . ?
H3AA C3AA H3AC 109.5 . . ?
H3AB C3AA H3AC 109.5 . . ?
O1 C3AA H3AD 48.6 . . ?
O1 C3AA H3AE 122.1 . . ?
O1 C3AA H3AF 128.0 . . ?
O1 C3AA H3AA 109.5 . . ?
O1 C3AA H3AB 109.5 . . ?
O1 C3AA H3AC 109.5 . . ?
C6AA O2 Na07 119.8(12) . . ?
C6AA O2 C5AA 109.3 . . ?
C6AA O2 C11 114.3(14) . . ?
C5AA O2 Na07 129.9(12) . . ?
C5AA O2 C11 30.9(15) . . ?
C11 O2 Na07 111.8(13) . . ?
C16 O2 Na07 133.4(19) . . ?
C16 O2 C6AA 46.0(16) . . ?
C16 O2 C5AA 88.0(14) . . ?
C16 O2 C11 113.6(17) . . ?
O2 C6AA H6AA 110.4 . . ?
O2 C6AA H6AB 110.4 . . ?
O2 C6AA C5 106.5 . . ?
H6AA C6AA H6AB 108.6 . . ?
C5 C6AA H6AA 110.4 . . ?
C5 C6AA H6AB 110.4 . . ?
O3 C6AA O2 9.8(15) . . ?
O3 C6AA H6AA 116.9 . . ?
O3 C6AA H6AB 100.9 . . ?
O3 C6AA C5 109.1(11) . . ?
C16 C6AA O2 61.6(15) . . ?
C16 C6AA H6AA 79.6 . . ?
C16 C6AA H6AB 170.7 . . ?
C16 C6AA C5 69.5(15) . . ?
C16 C6AA O3 70.9(18) . . ?
C6AA C5 H5A 111.5 . . ?
C6AA C5 H5B 111.5 . . ?
C6AA C5 C8 101.5 . . ?
C6AA C5 C15 94.2(11) . . ?
C6AA C5 C16 41.5(13) . . ?
H5A C5 H5B 109.3 . . ?
C8 C5 H5A 111.5 . . ?
C8 C5 H5B 111.5 . . ?
C8 C5 C15 61.3(14) . . ?
C8 C5 C16 93.1(12) . . ?
C15 C5 H5A 58.1 . . ?
C15 C5 H5B 154.3 . . ?
C16 C5 H5A 77.4 . . ?
C16 C5 H5B 148.4 . . ?
C16 C5 C15 55.6(12) . . ?
C5 C8 H8A 111.5 . . ?
C5 C8 H8B 111.5 . . ?
C5 C8 C11 108.9(11) . . ?
C5 C8 C15 65.1(13) . . ?
H8A C8 H8B 109.3 . . ?
C5AA C8 C5 101.5 . . ?
C5AA C8 H8A 111.5 . . ?
C5AA C8 H8B 111.5 . . ?
C5AA C8 C11 25.7(14) . . ?
C5AA C8 C15 61.7(11) . . ?
C11 C8 H8A 86.1 . . ?
C11 C8 H8B 126.6 . . ?
C12 C8 C5 131(3) . . ?
C12 C8 H8A 114.3 . . ?
C12 C8 H8B 69.4 . . ?
C12 C8 C5AA 44(2) . . ?
C12 C8 C11 57.9(19) . . ?
C12 C8 C15 67(3) . . ?
C15 C8 H8A 170.1 . . ?
C15 C8 H8B 80.4 . . ?
C15 C8 C11 86.5(14) . . ?
O2 C5AA C8 106.4 . . ?
O2 C5AA H5AA 110.4 . . ?
O2 C5AA H5AB 110.4 . . ?
O2 C5AA O3 9.3(14) . . ?
O2 C5AA C15 92.9(13) . . ?
O2 C5AA C16 43.5(9) . . ?
C8 C5AA H5AA 110.4 . . ?
C8 C5AA H5AB 110.4 . . ?
C8 C5AA C15 63.3(15) . . ?
C8 C5AA C16 79.4(9) . . ?
H5AA C5AA H5AB 108.6 . . ?
O3 C5AA C8 101.3(12) . . ?
O3 C5AA H5AA 105.9 . . ?
O3 C5AA H5AB 119.8 . . ?
O3 C5AA C15 97.6(17) . . ?
O3 C5AA C16 47.6(9) . . ?
C11 C5AA O2 77(3) . . ?
C11 C5AA C8 96(3) . . ?
C11 C5AA H5AA 42.7 . . ?
C11 C5AA H5AB 147.8 . . ?
C11 C5AA O3 70(2) . . ?
C11 C5AA C12 105(4) . . ?
C11 C5AA C15 154(3) . . ?
C11 C5AA C16 114(3) . . ?
C12 C5AA O2 132.9(16) . . ?
C12 C5AA C8 27.0(18) . . ?
C12 C5AA H5AA 99.8 . . ?
C12 C5AA H5AB 92.0 . . ?
C12 C5AA O3 128(2) . . ?
C12 C5AA C15 64.0(14) . . ?
C12 C5AA C16 98.8(16) . . ?
C15 C5AA H5AA 156.5 . . ?
C15 C5AA H5AB 58.1 . . ?
C15 C5AA C16 50.0(9) . . ?
C16 C5AA H5AA 153.5 . . ?
C16 C5AA H5AB 89.4 . . ?
C6AA O3 Na07 123.3(13) . . ?
C6AA O3 C5AA 109.6(14) . . ?
C6AA O3 C11 122.0(13) . . ?
C6AA O3 C16 45.5(16) . . ?
C5AA O3 Na07 125.1(13) . . ?
C11 O3 Na07 113.1(7) . . ?
C11 O3 C5AA 30.5(14) . . ?
C16 O3 Na07 125.5(6) . . ?
C16 O3 C5AA 81.5(12) . . ?
C16 O3 C11 109.5 . . ?
O2 C11 C8 92.9(14) . . ?
O2 C11 H11A 119.9 . . ?
O2 C11 H11B 103.9 . . ?
O2 C11 C12 103.1(9) . . ?
C8 C11 H11A 98.3 . . ?
C8 C11 H11B 134.4 . . ?
C5AA C11 O2 72(2) . . ?
C5AA C11 C8 58.1(18) . . ?
C5AA C11 O3 80(2) . . ?
C5AA C11 H11A 155.4 . . ?
C5AA C11 H11B 87.1 . . ?
C5AA C11 C12 45(2) . . ?
O3 C11 O2 9.7(14) . . ?
O3 C11 C8 92.8(10) . . ?
O3 C11 H11A 110.4 . . ?
O3 C11 H11B 110.4 . . ?
O3 C11 C12 106.5 . . ?
H11A C11 H11B 108.6 . . ?
C12 C11 C8 23.9(12) . . ?
C12 C11 H11A 110.4 . . ?
C12 C11 H11B 110.4 . . ?
C8 C12 C5AA 109(3) . . ?
C8 C12 C11 98(2) . . ?
C8 C12 H12A 31.7 . . ?
C8 C12 H12B 139.8 . . ?
C8 C12 C15 87(3) . . ?
C5AA C12 C11 29(2) . . ?
C5AA C12 H12A 133.4 . . ?
C5AA C12 H12B 110.4 . . ?
C5AA C12 C15 74.6(19) . . ?
C11 C12 H12A 111.5 . . ?
C11 C12 H12B 111.5 . . ?
C11 C12 C15 101.3 . . ?
H12A C12 H12B 109.3 . . ?
C15 C12 H12A 111.5 . . ?
C15 C12 H12B 111.5 . . ?
C5 C15 H15A 165.8 . . ?
C5 C15 H15B 73.4 . . ?
C8 C15 C5 53.7(12) . . ?
C8 C15 H15A 137.5 . . ?
C8 C15 H15B 96.6 . . ?
C5AA C15 C5 89.4(15) . . ?
C5AA C15 C8 54.9(12) . . ?
C5AA C15 H15A 93.1 . . ?
C5AA C15 H15B 151.3 . . ?
C12 C15 C5 79.4(13) . . ?
C12 C15 C8 26.1(11) . . ?
C12 C15 C5AA 41.3(12) . . ?
C12 C15 H15A 111.4 . . ?
C12 C15 H15B 111.4 . . ?
H15A C15 H15B 109.3 . . ?
C16 C15 C5 55.8(10) . . ?
C16 C15 C8 88.2(11) . . ?
C16 C15 C5AA 74.6(11) . . ?
C16 C15 C12 101.6 . . ?
C16 C15 H15A 111.4 . . ?
C16 C15 H15B 111.4 . . ?
O2 C16 C5 112(2) . . ?
O2 C16 C5AA 48.4(10) . . ?
O2 C16 O3 9.3(16) . . ?
O2 C16 C15 103.1(14) . . ?
O2 C16 H16A 104.2 . . ?
O2 C16 H16B 119.6 . . ?
C6AA C16 O2 72.4(18) . . ?
C6AA C16 C5 69.0(18) . . ?
C6AA C16 C5AA 99(2) . . ?
C6AA C16 O3 63.6(18) . . ?
C6AA C16 C15 131.3(17) . . ?
C6AA C16 H16A 117.7 . . ?
C6AA C16 H16B 47.6 . . ?
C5 C16 C5AA 85.8(14) . . ?
C5 C16 H16A 142.8 . . ?
C5 C16 H16B 46.1 . . ?
C5AA C16 H16A 125.7 . . ?
C5AA C16 H16B 125.6 . . ?
O3 C16 C5 105.0(15) . . ?
O3 C16 C5AA 50.9(10) . . ?
O3 C16 C15 106.3 . . ?
O3 C16 H16A 110.5 . . ?
O3 C16 H16B 110.5 . . ?
C15 C16 C5 68.6(13) . . ?
C15 C16 C5AA 55.5(10) . . ?
C15 C16 H16A 110.5 . . ?
C15 C16 H16B 110.5 . . ?
H16A C16 H16B 108.7 . . ?
O00X O1 Na07 72.1(12) . . ?
O00X O1 C3AA 54.3(15) . . ?
C3AA O1 Na07 116.7(15) . . ?
C4 O1 Na07 111(3) . . ?
C4 O1 O00X 142(5) . . ?
C4 O1 C3AA 95(4) . . ?
O00L C7AA H7AA 109.5 . . ?
O00L C7AA H7AB 109.5 . . ?
O00L C7AA H7AC 109.5 . . ?
C01H C7AA O00L 83.4(15) . . ?
C01H C7AA C14 67(3) . . ?
C01H C7AA C19 107(3) . . ?
C01H C7AA H7AA 26.6 . . ?
C01H C7AA H7AB 115.3 . . ?
C01H C7AA H7AC 125.5 . . ?
C14 C7AA O00L 89(2) . . ?
C14 C7AA C19 66(2) . . ?
C14 C7AA H7AA 73.6 . . ?
C14 C7AA H7AB 50.8 . . ?
C14 C7AA H7AC 157.5 . . ?
C19 C7AA O00L 44.1(10) . . ?
C19 C7AA H7AA 129.8 . . ?
C19 C7AA H7AB 65.7 . . ?
C19 C7AA H7AC 119.2 . . ?
H7AA C7AA H7AB 109.5 . . ?
H7AA C7AA H7AC 109.5 . . ?
H7AB C7AA H7AC 109.5 . . ?
O1 C4 H4A 107.4 . . ?
O1 C4 H4B 107.4 . . ?
O1 C4 C10 120(7) . . ?
H4A C4 H4B 107.0 . . ?
C10 C4 H4A 107.4 . . ?
C10 C4 H4B 107.4 . . ?
O00L C10 H10A 110.6 . . ?
O00L C10 H10B 110.6 . . ?
C19 C10 O00L 60(4) . . ?
C19 C10 C4 162(10) . . ?
C19 C10 H10A 86.6 . . ?
C19 C10 H10B 67.8 . . ?
C4 C10 O00L 106(7) . . ?
C4 C10 H10A 110.6 . . ?
C4 C10 H10B 110.6 . . ?
H10A C10 H10B 108.7 . . ?

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
P001 P003 C00V N00B 0.7(8) . . . . ?
P001 P003 C00V C010 -178.7(11) . . . . ?
P002 P004 C00S N00C 0.2(8) . . . . ?
P002 P004 C00S C00U 177.2(10) . . . . ?
P003 P001 C00E O00A -179.2(8) . . . . ?
P003 P001 C00E N00B 1.2(8) . . . . ?
P003 C00V C010 C014 179.4(12) . . . . ?
P004 P002 C00G O08 179.4(9) . . . . ?
P004 P002 C00G N00C 1.7(8) . . . . ?
P004 C00S C00U C00Q -179.3(10) . . . . ?
Na07 O00K C01G C01D -40.9(19) . . . . ?
Na07 O00L C3 C01H 145.5(12) . . . . ?
Na07 O00L C19 C14 -162.7(13) . . . . ?
Na07 O00L C19 C7AA -119(2) . . . . ?
Na07 O00L C19 C10 63(6) . . . . ?
Na07 O00L C10 C19 -135(4) . . . . ?
Na07 O00L C10 C4 32(7) . . . . ?
Na07 O00W C019 C01I -8(2) . . . . ?
Na07 O00X C01D C01G -48.5(17) . . . . ?
Na07 O00X C3AA O1 44.1(17) . . . . ?
Na07 O00X O1 C3AA -144.5(16) . . . . ?
Na07 O00X O1 C4 -102(6) . . . . ?
Na07 O013 C01I C019 12(3) . . . . ?
Na07 O2 C6AA C5 178.0(19) . . . . ?
Na07 O2 C6AA O3 -75(7) . . . . ?
Na07 O2 C6AA C16 123(2) . . . . ?
Na07 O2 C5AA C8 156(2) . . . . ?
Na07 O2 C5AA O3 98(7) . . . . ?
Na07 O2 C5AA C11 63(3) . . . . ?
Na07 O2 C5AA C12 162(4) . . . . ?
Na07 O2 C5AA C15 -141(2) . . . . ?
Na07 O2 C5AA C16 -150(3) . . . . ?
Na07 O2 C11 C8 172.5(16) . . . . ?
Na07 O2 C11 C5AA -132(2) . . . . ?
Na07 O2 C11 O3 83(5) . . . . ?
Na07 O2 C11 C12 -165.6(11) . . . . ?
Na07 O2 C16 C6AA -92(3) . . . . ?
Na07 O2 C16 C5 -150(2) . . . . ?
Na07 O2 C16 C5AA 148(3) . . . . ?
Na07 O2 C16 O3 -110(9) . . . . ?
Na07 O2 C16 C15 138(2) . . . . ?
Na07 O3 C11 O2 -86(6) . . . . ?
Na07 O3 C11 C8 -177.4(15) . . . . ?
Na07 O3 C11 C5AA -121(3) . . . . ?
Na07 O3 C11 C12 -157.4(8) . . . . ?
Na07 O3 C16 O2 56(8) . . . . ?
Na07 O3 C16 C6AA -104(2) . . . . ?
Na07 O3 C16 C5 -161.1(15) . . . . ?
Na07 O3 C16 C5AA 127.4(18) . . . . ?
Na07 O3 C16 C15 127.3(10) . . . . ?
Na07 O1 C4 C10 44(9) . . . . ?
N00B C00P C00Z C014 -2(2) . . . . ?
N00B C00V C010 C014 0.0(19) . . . . ?
N00C C00S C00U C00Q -2.4(17) . . . . ?
C00E O00A B2 O08 -168.8(8) . . . . ?
C00E O00A B2 C00J 67.4(13) . . . . ?
C00E O00A B2 O0AA -52.0(13) . . . . ?
C00E N00B C00P C00Z -178.3(12) . . . . ?
C00E N00B C00V P003 0.0(12) . . . . ?
C00E N00B C00V C010 179.4(10) . . . . ?
C00G O08 B2 O00A -60.0(13) . . . . ?
C00G O08 B2 C00J 65.2(13) . . . . ?
C00G O08 B2 O0AA -179.2(8) . . . . ?
C00G N00C C00O C00I 177.1(10) . . . . ?
C00G N00C C00S P004 0.9(12) . . . . ?
C00G N00C C00S C00U -176.3(9) . . . . ?
C00H C00J C012 C016 2(2) . . . . ?
C00H C00J B2 O08 -108.0(12) . . . . ?
C00H C00J B2 O00A 13.2(15) . . . . ?
C00H C00J B2 O0AA 135.5(10) . . . . ?
C00H C00N C011 C016 -1(2) . . . . ?
C00I C00Q C00U C00S 0.3(18) . . . . ?
C00J C00H C00N C011 -1(2) . . . . ?
C00J C012 C016 C011 -4(3) . . . . ?
O00L C19 C7AA C01H -61(3) . . . . ?
O00L C19 C7AA C14 -116.0(19) . . . . ?
O00L C19 C10 C4 -43(32) . . . . ?
C00N C00H C00J C012 0.0(18) . . . . ?
C00N C00H C00J B2 178.8(11) . . . . ?
C00N C011 C016 C012 3(3) . . . . ?
C00O N00C C00G P002 178.3(7) . . . . ?
C00O N00C C00G O08 0.3(13) . . . . ?
C00O N00C C00S P004 -179.3(7) . . . . ?
C00O N00C C00S C00U 3.5(14) . . . . ?
C00O C00I C00Q C00U 0.6(18) . . . . ?
C00P N00B C00E P001 176.9(8) . . . . ?
C00P N00B C00E O00A -2.8(13) . . . . ?
C00P N00B C00V P003 -177.8(8) . . . . ?
C00P N00B C00V C010 1.6(15) . . . . ?
C00P C00Z C014 C010 4(3) . . . . ?
C00Q C00I C00O N00C 0.6(17) . . . . ?
C00S N00C C00G P002 -1.9(12) . . . . ?
C00S N00C C00G O08 -179.9(9) . . . . ?
C00S N00C C00O C00I -2.7(15) . . . . ?
C00V N00B C00E P001 -0.9(11) . . . . ?
C00V N00B C00E O00A 179.4(8) . . . . ?
C00V N00B C00P C00Z -0.7(17) . . . . ?
C00V C010 C014 C00Z -3(2) . . . . ?
O00W C019 C01I O013 -3(3) . . . . ?
O00X C01D C01G O00K 60(2) . . . . ?
O00X C3AA O1 Na07 -38.2(19) . . . . ?
O00X C3AA O1 C4 -155(4) . . . . ?
O00X O1 C4 C10 131(7) . . . . ?
C012 C00J B2 O08 70.7(15) . . . . ?
C012 C00J B2 O00A -168.1(12) . . . . ?
C012 C00J B2 O0AA -45.8(15) . . . . ?
C01A O00W C019 C01I 176.2(19) . . . . ?
C01C O00K C01G C01D 168.9(15) . . . . ?
C01D O00X C3AA O1 -176.6(17) . . . . ?
C01H C14 C19 O00L 23(2) . . . . ?
C01H C14 C19 C7AA -44.7(18) . . . . ?
C01H C14 C19 C10 122(9) . . . . ?
C01H C14 C7AA O00L 83.1(15) . . . . ?
C01H C14 C7AA C19 121.8(16) . . . . ?
O0AA C0AA P0 P1 -173.9(8) . . . . ?
O0AA C0AA N00E C1AA 175.3(8) . . . . ?
O0AA C0AA N00E C2AA -6.4(13) . . . . ?
B2 O08 C00G P002 19.8(15) . . . . ?
B2 O08 C00G N00C -162.5(9) . . . . ?
B2 O00A C00E P001 -10.4(14) . . . . ?
B2 O00A C00E N00B 169.2(9) . . . . ?
B2 C00J C012 C016 -176.6(15) . . . . ?
B2 O0AA C0AA P0 -25.0(13) . . . . ?
B2 O0AA C0AA N00E 160.1(9) . . . . ?
C3 O00L C19 C14 0(2) . . . . ?
C3 O00L C19 C7AA 43(3) . . . . ?
C3 O00L C19 C10 -135(6) . . . . ?
C3 O00L C10 C19 63(7) . . . . ?
C3 O00L C10 C4 -130(5) . . . . ?
C3 C01H C14 C19 -38(2) . . . . ?
C3 C01H C14 C7AA -90(2) . . . . ?
C3 C01H C7AA O00L 16(2) . . . . ?
C3 C01H C7AA C14 107.9(19) . . . . ?
C3 C01H C7AA C19 54(3) . . . . ?
C6 O013 C01I C019 175(2) . . . . ?
C14 C01H C3 O00L 38(2) . . . . ?
C14 C01H C7AA O00L -92.2(19) . . . . ?
C14 C01H C7AA C19 -54(3) . . . . ?
C14 C19 C7AA O00L 116.0(19) . . . . ?
C14 C19 C7AA C01H 55(3) . . . . ?
C14 C19 C10 O00L -107(6) . . . . ?
C14 C19 C10 C4 -151(27) . . . . ?
C0AA O0AA B2 O08 53.5(12) . . . . ?
C0AA O0AA B2 O00A -63.1(12) . . . . ?
C0AA O0AA B2 C00J 172.9(8) . . . . ?
C0AA N00E C2AA C0 -179.4(12) . . . . ?
P0 C0AA N00E C1AA -0.3(12) . . . . ?
P0 C0AA N00E C2AA 178.0(8) . . . . ?
P0 P1 C1AA N00E 0.8(9) . . . . ?
P0 P1 C1AA C2 177.6(11) . . . . ?
P1 C1AA N00E C0AA -0.5(13) . . . . ?
P1 C1AA N00E C2AA -178.8(8) . . . . ?
P1 C1AA C2 C4AA 179.3(13) . . . . ?
C1AA N00E C2AA C0 -1.1(17) . . . . ?
N00E C0AA P0 P1 0.8(8) . . . . ?
N00E C1AA C2 C4AA -4(2) . . . . ?
N00E C2AA C0 C4AA -2(2) . . . . ?
C2AA C0 C4AA C2 2(3) . . . . ?
C0 C4AA C2 C1AA 1(3) . . . . ?
C2 C1AA N00E C0AA -177.5(10) . . . . ?
C2 C1AA N00E C2AA 4.1(15) . . . . ?
C19 O00L C3 C01H -21(2) . . . . ?
C19 O00L C10 C4 167(10) . . . . ?
C19 C14 C7AA O00L -38.7(12) . . . . ?
C19 C14 C7AA C01H -121.8(16) . . . . ?
C3AA O00X C01D C01G 164.9(19) . . . . ?
C3AA O00X O1 Na07 144.5(16) . . . . ?
C3AA O00X O1 C4 42(6) . . . . ?
C3AA O1 C4 C10 165(7) . . . . ?
O2 C6AA C5 C8 31.5 . . . . ?
O2 C6AA C5 C15 -30.0(14) . . . . ?
O2 C6AA C5 C16 -50.1(17) . . . . ?
O2 C6AA O3 Na07 92(7) . . . . ?
O2 C6AA O3 C5AA -72(6) . . . . ?
O2 C6AA O3 C11 -103(7) . . . . ?
O2 C6AA O3 C16 -17(8) . . . . ?
O2 C6AA C16 C5 123.2(13) . . . . ?
O2 C6AA C16 C5AA 41.2(7) . . . . ?
O2 C6AA C16 O3 3.2(16) . . . . ?
O2 C6AA C16 C15 92(2) . . . . ?
O2 C5AA O3 Na07 -68(6) . . . . ?
O2 C5AA O3 C6AA 96(7) . . . . ?
O2 C5AA O3 C11 -143(6) . . . . ?
O2 C5AA O3 C16 60(6) . . . . ?
O2 C5AA C11 C8 105.5(6) . . . . ?
O2 C5AA C11 O3 5.7(10) . . . . ?
O2 C5AA C11 C12 131.4(19) . . . . ?
O2 C5AA C12 C8 -14(6) . . . . ?
O2 C5AA C12 C11 -87(4) . . . . ?
O2 C5AA C12 C15 68(3) . . . . ?
O2 C5AA C15 C5 -62.7(14) . . . . ?
O2 C5AA C15 C8 -107.0(6) . . . . ?
O2 C5AA C15 C12 -137.2(19) . . . . ?
O2 C5AA C15 C16 -8.1(10) . . . . ?
O2 C11 C12 C8 -67(3) . . . . ?
O2 C11 C12 C5AA 47(2) . . . . ?
O2 C11 C12 C15 22.1(14) . . . . ?
C6AA O2 C5AA C8 -12.4 . . . . ?
C6AA O2 C5AA O3 -70(6) . . . . ?
C6AA O2 C5AA C11 -105(3) . . . . ?
C6AA O2 C5AA C12 -6(3) . . . . ?
C6AA O2 C5AA C15 50.6(14) . . . . ?
C6AA O2 C5AA C16 41.6(16) . . . . ?
C6AA O2 C11 C8 32(2) . . . . ?
C6AA O2 C11 C5AA 87(3) . . . . ?
C6AA O2 C11 O3 -57(6) . . . . ?
C6AA O2 C11 C12 54.3(19) . . . . ?
C6AA O2 C16 C5 -57.6(19) . . . . ?
C6AA O2 C16 C5AA -119.6(13) . . . . ?
C6AA O2 C16 O3 -18(9) . . . . ?
C6AA O2 C16 C15 -129.5(17) . . . . ?
C6AA C5 C8 C5AA -37.4 . . . . ?
C6AA C5 C8 C11 -11.9(16) . . . . ?
C6AA C5 C8 C12 -75(3) . . . . ?
C6AA C5 C8 C15 -88.5(11) . . . . ?
C6AA C5 C15 C8 100.8(6) . . . . ?
C6AA C5 C15 C5AA 55.6(15) . . . . ?
C6AA C5 C15 C12 96.0(11) . . . . ?
C6AA C5 C15 C16 -16.1(11) . . . . ?
C6AA C5 C16 O2 59.5(19) . . . . ?
C6AA C5 C16 C5AA 101.0(16) . . . . ?
C6AA C5 C16 O3 53.4(17) . . . . ?
C6AA C5 C16 C15 155.4(14) . . . . ?
C6AA O3 C11 O2 108(6) . . . . ?
C6AA O3 C11 C8 17(2) . . . . ?
C6AA O3 C11 C5AA 74(3) . . . . ?
C6AA O3 C11 C12 37(2) . . . . ?
C6AA O3 C16 O2 161(10) . . . . ?
C6AA O3 C16 C5 -56.8(18) . . . . ?
C6AA O3 C16 C5AA -128(3) . . . . ?
C6AA O3 C16 C15 -128.5(19) . . . . ?
C5 C6AA O3 Na07 168.3(12) . . . . ?
C5 C6AA O3 C5AA 4(3) . . . . ?
C5 C6AA O3 C11 -27(2) . . . . ?
C5 C6AA O3 C16 59.1(15) . . . . ?
C5 C6AA C16 O2 -123.2(13) . . . . ?
C5 C6AA C16 C5AA -82.0(12) . . . . ?
C5 C6AA C16 O3 -120.0(10) . . . . ?
C5 C6AA C16 C15 -31.0(17) . . . . ?
C5 C8 C5AA O2 31.6 . . . . ?
C5 C8 C5AA O3 39.6(13) . . . . ?
C5 C8 C5AA C11 110(3) . . . . ?
C5 C8 C5AA C12 -138(5) . . . . ?
C5 C8 C5AA C15 -53.3(14) . . . . ?
C5 C8 C5AA C16 -3.0(10) . . . . ?
C5 C8 C11 O2 -10(2) . . . . ?
C5 C8 C11 C5AA -77(3) . . . . ?
C5 C8 C11 O3 -0.6(18) . . . . ?
C5 C8 C11 C12 -127(4) . . . . ?
C5 C8 C12 C5AA 60(5) . . . . ?
C5 C8 C12 C11 88(3) . . . . ?
C5 C8 C12 C15 -13(3) . . . . ?
C5 C8 C15 C5AA 120.0(9) . . . . ?
C5 C8 C15 C12 169(2) . . . . ?
C5 C8 C15 C16 47.6(9) . . . . ?
C5 C15 C16 O2 109(2) . . . . ?
C5 C15 C16 C6AA 31.1(18) . . . . ?
C5 C15 C16 C5AA 100(2) . . . . ?
C5 C15 C16 O3 100.0(15) . . . . ?
C8 C5 C15 C5AA -45.1(11) . . . . ?
C8 C5 C15 C12 -4.8(10) . . . . ?
C8 C5 C15 C16 -116.8(11) . . . . ?
C8 C5 C16 O2 -44(2) . . . . ?
C8 C5 C16 C6AA -103.8(13) . . . . ?
C8 C5 C16 C5AA -2.8(10) . . . . ?
C8 C5 C16 O3 -50.4(15) . . . . ?
C8 C5 C16 C15 51.6(12) . . . . ?
C8 C5AA O3 Na07 168.1(12) . . . . ?
C8 C5AA O3 C6AA -28(2) . . . . ?
C8 C5AA O3 C11 92(3) . . . . ?
C8 C5AA O3 C16 -64.2(13) . . . . ?
C8 C5AA C11 O2 -105.5(6) . . . . ?
C8 C5AA C11 O3 -99.8(9) . . . . ?
C8 C5AA C11 C12 26(2) . . . . ?
C8 C5AA C12 C11 -73(5) . . . . ?
C8 C5AA C12 C15 82(4) . . . . ?
C8 C5AA C15 C5 44.3(10) . . . . ?
C8 C5AA C15 C12 -30.2(19) . . . . ?
C8 C5AA C15 C16 98.8(9) . . . . ?
C8 C11 C12 C5AA 114(5) . . . . ?
C8 C11 C12 C15 89(3) . . . . ?
C8 C12 C15 C5 8.9(18) . . . . ?
C8 C12 C15 C5AA 110(3) . . . . ?
C8 C12 C15 C16 60(2) . . . . ?
C8 C15 C16 O2 63.1(15) . . . . ?
C8 C15 C16 C6AA -15(2) . . . . ?
C8 C15 C16 C5 -46.0(12) . . . . ?
C8 C15 C16 C5AA 54.0(11) . . . . ?
C8 C15 C16 O3 54.1(11) . . . . ?
C5AA O2 C6AA C5 -12.3 . . . . ?
C5AA O2 C6AA O3 95(7) . . . . ?
C5AA O2 C6AA C16 -67.1(18) . . . . ?
C5AA O2 C11 C8 -55.0(15) . . . . ?
C5AA O2 C11 O3 -144(5) . . . . ?
C5AA O2 C11 C12 -33.1(19) . . . . ?
C5AA O2 C16 C6AA 119.6(13) . . . . ?
C5AA O2 C16 C5 62(2) . . . . ?
C5AA O2 C16 O3 101(8) . . . . ?
C5AA O2 C16 C15 -10.0(13) . . . . ?
C5AA C8 C11 O2 67(2) . . . . ?
C5AA C8 C11 O3 76(2) . . . . ?
C5AA C8 C11 C12 -50(4) . . . . ?
C5AA C8 C12 C11 28(3) . . . . ?
C5AA C8 C12 C15 -73(3) . . . . ?
C5AA C8 C15 C5 -120.0(9) . . . . ?
C5AA C8 C15 C12 49(2) . . . . ?
C5AA C8 C15 C16 -72.4(10) . . . . ?
C5AA O3 C11 O2 34(5) . . . . ?
C5AA O3 C11 C8 -56.9(18) . . . . ?
C5AA O3 C11 C12 -37(2) . . . . ?
C5AA O3 C16 O2 -71(8) . . . . ?
C5AA O3 C16 C6AA 128(3) . . . . ?
C5AA O3 C16 C5 71.6(16) . . . . ?
C5AA O3 C16 C15 0.0(14) . . . . ?
C5AA C11 C12 C8 -114(5) . . . . ?
C5AA C11 C12 C15 -25(3) . . . . ?
C5AA C12 C15 C5 -101.4(19) . . . . ?
C5AA C12 C15 C8 -110(3) . . . . ?
C5AA C12 C15 C16 -49.8(17) . . . . ?
C5AA C15 C16 O2 9.1(11) . . . . ?
C5AA C15 C16 C6AA -69(2) . . . . ?
C5AA C15 C16 C5 -100(2) . . . . ?
C5AA C15 C16 O3 0.0(13) . . . . ?
O3 C6AA C5 C8 21.6(17) . . . . ?
O3 C6AA C5 C15 -39.9(18) . . . . ?
O3 C6AA C5 C16 -60.0(17) . . . . ?
O3 C6AA C16 O2 -3.2(16) . . . . ?
O3 C6AA C16 C5 120.0(10) . . . . ?
O3 C6AA C16 C5AA 37.9(15) . . . . ?
O3 C6AA C16 C15 89.0(17) . . . . ?
O3 C5AA C11 O2 -5.7(10) . . . . ?
O3 C5AA C11 C8 99.8(9) . . . . ?
O3 C5AA C11 C12 126(2) . . . . ?
O3 C5AA C12 C8 -3(7) . . . . ?
O3 C5AA C12 C11 -76(4) . . . . ?
O3 C5AA C12 C15 79(3) . . . . ?
O3 C5AA C15 C5 -55(2) . . . . ?
O3 C5AA C15 C8 -98.9(14) . . . . ?
O3 C5AA C15 C12 -129(3) . . . . ?
O3 C5AA C15 C16 0.0(12) . . . . ?
O3 C11 C12 C8 -57(3) . . . . ?
O3 C11 C12 C5AA 56(3) . . . . ?
O3 C11 C12 C15 31.5 . . . . ?
C11 O2 C6AA C5 -45.3(17) . . . . ?
C11 O2 C6AA O3 62(7) . . . . ?
C11 O2 C6AA C16 -100(2) . . . . ?
C11 O2 C5AA C8 93(3) . . . . ?
C11 O2 C5AA O3 35(6) . . . . ?
C11 O2 C5AA C12 99(5) . . . . ?
C11 O2 C5AA C15 156(3) . . . . ?
C11 O2 C5AA C16 147(3) . . . . ?
C11 O2 C16 C6AA 102(2) . . . . ?
C11 O2 C16 C5 44(3) . . . . ?
C11 O2 C16 C5AA -18(2) . . . . ?
C11 O2 C16 O3 84(8) . . . . ?
C11 O2 C16 C15 -28(3) . . . . ?
C11 C8 C5AA O2 -78(3) . . . . ?
C11 C8 C5AA O3 -70(2) . . . . ?
C11 C8 C5AA C12 112(5) . . . . ?
C11 C8 C5AA C15 -163(3) . . . . ?
C11 C8 C5AA C16 -113(3) . . . . ?
C11 C8 C12 C5AA -28(3) . . . . ?
C11 C8 C12 C15 -101.1(5) . . . . ?
C11 C8 C15 C5 -112.8(12) . . . . ?
C11 C8 C15 C5AA 7.2(15) . . . . ?
C11 C8 C15 C12 56.4(17) . . . . ?
C11 C8 C15 C16 -65.2(10) . . . . ?
C11 C5AA O3 Na07 76(3) . . . . ?
C11 C5AA O3 C6AA -120(2) . . . . ?
C11 C5AA O3 C16 -157(2) . . . . ?
C11 C5AA C12 C8 73(5) . . . . ?
C11 C5AA C12 C15 155(3) . . . . ?
C11 C5AA C15 C5 3(8) . . . . ?
C11 C5AA C15 C8 -41(8) . . . . ?
C11 C5AA C15 C12 -71(8) . . . . ?
C11 C5AA C15 C16 58(8) . . . . ?
C11 O3 C16 O2 -83(8) . . . . ?
C11 O3 C16 C6AA 116.1(19) . . . . ?
C11 O3 C16 C5 59.2(13) . . . . ?
C11 O3 C16 C5AA -12.3(14) . . . . ?
C11 O3 C16 C15 -12.4 . . . . ?
C11 C12 C15 C5 -88.9(9) . . . . ?
C11 C12 C15 C8 -98(2) . . . . ?
C11 C12 C15 C5AA 12.4(17) . . . . ?
C11 C12 C15 C16 -37.4 . . . . ?
C12 C8 C5AA O2 170(5) . . . . ?
C12 C8 C5AA O3 178(5) . . . . ?
C12 C8 C5AA C11 -112(5) . . . . ?
C12 C8 C5AA C15 85(4) . . . . ?
C12 C8 C5AA C16 135(5) . . . . ?
C12 C8 C11 O2 116(3) . . . . ?
C12 C8 C11 C5AA 50(4) . . . . ?
C12 C8 C11 O3 126(3) . . . . ?
C12 C8 C15 C5 -169(2) . . . . ?
C12 C8 C15 C5AA -49(2) . . . . ?
C12 C8 C15 C16 -122(2) . . . . ?
C12 C5AA O3 Na07 170(3) . . . . ?
C12 C5AA O3 C6AA -26(5) . . . . ?
C12 C5AA O3 C11 94(5) . . . . ?
C12 C5AA O3 C16 -63(4) . . . . ?
C12 C5AA C11 O2 -131.4(19) . . . . ?
C12 C5AA C11 C8 -26(2) . . . . ?
C12 C5AA C11 O3 -126(2) . . . . ?
C12 C5AA C15 C5 74.5(19) . . . . ?
C12 C5AA C15 C8 30.2(19) . . . . ?
C12 C5AA C15 C16 129.1(16) . . . . ?
C12 C15 C16 O2 40.6(15) . . . . ?
C12 C15 C16 C6AA -37(2) . . . . ?
C12 C15 C16 C5 -68.5(16) . . . . ?
C12 C15 C16 C5AA 31.5(13) . . . . ?
C12 C15 C16 O3 31.6 . . . . ?
C15 C5 C8 C5AA 51.1(11) . . . . ?
C15 C5 C8 C11 76.6(17) . . . . ?
C15 C5 C8 C12 13(3) . . . . ?
C15 C5 C16 O2 -95.9(18) . . . . ?
C15 C5 C16 C6AA -155.4(14) . . . . ?
C15 C5 C16 C5AA -54.4(12) . . . . ?
C15 C5 C16 O3 -102.0(7) . . . . ?
C15 C8 C5AA O2 84.8(14) . . . . ?
C15 C8 C5AA O3 92.9(18) . . . . ?
C15 C8 C5AA C11 163(3) . . . . ?
C15 C8 C5AA C12 -85(4) . . . . ?
C15 C8 C5AA C16 50.3(9) . . . . ?
C15 C8 C11 O2 52(2) . . . . ?
C15 C8 C11 C5AA -15(3) . . . . ?
C15 C8 C11 O3 61.5(11) . . . . ?
C15 C8 C11 C12 -65(3) . . . . ?
C15 C8 C12 C5AA 73(3) . . . . ?
C15 C8 C12 C11 101.1(4) . . . . ?
C15 C5AA O3 Na07 -127.7(10) . . . . ?
C15 C5AA O3 C6AA 36(3) . . . . ?
C15 C5AA O3 C11 157(3) . . . . ?
C15 C5AA O3 C16 0.0(13) . . . . ?
C15 C5AA C11 O2 -69(7) . . . . ?
C15 C5AA C11 C8 36(7) . . . . ?
C15 C5AA C11 O3 -64(7) . . . . ?
C15 C5AA C11 C12 62(7) . . . . ?
C15 C5AA C12 C8 -82(4) . . . . ?
C15 C5AA C12 C11 -155(3) . . . . ?
C16 O2 C6AA C5 54.8(18) . . . . ?
C16 O2 C6AA O3 162(8) . . . . ?
C16 O2 C5AA C8 -54.0(15) . . . . ?
C16 O2 C5AA O3 -112(7) . . . . ?
C16 O2 C5AA C11 -147(3) . . . . ?
C16 O2 C5AA C12 -47(3) . . . . ?
C16 O2 C5AA C15 9.0(12) . . . . ?
C16 O2 C11 C8 -18(3) . . . . ?
C16 O2 C11 C5AA 37(4) . . . . ?
C16 O2 C11 O3 -108(6) . . . . ?
C16 O2 C11 C12 4(3) . . . . ?
C16 C6AA C5 C8 81.6(17) . . . . ?
C16 C6AA C5 C15 20.1(12) . . . . ?
C16 C6AA O3 Na07 109.1(13) . . . . ?
C16 C6AA O3 C5AA -55(3) . . . . ?
C16 C6AA O3 C11 -86(2) . . . . ?
C16 C5 C8 C5AA 3.6(13) . . . . ?
C16 C5 C8 C11 29.1(19) . . . . ?
C16 C5 C8 C12 -34(3) . . . . ?
C16 C5 C8 C15 -47.5(12) . . . . ?
C16 C5 C15 C8 116.8(11) . . . . ?
C16 C5 C15 C5AA 71.7(16) . . . . ?
C16 C5 C15 C12 112.0(9) . . . . ?
C16 C5AA O3 Na07 -127.7(13) . . . . ?
C16 C5AA O3 C6AA 36(2) . . . . ?
C16 C5AA O3 C11 157(2) . . . . ?
C16 C5AA C11 O2 -24(2) . . . . ?
C16 C5AA C11 C8 81.1(17) . . . . ?
C16 C5AA C11 O3 -18.6(17) . . . . ?
C16 C5AA C11 C12 107(3) . . . . ?
C16 C5AA C12 C8 -45(5) . . . . ?
C16 C5AA C12 C11 -118(4) . . . . ?
C16 C5AA C12 C15 37.0(11) . . . . ?
C16 C5AA C15 C5 -54.6(12) . . . . ?
C16 C5AA C15 C8 -98.8(9) . . . . ?
C16 C5AA C15 C12 -129.1(16) . . . . ?
C16 O3 C11 O2 59(5) . . . . ?
C16 O3 C11 C8 -32.3(14) . . . . ?
C16 O3 C11 C5AA 25(2) . . . . ?
C16 O3 C11 C12 -12.3 . . . . ?
O1 C4 C10 O00L -51(9) . . . . ?
O1 C4 C10 C19 -12(36) . . . . ?
C7AA O00L C3 C01H 14(2) . . . . ?
C7AA O00L C19 C14 -44(2) . . . . ?
C7AA O00L C19 C10 -178(6) . . . . ?
C7AA O00L C10 C19 2(5) . . . . ?
C7AA O00L C10 C4 169(6) . . . . ?
C7AA C01H C3 O00L -22(3) . . . . ?
C7AA C01H C14 C19 51.7(18) . . . . ?
C7AA C14 C19 O00L 67(2) . . . . ?
C7AA C14 C19 C10 167(9) . . . . ?
C10 O00L C3 C01H -53(5) . . . . ?
C10 O00L C19 C14 134(6) . . . . ?
C10 O00L C19 C7AA 178(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_rs2097
_database_code_depnum_ccdc_archive 'CCDC 1495143'
_audit_update_record             
;
2016-07-21 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_audit_creation_date             2015-12-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
1-([1,3,4]azadiphospholo[1,2-a]pyridin-3-yloxy)-N,N,N',N'-tetraisopropylphosphanediamine
_chemical_formula_moiety         'C18 H32 N3 O P3'
_chemical_formula_sum            'C18 H32 N3 O P3'
_chemical_formula_weight         399.37
_chemical_melting_point          421
_chemical_oxdiff_formula         'P3 N3 C40 H40'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   12.9301(4)
_cell_length_b                   11.3677(4)
_cell_length_c                   29.4791(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4333.0(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4703
_cell_measurement_temperature    104.79(12)
_cell_measurement_theta_max      30.3350
_cell_measurement_theta_min      3.1920
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14270
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.575
_diffrn_reflns_theta_min         3.151
_diffrn_ambient_temperature      104.79(12)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -12.00   14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega  -50.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592    0.0000 -150.0000 130
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_UB_11      -0.0186792000
_diffrn_orient_matrix_UB_12      0.0139377000
_diffrn_orient_matrix_UB_13      0.0219861000
_diffrn_orient_matrix_UB_21      -0.0460403000
_diffrn_orient_matrix_UB_22      -0.0317983000
_diffrn_orient_matrix_UB_23      -0.0045252000
_diffrn_orient_matrix_UB_31      0.0232015000
_diffrn_orient_matrix_UB_32      -0.0518369000
_diffrn_orient_matrix_UB_33      0.0087030000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5195
_reflns_number_total             5923
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         5923
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0396
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0310P)²+2.0790P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0881
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C14(H14), C7(H7), C8(H8), C13(H13)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C11(H11A,H11B,
 H11C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C), C12(H12A,
 H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P3 P 0.51505(3) 0.50390(3) 0.65960(2) 0.01200(8) Uani 1 1 d . . . . .
P1 P 0.54797(3) 0.75445(3) 0.60503(2) 0.01906(9) Uani 1 1 d . . . . .
P2 P 0.48461(3) 0.88274(3) 0.56039(2) 0.02053(9) Uani 1 1 d . . . . .
O004 O 0.42416(7) 0.55972(8) 0.62246(3) 0.0150(2) Uani 1 1 d . . . . .
N1 N 0.35964(9) 0.69679(9) 0.57415(4) 0.0128(2) Uani 1 1 d . . . . .
N2 N 0.43503(9) 0.41437(10) 0.68744(4) 0.0132(2) Uani 1 1 d . . . . .
N3 N 0.58340(9) 0.42665(10) 0.62153(4) 0.0137(2) Uani 1 1 d . . . . .
C1 C 0.44124(11) 0.66310(11) 0.60123(5) 0.0136(3) Uani 1 1 d . . . . .
C6 C 0.27044(11) 0.62938(12) 0.56931(5) 0.0154(3) Uani 1 1 d . . . . .
H6 H 0.2646 0.5583 0.5847 0.019 Uiso 1 1 calc R . . . .
C2 C 0.37061(11) 0.80515(11) 0.55154(5) 0.0156(3) Uani 1 1 d . . . . .
C14 C 0.69478(11) 0.40846(13) 0.63213(5) 0.0163(3) Uani 1 1 d . . . . .
H14 H 0.7226 0.3571 0.6084 0.020 Uiso 1 1 calc R . . . .
C7 C 0.41260(11) 0.44277(12) 0.73571(5) 0.0161(3) Uani 1 1 d . . . . .
H7 H 0.3602 0.3866 0.7460 0.019 Uiso 1 1 calc R . . . .
C8 C 0.36985(11) 0.32317(12) 0.66624(5) 0.0162(3) Uani 1 1 d . . . . .
H8 H 0.3885 0.3201 0.6340 0.019 Uiso 1 1 calc R . . . .
C5 C 0.19247(12) 0.66605(13) 0.54246(5) 0.0198(3) Uani 1 1 d . . . . .
H5 H 0.1332 0.6204 0.5396 0.024 Uiso 1 1 calc R . . . .
C4 C 0.20050(12) 0.77469(13) 0.51845(5) 0.0218(3) Uani 1 1 d . . . . .
H4 H 0.1470 0.8000 0.4998 0.026 Uiso 1 1 calc R . . . .
C18 C 0.59939(13) 0.43207(13) 0.53769(5) 0.0227(3) Uani 1 1 d . . . . .
H18A H 0.5902 0.5158 0.5391 0.034 Uiso 1 1 calc GR . . . .
H18B H 0.5693 0.4025 0.5102 0.034 Uiso 1 1 calc GR . . . .
H18C H 0.6719 0.4139 0.5382 0.034 Uiso 1 1 calc GR . . . .
C13 C 0.54650(11) 0.37471(12) 0.57841(5) 0.0150(3) Uani 1 1 d . . . . .
H13 H 0.4724 0.3915 0.5760 0.018 Uiso 1 1 calc R . . . .
C3 C 0.28733(12) 0.84043(12) 0.52327(5) 0.0199(3) Uani 1 1 d . . . . .
H3 H 0.2925 0.9111 0.5075 0.024 Uiso 1 1 calc R . . . .
C17 C 0.55940(12) 0.24095(13) 0.57695(5) 0.0207(3) Uani 1 1 d . . . . .
H17A H 0.6312 0.2213 0.5803 0.031 Uiso 1 1 calc GR . . . .
H17B H 0.5345 0.2116 0.5484 0.031 Uiso 1 1 calc GR . . . .
H17C H 0.5206 0.2060 0.6012 0.031 Uiso 1 1 calc GR . . . .
C16 C 0.71050(12) 0.34453(14) 0.67710(5) 0.0219(3) Uani 1 1 d . . . . .
H16A H 0.6909 0.3953 0.7017 0.033 Uiso 1 1 calc GR . . . .
H16B H 0.7820 0.3231 0.6803 0.033 Uiso 1 1 calc GR . . . .
H16C H 0.6685 0.2749 0.6777 0.033 Uiso 1 1 calc GR . . . .
C11 C 0.25427(12) 0.35164(15) 0.66870(5) 0.0238(3) Uani 1 1 d . . . . .
H11A H 0.2329 0.3547 0.6999 0.036 Uiso 1 1 calc GR . . . .
H11B H 0.2158 0.2917 0.6532 0.036 Uiso 1 1 calc GR . . . .
H11C H 0.2416 0.4264 0.6546 0.036 Uiso 1 1 calc GR . . . .
C10 C 0.50710(13) 0.42542(14) 0.76581(5) 0.0229(3) Uani 1 1 d . . . . .
H10A H 0.5339 0.3474 0.7616 0.034 Uiso 1 1 calc GR . . . .
H10B H 0.4878 0.4360 0.7970 0.034 Uiso 1 1 calc GR . . . .
H10C H 0.5592 0.4819 0.7578 0.034 Uiso 1 1 calc GR . . . .
C15 C 0.75635(12) 0.52261(15) 0.63012(7) 0.0291(4) Uani 1 1 d . . . . .
H15A H 0.7477 0.5583 0.6008 0.044 Uiso 1 1 calc GR . . . .
H15B H 0.8283 0.5061 0.6351 0.044 Uiso 1 1 calc GR . . . .
H15C H 0.7319 0.5754 0.6532 0.044 Uiso 1 1 calc GR . . . .
C9 C 0.36633(14) 0.56534(14) 0.74140(6) 0.0266(3) Uani 1 1 d . . . . .
H9A H 0.4165 0.6234 0.7328 0.040 Uiso 1 1 calc GR . . . .
H9B H 0.3471 0.5771 0.7725 0.040 Uiso 1 1 calc GR . . . .
H9C H 0.3062 0.5727 0.7225 0.040 Uiso 1 1 calc GR . . . .
C12 C 0.39322(14) 0.20210(13) 0.68627(6) 0.0255(3) Uani 1 1 d . . . . .
H12A H 0.4658 0.1859 0.6835 0.038 Uiso 1 1 calc GR . . . .
H12B H 0.3546 0.1433 0.6702 0.038 Uiso 1 1 calc GR . . . .
H12C H 0.3739 0.2010 0.7177 0.038 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P3 O004 1.7269(10) . ?
P3 N2 1.6673(12) . ?
P3 N3 1.6767(12) . ?
P1 P2 2.1283(5) . ?
P1 C1 1.7307(14) . ?
P2 C2 1.7375(15) . ?
O004 C1 1.3496(16) . ?
N1 C1 1.3775(17) . ?
N1 C6 1.3921(17) . ?
N1 C2 1.4077(17) . ?
N2 C7 1.4877(18) . ?
N2 C8 1.4751(18) . ?
N3 C14 1.4881(17) . ?
N3 C13 1.4805(18) . ?
C6 H6 0.9300 . ?
C6 C5 1.348(2) . ?
C2 C3 1.419(2) . ?
C14 H14 0.9800 . ?
C14 C16 1.525(2) . ?
C14 C15 1.524(2) . ?
C7 H7 0.9800 . ?
C7 C10 1.523(2) . ?
C7 C9 1.526(2) . ?
C8 H8 0.9800 . ?
C8 C11 1.531(2) . ?
C8 C12 1.528(2) . ?
C5 H5 0.9300 . ?
C5 C4 1.427(2) . ?
C4 H4 0.9300 . ?
C4 C3 1.356(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 C13 1.528(2) . ?
C13 H13 0.9800 . ?
C13 C17 1.5302(19) . ?
C3 H3 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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
N2 P3 O004 96.55(5) . . ?
N2 P3 N3 109.69(6) . . ?
N3 P3 O004 97.29(5) . . ?
C1 P1 P2 93.68(5) . . ?
C2 P2 P1 94.11(5) . . ?
C1 O004 P3 120.17(9) . . ?
C1 N1 C6 122.75(11) . . ?
C1 N1 C2 116.14(11) . . ?
C6 N1 C2 121.10(12) . . ?
C7 N2 P3 117.35(9) . . ?
C8 N2 P3 125.10(9) . . ?
C8 N2 C7 116.51(11) . . ?
C14 N3 P3 116.25(9) . . ?
C13 N3 P3 127.85(9) . . ?
C13 N3 C14 115.90(11) . . ?
O004 C1 P1 128.53(10) . . ?
O004 C1 N1 112.68(11) . . ?
N1 C1 P1 118.78(10) . . ?
N1 C6 H6 119.7 . . ?
C5 C6 N1 120.64(13) . . ?
C5 C6 H6 119.7 . . ?
N1 C2 P2 117.29(10) . . ?
N1 C2 C3 116.67(13) . . ?
C3 C2 P2 126.04(11) . . ?
N3 C14 H14 106.7 . . ?
N3 C14 C16 112.19(12) . . ?
N3 C14 C15 112.28(12) . . ?
C16 C14 H14 106.7 . . ?
C15 C14 H14 106.7 . . ?
C15 C14 C16 111.72(13) . . ?
N2 C7 H7 106.9 . . ?
N2 C7 C10 111.89(12) . . ?
N2 C7 C9 112.32(12) . . ?
C10 C7 H7 106.9 . . ?
C10 C7 C9 111.64(13) . . ?
C9 C7 H7 106.9 . . ?
N2 C8 H8 107.1 . . ?
N2 C8 C11 112.90(12) . . ?
N2 C8 C12 110.87(12) . . ?
C11 C8 H8 107.1 . . ?
C12 C8 H8 107.1 . . ?
C12 C8 C11 111.43(13) . . ?
C6 C5 H5 119.9 . . ?
C6 C5 C4 120.29(14) . . ?
C4 C5 H5 119.9 . . ?
C5 C4 H4 120.5 . . ?
C3 C4 C5 119.02(14) . . ?
C3 C4 H4 120.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
N3 C13 C18 111.11(12) . . ?
N3 C13 H13 107.4 . . ?
N3 C13 C17 112.67(12) . . ?
C18 C13 H13 107.4 . . ?
C18 C13 C17 110.68(12) . . ?
C17 C13 H13 107.4 . . ?
C2 C3 H3 118.9 . . ?
C4 C3 C2 122.27(13) . . ?
C4 C3 H3 118.9 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P3 O004 C1 P1 0.88(17) . . . . ?
P3 O004 C1 N1 -177.80(9) . . . . ?
P3 N2 C7 C10 -68.41(14) . . . . ?
P3 N2 C7 C9 58.07(15) . . . . ?
P3 N2 C8 C11 -111.51(13) . . . . ?
P3 N2 C8 C12 122.66(12) . . . . ?
P3 N3 C14 C16 58.90(14) . . . . ?
P3 N3 C14 C15 -67.90(15) . . . . ?
P3 N3 C13 C18 115.52(12) . . . . ?
P3 N3 C13 C17 -119.63(12) . . . . ?
P1 P2 C2 N1 0.09(10) . . . . ?
P1 P2 C2 C3 -179.44(12) . . . . ?
P2 P1 C1 O004 -178.47(12) . . . . ?
P2 P1 C1 N1 0.15(11) . . . . ?
P2 C2 C3 C4 -179.61(12) . . . . ?
O004 P3 N2 C7 -112.77(10) . . . . ?
O004 P3 N2 C8 55.13(12) . . . . ?
O004 P3 N3 C14 152.16(10) . . . . ?
O004 P3 N3 C13 -27.49(12) . . . . ?
N1 C6 C5 C4 0.2(2) . . . . ?
N1 C2 C3 C4 0.9(2) . . . . ?
N2 P3 O004 C1 159.41(10) . . . . ?
N2 P3 N3 C14 -108.17(10) . . . . ?
N2 P3 N3 C13 72.18(13) . . . . ?
N3 P3 O004 C1 -89.70(10) . . . . ?
N3 P3 N2 C7 147.05(10) . . . . ?
N3 P3 N2 C8 -45.05(13) . . . . ?
C1 N1 C6 C5 179.89(13) . . . . ?
C1 N1 C2 P2 -0.01(16) . . . . ?
C1 N1 C2 C3 179.57(12) . . . . ?
C6 N1 C1 P1 -179.53(10) . . . . ?
C6 N1 C1 O004 -0.71(18) . . . . ?
C6 N1 C2 P2 179.42(10) . . . . ?
C6 N1 C2 C3 -1.00(19) . . . . ?
C6 C5 C4 C3 -0.3(2) . . . . ?
C2 N1 C1 P1 -0.11(16) . . . . ?
C2 N1 C1 O004 178.71(11) . . . . ?
C2 N1 C6 C5 0.5(2) . . . . ?
C14 N3 C13 C18 -64.13(15) . . . . ?
C14 N3 C13 C17 60.72(15) . . . . ?
C7 N2 C8 C11 56.48(16) . . . . ?
C7 N2 C8 C12 -69.36(15) . . . . ?
C8 N2 C7 C10 122.64(13) . . . . ?
C8 N2 C7 C9 -110.87(14) . . . . ?
C5 C4 C3 C2 -0.2(2) . . . . ?
C13 N3 C14 C16 -121.40(13) . . . . ?
C13 N3 C14 C15 111.80(14) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_pmmm
_database_code_depnum_ccdc_archive 'CCDC 1494719'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_pmmm                
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          12 Note
RESPONSE: the mask of the beam-stopper is increased
;
# Added during the CSD deposition process: Tuesday 19 July 2016 09:44 AM
# end Validation Reply Form

_audit_creation_date             2016-06-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H17 Mo N3 O6 P6 Si, 3(C4 H8 O)'
_chemical_formula_sum            'C39 H41 Mo N3 O9 P6 Si'
_chemical_formula_weight         1005.60
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mo1 Si1 P6 N3 C40 H60 O9'
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'
Mo Mo -1.6832 0.6857 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   28.4804(10)
_cell_length_b                   18.1858(6)
_cell_length_c                   16.8840(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8744.9(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5430
_cell_measurement_temperature    106.48(14)
_cell_measurement_theta_max      23.7860
_cell_measurement_theta_min      2.9200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1278
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47716
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.108
_diffrn_reflns_theta_max         24.108
_diffrn_reflns_theta_min         2.805
_diffrn_ambient_temperature      106.48(14)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -70.00   12.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303   19.0000 -120.0000 82

#__ type_ start__ end____ width___ exp.time_
  2 omega  -42.00   45.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990  -57.0000 -120.0000 87

#__ type_ start__ end____ width___ exp.time_
  3 omega   46.00   96.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990 -144.0000 -122.0000 50

#__ type_ start__ end____ width___ exp.time_
  4 omega   -3.00   62.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990   77.0000   60.0000 65

#__ type_ start__ end____ width___ exp.time_
  5 omega    1.00   99.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990   38.0000 -120.0000 98
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_UB_11      0.0247434000
_diffrn_orient_matrix_UB_12      0.0043938000
_diffrn_orient_matrix_UB_13      -0.0010697000
_diffrn_orient_matrix_UB_21      -0.0027622000
_diffrn_orient_matrix_UB_22      0.0386780000
_diffrn_orient_matrix_UB_23      0.0026820000
_diffrn_orient_matrix_UB_31      0.0008114000
_diffrn_orient_matrix_UB_32      -0.0023517000
_diffrn_orient_matrix_UB_33      0.0419075000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5726
_reflns_number_total             6938
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.335
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         6938
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_gt           0.0972
_refine_ls_restrained_S_all      1.335
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0188P)²+61.7095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1639
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C30(H30A,H30B), C28(H28A,H28B), C33(H33A,
 H33B), C39(H39A,H39B), C36(H36A,H36B), C29(H29A,H29B), C38(H38A,H38B),
 C35(H35A,H35B), C34(H34A,H34B), C37(H37A,H37B)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C3(H3), C24(H24), C6(H6), C4(H4), C20(H20), C9(H9), C12(H12),
 C5(H5), C15(H15), C18(H18), C21(H21), C10(H10), C16(H16), C22(H22), C17(H17),
 C11(H11)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.16885(3) 0.41824(4) 0.73505(4) 0.01525(19) Uani 1 1 d . . . . .
P1 P 0.22327(8) 0.50695(12) 0.79899(13) 0.0172(5) Uani 1 1 d . . . . .
P3 P 0.23451(8) 0.33829(12) 0.69584(12) 0.0162(5) Uani 1 1 d . . . . .
P2 P 0.21302(8) 0.56714(13) 0.90391(13) 0.0205(5) Uani 1 1 d . . . . .
P4 P 0.24928(8) 0.22746(12) 0.72094(12) 0.0190(5) Uani 1 1 d . . . . .
Si1 Si 0.30199(8) 0.50621(13) 0.62756(13) 0.0135(5) Uani 1 1 d . . . . .
P5 P 0.17100(8) 0.47720(12) 0.60425(12) 0.0178(5) Uani 1 1 d . . . . .
P6 P 0.12210(8) 0.49520(14) 0.51367(13) 0.0230(6) Uani 1 1 d . . . . .
O3 O 0.25468(19) 0.5520(3) 0.6029(3) 0.0163(13) Uani 1 1 d . . . . .
O2 O 0.29772(19) 0.4185(3) 0.6054(3) 0.0164(13) Uani 1 1 d . . . . .
O1 O 0.30905(19) 0.5157(3) 0.7231(3) 0.0203(14) Uani 1 1 d . . . . .
N00C N 0.3157(2) 0.2983(4) 0.6342(4) 0.0133(15) Uani 1 1 d . . . . .
O6 O 0.1630(2) 0.3446(4) 0.9025(4) 0.0329(16) Uani 1 1 d . . . . .
O5 O 0.0851(2) 0.5231(4) 0.7774(4) 0.0360(17) Uani 1 1 d . . . . .
N00F N 0.2025(2) 0.5743(4) 0.5011(4) 0.0173(16) Uani 1 1 d . . . . .
N00G N 0.2987(2) 0.5857(4) 0.8361(4) 0.0166(16) Uani 1 1 d . . . . .
O4 O 0.0949(2) 0.3017(4) 0.6808(4) 0.0426(19) Uani 1 1 d . . . . .
O8 O 0.4123(2) 0.3560(4) 0.4347(4) 0.0346(17) Uani 1 1 d . . . . .
C13 C 0.2135(3) 0.5348(5) 0.5686(5) 0.0161(19) Uani 1 1 d . . . . .
O7 O 0.4744(3) 0.7159(4) 0.9290(4) 0.0417(19) Uani 1 1 d . . . . .
C26 C 0.1161(3) 0.4849(5) 0.7626(5) 0.021(2) Uani 1 1 d . . . . .
C1 C 0.2794(3) 0.5358(5) 0.7827(4) 0.0157(19) Uani 1 1 d . . . . .
C25 C 0.1227(3) 0.3438(5) 0.6980(5) 0.027(2) Uani 1 1 d . . . . .
C7 C 0.2846(3) 0.3560(4) 0.6444(4) 0.0134(18) Uani 1 1 d . . . . .
O9 O 0.0496(3) 0.5681(5) 0.2913(4) 0.054(2) Uani 1 1 d . . . . .
C23 C 0.4154(3) 0.5476(5) 0.4825(5) 0.023(2) Uani 1 1 d . . . . .
H23 H 0.4322 0.5235 0.4431 0.028 Uiso 1 1 calc R . . . .
C27 C 0.1657(3) 0.3714(5) 0.8414(5) 0.023(2) Uani 1 1 d . . . . .
C3 C 0.2871(3) 0.6559(5) 0.9540(5) 0.020(2) Uani 1 1 d . . . . .
H3 H 0.2686 0.6694 0.9969 0.024 Uiso 1 1 calc R . . . .
C8 C 0.3030(3) 0.2323(4) 0.6710(5) 0.0163(19) Uani 1 1 d . . . . .
C2 C 0.2694(3) 0.6047(5) 0.8988(4) 0.017(2) Uani 1 1 d . . . . .
C19 C 0.3532(3) 0.5476(5) 0.5779(5) 0.0141(19) Uani 1 1 d . . . . .
C24 C 0.3796(3) 0.5114(5) 0.5202(5) 0.023(2) Uani 1 1 d . . . . .
H24 H 0.3730 0.4628 0.5073 0.027 Uiso 1 1 calc R . . . .
C6 C 0.3432(3) 0.6156(5) 0.8274(5) 0.019(2) Uani 1 1 d . . . . .
H6 H 0.3624 0.6012 0.7857 0.023 Uiso 1 1 calc R . . . .
C4 C 0.3307(3) 0.6862(5) 0.9461(5) 0.025(2) Uani 1 1 d . . . . .
H4 H 0.3419 0.7196 0.9833 0.030 Uiso 1 1 calc R . . . .
C20 C 0.3653(3) 0.6197(5) 0.5973(5) 0.021(2) Uani 1 1 d . . . . .
H20 H 0.3484 0.6443 0.6364 0.026 Uiso 1 1 calc R . . . .
C9 C 0.3350(3) 0.1738(4) 0.6654(5) 0.020(2) Uani 1 1 d . . . . .
H9 H 0.3280 0.1299 0.6911 0.024 Uiso 1 1 calc R . . . .
C14 C 0.1585(3) 0.5585(5) 0.4667(5) 0.020(2) Uani 1 1 d . . . . .
C12 C 0.3571(3) 0.3031(5) 0.5906(5) 0.021(2) Uani 1 1 d . . . . .
H12 H 0.3647 0.3467 0.5650 0.025 Uiso 1 1 calc R . . . .
C5 C 0.3583(3) 0.6661(5) 0.8808(5) 0.026(2) Uani 1 1 d . . . . .
H5 H 0.3876 0.6878 0.8739 0.031 Uiso 1 1 calc R . . . .
C15 C 0.1476(3) 0.5968(5) 0.3959(5) 0.026(2) Uani 1 1 d . . . . .
H15 H 0.1196 0.5867 0.3698 0.031 Uiso 1 1 calc R . . . .
C18 C 0.2320(3) 0.6277(5) 0.4693(5) 0.019(2) Uani 1 1 d . . . . .
H18 H 0.2603 0.6382 0.4941 0.023 Uiso 1 1 calc R . . . .
C21 C 0.4016(3) 0.6546(5) 0.5597(5) 0.024(2) Uani 1 1 d . . . . .
H21 H 0.4092 0.7027 0.5731 0.029 Uiso 1 1 calc R . . . .
C10 C 0.3755(3) 0.1785(5) 0.6242(5) 0.023(2) Uani 1 1 d . . . . .
H10 H 0.3960 0.1387 0.6215 0.028 Uiso 1 1 calc R . . . .
C16 C 0.1770(3) 0.6472(5) 0.3658(5) 0.028(2) Uani 1 1 d . . . . .
H16 H 0.1689 0.6715 0.3194 0.034 Uiso 1 1 calc R . . . .
C22 C 0.4269(3) 0.6182(5) 0.5016(5) 0.025(2) Uani 1 1 d . . . . .
H22 H 0.4516 0.6417 0.4758 0.030 Uiso 1 1 calc R . . . .
C17 C 0.2201(3) 0.6641(5) 0.4035(5) 0.026(2) Uani 1 1 d . . . . .
H17 H 0.2398 0.7001 0.3829 0.031 Uiso 1 1 calc R . . . .
C11 C 0.3862(3) 0.2447(5) 0.5855(5) 0.027(2) Uani 1 1 d . . . . .
H11 H 0.4137 0.2484 0.5560 0.033 Uiso 1 1 calc R . . . .
C31 C 0.3898(3) 0.3122(6) 0.3766(6) 0.034(2) Uani 1 1 d . . . . .
H31A H 0.3746 0.3430 0.3374 0.041 Uiso 1 1 calc R . . . .
H31B H 0.3663 0.2809 0.4009 0.041 Uiso 1 1 calc R . . . .
C32 C 0.0039(3) 0.6000(6) 0.2840(5) 0.036(3) Uani 1 1 d . . . . .
H32A H 0.0013 0.6432 0.3174 0.043 Uiso 1 1 calc R . . . .
H32B H -0.0200 0.5649 0.2996 0.043 Uiso 1 1 calc R . . . .
C30 C 0.4275(3) 0.2665(6) 0.3387(6) 0.040(3) Uani 1 1 d . . . . .
H30A H 0.4198 0.2550 0.2841 0.048 Uiso 1 1 calc R . . . .
H30B H 0.4326 0.2212 0.3676 0.048 Uiso 1 1 calc R . . . .
C28 C 0.4614(3) 0.3510(6) 0.4236(6) 0.034(3) Uani 1 1 d . . . . .
H28A H 0.4753 0.3210 0.4650 0.041 Uiso 1 1 calc R . . . .
H28B H 0.4755 0.3995 0.4257 0.041 Uiso 1 1 calc R . . . .
C33 C -0.0016(4) 0.6203(6) 0.1990(6) 0.044(3) Uani 1 1 d . . . . .
H33A H -0.0342 0.6173 0.1828 0.053 Uiso 1 1 calc R . . . .
H33B H 0.0098 0.6697 0.1892 0.053 Uiso 1 1 calc R . . . .
C39 C 0.4711(4) 0.6731(5) 0.9990(5) 0.031(2) Uani 1 1 d . . . . .
H39A H 0.4391 0.6566 1.0070 0.038 Uiso 1 1 calc R . . . .
H39B H 0.4806 0.7019 1.0447 0.038 Uiso 1 1 calc R . . . .
C36 C 0.4907(4) 0.6694(6) 0.8665(6) 0.042(3) Uani 1 1 d . . . . .
H36A H 0.5204 0.6876 0.8460 0.050 Uiso 1 1 calc R . . . .
H36B H 0.4681 0.6686 0.8235 0.050 Uiso 1 1 calc R . . . .
C29 C 0.4697(4) 0.3165(6) 0.3438(6) 0.038(3) Uani 1 1 d . . . . .
H29A H 0.4989 0.2890 0.3425 0.045 Uiso 1 1 calc R . . . .
H29B H 0.4698 0.3529 0.3018 0.045 Uiso 1 1 calc R . . . .
C38 C 0.5036(4) 0.6079(6) 0.9879(6) 0.038(3) Uani 1 1 d . . . . .
H38A H 0.5359 0.6204 1.0002 0.046 Uiso 1 1 calc R . . . .
H38B H 0.4940 0.5662 1.0199 0.046 Uiso 1 1 calc R . . . .
C35 C 0.0636(5) 0.5427(9) 0.2162(7) 0.078(5) Uani 1 1 d . . . . .
H35A H 0.0667 0.4896 0.2170 0.094 Uiso 1 1 calc R . . . .
H35B H 0.0938 0.5636 0.2023 0.094 Uiso 1 1 calc R . . . .
C34 C 0.0275(4) 0.5649(9) 0.1565(6) 0.072(5) Uani 1 1 d . . . . .
H34A H 0.0421 0.5862 0.1100 0.086 Uiso 1 1 calc R . . . .
H34B H 0.0086 0.5231 0.1404 0.086 Uiso 1 1 calc R . . . .
C37 C 0.4970(4) 0.5931(6) 0.9003(6) 0.047(3) Uani 1 1 d . . . . .
H37A H 0.5243 0.5690 0.8778 0.057 Uiso 1 1 calc R . . . .
H37B H 0.4694 0.5630 0.8909 0.057 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 P1 2.484(2) . ?
Mo1 P3 2.460(2) . ?
Mo1 P5 2.456(2) . ?
Mo1 C26 1.984(9) . ?
Mo1 C25 1.988(9) . ?
Mo1 C27 1.990(9) . ?
P1 P2 2.103(3) . ?
P1 C1 1.705(9) . ?
P3 P4 2.102(3) . ?
P3 C7 1.700(8) . ?
P2 C2 1.748(9) . ?
P4 C8 1.749(9) . ?
Si1 O3 1.638(6) . ?
Si1 O2 1.643(6) . ?
Si1 O1 1.635(6) . ?
Si1 C19 1.844(9) . ?
P5 P6 2.094(3) . ?
P5 C13 1.710(9) . ?
P6 C14 1.741(9) . ?
O3 C13 1.345(9) . ?
O2 C7 1.366(9) . ?
O1 C1 1.364(9) . ?
N00C C7 1.384(10) . ?
N00C C8 1.400(10) . ?
N00C C12 1.392(10) . ?
O6 C27 1.143(10) . ?
O5 C26 1.151(10) . ?
N00F C13 1.382(10) . ?
N00F C14 1.412(10) . ?
N00F C18 1.391(11) . ?
N00G C1 1.392(10) . ?
N00G C2 1.392(10) . ?
N00G C6 1.386(10) . ?
O4 C25 1.139(10) . ?
O8 C31 1.417(11) . ?
O8 C28 1.413(11) . ?
O7 C39 1.418(11) . ?
O7 C36 1.429(11) . ?
O9 C32 1.428(11) . ?
O9 C35 1.408(13) . ?
C23 H23 0.9300 . ?
C23 C24 1.369(12) . ?
C23 C22 1.363(12) . ?
C3 H3 0.9300 . ?
C3 C2 1.410(11) . ?
C3 C4 1.363(12) . ?
C8 C9 1.404(11) . ?
C19 C24 1.396(12) . ?
C19 C20 1.394(12) . ?
C24 H24 0.9300 . ?
C6 H6 0.9300 . ?
C6 C5 1.357(12) . ?
C4 H4 0.9300 . ?
C4 C5 1.404(12) . ?
C20 H20 0.9300 . ?
C20 C21 1.370(12) . ?
C9 H9 0.9300 . ?
C9 C10 1.351(12) . ?
C14 C15 1.417(12) . ?
C12 H12 0.9300 . ?
C12 C11 1.350(12) . ?
C5 H5 0.9300 . ?
C15 H15 0.9300 . ?
C15 C16 1.340(13) . ?
C18 H18 0.9300 . ?
C18 C17 1.336(12) . ?
C21 H21 0.9300 . ?
C21 C22 1.387(12) . ?
C10 H10 0.9300 . ?
C10 C11 1.402(12) . ?
C16 H16 0.9300 . ?
C16 C17 1.417(13) . ?
C22 H22 0.9300 . ?
C17 H17 0.9300 . ?
C11 H11 0.9300 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C30 1.499(13) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.491(13) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C29 1.510(14) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.506(13) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.488(15) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C38 1.518(13) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.511(15) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C37 1.515(14) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C34 1.496(16) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?

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
P3 Mo1 P1 91.53(8) . . ?
P5 Mo1 P1 95.26(8) . . ?
P5 Mo1 P3 89.83(8) . . ?
C26 Mo1 P1 88.5(2) . . ?
C26 Mo1 P3 177.7(3) . . ?
C26 Mo1 P5 87.9(3) . . ?
C26 Mo1 C25 89.4(4) . . ?
C26 Mo1 C27 90.9(4) . . ?
C25 Mo1 P1 172.6(3) . . ?
C25 Mo1 P3 90.9(3) . . ?
C25 Mo1 P5 91.8(3) . . ?
C25 Mo1 C27 87.9(4) . . ?
C27 Mo1 P1 85.0(3) . . ?
C27 Mo1 P3 91.4(3) . . ?
C27 Mo1 P5 178.8(3) . . ?
P2 P1 Mo1 128.14(12) . . ?
C1 P1 Mo1 135.6(3) . . ?
C1 P1 P2 96.1(3) . . ?
P4 P3 Mo1 131.66(12) . . ?
C7 P3 Mo1 131.5(3) . . ?
C7 P3 P4 96.7(3) . . ?
C2 P2 P1 92.0(3) . . ?
C8 P4 P3 91.7(3) . . ?
O3 Si1 O2 112.0(3) . . ?
O3 Si1 C19 109.2(3) . . ?
O2 Si1 C19 110.6(3) . . ?
O1 Si1 O3 107.4(3) . . ?
O1 Si1 O2 109.6(3) . . ?
O1 Si1 C19 108.0(3) . . ?
P6 P5 Mo1 135.10(13) . . ?
C13 P5 Mo1 127.0(3) . . ?
C13 P5 P6 96.8(3) . . ?
C14 P6 P5 92.3(3) . . ?
C13 O3 Si1 135.1(5) . . ?
C7 O2 Si1 136.0(5) . . ?
C1 O1 Si1 132.9(5) . . ?
C7 N00C C8 115.4(7) . . ?
C7 N00C C12 124.1(7) . . ?
C12 N00C C8 120.5(7) . . ?
C13 N00F C14 115.8(7) . . ?
C13 N00F C18 123.0(7) . . ?
C18 N00F C14 121.2(7) . . ?
C2 N00G C1 114.7(7) . . ?
C6 N00G C1 123.3(7) . . ?
C6 N00G C2 122.1(7) . . ?
C28 O8 C31 108.6(7) . . ?
O3 C13 P5 127.4(6) . . ?
O3 C13 N00F 115.6(7) . . ?
N00F C13 P5 116.7(6) . . ?
C39 O7 C36 108.3(7) . . ?
O5 C26 Mo1 178.8(8) . . ?
O1 C1 P1 128.1(6) . . ?
O1 C1 N00G 114.1(7) . . ?
N00G C1 P1 117.8(6) . . ?
O4 C25 Mo1 176.1(8) . . ?
O2 C7 P3 129.3(6) . . ?
O2 C7 N00C 113.2(7) . . ?
N00C C7 P3 117.2(6) . . ?
C35 O9 C32 108.3(8) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C22 C23 C24 121.4(9) . . ?
O6 C27 Mo1 178.7(8) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C4 C3 C2 121.9(8) . . ?
N00C C8 P4 118.9(6) . . ?
N00C C8 C9 116.9(7) . . ?
C9 C8 P4 124.2(6) . . ?
N00G C2 P2 119.4(6) . . ?
N00G C2 C3 116.9(8) . . ?
C3 C2 P2 123.7(7) . . ?
C24 C19 Si1 123.5(7) . . ?
C20 C19 Si1 118.1(6) . . ?
C20 C19 C24 118.4(8) . . ?
C23 C24 C19 119.9(9) . . ?
C23 C24 H24 120.0 . . ?
C19 C24 H24 120.0 . . ?
N00G C6 H6 120.5 . . ?
C5 C6 N00G 119.0(8) . . ?
C5 C6 H6 120.5 . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.7(8) . . ?
C5 C4 H4 120.6 . . ?
C19 C20 H20 119.6 . . ?
C21 C20 C19 120.8(8) . . ?
C21 C20 H20 119.6 . . ?
C8 C9 H9 118.6 . . ?
C10 C9 C8 122.8(8) . . ?
C10 C9 H9 118.6 . . ?
N00F C14 P6 118.4(6) . . ?
N00F C14 C15 116.2(8) . . ?
C15 C14 P6 125.4(7) . . ?
N00C C12 H12 119.9 . . ?
C11 C12 N00C 120.3(8) . . ?
C11 C12 H12 119.9 . . ?
C6 C5 C4 121.4(9) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C14 C15 H15 119.4 . . ?
C16 C15 C14 121.2(9) . . ?
C16 C15 H15 119.4 . . ?
N00F C18 H18 119.5 . . ?
C17 C18 N00F 121.0(8) . . ?
C17 C18 H18 119.5 . . ?
C20 C21 H21 120.0 . . ?
C20 C21 C22 120.0(8) . . ?
C22 C21 H21 120.0 . . ?
C9 C10 H10 120.7 . . ?
C9 C10 C11 118.6(8) . . ?
C11 C10 H10 120.7 . . ?
C15 C16 H16 119.4 . . ?
C15 C16 C17 121.3(8) . . ?
C17 C16 H16 119.4 . . ?
C23 C22 C21 119.4(9) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C18 C17 C16 119.0(9) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C12 C11 C10 120.8(8) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
O8 C31 H31A 110.4 . . ?
O8 C31 H31B 110.4 . . ?
O8 C31 C30 106.5(8) . . ?
H31A C31 H31B 108.6 . . ?
C30 C31 H31A 110.4 . . ?
C30 C31 H31B 110.4 . . ?
O9 C32 H32A 110.5 . . ?
O9 C32 H32B 110.5 . . ?
O9 C32 C33 106.3(8) . . ?
H32A C32 H32B 108.7 . . ?
C33 C32 H32A 110.5 . . ?
C33 C32 H32B 110.5 . . ?
C31 C30 H30A 111.3 . . ?
C31 C30 H30B 111.3 . . ?
C31 C30 C29 102.3(8) . . ?
H30A C30 H30B 109.2 . . ?
C29 C30 H30A 111.3 . . ?
C29 C30 H30B 111.3 . . ?
O8 C28 H28A 110.2 . . ?
O8 C28 H28B 110.2 . . ?
O8 C28 C29 107.5(8) . . ?
H28A C28 H28B 108.5 . . ?
C29 C28 H28A 110.2 . . ?
C29 C28 H28B 110.2 . . ?
C32 C33 H33A 111.0 . . ?
C32 C33 H33B 111.0 . . ?
H33A C33 H33B 109.0 . . ?
C34 C33 C32 103.7(9) . . ?
C34 C33 H33A 111.0 . . ?
C34 C33 H33B 111.0 . . ?
O7 C39 H39A 110.4 . . ?
O7 C39 H39B 110.4 . . ?
O7 C39 C38 106.6(7) . . ?
H39A C39 H39B 108.6 . . ?
C38 C39 H39A 110.4 . . ?
C38 C39 H39B 110.4 . . ?
O7 C36 H36A 110.2 . . ?
O7 C36 H36B 110.2 . . ?
O7 C36 C37 107.5(8) . . ?
H36A C36 H36B 108.5 . . ?
C37 C36 H36A 110.2 . . ?
C37 C36 H36B 110.2 . . ?
C30 C29 H29A 111.7 . . ?
C30 C29 H29B 111.7 . . ?
C28 C29 C30 100.1(8) . . ?
C28 C29 H29A 111.7 . . ?
C28 C29 H29B 111.7 . . ?
H29A C29 H29B 109.5 . . ?
C39 C38 H38A 111.7 . . ?
C39 C38 H38B 111.7 . . ?
H38A C38 H38B 109.4 . . ?
C37 C38 C39 100.5(8) . . ?
C37 C38 H38A 111.7 . . ?
C37 C38 H38B 111.7 . . ?
O9 C35 H35A 109.9 . . ?
O9 C35 H35B 109.9 . . ?
O9 C35 C34 108.9(9) . . ?
H35A C35 H35B 108.3 . . ?
C34 C35 H35A 109.9 . . ?
C34 C35 H35B 109.9 . . ?
C33 C34 C35 103.9(9) . . ?
C33 C34 H34A 111.0 . . ?
C33 C34 H34B 111.0 . . ?
C35 C34 H34A 111.0 . . ?
C35 C34 H34B 111.0 . . ?
H34A C34 H34B 109.0 . . ?
C36 C37 C38 102.8(8) . . ?
C36 C37 H37A 111.2 . . ?
C36 C37 H37B 111.2 . . ?
C38 C37 H37A 111.2 . . ?
C38 C37 H37B 111.2 . . ?
H37A C37 H37B 109.1 . . ?

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
Mo1 P1 C1 O1 2.5(10) . . . . ?
Mo1 P1 C1 N00G -176.9(4) . . . . ?
Mo1 P3 C7 O2 -7.5(9) . . . . ?
Mo1 P3 C7 N00C 178.0(4) . . . . ?
Mo1 P5 C13 O3 6.8(9) . . . . ?
Mo1 P5 C13 N00F -165.9(4) . . . . ?
P1 P2 C2 N00G 0.1(6) . . . . ?
P1 P2 C2 C3 178.1(7) . . . . ?
P3 P4 C8 N00C -1.7(6) . . . . ?
P3 P4 C8 C9 178.0(7) . . . . ?
P2 P1 C1 O1 178.1(7) . . . . ?
P2 P1 C1 N00G -1.4(6) . . . . ?
P4 P3 C7 O2 175.9(7) . . . . ?
P4 P3 C7 N00C 1.4(6) . . . . ?
P4 C8 C9 C10 177.8(7) . . . . ?
Si1 O3 C13 P5 63.5(10) . . . . ?
Si1 O3 C13 N00F -123.7(7) . . . . ?
Si1 O2 C7 P3 52.6(11) . . . . ?
Si1 O2 C7 N00C -132.7(6) . . . . ?
Si1 O1 C1 P1 44.9(11) . . . . ?
Si1 O1 C1 N00G -135.6(6) . . . . ?
Si1 C19 C24 C23 175.9(7) . . . . ?
Si1 C19 C20 C21 -176.8(7) . . . . ?
P5 P6 C14 N00F -0.3(6) . . . . ?
P5 P6 C14 C15 -179.8(7) . . . . ?
P6 P5 C13 O3 176.0(7) . . . . ?
P6 P5 C13 N00F 3.3(6) . . . . ?
P6 C14 C15 C16 176.8(7) . . . . ?
O3 Si1 O2 C7 -94.4(8) . . . . ?
O3 Si1 O1 C1 19.0(8) . . . . ?
O3 Si1 C19 C24 -114.4(7) . . . . ?
O3 Si1 C19 C20 63.6(7) . . . . ?
O2 Si1 O3 C13 -0.5(8) . . . . ?
O2 Si1 O1 C1 -102.9(8) . . . . ?
O2 Si1 C19 C24 9.3(8) . . . . ?
O2 Si1 C19 C20 -172.7(6) . . . . ?
O1 Si1 O3 C13 -120.9(7) . . . . ?
O1 Si1 O2 C7 24.6(8) . . . . ?
O1 Si1 C19 C24 129.2(7) . . . . ?
O1 Si1 C19 C20 -52.8(7) . . . . ?
N00C C8 C9 C10 -2.5(12) . . . . ?
N00C C12 C11 C10 -0.4(13) . . . . ?
N00F C14 C15 C16 -2.7(12) . . . . ?
N00F C18 C17 C16 -0.6(13) . . . . ?
N00G C6 C5 C4 2.8(13) . . . . ?
O8 C31 C30 C29 -31.6(10) . . . . ?
O8 C28 C29 C30 -32.2(10) . . . . ?
C13 N00F C14 P6 2.6(9) . . . . ?
C13 N00F C14 C15 -177.9(7) . . . . ?
C13 N00F C18 C17 179.5(8) . . . . ?
O7 C39 C38 C37 -36.2(10) . . . . ?
O7 C36 C37 C38 -23.7(11) . . . . ?
C1 N00G C2 P2 -1.1(9) . . . . ?
C1 N00G C2 C3 -179.2(7) . . . . ?
C1 N00G C6 C5 177.3(8) . . . . ?
C7 N00C C8 P4 3.0(9) . . . . ?
C7 N00C C8 C9 -176.7(7) . . . . ?
C7 N00C C12 C11 178.1(8) . . . . ?
O9 C32 C33 C34 30.3(12) . . . . ?
O9 C35 C34 C33 13.8(16) . . . . ?
C3 C4 C5 C6 -2.3(13) . . . . ?
C8 N00C C7 P3 -2.7(9) . . . . ?
C8 N00C C7 O2 -178.1(6) . . . . ?
C8 N00C C12 C11 -2.1(12) . . . . ?
C8 C9 C10 C11 0.1(13) . . . . ?
C2 N00G C1 P1 1.7(9) . . . . ?
C2 N00G C1 O1 -177.8(6) . . . . ?
C2 N00G C6 C5 -1.4(12) . . . . ?
C2 C3 C4 C5 0.5(13) . . . . ?
C19 Si1 O3 C13 122.3(7) . . . . ?
C19 Si1 O2 C7 143.6(7) . . . . ?
C19 Si1 O1 C1 136.6(7) . . . . ?
C19 C20 C21 C22 -0.2(13) . . . . ?
C24 C23 C22 C21 -0.8(14) . . . . ?
C24 C19 C20 C21 1.2(12) . . . . ?
C6 N00G C1 P1 -177.2(6) . . . . ?
C6 N00G C1 O1 3.3(11) . . . . ?
C6 N00G C2 P2 177.8(6) . . . . ?
C6 N00G C2 C3 -0.3(11) . . . . ?
C4 C3 C2 P2 -177.3(7) . . . . ?
C4 C3 C2 N00G 0.8(12) . . . . ?
C20 C19 C24 C23 -2.0(12) . . . . ?
C20 C21 C22 C23 -0.1(13) . . . . ?
C9 C10 C11 C12 1.4(14) . . . . ?
C14 N00F C13 P5 -4.0(9) . . . . ?
C14 N00F C13 O3 -177.6(6) . . . . ?
C14 N00F C18 C17 -2.1(12) . . . . ?
C14 C15 C16 C17 0.1(14) . . . . ?
C12 N00C C7 P3 177.1(6) . . . . ?
C12 N00C C7 O2 1.7(10) . . . . ?
C12 N00C C8 P4 -176.9(6) . . . . ?
C12 N00C C8 C9 3.5(11) . . . . ?
C15 C16 C17 C18 1.6(14) . . . . ?
C18 N00F C13 P5 174.4(6) . . . . ?
C18 N00F C13 O3 0.8(11) . . . . ?
C18 N00F C14 P6 -175.9(6) . . . . ?
C18 N00F C14 C15 3.7(11) . . . . ?
C22 C23 C24 C19 1.8(13) . . . . ?
C31 O8 C28 C29 13.4(10) . . . . ?
C31 C30 C29 C28 37.6(10) . . . . ?
C32 O9 C35 C34 5.2(16) . . . . ?
C32 C33 C34 C35 -26.3(14) . . . . ?
C28 O8 C31 C30 11.6(11) . . . . ?
C39 O7 C36 C37 1.0(11) . . . . ?
C39 C38 C37 C36 35.2(10) . . . . ?
C36 O7 C39 C38 22.5(10) . . . . ?
C35 O9 C32 C33 -22.3(13) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_rs2_197
_database_code_depnum_ccdc_archive 'CCDC 1494717'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_rs2_197             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          15 Note
RESPONSE: the mask of the beam-stopper is increased
;
# Added during the CSD deposition process: Tuesday 19 July 2016 09:44 AM
# end Validation Reply Form

_audit_creation_date             2016-06-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
Titanium(tris(1,3,4-azadiphospholo-1,2-pyridin-3-olate))-cyclopentadiene
_chemical_formula_moiety         'C23 H17 N3 O3 P6 Ti, C7 H8'
_chemical_formula_sum            'C30 H25 N3 O3 P6 Ti'
_chemical_formula_weight         709.25
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ti1 P4 O2 N2 C50 H50 Cl2'
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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   13.1587(2)
_cell_length_b                   20.1174(3)
_cell_length_c                   24.1036(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6380.68(17)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    11287
_cell_measurement_temperature    104.7(10)
_cell_measurement_theta_max      29.7250
_cell_measurement_theta_min      3.1310
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
_exptl_crystal_preparation       
'Cyclopentadienyltitaniumtrichloride and sodium azadiphospholate in toluene'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30300
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.283
_diffrn_reflns_theta_min         3.059
_diffrn_ambient_temperature      104.7(10)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -6.00   20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega  -52.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904   77.0000 -150.0000 93

#__ type_ start__ end____ width___ exp.time_
  3 omega  -89.00  -63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  161.0000 -148.0000 26

#__ type_ start__ end____ width___ exp.time_
  4 omega   13.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000  -60.0000 74
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_UB_11      0.0155916000
_diffrn_orient_matrix_UB_12      0.0046234000
_diffrn_orient_matrix_UB_13      -0.0278943000
_diffrn_orient_matrix_UB_21      -0.0515763000
_diffrn_orient_matrix_UB_22      0.0016997000
_diffrn_orient_matrix_UB_23      -0.0084314000
_diffrn_orient_matrix_UB_31      0.0004449000
_diffrn_orient_matrix_UB_32      0.0349275000
_diffrn_orient_matrix_UB_33      0.0040854000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                13534
_reflns_number_total             15821
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.501
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 
;
 Flack x determined using 4898 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         15821
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0521
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²+2.8533P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1141
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C21(H21), C29(H29), C30(H30), C24(H24), C43(H43), C33(H33),
 C27(H27), C35(H35), C44(H44), C28(H28), C45(H45), C34(H34), C23(H23), C22(H22),
  C42(H42), C46(H46), C12(H12), C9(H9), C3(H3), C5(H5), C37(H37), C10(H10),
 C4(H4), C16(H16), C6(H6), C38(H38), C41(H41), C18(H18), C17(H17), C56(H56),
 C15(H15), C57(H57), C11(H11), C39(H39), C59(H59), C40(H40), C58(H58), C60(H60),
  C52(H52), C50(H50), C49(H49), C51(H51), C53(H53)
2.b Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C47(H47A,H47B,H47C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti2 Ti 0.33376(6) 0.45616(4) 0.13913(3) 0.01676(17) Uani 1 1 d . . . . .
P8 P 0.40351(13) 0.66499(7) 0.30199(7) 0.0343(4) Uani 1 1 d . . . . .
P10 P 0.66849(10) 0.28220(6) 0.07389(5) 0.0245(3) Uani 1 1 d . . . . .
P9 P 0.62823(10) 0.37222(6) 0.11376(6) 0.0265(3) Uani 1 1 d . . . . .
P12 P -0.08028(11) 0.38722(8) 0.09273(6) 0.0326(3) Uani 1 1 d . . . . .
P11 P 0.07134(11) 0.35279(7) 0.08540(6) 0.0299(3) Uani 1 1 d . . . . .
P7 P 0.29301(11) 0.61086(7) 0.25683(6) 0.0313(3) Uani 1 1 d . . . . .
O4 O 0.3544(2) 0.49607(15) 0.20695(14) 0.0219(7) Uani 1 1 d . . . . .
N4 N 0.4772(3) 0.55395(18) 0.25446(16) 0.0180(8) Uani 1 1 d . . . . .
C36 C 0.0784(4) 0.4892(2) 0.20656(19) 0.0228(10) Uani 1 1 d . . . . .
H36 H 0.1459 0.4904 0.2181 0.027 Uiso 1 1 calc R . . . .
O5 O 0.4285(2) 0.38933(15) 0.14071(14) 0.0236(7) Uani 1 1 d . . . . .
C21 C 0.6017(4) 0.6140(3) 0.3066(2) 0.0293(12) Uani 1 1 d . . . . .
H21 H 0.6197 0.6498 0.3289 0.035 Uiso 1 1 calc R . . . .
N6 N 0.4684(3) 0.29189(18) 0.09615(16) 0.0178(8) Uani 1 1 d . . . . .
C32 C -0.0515(4) 0.4431(2) 0.1457(2) 0.0247(10) Uani 1 1 d . . . . .
C26 C 0.5444(4) 0.2516(2) 0.07312(19) 0.0215(10) Uani 1 1 d . . . . .
C31 C 0.1165(3) 0.4052(2) 0.1364(2) 0.0210(10) Uani 1 1 d . . . . .
C29 C 0.3394(4) 0.2136(2) 0.0739(2) 0.0254(10) Uani 1 1 d . . . . .
H29 H 0.2712 0.2015 0.0731 0.030 Uiso 1 1 calc R . . . .
N5 N 0.0492(3) 0.44657(19) 0.16341(16) 0.0204(8) Uani 1 1 d . . . . .
C30 C 0.3670(4) 0.2729(2) 0.0961(2) 0.0207(10) Uani 1 1 d . . . . .
H30 H 0.3179 0.3008 0.1113 0.025 Uiso 1 1 calc R . . . .
C25 C 0.5010(4) 0.3520(2) 0.1174(2) 0.0215(10) Uani 1 1 d . . . . .
C24 C 0.5509(4) 0.5069(2) 0.2409(2) 0.0222(10) Uani 1 1 d . . . . .
H24 H 0.5340 0.4708 0.2187 0.027 Uiso 1 1 calc R . . . .
C43 C 0.4152(5) 0.5365(3) 0.0865(3) 0.0478(17) Uani 1 1 d . . . . .
H43 H 0.4782 0.5525 0.0978 0.057 Uiso 1 1 calc R . . . .
C33 C -0.1225(4) 0.4849(3) 0.1729(2) 0.0308(12) Uani 1 1 d . . . . .
H33 H -0.1904 0.4836 0.1622 0.037 Uiso 1 1 calc R . . . .
C20 C 0.5006(4) 0.6092(2) 0.28704(19) 0.0221(10) Uani 1 1 d . . . . .
C27 C 0.5133(4) 0.1893(2) 0.0518(2) 0.0240(11) Uani 1 1 d . . . . .
H27 H 0.5619 0.1605 0.0374 0.029 Uiso 1 1 calc R . . . .
C35 C 0.0093(4) 0.5284(2) 0.2313(2) 0.0275(11) Uani 1 1 d . . . . .
H35 H 0.0292 0.5568 0.2597 0.033 Uiso 1 1 calc R . . . .
C44 C 0.3973(5) 0.4817(3) 0.0516(3) 0.0473(18) Uani 1 1 d . . . . .
H44 H 0.4465 0.4550 0.0352 0.057 Uiso 1 1 calc R . . . .
C28 C 0.4136(4) 0.1703(2) 0.0520(2) 0.0277(12) Uani 1 1 d . . . . .
H28 H 0.3947 0.1292 0.0378 0.033 Uiso 1 1 calc R . . . .
C45 C 0.2938(6) 0.4750(3) 0.0462(2) 0.0499(18) Uani 1 1 d . . . . .
H45 H 0.2608 0.4425 0.0255 0.060 Uiso 1 1 calc R . . . .
C19 C 0.3780(4) 0.5495(2) 0.23698(19) 0.0201(9) Uani 1 1 d . . . . .
C34 C -0.0941(4) 0.5267(3) 0.2142(2) 0.0321(12) Uani 1 1 d . . . . .
H34 H -0.1418 0.5541 0.2311 0.038 Uiso 1 1 calc R . . . .
C23 C 0.6462(4) 0.5136(2) 0.2599(2) 0.0267(11) Uani 1 1 d . . . . .
H23 H 0.6950 0.4821 0.2506 0.032 Uiso 1 1 calc R . . . .
C22 C 0.6730(4) 0.5680(3) 0.2938(2) 0.0335(12) Uani 1 1 d . . . . .
H22 H 0.7390 0.5722 0.3072 0.040 Uiso 1 1 calc R . . . .
C42 C 0.3206(6) 0.5624(3) 0.1011(2) 0.0479(18) Uani 1 1 d . . . . .
H42 H 0.3097 0.5991 0.1237 0.057 Uiso 1 1 calc R . . . .
C46 C 0.2468(5) 0.5248(4) 0.0766(3) 0.0505(18) Uani 1 1 d . . . . .
H46 H 0.1771 0.5315 0.0797 0.061 Uiso 1 1 calc R . . . .
Ti1 Ti 0.83295(6) 0.89535(4) 0.14386(3) 0.01686(17) Uani 1 1 d . . . . .
P2 P 1.16245(10) 1.05999(6) 0.06232(6) 0.0253(3) Uani 1 1 d . . . . .
P5 P 0.57604(11) 0.99919(8) 0.08004(7) 0.0352(3) Uani 1 1 d . . . . .
P6 P 0.42406(11) 0.96495(8) 0.08545(7) 0.0357(3) Uani 1 1 d . . . . .
P1 P 1.12753(10) 0.97332(6) 0.10890(6) 0.0258(3) Uani 1 1 d . . . . .
P3 P 0.78522(11) 0.74499(7) 0.26678(6) 0.0283(3) Uani 1 1 d . . . . .
P4 P 0.89787(12) 0.68929(7) 0.30891(6) 0.0326(3) Uani 1 1 d . . . . .
O2 O 0.8464(2) 0.85734(15) 0.21331(13) 0.0204(7) Uani 1 1 d . . . . .
O3 O 0.7144(2) 0.94398(15) 0.15087(14) 0.0220(7) Uani 1 1 d . . . . .
N2 N 0.9711(3) 0.79788(18) 0.25740(16) 0.0192(8) Uani 1 1 d . . . . .
N1 N 0.9674(3) 1.05427(18) 0.09573(16) 0.0168(8) Uani 1 1 d . . . . .
C1 C 1.0017(3) 0.9952(2) 0.1181(2) 0.0192(9) Uani 1 1 d . . . . .
C12 C 1.0445(4) 0.8433(2) 0.2410(2) 0.0215(10) Uani 1 1 d . . . . .
H12 H 1.0264 0.8797 0.2194 0.026 Uiso 1 1 calc R . . . .
C9 C 1.0991(4) 0.7348(3) 0.3049(2) 0.0314(12) Uani 1 1 d . . . . .
H9 H 1.1177 0.6983 0.3263 0.038 Uiso 1 1 calc R . . . .
N3 N 0.5486(3) 0.90880(18) 0.16034(17) 0.0204(8) Uani 1 1 d . . . . .
C7 C 0.8697(4) 0.8042(2) 0.24375(19) 0.0196(9) Uani 1 1 d . . . . .
C3 C 1.0059(4) 1.1531(2) 0.0449(2) 0.0270(11) Uani 1 1 d . . . . .
H3 H 1.0525 1.1799 0.0264 0.032 Uiso 1 1 calc R . . . .
C5 C 0.8380(4) 1.1342(2) 0.0779(2) 0.0241(10) Uani 1 1 d . . . . .
H5 H 0.7708 1.1481 0.0813 0.029 Uiso 1 1 calc R . . . .
C37 C 0.8883(4) 0.8723(3) 0.0538(2) 0.0317(13) Uani 1 1 d . . . . .
H37 H 0.9280 0.9027 0.0344 0.038 Uiso 1 1 calc R . . . .
C10 C 1.1720(4) 0.7790(3) 0.2894(2) 0.0333(12) Uani 1 1 d . . . . .
H10 H 1.2394 0.7730 0.2999 0.040 Uiso 1 1 calc R . . . .
C4 C 0.9090(4) 1.1743(2) 0.0493(2) 0.0280(12) Uani 1 1 d . . . . .
H4 H 0.8893 1.2146 0.0338 0.034 Uiso 1 1 calc R . . . .
C16 C 0.4031(4) 0.8281(3) 0.2086(3) 0.0336(13) Uani 1 1 d . . . . .
H16 H 0.3547 0.8001 0.2242 0.040 Uiso 1 1 calc R . . . .
C6 C 0.8673(4) 1.0758(2) 0.10043(19) 0.0201(10) Uani 1 1 d . . . . .
H6 H 0.8202 1.0498 0.1192 0.024 Uiso 1 1 calc R . . . .
C14 C 0.4488(4) 0.9109(2) 0.1399(2) 0.0264(11) Uani 1 1 d . . . . .
C38 C 0.9239(5) 0.8215(3) 0.0886(3) 0.0401(15) Uani 1 1 d . . . . .
H38 H 0.9917 0.8124 0.0964 0.048 Uiso 1 1 calc R . . . .
C41 C 0.7826(4) 0.8690(3) 0.0538(2) 0.0288(12) Uani 1 1 d . . . . .
H41 H 0.7390 0.8966 0.0340 0.035 Uiso 1 1 calc R . . . .
C13 C 0.6186(4) 0.9486(2) 0.1331(2) 0.0230(10) Uani 1 1 d . . . . .
C8 C 0.9965(4) 0.7425(2) 0.2898(2) 0.0246(11) Uani 1 1 d . . . . .
C55 C 0.6759(6) 0.6156(4) 0.0768(3) 0.0564(18) Uani 1 1 d . . . . .
C18 C 0.5751(4) 0.8679(2) 0.2052(2) 0.0227(10) Uani 1 1 d . . . . .
H18 H 0.6414 0.8681 0.2187 0.027 Uiso 1 1 calc R . . . .
C17 C 0.5046(4) 0.8283(2) 0.2288(2) 0.0267(11) Uani 1 1 d . . . . .
H17 H 0.5225 0.8011 0.2585 0.032 Uiso 1 1 calc R . . . .
C56 C 0.6725(5) 0.6298(3) 0.1342(3) 0.0417(14) Uani 1 1 d . . . . .
H56 H 0.7189 0.6116 0.1590 0.050 Uiso 1 1 calc R . . . .
C2 C 1.0398(4) 1.0918(2) 0.06720(19) 0.0193(9) Uani 1 1 d . . . . .
C15 C 0.3782(4) 0.8687(2) 0.1669(2) 0.0303(12) Uani 1 1 d . . . . .
H15 H 0.3110 0.8692 0.1549 0.036 Uiso 1 1 calc R . . . .
C57 C 0.5960(5) 0.6722(3) 0.1511(3) 0.0436(15) Uani 1 1 d . . . . .
H57 H 0.5908 0.6815 0.1888 0.052 Uiso 1 1 calc R . . . .
C11 C 1.1428(4) 0.8347(2) 0.2566(2) 0.0283(11) Uani 1 1 d . . . . .
H11 H 1.1916 0.8654 0.2456 0.034 Uiso 1 1 calc R . . . .
C39 C 0.8409(6) 0.7870(3) 0.1091(2) 0.0426(15) Uani 1 1 d . . . . .
H39 H 0.8433 0.7502 0.1324 0.051 Uiso 1 1 calc R . . . .
C59 C 0.5371(6) 0.6891(3) 0.0677(4) 0.063(2) Uani 1 1 d . . . . .
H59 H 0.4918 0.7107 0.0442 0.076 Uiso 1 1 calc R . . . .
C40 C 0.7537(4) 0.8171(3) 0.0888(2) 0.0331(13) Uani 1 1 d . . . . .
H40 H 0.6873 0.8047 0.0970 0.040 Uiso 1 1 calc R . . . .
C58 C 0.5273(7) 0.7016(4) 0.1163(4) 0.070(2) Uani 1 1 d . . . . .
H58 H 0.4762 0.7295 0.1293 0.083 Uiso 1 1 calc R . . . .
C60 C 0.6051(6) 0.6476(4) 0.0419(3) 0.064(2) Uani 1 1 d . . . . .
H60 H 0.6045 0.6410 0.0037 0.076 Uiso 1 1 calc R . . . .
C54 C 0.7490(7) 0.5669(4) 0.0544(4) 0.087(3) Uani 1 1 d . . . . .
H54A H 0.8074 0.5646 0.0783 0.131 Uiso 1 1 calc GR . . . .
H54B H 0.7698 0.5803 0.0179 0.131 Uiso 1 1 calc GR . . . .
H54C H 0.7174 0.5239 0.0525 0.131 Uiso 1 1 calc GR . . . .
C52 C 0.0852(7) 0.6769(3) 0.1510(3) 0.063(2) Uani 1 1 d . . . . .
H52 H 0.0786 0.6702 0.1890 0.075 Uiso 1 1 calc R . . . .
C50 C 0.0265(6) 0.6544(4) 0.0602(3) 0.060(2) Uani 1 1 d . . . . .
H50 H -0.0190 0.6341 0.0360 0.072 Uiso 1 1 calc R . . . .
C49 C 0.1041(5) 0.6936(4) 0.0402(3) 0.0569(19) Uani 1 1 d . . . . .
H49 H 0.1115 0.6985 0.0021 0.068 Uiso 1 1 calc R . . . .
C48 C 0.1712(6) 0.7260(4) 0.0751(4) 0.064(2) Uani 1 1 d . . . . .
C47 C 0.2553(6) 0.7680(5) 0.0542(4) 0.102(4) Uani 1 1 d . . . . .
H47A H 0.2629 0.7614 0.0150 0.153 Uiso 1 1 calc GR . . . .
H47B H 0.3173 0.7560 0.0727 0.153 Uiso 1 1 calc GR . . . .
H47C H 0.2403 0.8139 0.0615 0.153 Uiso 1 1 calc GR . . . .
C51 C 0.0181(7) 0.6462(4) 0.1156(3) 0.062(2) Uani 1 1 d . . . . .
H51 H -0.0334 0.6195 0.1298 0.074 Uiso 1 1 calc R . . . .
C53 C 0.1607(7) 0.7168(4) 0.1320(3) 0.062(2) Uani 1 1 d . . . . .
H53 H 0.2047 0.7378 0.1566 0.074 Uiso 1 1 calc R . . . .
O1 O 0.9321(2) 0.95983(14) 0.14566(14) 0.0205(7) Uani 1 1 d . . . . .
O6 O 0.2141(2) 0.41086(15) 0.15129(14) 0.0211(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti2 O4 1.841(3) . ?
Ti2 O5 1.834(3) . ?
Ti2 C43 2.317(6) . ?
Ti2 C44 2.327(6) . ?
Ti2 C45 2.333(6) . ?
Ti2 C42 2.332(5) . ?
Ti2 C46 2.343(6) . ?
Ti2 O6 1.843(3) . ?
P8 P7 2.118(2) . ?
P8 C20 1.738(5) . ?
P10 P9 2.1174(18) . ?
P10 C26 1.746(5) . ?
P9 C25 1.725(5) . ?
P12 P11 2.119(2) . ?
P12 C32 1.742(5) . ?
P11 C31 1.725(5) . ?
P7 C19 1.732(5) . ?
O4 C19 1.333(5) . ?
N4 C24 1.394(6) . ?
N4 C20 1.395(6) . ?
N4 C19 1.375(6) . ?
C36 H36 0.9300 . ?
C36 N5 1.402(6) . ?
C36 C35 1.343(7) . ?
O5 C25 1.337(5) . ?
C21 H21 0.9300 . ?
C21 C20 1.415(7) . ?
C21 C22 1.354(8) . ?
N6 C26 1.402(6) . ?
N6 C30 1.388(6) . ?
N6 C25 1.382(6) . ?
C32 N5 1.395(6) . ?
C32 C33 1.418(7) . ?
C26 C27 1.415(7) . ?
C31 N5 1.379(6) . ?
C31 O6 1.338(5) . ?
C29 H29 0.9300 . ?
C29 C30 1.356(6) . ?
C29 C28 1.411(7) . ?
C30 H30 0.9300 . ?
C24 H24 0.9300 . ?
C24 C23 1.342(7) . ?
C43 H43 0.9300 . ?
C43 C44 1.406(9) . ?
C43 C42 1.394(9) . ?
C33 H33 0.9300 . ?
C33 C34 1.354(7) . ?
C27 H27 0.9300 . ?
C27 C28 1.366(7) . ?
C35 H35 0.9300 . ?
C35 C34 1.422(7) . ?
C44 H44 0.9300 . ?
C44 C45 1.375(9) . ?
C28 H28 0.9300 . ?
C45 H45 0.9300 . ?
C45 C46 1.387(9) . ?
C34 H34 0.9300 . ?
C23 H23 0.9300 . ?
C23 C22 1.410(7) . ?
C22 H22 0.9300 . ?
C42 H42 0.9300 . ?
C42 C46 1.365(10) . ?
C46 H46 0.9300 . ?
Ti1 O2 1.849(3) . ?
Ti1 O3 1.850(3) . ?
Ti1 C37 2.335(5) . ?
Ti1 C38 2.328(5) . ?
Ti1 C41 2.330(5) . ?
Ti1 C39 2.337(5) . ?
Ti1 C40 2.309(5) . ?
Ti1 O1 1.841(3) . ?
P2 P1 2.1241(18) . ?
P2 C2 1.740(5) . ?
P5 P6 2.119(2) . ?
P5 C13 1.727(5) . ?
P6 C14 1.736(6) . ?
P1 C1 1.727(5) . ?
P3 P4 2.118(2) . ?
P3 C7 1.720(5) . ?
P4 C8 1.744(5) . ?
O2 C7 1.333(5) . ?
O3 C13 1.335(5) . ?
N2 C12 1.388(6) . ?
N2 C7 1.381(6) . ?
N2 C8 1.402(6) . ?
N1 C1 1.381(6) . ?
N1 C6 1.391(6) . ?
N1 C2 1.396(6) . ?
C1 O1 1.336(5) . ?
C12 H12 0.9300 . ?
C12 C11 1.358(7) . ?
C9 H9 0.9300 . ?
C9 C10 1.361(8) . ?
C9 C8 1.407(7) . ?
N3 C14 1.402(6) . ?
N3 C13 1.386(6) . ?
N3 C18 1.403(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.348(7) . ?
C3 C2 1.418(7) . ?
C5 H5 0.9300 . ?
C5 C4 1.416(7) . ?
C5 C6 1.350(6) . ?
C37 H37 0.9300 . ?
C37 C38 1.403(8) . ?
C37 C41 1.393(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.424(7) . ?
C4 H4 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.422(7) . ?
C16 C15 1.336(8) . ?
C6 H6 0.9300 . ?
C14 C15 1.417(7) . ?
C38 H38 0.9300 . ?
C38 C39 1.385(9) . ?
C41 H41 0.9300 . ?
C41 C40 1.395(8) . ?
C55 C56 1.412(9) . ?
C55 C60 1.412(10) . ?
C55 C54 1.476(10) . ?
C18 H18 0.9300 . ?
C18 C17 1.349(7) . ?
C17 H17 0.9300 . ?
C56 H56 0.9300 . ?
C56 C57 1.382(9) . ?
C15 H15 0.9300 . ?
C57 H57 0.9300 . ?
C57 C58 1.368(10) . ?
C11 H11 0.9300 . ?
C39 H39 0.9300 . ?
C39 C40 1.387(8) . ?
C59 H59 0.9300 . ?
C59 C58 1.205(11) . ?
C59 C60 1.372(10) . ?
C40 H40 0.9300 . ?
C58 H58 0.9300 . ?
C60 H60 0.9300 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C52 H52 0.9300 . ?
C52 C51 1.376(11) . ?
C52 C53 1.358(11) . ?
C50 H50 0.9300 . ?
C50 C49 1.377(10) . ?
C50 C51 1.350(10) . ?
C49 H49 0.9300 . ?
C49 C48 1.383(11) . ?
C48 C47 1.482(11) . ?
C48 C53 1.390(11) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C51 H51 0.9300 . ?
C53 H53 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
O4 Ti2 C43 96.5(2) . . ?
O4 Ti2 C44 131.0(2) . . ?
O4 Ti2 C45 144.6(2) . . ?
O4 Ti2 C42 87.75(19) . . ?
O4 Ti2 C46 112.7(2) . . ?
O4 Ti2 O6 101.57(15) . . ?
O5 Ti2 O4 101.58(15) . . ?
O5 Ti2 C43 102.0(2) . . ?
O5 Ti2 C44 86.36(19) . . ?
O5 Ti2 C45 107.0(2) . . ?
O5 Ti2 C42 136.9(2) . . ?
O5 Ti2 C46 141.0(2) . . ?
O5 Ti2 O6 102.43(14) . . ?
C43 Ti2 C44 35.3(2) . . ?
C43 Ti2 C45 57.6(2) . . ?
C43 Ti2 C42 34.9(2) . . ?
C43 Ti2 C46 57.5(2) . . ?
C44 Ti2 C45 34.3(2) . . ?
C44 Ti2 C42 57.8(2) . . ?
C44 Ti2 C46 57.4(2) . . ?
C45 Ti2 C46 34.5(2) . . ?
C42 Ti2 C45 57.1(2) . . ?
C42 Ti2 C46 34.0(2) . . ?
O6 Ti2 C43 145.8(2) . . ?
O6 Ti2 C44 124.1(2) . . ?
O6 Ti2 C45 92.3(2) . . ?
O6 Ti2 C42 116.9(2) . . ?
O6 Ti2 C46 88.65(19) . . ?
C20 P8 P7 93.78(17) . . ?
C26 P10 P9 94.16(16) . . ?
C25 P9 P10 93.70(17) . . ?
C32 P12 P11 93.87(17) . . ?
C31 P11 P12 93.75(17) . . ?
C19 P7 P8 93.73(17) . . ?
C19 O4 Ti2 150.3(3) . . ?
C24 N4 C20 121.3(4) . . ?
C19 N4 C24 123.0(4) . . ?
C19 N4 C20 115.7(4) . . ?
N5 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C35 C36 N5 120.2(5) . . ?
C25 O5 Ti2 152.6(3) . . ?
C20 C21 H21 119.0 . . ?
C22 C21 H21 119.0 . . ?
C22 C21 C20 121.9(5) . . ?
C30 N6 C26 121.8(4) . . ?
C25 N6 C26 115.5(4) . . ?
C25 N6 C30 122.7(4) . . ?
N5 C32 P12 117.6(4) . . ?
N5 C32 C33 117.0(4) . . ?
C33 C32 P12 125.4(4) . . ?
N6 C26 P10 117.3(3) . . ?
N6 C26 C27 116.7(4) . . ?
C27 C26 P10 125.9(4) . . ?
N5 C31 P11 119.0(3) . . ?
O6 C31 P11 125.0(4) . . ?
O6 C31 N5 116.0(4) . . ?
C30 C29 H29 119.8 . . ?
C30 C29 C28 120.4(5) . . ?
C28 C29 H29 119.8 . . ?
C32 N5 C36 121.2(4) . . ?
C31 N5 C36 122.9(4) . . ?
C31 N5 C32 115.8(4) . . ?
N6 C30 H30 120.0 . . ?
C29 C30 N6 119.9(5) . . ?
C29 C30 H30 120.0 . . ?
O5 C25 P9 125.5(3) . . ?
O5 C25 N6 115.2(4) . . ?
N6 C25 P9 119.3(3) . . ?
N4 C24 H24 119.9 . . ?
C23 C24 N4 120.1(4) . . ?
C23 C24 H24 119.9 . . ?
Ti2 C43 H43 119.6 . . ?
C44 C43 Ti2 72.8(3) . . ?
C44 C43 H43 126.4 . . ?
C42 C43 Ti2 73.1(3) . . ?
C42 C43 H43 126.4 . . ?
C42 C43 C44 107.1(6) . . ?
C32 C33 H33 119.1 . . ?
C34 C33 C32 121.8(5) . . ?
C34 C33 H33 119.1 . . ?
N4 C20 P8 118.0(4) . . ?
N4 C20 C21 116.8(5) . . ?
C21 C20 P8 125.3(4) . . ?
C26 C27 H27 119.2 . . ?
C28 C27 C26 121.6(5) . . ?
C28 C27 H27 119.2 . . ?
C36 C35 H35 119.8 . . ?
C36 C35 C34 120.3(5) . . ?
C34 C35 H35 119.8 . . ?
Ti2 C44 H44 120.5 . . ?
C43 C44 Ti2 72.0(3) . . ?
C43 C44 H44 126.3 . . ?
C45 C44 Ti2 73.1(4) . . ?
C45 C44 C43 107.4(6) . . ?
C45 C44 H44 126.3 . . ?
C29 C28 H28 120.2 . . ?
C27 C28 C29 119.5(5) . . ?
C27 C28 H28 120.2 . . ?
Ti2 C45 H45 120.3 . . ?
C44 C45 Ti2 72.6(4) . . ?
C44 C45 H45 125.6 . . ?
C44 C45 C46 108.7(6) . . ?
C46 C45 Ti2 73.2(4) . . ?
C46 C45 H45 125.6 . . ?
O4 C19 P7 125.1(4) . . ?
O4 C19 N4 116.1(4) . . ?
N4 C19 P7 118.8(3) . . ?
C33 C34 C35 119.5(5) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C24 C23 H23 119.7 . . ?
C24 C23 C22 120.6(5) . . ?
C22 C23 H23 119.7 . . ?
C21 C22 C23 119.3(5) . . ?
C21 C22 H22 120.4 . . ?
C23 C22 H22 120.4 . . ?
Ti2 C42 H42 120.6 . . ?
C43 C42 Ti2 72.0(3) . . ?
C43 C42 H42 125.7 . . ?
C46 C42 Ti2 73.5(3) . . ?
C46 C42 C43 108.6(5) . . ?
C46 C42 H42 125.7 . . ?
Ti2 C46 H46 120.9 . . ?
C45 C46 Ti2 72.3(3) . . ?
C45 C46 H46 125.9 . . ?
C42 C46 Ti2 72.6(3) . . ?
C42 C46 C45 108.1(6) . . ?
C42 C46 H46 125.9 . . ?
O2 Ti1 O3 102.51(15) . . ?
O2 Ti1 C37 136.85(18) . . ?
O2 Ti1 C38 101.85(19) . . ?
O2 Ti1 C41 140.93(17) . . ?
O2 Ti1 C39 86.25(17) . . ?
O2 Ti1 C40 106.37(18) . . ?
O3 Ti1 C37 116.92(19) . . ?
O3 Ti1 C38 145.48(19) . . ?
O3 Ti1 C41 88.02(17) . . ?
O3 Ti1 C39 124.3(2) . . ?
O3 Ti1 C40 91.84(18) . . ?
C37 Ti1 C39 57.9(2) . . ?
C38 Ti1 C37 35.0(2) . . ?
C38 Ti1 C41 57.8(2) . . ?
C38 Ti1 C39 34.5(2) . . ?
C41 Ti1 C37 34.73(18) . . ?
C41 Ti1 C39 57.8(2) . . ?
C40 Ti1 C37 58.07(19) . . ?
C40 Ti1 C38 57.8(2) . . ?
C40 Ti1 C41 34.99(19) . . ?
C40 Ti1 C39 34.7(2) . . ?
O1 Ti1 O2 101.68(15) . . ?
O1 Ti1 O3 102.91(14) . . ?
O1 Ti1 C37 86.59(17) . . ?
O1 Ti1 C38 95.67(19) . . ?
O1 Ti1 C41 112.57(18) . . ?
O1 Ti1 C39 129.3(2) . . ?
O1 Ti1 C40 144.54(18) . . ?
C2 P2 P1 93.74(16) . . ?
C13 P5 P6 93.94(18) . . ?
C14 P6 P5 94.19(17) . . ?
C1 P1 P2 93.82(16) . . ?
C7 P3 P4 93.95(17) . . ?
C8 P4 P3 93.99(17) . . ?
C7 O2 Ti1 148.5(3) . . ?
C13 O3 Ti1 143.6(3) . . ?
C12 N2 C8 121.1(4) . . ?
C7 N2 C12 123.0(4) . . ?
C7 N2 C8 115.9(4) . . ?
C1 N1 C6 123.1(4) . . ?
C1 N1 C2 115.8(4) . . ?
C6 N1 C2 121.1(4) . . ?
N1 C1 P1 118.8(3) . . ?
O1 C1 P1 125.8(3) . . ?
O1 C1 N1 115.4(4) . . ?
N2 C12 H12 120.0 . . ?
C11 C12 N2 120.0(4) . . ?
C11 C12 H12 120.0 . . ?
C10 C9 H9 118.9 . . ?
C10 C9 C8 122.2(5) . . ?
C8 C9 H9 118.9 . . ?
C14 N3 C18 121.4(4) . . ?
C13 N3 C14 116.0(4) . . ?
C13 N3 C18 122.6(4) . . ?
O2 C7 P3 125.8(4) . . ?
O2 C7 N2 115.3(4) . . ?
N2 C7 P3 119.0(3) . . ?
C4 C3 H3 118.6 . . ?
C4 C3 C2 122.9(5) . . ?
C2 C3 H3 118.6 . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C6 C5 C4 120.2(5) . . ?
Ti1 C37 H37 120.9 . . ?
C38 C37 Ti1 72.2(3) . . ?
C38 C37 H37 126.3 . . ?
C41 C37 Ti1 72.4(3) . . ?
C41 C37 H37 126.3 . . ?
C41 C37 C38 107.4(5) . . ?
C9 C10 H10 120.8 . . ?
C9 C10 C11 118.5(5) . . ?
C11 C10 H10 120.8 . . ?
C3 C4 C5 118.8(5) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C15 C16 C17 119.1(5) . . ?
N1 C6 H6 119.7 . . ?
C5 C6 N1 120.6(5) . . ?
C5 C6 H6 119.7 . . ?
N3 C14 P6 117.4(4) . . ?
N3 C14 C15 115.8(5) . . ?
C15 C14 P6 126.8(4) . . ?
Ti1 C38 H38 120.1 . . ?
C37 C38 Ti1 72.8(3) . . ?
C37 C38 H38 125.8 . . ?
C39 C38 Ti1 73.1(3) . . ?
C39 C38 C37 108.3(5) . . ?
C39 C38 H38 125.8 . . ?
Ti1 C41 H41 121.2 . . ?
C37 C41 Ti1 72.8(3) . . ?
C37 C41 H41 126.0 . . ?
C37 C41 C40 107.9(5) . . ?
C40 C41 Ti1 71.7(3) . . ?
C40 C41 H41 126.0 . . ?
O3 C13 P5 125.8(4) . . ?
O3 C13 N3 115.8(4) . . ?
N3 C13 P5 118.4(3) . . ?
N2 C8 P4 117.2(4) . . ?
N2 C8 C9 117.4(5) . . ?
C9 C8 P4 125.3(4) . . ?
C56 C55 C60 118.1(7) . . ?
C56 C55 C54 120.8(7) . . ?
C60 C55 C54 121.0(7) . . ?
N3 C18 H18 120.0 . . ?
C17 C18 N3 120.0(5) . . ?
C17 C18 H18 120.0 . . ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.2(5) . . ?
C18 C17 H17 119.9 . . ?
C55 C56 H56 122.0 . . ?
C57 C56 C55 115.9(6) . . ?
C57 C56 H56 122.0 . . ?
N1 C2 P2 117.8(3) . . ?
N1 C2 C3 116.3(4) . . ?
C3 C2 P2 125.9(4) . . ?
C16 C15 C14 123.4(5) . . ?
C16 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
C56 C57 H57 117.7 . . ?
C58 C57 C56 124.5(7) . . ?
C58 C57 H57 117.7 . . ?
C12 C11 C10 120.7(5) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
Ti1 C39 H39 121.8 . . ?
C38 C39 Ti1 72.4(3) . . ?
C38 C39 H39 126.0 . . ?
C38 C39 C40 108.0(5) . . ?
C40 C39 Ti1 71.5(3) . . ?
C40 C39 H39 126.0 . . ?
C58 C59 H59 115.2 . . ?
C58 C59 C60 129.6(10) . . ?
C60 C59 H59 115.2 . . ?
Ti1 C40 H40 118.9 . . ?
C41 C40 Ti1 73.3(3) . . ?
C41 C40 H40 125.8 . . ?
C39 C40 Ti1 73.7(3) . . ?
C39 C40 C41 108.3(5) . . ?
C39 C40 H40 125.8 . . ?
C57 C58 H58 122.1 . . ?
C59 C58 C57 115.8(9) . . ?
C59 C58 H58 122.1 . . ?
C55 C60 H60 122.0 . . ?
C59 C60 C55 115.9(8) . . ?
C59 C60 H60 122.0 . . ?
C55 C54 H54A 109.5 . . ?
C55 C54 H54B 109.5 . . ?
C55 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C51 C52 H52 119.1 . . ?
C53 C52 H52 119.1 . . ?
C53 C52 C51 121.7(8) . . ?
C49 C50 H50 120.8 . . ?
C51 C50 H50 120.8 . . ?
C51 C50 C49 118.5(8) . . ?
C50 C49 H49 119.0 . . ?
C50 C49 C48 122.1(7) . . ?
C48 C49 H49 119.0 . . ?
C49 C48 C47 122.6(8) . . ?
C49 C48 C53 118.3(8) . . ?
C53 C48 C47 119.0(9) . . ?
C48 C47 H47A 109.5 . . ?
C48 C47 H47B 109.5 . . ?
C48 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C52 C51 H51 119.8 . . ?
C50 C51 C52 120.5(9) . . ?
C50 C51 H51 119.8 . . ?
C52 C53 C48 119.0(8) . . ?
C52 C53 H53 120.5 . . ?
C48 C53 H53 120.5 . . ?
C1 O1 Ti1 148.1(3) . . ?
C31 O6 Ti2 145.0(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
Ti2 O4 C19 P7 84.5(7) . . . . ?
Ti2 O4 C19 N4 -97.6(6) . . . . ?
Ti2 O5 C25 P9 85.4(8) . . . . ?
Ti2 O5 C25 N6 -96.2(7) . . . . ?
Ti2 C43 C44 C45 65.0(4) . . . . ?
Ti2 C43 C42 C46 -64.8(4) . . . . ?
Ti2 C44 C45 C46 64.8(4) . . . . ?
Ti2 C45 C46 C42 64.2(4) . . . . ?
Ti2 C42 C46 C45 -64.1(4) . . . . ?
P8 P7 C19 O4 178.1(4) . . . . ?
P8 P7 C19 N4 0.3(4) . . . . ?
P10 P9 C25 O5 178.2(4) . . . . ?
P10 P9 C25 N6 -0.2(4) . . . . ?
P10 C26 C27 C28 -178.5(4) . . . . ?
P9 P10 C26 N6 0.2(4) . . . . ?
P9 P10 C26 C27 -179.1(4) . . . . ?
P12 P11 C31 N5 1.3(4) . . . . ?
P12 P11 C31 O6 -176.5(4) . . . . ?
P12 C32 N5 C36 -178.7(3) . . . . ?
P12 C32 N5 C31 0.5(6) . . . . ?
P12 C32 C33 C34 179.4(4) . . . . ?
P11 P12 C32 N5 0.3(4) . . . . ?
P11 P12 C32 C33 -178.8(4) . . . . ?
P11 C31 N5 C36 177.9(3) . . . . ?
P11 C31 N5 C32 -1.3(6) . . . . ?
P11 C31 O6 Ti2 91.6(6) . . . . ?
P7 P8 C20 N4 -0.1(4) . . . . ?
P7 P8 C20 C21 -178.2(4) . . . . ?
O4 Ti2 O5 C25 -137.7(7) . . . . ?
O4 Ti2 O6 C31 116.8(5) . . . . ?
N4 C24 C23 C22 0.2(7) . . . . ?
C36 C35 C34 C33 0.4(8) . . . . ?
O5 Ti2 O4 C19 120.7(6) . . . . ?
O5 Ti2 O6 C31 -138.5(5) . . . . ?
N6 C26 C27 C28 2.2(7) . . . . ?
C32 C33 C34 C35 -0.8(8) . . . . ?
C26 N6 C30 C29 0.7(7) . . . . ?
C26 N6 C25 P9 0.3(6) . . . . ?
C26 N6 C25 O5 -178.2(4) . . . . ?
C26 C27 C28 C29 -0.1(7) . . . . ?
N5 C36 C35 C34 0.4(7) . . . . ?
N5 C32 C33 C34 0.3(7) . . . . ?
N5 C31 O6 Ti2 -86.3(6) . . . . ?
C30 N6 C26 P10 178.1(3) . . . . ?
C30 N6 C26 C27 -2.5(6) . . . . ?
C30 N6 C25 P9 -178.1(4) . . . . ?
C30 N6 C25 O5 3.3(6) . . . . ?
C30 C29 C28 C27 -1.9(7) . . . . ?
C25 N6 C26 P10 -0.3(5) . . . . ?
C25 N6 C26 C27 179.0(4) . . . . ?
C25 N6 C30 C29 179.0(4) . . . . ?
C24 N4 C20 P8 -179.7(3) . . . . ?
C24 N4 C20 C21 -1.5(6) . . . . ?
C24 N4 C19 P7 179.6(3) . . . . ?
C24 N4 C19 O4 1.6(6) . . . . ?
C24 C23 C22 C21 -0.7(8) . . . . ?
C43 Ti2 O4 C19 16.9(7) . . . . ?
C43 Ti2 O5 C25 -38.4(7) . . . . ?
C43 Ti2 O6 C31 -3.7(7) . . . . ?
C43 C44 C45 Ti2 -64.3(4) . . . . ?
C43 C44 C45 C46 0.5(7) . . . . ?
C43 C42 C46 Ti2 63.8(4) . . . . ?
C43 C42 C46 C45 -0.2(7) . . . . ?
C33 C32 N5 C36 0.5(7) . . . . ?
C33 C32 N5 C31 179.7(4) . . . . ?
C20 N4 C24 C23 0.9(7) . . . . ?
C20 N4 C19 P7 -0.5(5) . . . . ?
C20 N4 C19 O4 -178.5(4) . . . . ?
C20 C21 C22 C23 0.0(8) . . . . ?
C35 C36 N5 C32 -0.9(7) . . . . ?
C35 C36 N5 C31 180.0(4) . . . . ?
C44 Ti2 O4 C19 25.4(7) . . . . ?
C44 Ti2 O5 C25 -6.6(7) . . . . ?
C44 Ti2 O6 C31 -44.4(6) . . . . ?
C44 C43 C42 Ti2 65.3(4) . . . . ?
C44 C43 C42 C46 0.5(7) . . . . ?
C44 C45 C46 Ti2 -64.4(4) . . . . ?
C44 C45 C46 C42 -0.2(7) . . . . ?
C28 C29 C30 N6 1.6(7) . . . . ?
C45 Ti2 O4 C19 -22.8(8) . . . . ?
C45 Ti2 O5 C25 21.1(7) . . . . ?
C45 Ti2 O6 C31 -30.5(6) . . . . ?
C19 N4 C24 C23 -179.1(4) . . . . ?
C19 N4 C20 P8 0.4(5) . . . . ?
C19 N4 C20 C21 178.6(4) . . . . ?
C22 C21 C20 P8 179.1(4) . . . . ?
C22 C21 C20 N4 1.0(7) . . . . ?
C42 Ti2 O4 C19 -16.9(6) . . . . ?
C42 Ti2 O5 C25 -38.5(8) . . . . ?
C42 Ti2 O6 C31 23.4(6) . . . . ?
C42 C43 C44 Ti2 -65.6(4) . . . . ?
C42 C43 C44 C45 -0.6(7) . . . . ?
C46 Ti2 O4 C19 -40.5(7) . . . . ?
C46 Ti2 O5 C25 13.9(8) . . . . ?
C46 Ti2 O6 C31 3.8(6) . . . . ?
Ti1 O2 C7 P3 -92.5(6) . . . . ?
Ti1 O2 C7 N2 87.8(6) . . . . ?
Ti1 O3 C13 P5 -95.6(6) . . . . ?
Ti1 O3 C13 N3 84.4(6) . . . . ?
Ti1 C37 C38 C39 64.9(4) . . . . ?
Ti1 C37 C41 C40 -63.5(4) . . . . ?
Ti1 C38 C39 C40 63.1(4) . . . . ?
Ti1 C41 C40 C39 -66.0(4) . . . . ?
Ti1 C39 C40 C41 65.7(4) . . . . ?
P2 P1 C1 N1 -0.3(4) . . . . ?
P2 P1 C1 O1 179.9(4) . . . . ?
P5 P6 C14 N3 0.8(4) . . . . ?
P5 P6 C14 C15 180.0(4) . . . . ?
P6 P5 C13 O3 177.8(4) . . . . ?
P6 P5 C13 N3 -2.2(4) . . . . ?
P6 C14 C15 C16 179.8(4) . . . . ?
P1 P2 C2 N1 -0.9(3) . . . . ?
P1 P2 C2 C3 178.9(4) . . . . ?
P1 C1 O1 Ti1 -90.0(6) . . . . ?
P3 P4 C8 N2 0.6(4) . . . . ?
P3 P4 C8 C9 179.6(4) . . . . ?
P4 P3 C7 O2 -179.2(4) . . . . ?
P4 P3 C7 N2 0.5(4) . . . . ?
O2 Ti1 O3 C13 -114.0(5) . . . . ?
O2 Ti1 O1 C1 146.9(5) . . . . ?
O3 Ti1 O2 C7 138.7(6) . . . . ?
O3 Ti1 O1 C1 -107.2(5) . . . . ?
N2 C12 C11 C10 0.4(7) . . . . ?
N1 C1 O1 Ti1 90.2(6) . . . . ?
C1 N1 C6 C5 179.7(4) . . . . ?
C1 N1 C2 P2 0.8(5) . . . . ?
C1 N1 C2 C3 -179.0(4) . . . . ?
C12 N2 C7 P3 -179.6(3) . . . . ?
C12 N2 C7 O2 0.1(6) . . . . ?
C12 N2 C8 P4 179.0(3) . . . . ?
C12 N2 C8 C9 -0.1(7) . . . . ?
C9 C10 C11 C12 -0.2(8) . . . . ?
N3 C14 C15 C16 -1.1(7) . . . . ?
N3 C18 C17 C16 -0.3(7) . . . . ?
C7 N2 C12 C11 179.0(5) . . . . ?
C7 N2 C8 P4 -0.3(6) . . . . ?
C7 N2 C8 C9 -179.4(4) . . . . ?
C37 Ti1 O2 C7 -17.5(7) . . . . ?
C37 Ti1 O3 C13 48.0(6) . . . . ?
C37 Ti1 O1 C1 9.6(6) . . . . ?
C37 C38 C39 Ti1 -64.7(4) . . . . ?
C37 C38 C39 C40 -1.6(6) . . . . ?
C37 C41 C40 Ti1 64.3(4) . . . . ?
C37 C41 C40 C39 -1.7(6) . . . . ?
C10 C9 C8 P4 -178.8(4) . . . . ?
C10 C9 C8 N2 0.3(8) . . . . ?
C4 C3 C2 P2 178.8(4) . . . . ?
C4 C3 C2 N1 -1.5(7) . . . . ?
C4 C5 C6 N1 -0.1(7) . . . . ?
C6 N1 C1 P1 179.3(3) . . . . ?
C6 N1 C1 O1 -0.9(6) . . . . ?
C6 N1 C2 P2 -178.7(3) . . . . ?
C6 N1 C2 C3 1.5(6) . . . . ?
C6 C5 C4 C3 0.1(8) . . . . ?
C14 N3 C13 P5 3.2(6) . . . . ?
C14 N3 C13 O3 -176.8(4) . . . . ?
C14 N3 C18 C17 1.6(7) . . . . ?
C38 Ti1 O2 C7 -16.6(6) . . . . ?
C38 Ti1 O3 C13 20.0(7) . . . . ?
C38 Ti1 O1 C1 43.5(6) . . . . ?
C38 C37 C41 Ti1 64.2(4) . . . . ?
C38 C37 C41 C40 0.7(6) . . . . ?
C38 C39 C40 Ti1 -63.6(4) . . . . ?
C38 C39 C40 C41 2.1(6) . . . . ?
C41 Ti1 O2 C7 36.2(7) . . . . ?
C41 Ti1 O3 C13 28.0(5) . . . . ?
C41 Ti1 O1 C1 -14.0(6) . . . . ?
C41 C37 C38 Ti1 -64.4(4) . . . . ?
C41 C37 C38 C39 0.6(6) . . . . ?
C13 N3 C14 P6 -2.5(6) . . . . ?
C13 N3 C14 C15 178.3(4) . . . . ?
C13 N3 C18 C17 -177.5(4) . . . . ?
C8 N2 C12 C11 -0.3(7) . . . . ?
C8 N2 C7 P3 -0.2(6) . . . . ?
C8 N2 C7 O2 179.5(4) . . . . ?
C8 C9 C10 C11 -0.1(8) . . . . ?
C55 C56 C57 C58 -1.7(9) . . . . ?
C18 N3 C14 P6 178.3(3) . . . . ?
C18 N3 C14 C15 -0.9(6) . . . . ?
C18 N3 C13 P5 -177.6(3) . . . . ?
C18 N3 C13 O3 2.4(6) . . . . ?
C17 C16 C15 C14 2.3(8) . . . . ?
C56 C55 C60 C59 -1.3(10) . . . . ?
C56 C57 C58 C59 -0.8(11) . . . . ?
C2 N1 C1 P1 -0.2(5) . . . . ?
C2 N1 C1 O1 179.5(4) . . . . ?
C2 N1 C6 C5 -0.8(7) . . . . ?
C2 C3 C4 C5 0.7(8) . . . . ?
C15 C16 C17 C18 -1.6(8) . . . . ?
C39 Ti1 O2 C7 14.4(6) . . . . ?
C39 Ti1 O3 C13 -19.9(6) . . . . ?
C39 Ti1 O1 C1 52.1(6) . . . . ?
C40 Ti1 O2 C7 43.0(6) . . . . ?
C40 Ti1 O3 C13 -6.7(6) . . . . ?
C40 Ti1 O1 C1 5.0(7) . . . . ?
C58 C59 C60 C55 -1.5(12) . . . . ?
C60 C55 C56 C57 2.6(9) . . . . ?
C60 C59 C58 C57 2.6(13) . . . . ?
C54 C55 C56 C57 -175.1(7) . . . . ?
C54 C55 C60 C59 176.4(7) . . . . ?
C50 C49 C48 C47 179.7(7) . . . . ?
C50 C49 C48 C53 1.6(11) . . . . ?
C49 C50 C51 C52 0.6(11) . . . . ?
C49 C48 C53 C52 -0.2(10) . . . . ?
C47 C48 C53 C52 -178.3(7) . . . . ?
C51 C52 C53 C48 -1.0(11) . . . . ?
C51 C50 C49 C48 -1.8(11) . . . . ?
C53 C52 C51 C50 0.8(11) . . . . ?
O1 Ti1 O2 C7 -115.0(6) . . . . ?
O1 Ti1 O3 C13 140.8(5) . . . . ?
O6 Ti2 O4 C19 -133.9(6) . . . . ?
O6 Ti2 O5 C25 117.5(7) . . . . ?
O6 C31 N5 C36 -4.1(6) . . . . ?
O6 C31 N5 C32 176.7(4) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2013-10-01
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_rs3023_green
_database_code_depnum_ccdc_archive 'CCDC 1494802'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_audit_creation_date             2016-07-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C23 H17 N3 O3 P6 Ti, C H2 Cl2'
_chemical_formula_sum            'C24 H19 Cl2 N3 O3 P6 Ti'
_chemical_formula_weight         702.04
_chemical_melting_point          ?
_chemical_oxdiff_formula         'P8 O4 N4 Ti Na O10 C40 H40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.4263(3)
_cell_length_b                   15.2635(8)
_cell_length_c                   26.3095(15)
_cell_angle_alpha                90
_cell_angle_beta                 92.364(4)
_cell_angle_gamma                90
_cell_volume                     2979.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6302
_cell_measurement_temperature    104.6(2)
_cell_measurement_theta_max      34.5700
_cell_measurement_theta_min      3.0720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            26042
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         34.885
_diffrn_reflns_theta_min         3.053
_diffrn_ambient_temperature      104.6(2)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -46.00   31.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.6391   38.0000 -120.0000 77

#__ type_ start__ end____ width___ exp.time_
  2 omega  -93.00  -34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.6391 -179.0000 -150.0000 59

#__ type_ start__ end____ width___ exp.time_
  3 omega   66.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1078 -158.0000   85.0000 42

#__ type_ start__ end____ width___ exp.time_
  4 omega   81.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1078  179.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
  5 omega   27.00  101.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1078   57.0000   90.0000 74

#__ type_ start__ end____ width___ exp.time_
  6 omega   12.00   47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1078   57.0000  -90.0000 35
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_UB_11      0.0033192000
_diffrn_orient_matrix_UB_12      0.0454254000
_diffrn_orient_matrix_UB_13      -0.0055608000
_diffrn_orient_matrix_UB_21      -0.0084453000
_diffrn_orient_matrix_UB_22      0.0098270000
_diffrn_orient_matrix_UB_23      0.0261292000
_diffrn_orient_matrix_UB_31      0.0952091000
_diffrn_orient_matrix_UB_32      -0.0007111000
_diffrn_orient_matrix_UB_33      0.0036640000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8888
_reflns_number_total             12040
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.327
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         12040
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0671
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0911P)²+0.9700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.1938
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C18(H18), C11(H11), C6(H6), C15(H15), C17(H17), C16(H16), C9(H9),
 C10(H10), C5(H5), C23(H23), C22(H22), C3(H3), C4(H4), C21(H21), C20(H20),
 C19(H19)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti01 Ti 0.36367(6) 0.33841(3) 0.60584(2) 0.01365(10) Uani 1 1 d . . . . .
P5 P 0.17376(9) 0.18409(5) 0.48370(3) 0.01930(15) Uani 1 1 d . . . . .
P6 P 0.25293(10) 0.16827(5) 0.40798(3) 0.02055(15) Uani 1 1 d . . . . .
P3 P 0.70609(10) 0.56257(5) 0.60277(3) 0.02107(15) Uani 1 1 d . . . . .
P4 P 0.84072(9) 0.62436(5) 0.66570(3) 0.02160(16) Uani 1 1 d . . . . .
P1 P 0.23395(11) 0.23359(5) 0.74910(3) 0.02529(17) Uani 1 1 d . . . . .
Cl2 Cl 0.65260(11) 0.07663(6) 0.52833(4) 0.0366(2) Uani 1 1 d . . . . .
P2 P 0.11866(11) 0.11040(6) 0.76588(4) 0.03053(19) Uani 1 1 d . . . . .
Cl1 Cl 0.79357(14) 0.15788(7) 0.62212(5) 0.0533(3) Uani 1 1 d . . . . .
O1 O 0.3752(2) 0.25344(12) 0.65579(8) 0.0188(4) Uani 1 1 d . . . . .
O2 O 0.5809(2) 0.39602(12) 0.61703(8) 0.0179(4) Uani 1 1 d . . . . .
O3 O 0.4049(2) 0.27349(13) 0.54862(7) 0.0188(4) Uani 1 1 d . . . . .
N3 N 0.4934(3) 0.25740(13) 0.46702(8) 0.0133(4) Uani 1 1 d . . . . .
N2 N 0.7336(3) 0.45925(13) 0.68527(8) 0.0139(4) Uani 1 1 d . . . . .
N1 N 0.2538(3) 0.11830(14) 0.67248(9) 0.0167(4) Uani 1 1 d . . . . .
C13 C 0.3655(3) 0.24266(16) 0.50216(10) 0.0143(4) Uani 1 1 d . . . . .
C12 C 0.7166(3) 0.38339(17) 0.71403(11) 0.0181(5) Uani 1 1 d . . . . .
H12 H 0.6592 0.3346 0.6998 0.022 Uiso 1 1 calc R . . . .
C1 C 0.2925(3) 0.20288(17) 0.68885(10) 0.0167(4) Uani 1 1 d . . . . .
C7 C 0.6686(3) 0.46593(16) 0.63553(10) 0.0160(4) Uani 1 1 d . . . . .
C8 C 0.8220(3) 0.53335(16) 0.70501(11) 0.0168(5) Uani 1 1 d . . . . .
C14 C 0.4566(3) 0.22347(16) 0.41858(10) 0.0148(4) Uani 1 1 d . . . . .
C18 C 0.6527(3) 0.30286(16) 0.47871(11) 0.0181(5) Uani 1 1 d . . . . .
H18 H 0.6747 0.3249 0.5113 0.022 Uiso 1 1 calc R . . . .
C11 C 0.7835(4) 0.38030(19) 0.76268(11) 0.0226(5) Uani 1 1 d . . . . .
H11 H 0.7731 0.3291 0.7815 0.027 Uiso 1 1 calc R . . . .
C6 C 0.3003(4) 0.08713(18) 0.62536(12) 0.0217(5) Uani 1 1 d . . . . .
H6 H 0.3602 0.1235 0.6033 0.026 Uiso 1 1 calc R . . . .
C15 C 0.5862(4) 0.23813(19) 0.38179(11) 0.0217(5) Uani 1 1 d . . . . .
H15 H 0.5643 0.2172 0.3489 0.026 Uiso 1 1 calc R . . . .
C17 C 0.7747(3) 0.31500(18) 0.44302(12) 0.0228(6) Uani 1 1 d . . . . .
H17 H 0.8809 0.3451 0.4511 0.027 Uiso 1 1 calc R . . . .
C16 C 0.7420(4) 0.28199(19) 0.39300(12) 0.0240(6) Uani 1 1 d . . . . .
H16 H 0.8263 0.2903 0.3682 0.029 Uiso 1 1 calc R . . . .
C9 C 0.8869(4) 0.52897(19) 0.75657(12) 0.0228(5) Uani 1 1 d . . . . .
H9 H 0.9429 0.5778 0.7713 0.027 Uiso 1 1 calc R . . . .
C2 C 0.1662(3) 0.06523(19) 0.70725(13) 0.0231(6) Uani 1 1 d . . . . .
C10 C 0.8694(4) 0.4551(2) 0.78503(12) 0.0258(6) Uani 1 1 d . . . . .
H10 H 0.9131 0.4536 0.8187 0.031 Uiso 1 1 calc R . . . .
C5 C 0.2587(4) 0.0039(2) 0.61132(15) 0.0318(7) Uani 1 1 d . . . . .
H5 H 0.2909 -0.0170 0.5798 0.038 Uiso 1 1 calc R . . . .
C23 C 0.0675(4) 0.3628(2) 0.57509(14) 0.0332(8) Uani 1 1 d . . . . .
H23 H 0.0111 0.3241 0.5522 0.040 Uiso 1 1 calc R . . . .
C22 C 0.0637(4) 0.3588(2) 0.62747(14) 0.0296(7) Uani 1 1 d . . . . .
H22 H 0.0042 0.3166 0.6459 0.036 Uiso 1 1 calc R . . . .
C3 C 0.1222(4) -0.0213(2) 0.69144(16) 0.0340(8) Uani 1 1 d . . . . .
H3 H 0.0623 -0.0579 0.7134 0.041 Uiso 1 1 calc R . . . .
C24 C 0.8270(4) 0.0772(2) 0.57561(15) 0.0326(7) Uani 1 1 d . . . . .
H24A H 0.9409 0.0879 0.5599 0.039 Uiso 1 1 calc R . . . .
H24B H 0.8338 0.0201 0.5918 0.039 Uiso 1 1 calc R . . . .
C4 C 0.1653(4) -0.0518(2) 0.64517(17) 0.0363(9) Uani 1 1 d . . . . .
H4 H 0.1343 -0.1086 0.6355 0.044 Uiso 1 1 calc R . . . .
C21 C 0.1627(4) 0.4280(2) 0.64796(15) 0.0350(8) Uani 1 1 d . . . . .
H21 H 0.1813 0.4396 0.6825 0.042 Uiso 1 1 calc R . . . .
C20 C 0.2289(4) 0.4765(2) 0.60906(18) 0.0400(10) Uani 1 1 d . . . . .
H20 H 0.2984 0.5270 0.6127 0.048 Uiso 1 1 calc R . . . .
C19 C 0.1733(5) 0.4368(3) 0.56232(16) 0.0428(10) Uani 1 1 d . . . . .
H19 H 0.2005 0.4554 0.5299 0.051 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti01 O1 1.8459(19) . ?
Ti01 O2 1.8503(18) . ?
Ti01 O3 1.839(2) . ?
Ti01 C23 2.342(3) . ?
Ti01 C22 2.343(3) . ?
Ti01 C21 2.337(3) . ?
Ti01 C20 2.337(3) . ?
Ti01 C19 2.330(3) . ?
P5 P6 2.1141(11) . ?
P5 C13 1.734(2) . ?
P6 C14 1.744(3) . ?
P3 P4 2.1199(11) . ?
P3 C7 1.737(3) . ?
P4 C8 1.741(3) . ?
P1 P2 2.1201(12) . ?
P1 C1 1.726(3) . ?
Cl2 C24 1.758(3) . ?
P2 C2 1.739(3) . ?
Cl1 C24 1.761(4) . ?
O1 C1 1.332(3) . ?
O2 C7 1.332(3) . ?
O3 C13 1.331(3) . ?
N3 C13 1.371(3) . ?
N3 C14 1.392(3) . ?
N3 C18 1.395(3) . ?
N2 C12 1.392(3) . ?
N2 C7 1.380(3) . ?
N2 C8 1.397(3) . ?
N1 C1 1.387(3) . ?
N1 C6 1.385(4) . ?
N1 C2 1.402(4) . ?
C12 H12 0.9300 . ?
C12 C11 1.354(4) . ?
C8 C9 1.422(4) . ?
C14 C15 1.411(4) . ?
C18 H18 0.9300 . ?
C18 C17 1.344(4) . ?
C11 H11 0.9300 . ?
C11 C10 1.423(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.355(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.359(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.421(5) . ?
C16 H16 0.9300 . ?
C9 H9 0.9300 . ?
C9 C10 1.363(4) . ?
C2 C3 1.418(4) . ?
C10 H10 0.9300 . ?
C5 H5 0.9300 . ?
C5 C4 1.431(5) . ?
C23 H23 0.9300 . ?
C23 C22 1.381(5) . ?
C23 C19 1.424(5) . ?
C22 H22 0.9300 . ?
C22 C21 1.383(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.354(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C4 H4 0.9300 . ?
C21 H21 0.9300 . ?
C21 C20 1.371(6) . ?
C20 H20 0.9300 . ?
C20 C19 1.417(6) . ?
C19 H19 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
O1 Ti01 O2 101.89(9) . . ?
O1 Ti01 C23 111.91(12) . . ?
O1 Ti01 C22 86.40(11) . . ?
O1 Ti01 C21 94.89(12) . . ?
O1 Ti01 C20 127.99(13) . . ?
O1 Ti01 C19 144.30(11) . . ?
O2 Ti01 C23 141.25(11) . . ?
O2 Ti01 C22 136.88(10) . . ?
O2 Ti01 C21 102.50(11) . . ?
O2 Ti01 C20 86.42(10) . . ?
O2 Ti01 C19 106.21(13) . . ?
O3 Ti01 O1 101.52(9) . . ?
O3 Ti01 O2 102.29(9) . . ?
O3 Ti01 C23 89.34(10) . . ?
O3 Ti01 C22 117.56(11) . . ?
O3 Ti01 C21 146.60(11) . . ?
O3 Ti01 C20 127.02(13) . . ?
O3 Ti01 C19 93.63(12) . . ?
C23 Ti01 C22 34.29(13) . . ?
C21 Ti01 C23 57.43(12) . . ?
C21 Ti01 C22 34.38(12) . . ?
C20 Ti01 C23 58.09(12) . . ?
C20 Ti01 C22 57.19(12) . . ?
C20 Ti01 C21 34.12(14) . . ?
C19 Ti01 C23 35.50(14) . . ?
C19 Ti01 C22 58.00(13) . . ?
C19 Ti01 C21 57.97(14) . . ?
C19 Ti01 C20 35.34(15) . . ?
C13 P5 P6 93.77(9) . . ?
C14 P6 P5 93.86(9) . . ?
C7 P3 P4 94.03(9) . . ?
C8 P4 P3 93.57(9) . . ?
C1 P1 P2 93.99(10) . . ?
C2 P2 P1 93.92(10) . . ?
C1 O1 Ti01 149.64(17) . . ?
C7 O2 Ti01 148.09(17) . . ?
C13 O3 Ti01 154.78(17) . . ?
C13 N3 C14 116.2(2) . . ?
C13 N3 C18 122.5(2) . . ?
C14 N3 C18 121.3(2) . . ?
C12 N2 C8 121.5(2) . . ?
C7 N2 C12 122.8(2) . . ?
C7 N2 C8 115.7(2) . . ?
C1 N1 C2 115.5(2) . . ?
C6 N1 C1 122.8(2) . . ?
C6 N1 C2 121.7(2) . . ?
O3 C13 P5 125.92(19) . . ?
O3 C13 N3 115.4(2) . . ?
N3 C13 P5 118.66(19) . . ?
N2 C12 H12 119.8 . . ?
C11 C12 N2 120.3(2) . . ?
C11 C12 H12 119.8 . . ?
O1 C1 P1 125.7(2) . . ?
O1 C1 N1 115.6(2) . . ?
N1 C1 P1 118.8(2) . . ?
O2 C7 P3 125.8(2) . . ?
O2 C7 N2 115.7(2) . . ?
N2 C7 P3 118.46(18) . . ?
N2 C8 P4 118.2(2) . . ?
N2 C8 C9 116.9(2) . . ?
C9 C8 P4 124.9(2) . . ?
N3 C14 P6 117.53(18) . . ?
N3 C14 C15 117.1(2) . . ?
C15 C14 P6 125.4(2) . . ?
N3 C18 H18 119.9 . . ?
C17 C18 N3 120.3(3) . . ?
C17 C18 H18 119.9 . . ?
C12 C11 H11 119.9 . . ?
C12 C11 C10 120.2(3) . . ?
C10 C11 H11 119.9 . . ?
N1 C6 H6 119.9 . . ?
C5 C6 N1 120.3(3) . . ?
C5 C6 H6 119.9 . . ?
C14 C15 H15 119.1 . . ?
C16 C15 C14 121.9(3) . . ?
C16 C15 H15 119.1 . . ?
C18 C17 H17 119.9 . . ?
C18 C17 C16 120.3(3) . . ?
C16 C17 H17 119.9 . . ?
C15 C16 C17 119.1(3) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C8 C9 H9 119.1 . . ?
C10 C9 C8 121.8(3) . . ?
C10 C9 H9 119.1 . . ?
N1 C2 P2 117.8(2) . . ?
N1 C2 C3 117.0(3) . . ?
C3 C2 P2 125.2(3) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 C11 119.2(3) . . ?
C9 C10 H10 120.4 . . ?
C6 C5 H5 120.1 . . ?
C6 C5 C4 119.8(3) . . ?
C4 C5 H5 120.1 . . ?
Ti01 C23 H23 120.9 . . ?
C22 C23 Ti01 72.91(17) . . ?
C22 C23 H23 126.1 . . ?
C22 C23 C19 107.7(3) . . ?
C19 C23 Ti01 71.82(17) . . ?
C19 C23 H23 126.1 . . ?
Ti01 C22 H22 120.8 . . ?
C23 C22 Ti01 72.80(17) . . ?
C23 C22 H22 125.6 . . ?
C23 C22 C21 108.8(3) . . ?
C21 C22 Ti01 72.58(17) . . ?
C21 C22 H22 125.6 . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.6(3) . . ?
C4 C3 H3 119.2 . . ?
Cl2 C24 Cl1 111.97(17) . . ?
Cl2 C24 H24A 109.2 . . ?
Cl2 C24 H24B 109.2 . . ?
Cl1 C24 H24A 109.2 . . ?
Cl1 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C5 C4 H4 120.2 . . ?
C3 C4 C5 119.6(3) . . ?
C3 C4 H4 120.2 . . ?
Ti01 C21 H21 120.2 . . ?
C22 C21 Ti01 73.05(17) . . ?
C22 C21 H21 125.6 . . ?
C20 C21 Ti01 72.93(19) . . ?
C20 C21 C22 108.8(3) . . ?
C20 C21 H21 125.6 . . ?
Ti01 C20 H20 120.9 . . ?
C21 C20 Ti01 72.95(18) . . ?
C21 C20 H20 125.8 . . ?
C21 C20 C19 108.4(3) . . ?
C19 C20 Ti01 72.09(18) . . ?
C19 C20 H20 125.8 . . ?
Ti01 C19 H19 119.8 . . ?
C23 C19 Ti01 72.68(18) . . ?
C23 C19 H19 126.9 . . ?
C20 C19 Ti01 72.57(19) . . ?
C20 C19 C23 106.2(3) . . ?
C20 C19 H19 126.9 . . ?

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
Ti01 O1 C1 P1 -83.6(4) . . . . ?
Ti01 O1 C1 N1 97.2(4) . . . . ?
Ti01 O2 C7 P3 -87.9(4) . . . . ?
Ti01 O2 C7 N2 91.9(4) . . . . ?
Ti01 O3 C13 P5 -57.4(5) . . . . ?
Ti01 O3 C13 N3 124.7(4) . . . . ?
Ti01 C23 C22 C21 64.1(2) . . . . ?
Ti01 C23 C19 C20 -65.4(2) . . . . ?
Ti01 C22 C21 C20 64.6(2) . . . . ?
Ti01 C21 C20 C19 63.8(2) . . . . ?
Ti01 C20 C19 C23 65.4(2) . . . . ?
P5 P6 C14 N3 -1.37(19) . . . . ?
P5 P6 C14 C15 179.9(2) . . . . ?
P6 P5 C13 O3 -178.8(2) . . . . ?
P6 P5 C13 N3 -0.97(19) . . . . ?
P6 C14 C15 C16 179.9(2) . . . . ?
P3 P4 C8 N2 -0.85(19) . . . . ?
P3 P4 C8 C9 -179.5(2) . . . . ?
P4 P3 C7 O2 178.3(2) . . . . ?
P4 P3 C7 N2 -1.53(19) . . . . ?
P4 C8 C9 C10 -179.3(2) . . . . ?
P1 P2 C2 N1 -0.1(2) . . . . ?
P1 P2 C2 C3 -179.6(2) . . . . ?
P2 P1 C1 O1 180.0(2) . . . . ?
P2 P1 C1 N1 -0.82(19) . . . . ?
P2 C2 C3 C4 -179.5(2) . . . . ?
O1 Ti01 O2 C7 -103.4(3) . . . . ?
O1 Ti01 O3 C13 122.9(4) . . . . ?
O2 Ti01 O1 C1 147.4(4) . . . . ?
O2 Ti01 O3 C13 -132.1(4) . . . . ?
O3 Ti01 O1 C1 -107.3(4) . . . . ?
O3 Ti01 O2 C7 151.8(3) . . . . ?
N3 C14 C15 C16 1.2(4) . . . . ?
N3 C18 C17 C16 0.3(4) . . . . ?
N2 C12 C11 C10 0.9(4) . . . . ?
N2 C8 C9 C10 2.1(4) . . . . ?
N1 C6 C5 C4 0.5(4) . . . . ?
N1 C2 C3 C4 1.0(4) . . . . ?
C13 N3 C14 P6 1.0(3) . . . . ?
C13 N3 C14 C15 179.8(2) . . . . ?
C13 N3 C18 C17 179.5(2) . . . . ?
C12 N2 C7 P3 -177.39(18) . . . . ?
C12 N2 C7 O2 2.8(3) . . . . ?
C12 N2 C8 P4 178.61(18) . . . . ?
C12 N2 C8 C9 -2.7(3) . . . . ?
C12 C11 C10 C9 -1.4(4) . . . . ?
C1 N1 C6 C5 -179.9(2) . . . . ?
C1 N1 C2 P2 -0.4(3) . . . . ?
C1 N1 C2 C3 179.1(2) . . . . ?
C7 N2 C12 C11 179.8(2) . . . . ?
C7 N2 C8 P4 0.0(3) . . . . ?
C7 N2 C8 C9 178.7(2) . . . . ?
C8 N2 C12 C11 1.2(4) . . . . ?
C8 N2 C7 P3 1.2(3) . . . . ?
C8 N2 C7 O2 -178.6(2) . . . . ?
C8 C9 C10 C11 -0.2(4) . . . . ?
C14 N3 C13 P5 0.2(3) . . . . ?
C14 N3 C13 O3 178.3(2) . . . . ?
C14 N3 C18 C17 0.1(4) . . . . ?
C14 C15 C16 C17 -0.8(4) . . . . ?
C18 N3 C13 P5 -179.15(18) . . . . ?
C18 N3 C13 O3 -1.1(3) . . . . ?
C18 N3 C14 P6 -179.66(18) . . . . ?
C18 N3 C14 C15 -0.8(3) . . . . ?
C18 C17 C16 C15 0.0(4) . . . . ?
C6 N1 C1 P1 -178.12(19) . . . . ?
C6 N1 C1 O1 1.1(3) . . . . ?
C6 N1 C2 P2 178.59(19) . . . . ?
C6 N1 C2 C3 -1.9(4) . . . . ?
C6 C5 C4 C3 -1.3(4) . . . . ?
C2 N1 C1 P1 0.9(3) . . . . ?
C2 N1 C1 O1 -179.8(2) . . . . ?
C2 N1 C6 C5 1.2(4) . . . . ?
C2 C3 C4 C5 0.5(5) . . . . ?
C23 Ti01 O1 C1 -13.3(4) . . . . ?
C23 Ti01 O2 C7 47.2(4) . . . . ?
C23 Ti01 O3 C13 10.6(4) . . . . ?
C23 C22 C21 Ti01 -64.2(2) . . . . ?
C23 C22 C21 C20 0.4(3) . . . . ?
C22 Ti01 O1 C1 10.2(4) . . . . ?
C22 Ti01 O2 C7 -5.9(4) . . . . ?
C22 Ti01 O3 C13 30.9(5) . . . . ?
C22 C23 C19 Ti01 64.5(2) . . . . ?
C22 C23 C19 C20 -0.8(3) . . . . ?
C22 C21 C20 Ti01 -64.7(2) . . . . ?
C22 C21 C20 C19 -0.9(3) . . . . ?
C21 Ti01 O1 C1 43.5(4) . . . . ?
C21 Ti01 O2 C7 -5.6(4) . . . . ?
C21 Ti01 O3 C13 5.0(5) . . . . ?
C21 C20 C19 Ti01 -64.4(2) . . . . ?
C21 C20 C19 C23 1.1(3) . . . . ?
C20 Ti01 O1 C1 52.6(4) . . . . ?
C20 Ti01 O2 C7 24.7(4) . . . . ?
C20 Ti01 O3 C13 -37.2(5) . . . . ?
C19 Ti01 O1 C1 6.0(5) . . . . ?
C19 Ti01 O2 C7 54.3(4) . . . . ?
C19 Ti01 O3 C13 -24.6(4) . . . . ?
C19 C23 C22 Ti01 -63.8(2) . . . . ?
C19 C23 C22 C21 0.3(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_rs3155
_database_code_depnum_ccdc_archive 'CCDC 1494720'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_rs3155              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          13 Note
RESPONSE: the mask of the beam-stopper is increased
;
# Added during the CSD deposition process: Tuesday 19 July 2016 09:44 AM
# end Validation Reply Form

_audit_creation_date             2016-07-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C42 H24 Hf Mo2 N6 O12 P12, 2(C12 H30 Na O6), 2(C H1.93 Cl1.96)'
_chemical_formula_sum            'C68 H87.86 Cl3.92 Hf Mo2 N6 Na2 O24 P12'
_chemical_formula_weight         2300.25
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mo1 Hf1 P6 N3 C50 H50 O12'
_chemical_oxdiff_usercomment     '0.12 0.22 0.16'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.1135(3)
_cell_length_b                   13.1212(4)
_cell_length_c                   16.9409(4)
_cell_angle_alpha                83.345(2)
_cell_angle_beta                 68.758(2)
_cell_angle_gamma                60.501(3)
_cell_volume                     2357.64(12)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    24574
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      30.8810
_cell_measurement_theta_min      3.2230
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.754
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1154
_exptl_crystal_size_max          0.912
_exptl_crystal_size_mid          0.479
_exptl_crystal_size_min          0.393
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38086
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.000
_diffrn_reflns_theta_min         3.031
_diffrn_ambient_temperature      104(2)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -91.00  -64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987 -179.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega  -24.00   15.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987  -99.0000  150.0000 39

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987  -99.0000  -90.0000 45

#__ type_ start__ end____ width___ exp.time_
  4 omega  -20.00   16.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987  -99.0000   30.0000 36

#__ type_ start__ end____ width___ exp.time_
  5 omega  -36.00   27.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987   38.0000  -90.0000 63

#__ type_ start__ end____ width___ exp.time_
  6 omega  -81.00   49.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987    0.0000 -150.0000 130

#__ type_ start__ end____ width___ exp.time_
  7 omega  -36.00   36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987   57.0000   30.0000 72

#__ type_ start__ end____ width___ exp.time_
  8 omega  -86.00   -2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987  -57.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
  9 omega  -38.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987   38.0000  -30.0000 88

#__ type_ start__ end____ width___ exp.time_
 10 omega    3.00   48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.3674   57.0000   30.0000 45
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_UB_11      -0.0511251000
_diffrn_orient_matrix_UB_12      -0.0063524000
_diffrn_orient_matrix_UB_13      0.0288080000
_diffrn_orient_matrix_UB_21      0.0189160000
_diffrn_orient_matrix_UB_22      -0.0499199000
_diffrn_orient_matrix_UB_23      -0.0253585000
_diffrn_orient_matrix_UB_31      0.0379551000
_diffrn_orient_matrix_UB_32      -0.0367187000
_diffrn_orient_matrix_UB_33      0.0236007000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12528
_reflns_number_total             13365
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         13365
_refine_ls_number_restraints     534
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0230
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0233P)²+0.9960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0538
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(HC)=Sof(HD)=Sof(Cl2A)=1-FVAR(1)
 Sof(Cl2)=FVAR(1)
 Sof(Cl00)=Sof(H1AA)=Sof(HB)=Sof(Cl)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C01D(H01N,H01O), C01E(H01P,H01Q), C01I(H01U,H01V), C01J(H01W,H01X), C01L(H1AA,
 HB), C01L(HC,HD), C01M(H01Z,HE), C01N(H01,HF)
4.b Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00Y(H00Y), C00Z(H00Z), C014(H014), C015(H015), C016(H016),
 C017(H017), C018(H018), C01B(H01B), C01C(H01C), C01F(H01F), C01G(H01G)
4.c Idealised Me refined as rotating group:
 C011(H01A,H01D,H01E), C013(H01H,H01I,H01J), C01A(H01K,H01L,H01M), C01H(H01R,
 H01S,H01T), C01K(H01Y,H,HA), C01O(H0AA,HG,HH)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf01 Hf 0.0000 0.0000 0.0000 0.01147(3) Uani 1 2 d S TU P . .
Mo02 Mo -0.16952(2) 0.03465(2) 0.32312(2) 0.01491(3) Uani 1 1 d . U . . .
P03 P -0.06434(4) -0.15271(4) 0.23717(3) 0.01530(8) Uani 1 1 d . U . . .
P004 P -0.01061(4) 0.09198(4) 0.23761(3) 0.01575(8) Uani 1 1 d . U . . .
P005 P 0.30402(4) -0.14230(4) -0.23775(3) 0.01702(9) Uani 1 1 d . U . . .
P06 P 0.06542(5) 0.17803(4) 0.27561(3) 0.02038(9) Uani 1 1 d . U . . .
P007 P 0.49980(4) -0.24504(4) -0.27643(3) 0.02256(10) Uani 1 1 d . U . . .
P08 P -0.01009(4) -0.32366(4) 0.27709(3) 0.02045(9) Uani 1 1 d . U . . .
Na09 Na 0.49281(6) -0.70213(6) -0.28809(5) 0.01901(14) Uani 1 1 d . U . . .
O0A O 0.16170(10) -0.13931(10) -0.07332(7) 0.0162(2) Uani 1 1 d . U . . .
O0B O 0.09376(11) -0.00151(10) 0.07422(7) 0.0163(2) Uani 1 1 d . U . . .
Cl00 Cl -0.0190(3) -0.43734(19) 0.59925(15) 0.0711(8) Uani 0.480(2) 1 d . U . A
1
O00D O -0.04726(11) -0.11683(10) 0.07218(7) 0.0164(2) Uani 1 1 d . U . . .
O00F O 0.61536(11) -0.73959(11) -0.20145(8) 0.0213(3) Uani 1 1 d . U . . .
O00G O 0.39313(11) -0.81212(11) -0.20388(8) 0.0205(3) Uani 1 1 d . U . . .
O00H O 0.32332(12) -0.51979(11) -0.21438(9) 0.0236(3) Uani 1 1 d . U . . .
N00I N 0.02134(12) -0.30616(12) 0.11086(9) 0.0155(3) Uani 1 1 d . U . . .
O00J O 0.64144(13) -0.64027(12) -0.35388(9) 0.0279(3) Uani 1 1 d . U . . .
O00K O -0.00636(14) -0.09638(14) 0.43649(9) 0.0330(3) Uani 1 1 d . U . . .
O00L O -0.36791(15) -0.03763(16) 0.43835(10) 0.0431(4) Uani 1 1 d . U . . .
O00M O 0.36631(14) -0.60929(13) -0.36988(9) 0.0312(3) Uani 1 1 d . U . . .
O00N O 0.59569(12) -0.88944(11) -0.35095(8) 0.0248(3) Uani 1 1 d . U . . .
N00O N 0.17762(13) 0.09510(12) 0.11128(9) 0.0150(3) Uani 1 1 d . U . . .
N00P N 0.37540(13) -0.24922(12) -0.11088(9) 0.0162(3) Uani 1 1 d . U . . .
O00Q O -0.31462(18) 0.26481(14) 0.44181(10) 0.0460(4) Uani 1 1 d . U . . .
C00R C 0.08954(15) 0.05786(14) 0.13324(10) 0.0137(3) Uani 1 1 d . U . . .
C00S C -0.02869(15) -0.18829(14) 0.13214(10) 0.0144(3) Uani 1 1 d . U . . .
C00T C 0.05513(16) -0.34710(16) 0.02805(11) 0.0200(3) Uani 1 1 d . U . . .
H00T H 0.0478 -0.2953 -0.0146 0.024 Uiso 1 1 calc R . . . .
C00U C -0.06622(17) -0.04772(16) 0.39460(11) 0.0210(3) Uani 1 1 d . U . . .
C00V C -0.29582(18) -0.01082(18) 0.39595(12) 0.0250(4) Uani 1 1 d . U . . .
C00W C 0.17864(16) 0.15292(14) 0.17498(11) 0.0174(3) Uani 1 1 d . U . . .
C00X C 0.03413(15) -0.38278(15) 0.17565(11) 0.0177(3) Uani 1 1 d . U . . .
C00Y C 0.26445(16) 0.07269(15) 0.02943(11) 0.0193(3) Uani 1 1 d . U . . .
H00Y H 0.2604 0.0364 -0.0126 0.023 Uiso 1 1 calc R . . . .
C00Z C 0.36294(17) -0.28296(16) -0.02870(12) 0.0215(4) Uani 1 1 d . U . . .
H00Z H 0.2839 -0.2527 0.0134 0.026 Uiso 1 1 calc R . . . .
C010 C 0.27140(15) -0.17429(14) -0.13291(10) 0.0152(3) Uani 1 1 d . U . . .
C011 C 0.26411(17) -0.74320(18) -0.15589(13) 0.0280(4) Uani 1 1 d . U . . .
H01A H 0.2533 -0.6871 -0.1177 0.042 Uiso 1 1 calc GR . . . .
H01D H 0.2323 -0.7932 -0.1239 0.042 Uiso 1 1 calc GR . . . .
H01E H 0.2193 -0.7025 -0.1936 0.042 Uiso 1 1 calc GR . . . .
C012 C 0.49310(16) -0.29170(15) -0.17514(12) 0.0197(3) Uani 1 1 d . U . . .
C013 C 0.6299(2) -0.83979(17) -0.15468(14) 0.0293(4) Uani 1 1 d . U . . .
H01H H 0.5490 -0.8291 -0.1187 0.044 Uiso 1 1 calc GR . . . .
H01I H 0.6782 -0.8499 -0.1204 0.044 Uiso 1 1 calc GR . . . .
H01J H 0.6723 -0.9081 -0.1933 0.044 Uiso 1 1 calc GR . . . .
C014 C 0.27515(17) 0.18258(16) 0.15324(13) 0.0238(4) Uani 1 1 d . U . . .
H014 H 0.2793 0.2197 0.1946 0.029 Uiso 1 1 calc R . . . .
C015 C 0.35468(17) 0.10312(17) 0.01035(13) 0.0248(4) Uani 1 1 d . U . . .
H015 H 0.4125 0.0877 -0.0447 0.030 Uiso 1 1 calc R . . . .
C016 C 0.09839(17) -0.46153(16) 0.00949(13) 0.0252(4) Uani 1 1 d . U . . .
H016 H 0.1212 -0.4882 -0.0460 0.030 Uiso 1 1 calc R . . . .
C017 C 0.36166(17) 0.15840(17) 0.07380(14) 0.0266(4) Uani 1 1 d . U . . .
H017 H 0.4249 0.1779 0.0611 0.032 Uiso 1 1 calc R . . . .
C018 C 0.59764(17) -0.37281(16) -0.15270(14) 0.0249(4) Uani 1 1 d . U . . .
H018 H 0.6772 -0.4035 -0.1942 0.030 Uiso 1 1 calc R . . . .
C019 C -0.2598(2) 0.18076(17) 0.39789(12) 0.0267(4) Uani 1 1 d . U . . .
C01A C 0.3528(2) -0.46714(18) -0.16331(14) 0.0310(4) Uani 1 1 d . U . . .
H01K H 0.3799 -0.5197 -0.1218 0.046 Uiso 1 1 calc GR . . . .
H01L H 0.2799 -0.3950 -0.1350 0.046 Uiso 1 1 calc GR . . . .
H01M H 0.4186 -0.4512 -0.1986 0.046 Uiso 1 1 calc GR . . . .
C01B C 0.07866(17) -0.50200(16) 0.15396(13) 0.0236(4) Uani 1 1 d . U . . .
H01B H 0.0871 -0.5548 0.1959 0.028 Uiso 1 1 calc R . . . .
C01C C 0.46512(19) -0.35957(17) -0.00951(14) 0.0277(4) Uani 1 1 d . U . . .
H01C H 0.4560 -0.3812 0.0459 0.033 Uiso 1 1 calc R . . . .
C01D C 0.41303(19) -0.89646(17) -0.26146(13) 0.0278(4) Uani 1 1 d . U . . .
H01N H 0.3696 -0.8571 -0.3008 0.033 Uiso 1 1 calc R . . . .
H01O H 0.3806 -0.9474 -0.2305 0.033 Uiso 1 1 calc R . . . .
C01E C 0.73325(18) -0.7518(2) -0.25467(14) 0.0327(5) Uani 1 1 d . U . . .
H01P H 0.7801 -0.8226 -0.2924 0.039 Uiso 1 1 calc R . . . .
H01Q H 0.7811 -0.7578 -0.2205 0.039 Uiso 1 1 calc R . . . .
C01F C 0.58562(19) -0.40711(17) -0.07280(14) 0.0288(4) Uani 1 1 d . U . . .
H01F H 0.6557 -0.4612 -0.0598 0.035 Uiso 1 1 calc R . . . .
C01G C 0.10945(17) -0.54144(16) 0.07351(14) 0.0265(4) Uani 1 1 d . U . . .
H01G H 0.1374 -0.6200 0.0608 0.032 Uiso 1 1 calc R . . . .
C01H C 0.3517(2) -0.6689(2) -0.42657(15) 0.0394(5) Uani 1 1 d . U . . .
H01R H 0.4292 -0.7392 -0.4521 0.059 Uiso 1 1 calc GR . . . .
H01S H 0.3287 -0.6187 -0.4701 0.059 Uiso 1 1 calc GR . . . .
H01T H 0.2873 -0.6889 -0.3958 0.059 Uiso 1 1 calc GR . . . .
C01I C 0.7125(2) -0.6470(2) -0.30536(14) 0.0358(5) Uani 1 1 d . U . . .
H01U H 0.6679 -0.5763 -0.2678 0.043 Uiso 1 1 calc R . . . .
H01V H 0.7923 -0.6542 -0.3427 0.043 Uiso 1 1 calc R . . . .
C01J C 0.5505(2) -0.96731(17) -0.30917(14) 0.0300(4) Uani 1 1 d . U . . .
H01W H 0.5935 -1.0105 -0.2703 0.036 Uiso 1 1 calc R . . . .
H01X H 0.5660 -1.0233 -0.3505 0.036 Uiso 1 1 calc R . . . .
C01K C 0.72345(19) -0.94958(19) -0.40302(12) 0.0305(4) Uani 1 1 d . U . . .
H01Y H 0.7506 -0.8937 -0.4282 0.046 Uiso 1 1 calc GR . . . .
H H 0.7342 -0.9979 -0.4470 0.046 Uiso 1 1 calc GR . . . .
HA H 0.7723 -0.9980 -0.3693 0.046 Uiso 1 1 calc GR . . . .
C01L C -0.0540(2) -0.31925(19) 0.53147(14) 0.0340(5) Uani 1 1 d . U . . .
H1AA H -0.0365 -0.2623 0.5471 0.041 Uiso 0.480(2) 1 calc R . . A 1
HB H 0.0005 -0.3497 0.4733 0.041 Uiso 0.480(2) 1 calc R . . A 1
HC H -0.0344 -0.3319 0.4713 0.041 Uiso 0.487(2) 1 calc R . . A 2
HD H -0.0420 -0.2545 0.5395 0.041 Uiso 0.487(2) 1 calc R . . A 2
C01M C 0.2544(2) -0.50465(19) -0.32879(15) 0.0360(5) Uani 1 1 d . U . . .
H01Z H 0.1900 -0.5235 -0.2932 0.043 Uiso 1 1 calc R . . . .
HE H 0.2245 -0.4537 -0.3708 0.043 Uiso 1 1 calc R . . . .
C01N C 0.2810(2) -0.44376(18) -0.27581(15) 0.0343(5) Uani 1 1 d . U . . .
H01 H 0.3446 -0.4240 -0.3115 0.041 Uiso 1 1 calc R . . . .
HF H 0.2056 -0.3717 -0.2477 0.041 Uiso 1 1 calc R . . . .
C01O C 0.6341(2) -0.5541(2) -0.41402(14) 0.0385(5) Uani 1 1 d . U . . .
H0AA H 0.5805 -0.5484 -0.4426 0.058 Uiso 1 1 calc GR . . . .
HG H 0.7163 -0.5763 -0.4548 0.058 Uiso 1 1 calc GR . . . .
HH H 0.6007 -0.4795 -0.3852 0.058 Uiso 1 1 calc GR . . . .
Cl2 Cl -0.20266(14) -0.25167(13) 0.53655(15) 0.0614(5) Uani 0.513(2) 1 d . U .
A 1
Cl2A Cl 0.04246(16) -0.44188(18) 0.56647(15) 0.0523(6) Uani 0.487(2) 1 d . U .
A 2
Cl Cl -0.21499(11) -0.28335(13) 0.58927(11) 0.0450(4) Uani 0.480(2) 1 d . U . 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
Hf01 O0A 2.0447(11) 2 ?
Hf01 O0A 2.0447(11) . ?
Hf01 O0B 2.0454(11) . ?
Hf01 O0B 2.0454(11) 2 ?
Hf01 O00D 2.0448(11) 2 ?
Hf01 O00D 2.0449(11) . ?
Mo02 P03 2.4700(5) . ?
Mo02 P004 2.4720(5) . ?
Mo02 P005 2.4736(5) 2 ?
Mo02 C00U 1.9781(18) . ?
Mo02 C00V 1.9857(19) . ?
Mo02 C019 1.981(2) . ?
P03 P08 2.1023(6) . ?
P03 C00S 1.7256(17) . ?
P004 P06 2.1036(6) . ?
P004 C00R 1.7244(17) . ?
P005 Mo02 2.4736(5) 2 ?
P005 P007 2.1013(6) . ?
P005 C010 1.7226(17) . ?
P06 C00W 1.7417(19) . ?
P007 C012 1.7399(19) . ?
P08 C00X 1.7422(19) . ?
Na09 O00F 2.3965(14) . ?
Na09 O00G 2.4198(14) . ?
Na09 O00H 2.3807(15) . ?
Na09 O00J 2.3397(15) . ?
Na09 O00M 2.3324(15) . ?
Na09 O00N 2.3010(15) . ?
O0A C010 1.3054(19) . ?
O0B C00R 1.3066(19) . ?
Cl00 C01L 1.789(3) . ?
O00D C00S 1.3052(19) . ?
O00F C013 1.419(2) . ?
O00F C01E 1.417(2) . ?
O00G C011 1.417(2) . ?
O00G C01D 1.423(2) . ?
O00H C01A 1.421(2) . ?
O00H C01N 1.421(2) . ?
N00I C00S 1.382(2) . ?
N00I C00T 1.394(2) . ?
N00I C00X 1.398(2) . ?
O00J C01I 1.418(2) . ?
O00J C01O 1.422(2) . ?
O00K C00U 1.154(2) . ?
O00L C00V 1.145(2) . ?
O00M C01H 1.423(3) . ?
O00M C01M 1.421(3) . ?
O00N C01J 1.421(2) . ?
O00N C01K 1.413(2) . ?
N00O C00R 1.383(2) . ?
N00O C00W 1.397(2) . ?
N00O C00Y 1.388(2) . ?
N00P C00Z 1.387(2) . ?
N00P C010 1.389(2) . ?
N00P C012 1.398(2) . ?
O00Q C019 1.144(2) . ?
C00T H00T 0.9300 . ?
C00T C016 1.348(3) . ?
C00W C014 1.415(2) . ?
C00X C01B 1.415(2) . ?
C00Y H00Y 0.9300 . ?
C00Y C015 1.350(2) . ?
C00Z H00Z 0.9300 . ?
C00Z C01C 1.351(3) . ?
C011 H01A 0.9600 . ?
C011 H01D 0.9600 . ?
C011 H01E 0.9600 . ?
C012 C018 1.416(2) . ?
C013 H01H 0.9600 . ?
C013 H01I 0.9600 . ?
C013 H01J 0.9600 . ?
C014 H014 0.9300 . ?
C014 C017 1.355(3) . ?
C015 H015 0.9300 . ?
C015 C017 1.417(3) . ?
C016 H016 0.9300 . ?
C016 C01G 1.413(3) . ?
C017 H017 0.9300 . ?
C018 H018 0.9300 . ?
C018 C01F 1.354(3) . ?
C01A H01K 0.9600 . ?
C01A H01L 0.9600 . ?
C01A H01M 0.9600 . ?
C01B H01B 0.9300 . ?
C01B C01G 1.359(3) . ?
C01C H01C 0.9300 . ?
C01C C01F 1.411(3) . ?
C01D H01N 0.9700 . ?
C01D H01O 0.9700 . ?
C01D C01J 1.495(3) . ?
C01E H01P 0.9700 . ?
C01E H01Q 0.9700 . ?
C01E C01I 1.493(3) . ?
C01F H01F 0.9300 . ?
C01G H01G 0.9300 . ?
C01H H01R 0.9600 . ?
C01H H01S 0.9600 . ?
C01H H01T 0.9600 . ?
C01I H01U 0.9700 . ?
C01I H01V 0.9700 . ?
C01J H01W 0.9700 . ?
C01J H01X 0.9700 . ?
C01K H01Y 0.9600 . ?
C01K H 0.9600 . ?
C01K HA 0.9600 . ?
C01L H1AA 0.9700 . ?
C01L HB 0.9700 . ?
C01L HC 0.9700 . ?
C01L HD 0.9700 . ?
C01L Cl2 1.669(3) . ?
C01L Cl2A 1.691(3) . ?
C01L Cl 1.807(3) . ?
C01M H01Z 0.9700 . ?
C01M HE 0.9700 . ?
C01M C01N 1.494(3) . ?
C01N H01 0.9700 . ?
C01N HF 0.9700 . ?
C01O H0AA 0.9600 . ?
C01O HG 0.9600 . ?
C01O HH 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O0A Hf01 O0A 180.0 2 . ?
O0A Hf01 O0B 91.42(5) 2 . ?
O0A Hf01 O0B 88.58(5) . . ?
O0A Hf01 O0B 91.42(5) . 2 ?
O0A Hf01 O0B 88.58(5) 2 2 ?
O0B Hf01 O0B 180.0 2 . ?
O00D Hf01 O0A 91.46(5) . 2 ?
O00D Hf01 O0A 91.46(5) 2 . ?
O00D Hf01 O0A 88.54(5) . . ?
O00D Hf01 O0A 88.54(5) 2 2 ?
O00D Hf01 O0B 91.10(5) 2 2 ?
O00D Hf01 O0B 88.90(5) . 2 ?
O00D Hf01 O0B 88.90(5) 2 . ?
O00D Hf01 O0B 91.10(5) . . ?
O00D Hf01 O00D 180.0 2 . ?
P03 Mo02 P004 93.900(15) . . ?
P03 Mo02 P005 93.039(15) . 2 ?
P004 Mo02 P005 92.355(15) . 2 ?
C00U Mo02 P03 88.63(5) . . ?
C00U Mo02 P004 88.38(5) . . ?
C00U Mo02 P005 178.12(5) . 2 ?
C00U Mo02 C00V 89.71(8) . . ?
C00U Mo02 C019 90.30(8) . . ?
C00V Mo02 P03 87.37(6) . . ?
C00V Mo02 P004 177.68(6) . . ?
C00V Mo02 P005 89.51(6) . 2 ?
C019 Mo02 P03 176.32(6) . . ?
C019 Mo02 P004 89.59(6) . . ?
C019 Mo02 P005 87.98(6) . 2 ?
C019 Mo02 C00V 89.10(8) . . ?
P08 P03 Mo02 129.10(2) . . ?
C00S P03 Mo02 133.80(6) . . ?
C00S P03 P08 96.67(6) . . ?
P06 P004 Mo02 130.13(2) . . ?
C00R P004 Mo02 132.59(6) . . ?
C00R P004 P06 96.67(6) . . ?
P007 P005 Mo02 129.93(2) . 2 ?
C010 P005 Mo02 132.70(6) . 2 ?
C010 P005 P007 96.90(6) . . ?
C00W P06 P004 92.46(6) . . ?
C012 P007 P005 92.43(6) . . ?
C00X P08 P03 92.56(6) . . ?
O00F Na09 O00G 93.11(5) . . ?
O00H Na09 O00F 96.07(5) . . ?
O00H Na09 O00G 92.79(5) . . ?
O00J Na09 O00F 70.66(5) . . ?
O00J Na09 O00G 161.23(5) . . ?
O00J Na09 O00H 98.11(5) . . ?
O00M Na09 O00F 162.67(6) . . ?
O00M Na09 O00G 99.58(5) . . ?
O00M Na09 O00H 71.73(5) . . ?
O00M Na09 O00J 98.32(6) . . ?
O00N Na09 O00F 97.48(5) . . ?
O00N Na09 O00G 70.48(5) . . ?
O00N Na09 O00H 158.95(6) . . ?
O00N Na09 O00J 101.54(6) . . ?
O00N Na09 O00M 97.85(6) . . ?
C010 O0A Hf01 146.52(11) . . ?
C00R O0B Hf01 144.55(11) . . ?
C00S O00D Hf01 145.41(11) . . ?
C013 O00F Na09 112.87(11) . . ?
C01E O00F Na09 108.19(11) . . ?
C01E O00F C013 111.03(15) . . ?
C011 O00G Na09 114.83(11) . . ?
C011 O00G C01D 111.19(15) . . ?
C01D O00G Na09 106.33(11) . . ?
C01A O00H Na09 114.28(11) . . ?
C01A O00H C01N 111.14(15) . . ?
C01N O00H Na09 107.52(12) . . ?
C00S N00I C00T 121.22(14) . . ?
C00S N00I C00X 117.79(14) . . ?
C00T N00I C00X 120.97(15) . . ?
C01I O00J Na09 115.14(11) . . ?
C01I O00J C01O 112.09(16) . . ?
C01O O00J Na09 126.75(13) . . ?
C01H O00M Na09 124.57(13) . . ?
C01M O00M Na09 113.78(12) . . ?
C01M O00M C01H 112.65(17) . . ?
C01J O00N Na09 117.21(11) . . ?
C01K O00N Na09 124.87(13) . . ?
C01K O00N C01J 112.37(15) . . ?
C00R N00O C00W 117.68(14) . . ?
C00R N00O C00Y 121.20(14) . . ?
C00Y N00O C00W 121.10(14) . . ?
C00Z N00P C010 121.33(14) . . ?
C00Z N00P C012 121.17(14) . . ?
C010 N00P C012 117.48(14) . . ?
O0B C00R P004 127.57(12) . . ?
O0B C00R N00O 117.10(14) . . ?
N00O C00R P004 115.30(12) . . ?
O00D C00S P03 127.60(13) . . ?
O00D C00S N00I 117.11(14) . . ?
N00I C00S P03 115.25(12) . . ?
N00I C00T H00T 119.9 . . ?
C016 C00T N00I 120.25(17) . . ?
C016 C00T H00T 119.9 . . ?
O00K C00U Mo02 179.45(17) . . ?
O00L C00V Mo02 179.36(19) . . ?
N00O C00W P06 117.85(12) . . ?
N00O C00W C014 117.07(16) . . ?
C014 C00W P06 125.04(14) . . ?
N00I C00X P08 117.70(13) . . ?
N00I C00X C01B 117.16(16) . . ?
C01B C00X P08 125.11(14) . . ?
N00O C00Y H00Y 119.8 . . ?
C015 C00Y N00O 120.45(17) . . ?
C015 C00Y H00Y 119.8 . . ?
N00P C00Z H00Z 119.9 . . ?
C01C C00Z N00P 120.29(18) . . ?
C01C C00Z H00Z 119.9 . . ?
O0A C010 P005 127.84(12) . . ?
O0A C010 N00P 116.98(14) . . ?
N00P C010 P005 115.15(12) . . ?
O00G C011 H01A 109.5 . . ?
O00G C011 H01D 109.5 . . ?
O00G C011 H01E 109.5 . . ?
H01A C011 H01D 109.5 . . ?
H01A C011 H01E 109.5 . . ?
H01D C011 H01E 109.5 . . ?
N00P C012 P007 118.03(12) . . ?
N00P C012 C018 116.79(17) . . ?
C018 C012 P007 125.15(14) . . ?
O00F C013 H01H 109.5 . . ?
O00F C013 H01I 109.5 . . ?
O00F C013 H01J 109.5 . . ?
H01H C013 H01I 109.5 . . ?
H01H C013 H01J 109.5 . . ?
H01I C013 H01J 109.5 . . ?
C00W C014 H014 119.1 . . ?
C017 C014 C00W 121.84(18) . . ?
C017 C014 H014 119.1 . . ?
C00Y C015 H015 119.9 . . ?
C00Y C015 C017 120.27(18) . . ?
C017 C015 H015 119.9 . . ?
C00T C016 H016 119.7 . . ?
C00T C016 C01G 120.65(18) . . ?
C01G C016 H016 119.7 . . ?
C014 C017 C015 119.22(17) . . ?
C014 C017 H017 120.4 . . ?
C015 C017 H017 120.4 . . ?
C012 C018 H018 118.9 . . ?
C01F C018 C012 122.16(18) . . ?
C01F C018 H018 118.9 . . ?
O00Q C019 Mo02 178.3(2) . . ?
O00H C01A H01K 109.5 . . ?
O00H C01A H01L 109.5 . . ?
O00H C01A H01M 109.5 . . ?
H01K C01A H01L 109.5 . . ?
H01K C01A H01M 109.5 . . ?
H01L C01A H01M 109.5 . . ?
C00X C01B H01B 119.1 . . ?
C01G C01B C00X 121.80(17) . . ?
C01G C01B H01B 119.1 . . ?
C00Z C01C H01C 119.7 . . ?
C00Z C01C C01F 120.54(19) . . ?
C01F C01C H01C 119.7 . . ?
O00G C01D H01N 110.0 . . ?
O00G C01D H01O 110.0 . . ?
O00G C01D C01J 108.66(16) . . ?
H01N C01D H01O 108.3 . . ?
C01J C01D H01N 110.0 . . ?
C01J C01D H01O 110.0 . . ?
O00F C01E H01P 109.9 . . ?
O00F C01E H01Q 109.9 . . ?
O00F C01E C01I 108.82(16) . . ?
H01P C01E H01Q 108.3 . . ?
C01I C01E H01P 109.9 . . ?
C01I C01E H01Q 109.9 . . ?
C018 C01F C01C 119.02(17) . . ?
C018 C01F H01F 120.5 . . ?
C01C C01F H01F 120.5 . . ?
C016 C01G H01G 120.4 . . ?
C01B C01G C016 119.13(17) . . ?
C01B C01G H01G 120.4 . . ?
O00M C01H H01R 109.5 . . ?
O00M C01H H01S 109.5 . . ?
O00M C01H H01T 109.5 . . ?
H01R C01H H01S 109.5 . . ?
H01R C01H H01T 109.5 . . ?
H01S C01H H01T 109.5 . . ?
O00J C01I C01E 108.45(17) . . ?
O00J C01I H01U 110.0 . . ?
O00J C01I H01V 110.0 . . ?
C01E C01I H01U 110.0 . . ?
C01E C01I H01V 110.0 . . ?
H01U C01I H01V 108.4 . . ?
O00N C01J C01D 108.40(16) . . ?
O00N C01J H01W 110.0 . . ?
O00N C01J H01X 110.0 . . ?
C01D C01J H01W 110.0 . . ?
C01D C01J H01X 110.0 . . ?
H01W C01J H01X 108.4 . . ?
O00N C01K H01Y 109.5 . . ?
O00N C01K H 109.5 . . ?
O00N C01K HA 109.5 . . ?
H01Y C01K H 109.5 . . ?
H01Y C01K HA 109.5 . . ?
H C01K HA 109.5 . . ?
Cl00 C01L H1AA 108.9 . . ?
Cl00 C01L HB 108.9 . . ?
H1AA C01L HB 107.7 . . ?
HC C01L HD 108.2 . . ?
Cl2 C01L Cl00 113.21(18) . . ?
Cl2 C01L H1AA 108.9 . . ?
Cl2 C01L HB 108.9 . . ?
Cl2A C01L HC 109.7 . . ?
Cl2A C01L HD 109.7 . . ?
Cl2A C01L Cl 109.84(15) . . ?
Cl C01L HC 109.7 . . ?
Cl C01L HD 109.7 . . ?
O00M C01M H01Z 109.9 . . ?
O00M C01M HE 109.9 . . ?
O00M C01M C01N 108.85(17) . . ?
H01Z C01M HE 108.3 . . ?
C01N C01M H01Z 109.9 . . ?
C01N C01M HE 109.9 . . ?
O00H C01N C01M 108.76(17) . . ?
O00H C01N H01 109.9 . . ?
O00H C01N HF 109.9 . . ?
C01M C01N H01 109.9 . . ?
C01M C01N HF 109.9 . . ?
H01 C01N HF 108.3 . . ?
O00J C01O H0AA 109.5 . . ?
O00J C01O HG 109.5 . . ?
O00J C01O HH 109.5 . . ?
H0AA C01O HG 109.5 . . ?
H0AA C01O HH 109.5 . . ?
HG C01O HH 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Hf01 O0A C010 P005 -65.2(3) . . . . ?
Hf01 O0A C010 N00P 116.92(18) . . . . ?
Hf01 O0B C00R P004 67.6(2) . . . . ?
Hf01 O0B C00R N00O -114.68(17) . . . . ?
Hf01 O00D C00S P03 65.1(2) . . . . ?
Hf01 O00D C00S N00I -117.36(18) . . . . ?
Mo02 P03 C00S O00D 3.64(19) . . . . ?
Mo02 P03 C00S N00I -173.95(8) . . . . ?
Mo02 P004 C00R O0B 6.04(19) . . . . ?
Mo02 P004 C00R N00O -171.71(8) . . . . ?
Mo02 P005 C010 O0A -4.9(2) 2 . . . ?
Mo02 P005 C010 N00P 173.00(8) 2 . . . ?
P03 P08 C00X N00I 0.69(12) . . . . ?
P03 P08 C00X C01B -177.33(15) . . . . ?
P004 P06 C00W N00O 1.76(12) . . . . ?
P004 P06 C00W C014 -175.67(14) . . . . ?
P005 P007 C012 N00P -0.76(13) . . . . ?
P005 P007 C012 C018 177.11(15) . . . . ?
P06 P004 C00R O0B 177.54(14) . . . . ?
P06 P004 C00R N00O -0.20(12) . . . . ?
P06 C00W C014 C017 178.75(14) . . . . ?
P007 P005 C010 O0A -177.43(14) . . . . ?
P007 P005 C010 N00P 0.52(13) . . . . ?
P007 C012 C018 C01F -178.74(15) . . . . ?
P08 P03 C00S O00D 176.35(14) . . . . ?
P08 P03 C00S N00I -1.24(12) . . . . ?
P08 C00X C01B C01G 178.86(14) . . . . ?
Na09 O00F C01E C01I 52.88(19) . . . . ?
Na09 O00G C01D C01J 55.14(16) . . . . ?
Na09 O00H C01N C01M 52.90(19) . . . . ?
Na09 O00J C01I C01E 34.6(2) . . . . ?
Na09 O00M C01M C01N 35.3(2) . . . . ?
Na09 O00N C01J C01D 29.4(2) . . . . ?
O00F C01E C01I O00J -59.0(2) . . . . ?
O00G C01D C01J O00N -57.3(2) . . . . ?
N00I C00T C016 C01G 0.4(3) . . . . ?
N00I C00X C01B C01G 0.8(3) . . . . ?
O00M C01M C01N O00H -60.1(2) . . . . ?
N00O C00W C014 C017 1.3(2) . . . . ?
N00O C00Y C015 C017 0.0(3) . . . . ?
N00P C00Z C01C C01F -0.6(3) . . . . ?
N00P C012 C018 C01F -0.8(3) . . . . ?
C00R N00O C00W P06 -2.31(19) . . . . ?
C00R N00O C00W C014 175.32(14) . . . . ?
C00R N00O C00Y C015 -175.85(16) . . . . ?
C00S N00I C00T C016 -176.96(16) . . . . ?
C00S N00I C00X P08 -1.74(19) . . . . ?
C00S N00I C00X C01B 176.44(15) . . . . ?
C00T N00I C00S P03 -179.57(12) . . . . ?
C00T N00I C00S O00D 2.6(2) . . . . ?
C00T N00I C00X P08 179.80(12) . . . . ?
C00T N00I C00X C01B -2.0(2) . . . . ?
C00T C016 C01G C01B -1.6(3) . . . . ?
C00W N00O C00R P004 1.49(18) . . . . ?
C00W N00O C00R O0B -176.50(13) . . . . ?
C00W N00O C00Y C015 2.2(2) . . . . ?
C00W C014 C017 C015 0.7(3) . . . . ?
C00X N00I C00S P03 1.97(19) . . . . ?
C00X N00I C00S O00D -175.88(14) . . . . ?
C00X N00I C00T C016 1.4(2) . . . . ?
C00X C01B C01G C016 0.9(3) . . . . ?
C00Y N00O C00R P004 179.57(12) . . . . ?
C00Y N00O C00R O0B 1.6(2) . . . . ?
C00Y N00O C00W P06 179.60(12) . . . . ?
C00Y N00O C00W C014 -2.8(2) . . . . ?
C00Y C015 C017 C014 -1.4(3) . . . . ?
C00Z N00P C010 P005 -179.64(13) . . . . ?
C00Z N00P C010 O0A -1.5(2) . . . . ?
C00Z N00P C012 P007 179.79(13) . . . . ?
C00Z N00P C012 C018 1.7(2) . . . . ?
C00Z C01C C01F C018 1.5(3) . . . . ?
C010 N00P C00Z C01C 177.37(17) . . . . ?
C010 N00P C012 P007 1.3(2) . . . . ?
C010 N00P C012 C018 -176.75(15) . . . . ?
C011 O00G C01D C01J -179.20(15) . . . . ?
C012 N00P C00Z C01C -1.1(3) . . . . ?
C012 N00P C010 P005 -1.15(19) . . . . ?
C012 N00P C010 O0A 177.03(14) . . . . ?
C012 C018 C01F C01C -0.7(3) . . . . ?
C013 O00F C01E C01I 177.26(17) . . . . ?
C01A O00H C01N C01M 178.66(17) . . . . ?
C01H O00M C01M C01N -175.84(17) . . . . ?
C01K O00N C01J C01D -175.52(16) . . . . ?
C01O O00J C01I C01E -170.72(18) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_rs3033
_database_code_depnum_ccdc_archive 'CCDC 1494718'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_rs3033              
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.900 Note
RESPONSE: crystal was in needle shape and diffracted only very badly.
;
# Added during the CSD deposition process: Tuesday 19 July 2016 09:44 AM
# end Validation Reply Form

_audit_creation_date             2014-10-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C36 H24 Hf N6 O6 P12, 2(C12 H30 Na O6)'
_chemical_formula_sum            'C60 H84 Hf N6 Na2 O18 P12'
_chemical_formula_weight         1773.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Hf1 P4 O2 N2 C100 H100'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.9451(3)
_cell_length_b                   13.2815(2)
_cell_length_c                   18.8611(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.052(3)
_cell_angle_gamma                90.00
_cell_volume                     3994.33(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4727
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.5090
_cell_measurement_theta_min      2.9780
_exptl_absorpt_coefficient_mu    1.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13164
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.94
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    2.00   97.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990   38.0000  -60.0000 95

#__ type_ start__ end____ width___ exp.time_
  2 omega   36.00   68.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990   57.0000   60.0000 32

#__ type_ start__ end____ width___ exp.time_
  3 omega   13.00   69.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990  -99.0000  150.0000 56
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0381881000
_diffrn_orient_matrix_UB_12      0.0039967000
_diffrn_orient_matrix_UB_13      -0.0190894000
_diffrn_orient_matrix_UB_21      -0.0223068000
_diffrn_orient_matrix_UB_22      0.0043596000
_diffrn_orient_matrix_UB_23      0.0323938000
_diffrn_orient_matrix_UB_31      0.0046756000
_diffrn_orient_matrix_UB_32      0.0530723000
_diffrn_orient_matrix_UB_33      -0.0011985000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                6042
_reflns_number_total             7328
_reflns_odcompleteness_completeness 86.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0415
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0270P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0778
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C20(H20A,H20B), C21(H21A,H21B), C28(H28A,
 H28B), C29(H29A,H29B)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C10(H10), C11(H11), C6(H6), C12(H12), C3(H3), C4(H4), C15(H15),
 C9(H9), C16(H16), C5(H5), C17(H17)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C19(H19A,H19B,
 H19C), C30(H30A,H30B,H30C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Hf1 Hf 0.5000 0.5000 0.0000 0.01048(7) Uani 1 d . . 2 S T P
P2 P 0.14407(6) 0.59682(7) -0.05232(6) 0.0180(2) Uani 1 d . . 1 . . .
P1 P 0.27293(6) 0.57755(7) -0.07811(6) 0.0163(2) Uani 1 d . . 1 . . .
P6 P 0.44176(7) 0.83817(7) 0.19777(6) 0.0228(3) Uani 1 d . . 1 . . .
P3 P 0.48151(7) 0.40698(7) 0.20216(6) 0.0214(3) Uani 1 d . . 1 . . .
P5 P 0.40705(7) 0.73076(7) 0.11934(6) 0.0196(3) Uani 1 d . . 1 . . .
P4 P 0.51426(7) 0.29112(8) 0.27475(6) 0.0235(3) Uani 1 d . . 1 . . .
Na8 Na 0.70076(9) 0.40507(10) 0.55044(9) 0.0174(4) Uani 1 d . . 1 . . .
O2 O 0.51895(16) 0.37497(17) 0.06270(15) 0.0147(6) Uani 1 d . . 1 . . .
N3 N 0.56032(19) 0.6996(2) 0.17266(18) 0.0131(7) Uani 1 d . . 1 . . .
O7 O 0.65956(17) 0.24542(19) 0.50764(17) 0.0266(8) Uani 1 d . . 1 . . .
N6 N 0.23692(19) 0.5266(2) 0.05583(18) 0.0125(8) Uani 1 d . . 1 . . .
O5 O 0.67243(17) 0.57346(18) 0.58599(17) 0.0235(7) Uani 1 d . . 1 . . .
C2 C 0.1563(2) 0.5560(2) 0.0345(2) 0.0138(9) Uani 1 d . . 1 . . .
N10 N 0.55856(18) 0.2512(2) 0.14029(18) 0.0112(7) Uani 1 d . . 1 . . .
O6 O 0.56880(16) 0.36184(18) 0.60008(16) 0.0213(7) Uani 1 d . . 1 . . .
C13 C 0.5017(2) 0.6663(2) 0.1242(2) 0.0123(9) Uani 1 d . . 1 . . .
O8 O 0.78236(17) 0.37041(19) 0.65417(17) 0.0242(7) Uani 1 d . . 1 . . .
C7 C 0.5216(2) 0.3448(3) 0.1287(2) 0.0141(9) Uani 1 d . . 1 . . .
C18 C 0.6374(2) 0.6505(3) 0.1819(2) 0.0196(10) Uani 1 d . . 1 . . .
H18 H 0.6493 0.5927 0.1560 0.024 Uiso 1 calc . . 1 R . .
C14 C 0.5396(3) 0.7857(3) 0.2132(2) 0.0177(10) Uani 1 d . . 1 . . .
C10 C 0.6246(3) 0.0621(3) 0.1675(3) 0.0254(11) Uani 1 d . . 1 . . .
H10 H 0.6456 -0.0021 0.1759 0.031 Uiso 1 calc . . 1 R . .
C11 C 0.6262(2) 0.1041(3) 0.0978(2) 0.0211(10) Uani 1 d . . 1 . . .
H11 H 0.6497 0.0675 0.0607 0.025 Uiso 1 calc . . 1 R . .
C6 C 0.2519(2) 0.4931(3) 0.1240(2) 0.0191(9) Uani 1 d . . 1 . . .
H6 H 0.3059 0.4738 0.1370 0.023 Uiso 1 calc . . 1 R . .
C24 C 0.5566(3) 0.2553(3) 0.5977(2) 0.0229(10) Uani 1 d . . 1 . . .
H24A H 0.4992 0.2389 0.6102 0.027 Uiso 1 calc . . 1 R . .
H24B H 0.5937 0.2224 0.6313 0.027 Uiso 1 calc . . 1 R . .
C12 C 0.5943(2) 0.1959(3) 0.0853(2) 0.0180(9) Uani 1 d . . 1 . . .
H12 H 0.5959 0.2227 0.0398 0.022 Uiso 1 calc . . 1 R . .
C3 C 0.0921(2) 0.5504(3) 0.0861(2) 0.0191(10) Uani 1 d . . 1 . . .
H3 H 0.0380 0.5699 0.0738 0.023 Uiso 1 calc . . 1 R . .
C4 C 0.1071(3) 0.5177(3) 0.1527(3) 0.0243(11) Uani 1 d . . 1 . . .
H4 H 0.0639 0.5146 0.1857 0.029 Uiso 1 calc . . 1 R . .
C23 C 0.5417(3) 0.4040(3) 0.6659(2) 0.0276(11) Uani 1 d . . 1 . . .
H23A H 0.5746 0.3763 0.7039 0.041 Uiso 1 calc . . 1 GR . .
H23B H 0.4836 0.3883 0.6733 0.041 Uiso 1 calc . . 1 GR . .
H23C H 0.5489 0.4757 0.6647 0.041 Uiso 1 calc . . 1 GR . .
C15 C 0.6008(3) 0.8205(3) 0.2607(2) 0.0264(11) Uani 1 d . . 1 . . .
H15 H 0.5893 0.8776 0.2875 0.032 Uiso 1 calc . . 1 R . .
O4 O 0.68427(17) 0.50917(18) 0.44835(16) 0.0249(7) Uani 1 d . . 1 . . .
C8 C 0.5582(2) 0.2154(3) 0.2097(2) 0.0172(9) Uani 1 d . . 1 . . .
C9 C 0.5922(2) 0.1170(3) 0.2210(3) 0.0224(10) Uani 1 d . . 1 . . .
H9 H 0.5919 0.0901 0.2665 0.027 Uiso 1 calc . . 1 R . .
C25 C 0.5752(3) 0.2201(3) 0.5242(3) 0.0256(11) Uani 1 d . . 1 . . .
H25A H 0.5675 0.1478 0.5210 0.031 Uiso 1 calc . . 1 R . .
H25B H 0.5374 0.2521 0.4908 0.031 Uiso 1 calc . . 1 R . .
C16 C 0.6762(3) 0.7745(3) 0.2694(2) 0.0292(11) Uani 1 d . . 1 . . .
H16 H 0.7154 0.7995 0.3014 0.035 Uiso 1 calc . . 1 R . .
C22 C 0.6968(3) 0.6164(3) 0.6515(2) 0.0282(11) Uani 1 d . . 1 . . .
H22A H 0.6924 0.5667 0.6882 0.042 Uiso 1 calc . . 1 GR . .
H22B H 0.6607 0.6722 0.6623 0.042 Uiso 1 calc . . 1 GR . .
H22C H 0.7537 0.6395 0.6483 0.042 Uiso 1 calc . . 1 GR . .
C20 C 0.6392(3) 0.5997(3) 0.4643(3) 0.0319(12) Uani 1 d . . 1 . . .
H20A H 0.5803 0.5846 0.4720 0.038 Uiso 1 calc . . 1 R . .
H20B H 0.6435 0.6468 0.4252 0.038 Uiso 1 calc . . 1 R . .
C5 C 0.1896(2) 0.4880(3) 0.1718(2) 0.0220(10) Uani 1 d . . 1 . . .
H5 H 0.2006 0.4650 0.2174 0.026 Uiso 1 calc . . 1 R . .
C1 C 0.2999(2) 0.5321(2) 0.0049(2) 0.0126(9) Uani 1 d . . 1 . . .
C27 C 0.7651(3) 0.2991(3) 0.7083(3) 0.0326(12) Uani 1 d . . 1 . . .
H27A H 0.7062 0.2996 0.7188 0.049 Uiso 1 calc . . 1 GR . .
H27B H 0.7962 0.3163 0.7502 0.049 Uiso 1 calc . . 1 GR . .
H27C H 0.7812 0.2331 0.6926 0.049 Uiso 1 calc . . 1 GR . .
C19 C 0.6599(3) 0.4671(3) 0.3824(3) 0.0353(12) Uani 1 d . . 1 . . .
H19A H 0.6937 0.4090 0.3725 0.053 Uiso 1 calc . . 1 GR . .
H19B H 0.6676 0.5161 0.3455 0.053 Uiso 1 calc . . 1 GR . .
H19C H 0.6020 0.4478 0.3844 0.053 Uiso 1 calc . . 1 GR . .
C21 C 0.6767(3) 0.6443(3) 0.5300(3) 0.0304(12) Uani 1 d . . 1 . . .
H21A H 0.7347 0.6624 0.5212 0.036 Uiso 1 calc . . 1 R . .
H21B H 0.6464 0.7049 0.5430 0.036 Uiso 1 calc . . 1 R . .
C17 C 0.6940(3) 0.6867(3) 0.2282(2) 0.0251(10) Uani 1 d . . 1 . . .
H17 H 0.7453 0.6543 0.2334 0.030 Uiso 1 calc . . 1 R . .
C30 C 0.8958(3) 0.3391(3) 0.4766(3) 0.0410(14) Uani 1 d . . 1 . . .
H30A H 0.9014 0.2770 0.5023 0.062 Uiso 1 calc . . 1 GR . .
H30B H 0.9503 0.3680 0.4692 0.062 Uiso 1 calc . . 1 GR . .
H30C H 0.8698 0.3263 0.4316 0.062 Uiso 1 calc . . 1 GR . .
O1 O 0.37462(15) 0.50229(18) 0.02633(15) 0.0164(6) Uani 1 d . . 1 . . .
O9 O 0.84531(17) 0.4074(2) 0.51639(17) 0.0252(7) Uani 1 d . . 1 . . .
C26 C 0.6851(3) 0.2017(3) 0.4419(3) 0.0416(15) Uani 1 d . . 1 . . .
H26A H 0.6489 0.2250 0.4046 0.062 Uiso 1 calc . . 1 GR . .
H26B H 0.6816 0.1296 0.4451 0.062 Uiso 1 calc . . 1 GR . .
H26C H 0.7418 0.2210 0.4317 0.062 Uiso 1 calc . . 1 GR . .
C28 C 0.8707(3) 0.3761(3) 0.6404(3) 0.0294(12) Uani 1 d . . 1 . . .
H28A H 0.8927 0.3097 0.6299 0.035 Uiso 1 calc . . 1 R . .
H28B H 0.8998 0.4021 0.6818 0.035 Uiso 1 calc . . 1 R . .
C29 C 0.8839(3) 0.4445(3) 0.5788(3) 0.0310(12) Uani 1 d . . 1 . . .
H29A H 0.8611 0.5104 0.5898 0.037 Uiso 1 calc . . 1 R . .
H29B H 0.9436 0.4523 0.5705 0.037 Uiso 1 calc . . 1 R . .
O3 O 0.52547(16) 0.58958(17) 0.08499(15) 0.0161(6) Uani 1 d . . 1 . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O2 2.061(2) 3_665 ?
Hf1 O2 2.061(2) . ?
Hf1 O1 2.061(2) 3_665 ?
Hf1 O1 2.061(2) . ?
Hf1 O3 2.037(3) . ?
Hf1 O3 2.037(3) 3_665 ?
P2 P1 2.1274(14) . ?
P2 C2 1.736(4) . ?
P1 C1 1.731(4) . ?
P6 P5 2.1280(16) . ?
P6 C14 1.733(4) . ?
P3 P4 2.1247(16) . ?
P3 C7 1.735(4) . ?
P5 C13 1.738(4) . ?
P4 C8 1.735(4) . ?
Na8 O7 2.362(3) . ?
Na8 O5 2.378(3) . ?
Na8 O6 2.374(3) . ?
Na8 O8 2.393(4) . ?
Na8 O4 2.385(3) . ?
Na8 O9 2.393(3) . ?
O2 C7 1.309(5) . ?
N3 C13 1.380(5) . ?
N3 C18 1.402(5) . ?
N3 C14 1.415(4) . ?
O7 C25 1.421(4) . ?
O7 C26 1.429(5) . ?
N6 C2 1.403(5) . ?
N6 C6 1.382(5) . ?
N6 C1 1.392(4) . ?
O5 C22 1.414(5) . ?
O5 C21 1.416(5) . ?
C2 C3 1.414(5) . ?
N10 C7 1.392(4) . ?
N10 C12 1.393(5) . ?
N10 C8 1.393(5) . ?
O6 C24 1.429(4) . ?
O6 C23 1.429(5) . ?
C13 O3 1.315(4) . ?
O8 C27 1.421(5) . ?
O8 C28 1.435(5) . ?
C18 C17 1.344(6) . ?
C14 C15 1.403(6) . ?
C10 C11 1.429(6) . ?
C10 C9 1.348(6) . ?
C11 C12 1.342(5) . ?
C6 C5 1.343(5) . ?
C24 C25 1.494(6) . ?
C3 C4 1.351(6) . ?
C4 C5 1.420(6) . ?
C15 C16 1.358(6) . ?
O4 C20 1.433(4) . ?
O4 C19 1.418(6) . ?
C8 C9 1.431(5) . ?
C16 C17 1.430(6) . ?
C20 C21 1.498(7) . ?
C1 O1 1.319(5) . ?
C30 O9 1.427(4) . ?
O9 C29 1.416(6) . ?
C28 C29 1.491(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
O2 Hf1 O2 180.00(15) . 3_665 ?
O1 Hf1 O2 90.88(10) 3_665 3_665 ?
O1 Hf1 O2 89.12(10) . 3_665 ?
O1 Hf1 O2 89.12(10) 3_665 . ?
O1 Hf1 O2 90.88(10) . . ?
O1 Hf1 O1 180.00(14) 3_665 . ?
O3 Hf1 O2 90.57(10) 3_665 . ?
O3 Hf1 O2 89.43(10) 3_665 3_665 ?
O3 Hf1 O2 90.57(10) . 3_665 ?
O3 Hf1 O2 89.43(10) . . ?
O3 Hf1 O1 89.68(10) 3_665 3_665 ?
O3 Hf1 O1 90.32(10) 3_665 . ?
O3 Hf1 O1 89.68(10) . . ?
O3 Hf1 O1 90.32(10) . 3_665 ?
O3 Hf1 O3 180.00(14) 3_665 . ?
C2 P2 P1 94.06(13) . . ?
C1 P1 P2 94.26(13) . . ?
C14 P6 P5 94.62(14) . . ?
C7 P3 P4 94.54(14) . . ?
C13 P5 P6 93.94(15) . . ?
C8 P4 P3 93.64(15) . . ?
O7 Na8 O5 152.59(12) . . ?
O7 Na8 O6 70.81(9) . . ?
O7 Na8 O8 104.93(11) . . ?
O7 Na8 O4 102.36(12) . . ?
O7 Na8 O9 100.81(10) . . ?
O5 Na8 O8 93.08(12) . . ?
O5 Na8 O4 70.22(11) . . ?
O5 Na8 O9 104.29(10) . . ?
O6 Na8 O5 87.00(10) . . ?
O6 Na8 O8 96.46(11) . . ?
O6 Na8 O4 111.19(12) . . ?
O6 Na8 O9 164.35(12) . . ?
O8 Na8 O9 72.47(11) . . ?
O4 Na8 O8 146.20(11) . . ?
O4 Na8 O9 83.19(11) . . ?
C7 O2 Hf1 142.9(2) . . ?
C13 N3 C18 121.8(3) . . ?
C13 N3 C14 117.3(3) . . ?
C18 N3 C14 120.9(4) . . ?
C25 O7 Na8 113.6(2) . . ?
C25 O7 C26 111.4(4) . . ?
C26 O7 Na8 125.6(2) . . ?
C6 N6 C2 121.0(3) . . ?
C6 N6 C1 122.3(3) . . ?
C1 N6 C2 116.7(3) . . ?
C22 O5 Na8 125.0(3) . . ?
C22 O5 C21 111.7(3) . . ?
C21 O5 Na8 113.9(2) . . ?
N6 C2 P2 117.3(3) . . ?
N6 C2 C3 116.9(4) . . ?
C3 C2 P2 125.8(3) . . ?
C7 N10 C12 121.8(3) . . ?
C7 N10 C8 116.8(3) . . ?
C12 N10 C8 121.4(3) . . ?
C24 O6 Na8 110.3(2) . . ?
C23 O6 Na8 121.1(2) . . ?
C23 O6 C24 112.0(3) . . ?
N3 C13 P5 117.7(3) . . ?
O3 C13 P5 127.1(3) . . ?
O3 C13 N3 115.2(3) . . ?
C27 O8 Na8 127.6(3) . . ?
C27 O8 C28 110.9(3) . . ?
C28 O8 Na8 112.1(3) . . ?
O2 C7 P3 127.0(3) . . ?
O2 C7 N10 115.8(3) . . ?
N10 C7 P3 117.1(3) . . ?
C17 C18 N3 120.2(4) . . ?
N3 C14 P6 116.4(3) . . ?
C15 C14 P6 126.9(3) . . ?
C15 C14 N3 116.6(4) . . ?
C9 C10 C11 119.1(4) . . ?
C12 C11 C10 120.5(4) . . ?
C5 C6 N6 120.9(4) . . ?
O6 C24 C25 108.2(3) . . ?
C11 C12 N10 120.3(4) . . ?
C4 C3 C2 122.0(4) . . ?
C3 C4 C5 119.2(4) . . ?
C16 C15 C14 123.0(4) . . ?
C20 O4 Na8 111.8(3) . . ?
C19 O4 Na8 120.7(2) . . ?
C19 O4 C20 112.2(3) . . ?
N10 C8 P4 117.9(3) . . ?
N10 C8 C9 116.8(4) . . ?
C9 C8 P4 125.3(3) . . ?
C10 C9 C8 121.8(4) . . ?
O7 C25 C24 108.6(4) . . ?
C15 C16 C17 118.5(5) . . ?
O4 C20 C21 107.8(4) . . ?
C6 C5 C4 120.2(4) . . ?
N6 C1 P1 117.6(3) . . ?
O1 C1 P1 127.3(3) . . ?
O1 C1 N6 115.1(3) . . ?
O5 C21 C20 109.5(3) . . ?
C18 C17 C16 120.8(4) . . ?
C1 O1 Hf1 143.8(2) . . ?
C30 O9 Na8 132.6(3) . . ?
C29 O9 Na8 101.5(2) . . ?
C29 O9 C30 114.4(3) . . ?
O8 C28 C29 108.2(4) . . ?
O9 C29 C28 112.0(4) . . ?
C13 O3 Hf1 146.9(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
Hf1 O2 C7 P3 17.5(6) . . . . ?
Hf1 O2 C7 N10 -164.5(3) . . . . ?
P2 P1 C1 N6 -1.7(3) . . . . ?
P2 P1 C1 O1 178.9(3) . . . . ?
P2 C2 C3 C4 -180.0(3) . . . . ?
P1 P2 C2 N6 -0.5(3) . . . . ?
P1 P2 C2 C3 178.9(3) . . . . ?
P1 C1 O1 Hf1 11.2(6) . . . . ?
P6 P5 C13 N3 1.7(3) . . . . ?
P6 P5 C13 O3 -176.3(3) . . . . ?
P6 C14 C15 C16 -179.9(3) . . . . ?
P3 P4 C8 N10 0.7(3) . . . . ?
P3 P4 C8 C9 -177.2(3) . . . . ?
P5 P6 C14 N3 0.3(3) . . . . ?
P5 P6 C14 C15 179.1(3) . . . . ?
P5 C13 O3 Hf1 8.0(6) . . . . ?
P4 P3 C7 O2 177.3(3) . . . . ?
P4 P3 C7 N10 -0.7(3) . . . . ?
P4 C8 C9 C10 179.3(3) . . . . ?
Na8 O7 C25 C24 -39.4(4) . . . . ?
Na8 O5 C21 C20 39.5(4) . . . . ?
Na8 O6 C24 C25 -49.8(4) . . . . ?
Na8 O8 C28 C29 25.4(4) . . . . ?
Na8 O4 C20 C21 47.7(4) . . . . ?
Na8 O9 C29 C28 61.9(3) . . . . ?
O2 Hf1 O2 C7 -70(36) 3_665 . . . ?
O2 Hf1 O1 C1 -155.6(4) . . . . ?
O2 Hf1 O1 C1 24.4(4) 3_665 . . . ?
O2 Hf1 O3 C13 -130.2(4) . . . . ?
O2 Hf1 O3 C13 49.8(4) 3_665 . . . ?
N3 C13 O3 Hf1 -170.0(3) . . . . ?
N3 C18 C17 C16 1.1(6) . . . . ?
N3 C14 C15 C16 -1.1(6) . . . . ?
O7 Na8 O5 C22 127.1(3) . . . . ?
O7 Na8 O5 C21 -89.4(4) . . . . ?
O7 Na8 O6 C24 21.6(3) . . . . ?
O7 Na8 O6 C23 155.2(3) . . . . ?
O7 Na8 O8 C27 -42.5(3) . . . . ?
O7 Na8 O8 C28 100.4(3) . . . . ?
O7 Na8 O4 C20 131.9(3) . . . . ?
O7 Na8 O4 C19 -3.4(3) . . . . ?
O7 Na8 O9 C30 4.5(4) . . . . ?
O7 Na8 O9 C29 -134.9(2) . . . . ?
N6 C2 C3 C4 -0.5(5) . . . . ?
N6 C6 C5 C4 -0.3(6) . . . . ?
N6 C1 O1 Hf1 -168.2(3) . . . . ?
O5 Na8 O7 C25 -27.3(5) . . . . ?
O5 Na8 O7 C26 116.1(4) . . . . ?
O5 Na8 O6 C24 -174.7(3) . . . . ?
O5 Na8 O6 C23 -41.2(3) . . . . ?
O5 Na8 O8 C27 116.6(3) . . . . ?
O5 Na8 O8 C28 -100.4(3) . . . . ?
O5 Na8 O4 C20 -20.6(3) . . . . ?
O5 Na8 O4 C19 -155.9(3) . . . . ?
O5 Na8 O9 C30 -164.3(4) . . . . ?
O5 Na8 O9 C29 56.2(3) . . . . ?
C2 P2 P1 C1 1.13(17) . . . . ?
C2 N6 C6 C5 -0.1(5) . . . . ?
C2 N6 C1 P1 1.7(4) . . . . ?
C2 N6 C1 O1 -178.9(3) . . . . ?
C2 C3 C4 C5 0.1(6) . . . . ?
N10 C8 C9 C10 1.4(6) . . . . ?
O6 Na8 O7 C25 10.4(3) . . . . ?
O6 Na8 O7 C26 153.7(4) . . . . ?
O6 Na8 O5 C22 91.8(3) . . . . ?
O6 Na8 O5 C21 -124.7(3) . . . . ?
O6 Na8 O8 C27 29.3(3) . . . . ?
O6 Na8 O8 C28 172.2(2) . . . . ?
O6 Na8 O4 C20 57.9(3) . . . . ?
O6 Na8 O4 C19 -77.4(3) . . . . ?
O6 Na8 O9 C30 60.6(7) . . . . ?
O6 Na8 O9 C29 -78.9(5) . . . . ?
O6 C24 C25 O7 59.6(4) . . . . ?
C13 N3 C18 C17 178.1(4) . . . . ?
C13 N3 C14 P6 0.8(4) . . . . ?
C13 N3 C14 C15 -178.1(3) . . . . ?
O8 Na8 O7 C25 102.1(3) . . . . ?
O8 Na8 O7 C26 -114.5(4) . . . . ?
O8 Na8 O5 C22 -4.5(3) . . . . ?
O8 Na8 O5 C21 139.0(3) . . . . ?
O8 Na8 O6 C24 -82.0(3) . . . . ?
O8 Na8 O6 C23 51.6(3) . . . . ?
O8 Na8 O4 C20 -84.8(3) . . . . ?
O8 Na8 O4 C19 139.9(3) . . . . ?
O8 Na8 O9 C30 106.9(4) . . . . ?
O8 Na8 O9 C29 -32.5(2) . . . . ?
O8 C28 C29 O9 -62.1(5) . . . . ?
C7 P3 P4 C8 0.02(18) . . . . ?
C7 N10 C12 C11 -177.2(3) . . . . ?
C7 N10 C8 P4 -1.3(4) . . . . ?
C7 N10 C8 C9 176.8(3) . . . . ?
C18 N3 C13 P5 178.0(3) . . . . ?
C18 N3 C13 O3 -3.8(5) . . . . ?
C18 N3 C14 P6 -178.9(3) . . . . ?
C18 N3 C14 C15 2.1(5) . . . . ?
C14 P6 P5 C13 -0.97(18) . . . . ?
C14 N3 C13 P5 -1.8(4) . . . . ?
C14 N3 C13 O3 176.4(3) . . . . ?
C14 N3 C18 C17 -2.2(5) . . . . ?
C14 C15 C16 C17 0.1(7) . . . . ?
C10 C11 C12 N10 -0.4(6) . . . . ?
C11 C10 C9 C8 1.0(6) . . . . ?
C6 N6 C2 P2 -180.0(3) . . . . ?
C6 N6 C2 C3 0.6(5) . . . . ?
C6 N6 C1 P1 -178.9(3) . . . . ?
C6 N6 C1 O1 0.6(5) . . . . ?
C12 N10 C7 P3 -178.6(3) . . . . ?
C12 N10 C7 O2 3.2(5) . . . . ?
C12 N10 C8 P4 178.6(3) . . . . ?
C12 N10 C8 C9 -3.3(5) . . . . ?
C3 C4 C5 C6 0.4(6) . . . . ?
C23 O6 C24 C25 172.3(4) . . . . ?
C15 C16 C17 C18 0.0(6) . . . . ?
O4 Na8 O7 C25 -98.0(3) . . . . ?
O4 Na8 O7 C26 45.3(4) . . . . ?
O4 Na8 O5 C22 -154.4(3) . . . . ?
O4 Na8 O5 C21 -10.9(3) . . . . ?
O4 Na8 O6 C24 117.8(3) . . . . ?
O4 Na8 O6 C23 -108.6(3) . . . . ?
O4 Na8 O8 C27 174.7(3) . . . . ?
O4 Na8 O8 C28 -42.4(3) . . . . ?
O4 Na8 O9 C30 -96.8(4) . . . . ?
O4 Na8 O9 C29 123.7(2) . . . . ?
O4 C20 C21 O5 -57.8(5) . . . . ?
C8 N10 C7 P3 1.4(4) . . . . ?
C8 N10 C7 O2 -176.9(3) . . . . ?
C8 N10 C12 C11 2.8(6) . . . . ?
C9 C10 C11 C12 -1.5(6) . . . . ?
C22 O5 C21 C20 -172.1(3) . . . . ?
C1 N6 C2 P2 -0.5(4) . . . . ?
C1 N6 C2 C3 180.0(3) . . . . ?
C1 N6 C6 C5 -179.5(3) . . . . ?
C27 O8 C28 C29 174.7(4) . . . . ?
C19 O4 C20 C21 -173.1(3) . . . . ?
C30 O9 C29 C28 -86.5(4) . . . . ?
O1 Hf1 O2 C7 110.0(4) 3_665 . . . ?
O1 Hf1 O2 C7 -70.0(4) . . . . ?
O1 Hf1 O1 C1 -36(18) 3_665 . . . ?
O1 Hf1 O3 C13 140.7(4) 3_665 . . . ?
O1 Hf1 O3 C13 -39.3(4) . . . . ?
O9 Na8 O7 C25 176.7(3) . . . . ?
O9 Na8 O7 C26 -40.0(4) . . . . ?
O9 Na8 O5 C22 -77.2(3) . . . . ?
O9 Na8 O5 C21 66.3(3) . . . . ?
O9 Na8 O6 C24 -38.0(6) . . . . ?
O9 Na8 O6 C23 95.6(5) . . . . ?
O9 Na8 O8 C27 -139.3(3) . . . . ?
O9 Na8 O8 C28 3.6(2) . . . . ?
O9 Na8 O4 C20 -128.5(3) . . . . ?
O9 Na8 O4 C19 96.2(3) . . . . ?
C26 O7 C25 C24 172.0(3) . . . . ?
O3 Hf1 O2 C7 -160.3(4) 3_665 . . . ?
O3 Hf1 O2 C7 19.7(4) . . . . ?
O3 Hf1 O1 C1 115.0(4) . . . . ?
O3 Hf1 O1 C1 -65.0(4) 3_665 . . . ?
O3 Hf1 O3 C13 -35(19) 3_665 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DME/THF'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
