# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and 
#  data retrieval see:
#                         www.ccdc.cam.ac.uk 
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively. 
#
####################################################################### 

data_greme
_database_code_depnum_ccdc_archive 'CCDC 926716'
#TrackingRef 'agriw.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H21 Mo N O4 P2'
_chemical_formula_weight         617.36
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
loop_
_symmetry_equiv_pos_as_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                   15.5796(4)
_cell_length_b                   9.4484(2)
_cell_length_c                   19.0086(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2798.11(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19466
_cell_measurement_theta_min      2.1385
_cell_measurement_theta_max      30.7842
_exptl_crystal_description       tablet
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96238
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       \w-scan
_diffrn_detector_area_resol_mean 16.1419
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            70559
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         30.51
_reflns_number_total             8221
_reflns_number_gt                7704
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The NH hydrogen was refined freely but with a DFIX restraint to the NH
bond length. The methyl group was refined as an idealised rigid group
allowed to rotate but not tip. Other H were included at calculated
positions and refined using a riding model.
The structure was refined as a racemic twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+1.0112P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.392(18)
_refine_ls_number_reflns         8221
_refine_ls_number_parameters     349
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0242
_refine_ls_wR_factor_ref         0.0521
_refine_ls_wR_factor_gt          0.0497
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo Mo 0.641807(9) 0.309642(12) 0.220358(10) 0.01244(3) Uani 1 1 d . . .
N1 N 0.70929(10) 0.77084(16) 0.31682(8) 0.0146(3) Uani 1 1 d D . .
H01 H 0.7066(16) 0.8559(17) 0.3133(13) 0.027(6) Uiso 1 1 d D . .
C2 C 0.65584(11) 0.68282(18) 0.27999(9) 0.0119(3) Uani 1 1 d . . .
P3 P 0.68349(3) 0.50880(5) 0.29293(2) 0.01203(9) Uani 1 1 d . . .
C3A C 0.77172(11) 0.55541(18) 0.34567(9) 0.0131(3) Uani 1 1 d . . .
C4 C 0.83307(12) 0.47131(19) 0.38039(9) 0.0144(3) Uani 1 1 d . . .
H4 H 0.8313 0.3712 0.3758 0.017 Uiso 1 1 calc R . .
C5 C 0.89590(12) 0.5342(2) 0.42116(10) 0.0174(4) Uani 1 1 d . . .
C6 C 0.89623(13) 0.6837(2) 0.42841(11) 0.0195(4) Uani 1 1 d . . .
H6 H 0.9388 0.7266 0.4571 0.023 Uiso 1 1 calc R . .
C7 C 0.83695(13) 0.7684(2) 0.39521(10) 0.0191(4) Uani 1 1 d . . .
H7 H 0.8385 0.8684 0.4006 0.023 Uiso 1 1 calc R . .
C7A C 0.77440(12) 0.70399(18) 0.35327(9) 0.0142(3) Uani 1 1 d . . .
C8 C 0.96378(13) 0.4463(2) 0.45625(11) 0.0233(4) Uani 1 1 d . . .
H8A H 0.9365 0.3761 0.4870 0.035 Uiso 1 1 calc R . .
H8B H 1.0012 0.5076 0.4843 0.035 Uiso 1 1 calc R . .
H8C H 0.9980 0.3976 0.4204 0.035 Uiso 1 1 calc R . .
C9 C 0.67894(15) 0.1660(2) 0.28929(11) 0.0221(4) Uani 1 1 d . . .
O1 O 0.70102(12) 0.08257(16) 0.33024(8) 0.0336(4) Uani 1 1 d . . .
C10 C 0.61536(15) 0.1592(2) 0.14877(11) 0.0223(4) Uani 1 1 d . . .
O2 O 0.60372(13) 0.07202(17) 0.10780(9) 0.0378(4) Uani 1 1 d . . .
C11 C 0.52192(14) 0.3021(2) 0.26460(10) 0.0210(4) Uani 1 1 d . . .
O3 O 0.45737(11) 0.29560(18) 0.29277(9) 0.0361(4) Uani 1 1 d . . .
C12 C 0.76619(13) 0.3178(2) 0.18717(10) 0.0187(4) Uani 1 1 d . . .
O4 O 0.83733(10) 0.32405(17) 0.17335(8) 0.0295(4) Uani 1 1 d . . .
P1 P 0.59856(3) 0.51413(5) 0.14082(2) 0.01068(8) Uani 1 1 d . . .
C21 C 0.57951(12) 0.73479(18) 0.24320(9) 0.0130(3) Uani 1 1 d . . .
C22 C 0.54524(12) 0.66715(19) 0.18292(9) 0.0137(3) Uani 1 1 d . . .
C23 C 0.47000(12) 0.7210(2) 0.15312(10) 0.0188(4) Uani 1 1 d . . .
H23 H 0.4459 0.6749 0.1134 0.023 Uiso 1 1 calc R . .
C24 C 0.42970(13) 0.8402(2) 0.18013(11) 0.0219(4) Uani 1 1 d . . .
H24 H 0.3789 0.8753 0.1587 0.026 Uiso 1 1 calc R . .
C25 C 0.46380(12) 0.9078(2) 0.23846(9) 0.0189(4) Uani 1 1 d . . .
H25 H 0.4368 0.9899 0.2569 0.023 Uiso 1 1 calc R . .
C26 C 0.53754(12) 0.85507(19) 0.26967(10) 0.0166(4) Uani 1 1 d . . .
H26 H 0.5602 0.9014 0.3099 0.020 Uiso 1 1 calc R . .
C31 C 0.68538(11) 0.59742(19) 0.09107(9) 0.0134(3) Uani 1 1 d . . .
C32 C 0.73515(12) 0.5095(2) 0.04846(9) 0.0170(4) Uani 1 1 d . . .
H32 H 0.7261 0.4101 0.0495 0.020 Uiso 1 1 calc R . .
C33 C 0.79782(13) 0.5657(2) 0.00456(11) 0.0234(4) Uani 1 1 d . . .
H33 H 0.8309 0.5050 -0.0246 0.028 Uiso 1 1 calc R . .
C34 C 0.81193(14) 0.7106(2) 0.00337(11) 0.0264(5) Uani 1 1 d . . .
H34 H 0.8545 0.7495 -0.0268 0.032 Uiso 1 1 calc R . .
C35 C 0.76373(14) 0.7983(2) 0.04630(11) 0.0245(4) Uani 1 1 d . . .
H35 H 0.7741 0.8974 0.0461 0.029 Uiso 1 1 calc R . .
C36 C 0.70025(13) 0.7427(2) 0.08974(10) 0.0188(4) Uani 1 1 d . . .
H36 H 0.6670 0.8040 0.1185 0.023 Uiso 1 1 calc R . .
C41 C 0.52418(11) 0.46830(19) 0.06959(9) 0.0132(3) Uani 1 1 d . . .
C42 C 0.46100(12) 0.3671(2) 0.08287(10) 0.0178(4) Uani 1 1 d . . .
H42 H 0.4583 0.3227 0.1277 0.021 Uiso 1 1 calc R . .
C43 C 0.40221(13) 0.3307(2) 0.03124(10) 0.0209(4) Uani 1 1 d . . .
H43 H 0.3591 0.2623 0.0410 0.025 Uiso 1 1 calc R . .
C44 C 0.40600(13) 0.3933(2) -0.03447(10) 0.0194(4) Uani 1 1 d . . .
H44 H 0.3659 0.3676 -0.0699 0.023 Uiso 1 1 calc R . .
C45 C 0.46862(13) 0.4937(2) -0.04846(10) 0.0194(4) Uani 1 1 d . . .
H45 H 0.4713 0.5370 -0.0935 0.023 Uiso 1 1 calc R . .
C46 C 0.52731(13) 0.5312(2) 0.00315(10) 0.0160(4) Uani 1 1 d . . .
H46 H 0.5700 0.6002 -0.0068 0.019 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo 0.01798(6) 0.00882(5) 0.01053(6) -0.00039(7) -0.00270(7) -0.00094(5)
N1 0.0170(8) 0.0082(7) 0.0185(8) -0.0019(6) -0.0041(6) -0.0007(6)
C2 0.0134(8) 0.0120(8) 0.0102(8) -0.0020(6) 0.0017(6) -0.0002(6)
P3 0.0133(2) 0.01060(19) 0.0122(2) -0.00132(17) -0.00182(16) -0.00019(16)
C3A 0.0138(8) 0.0145(8) 0.0109(8) -0.0006(6) 0.0001(6) -0.0003(7)
C4 0.0145(8) 0.0157(8) 0.0129(8) -0.0005(6) 0.0006(6) 0.0016(7)
C5 0.0152(9) 0.0218(9) 0.0153(9) 0.0003(7) -0.0010(7) 0.0003(7)
C6 0.0165(9) 0.0231(10) 0.0191(9) -0.0006(8) -0.0068(7) -0.0026(8)
C7 0.0210(9) 0.0142(8) 0.0221(9) -0.0030(7) -0.0052(8) -0.0026(7)
C7A 0.0141(8) 0.0154(8) 0.0131(8) -0.0005(6) -0.0002(6) -0.0005(7)
C8 0.0193(10) 0.0263(10) 0.0244(10) 0.0003(8) -0.0065(8) 0.0034(8)
C9 0.0353(12) 0.0140(8) 0.0170(9) -0.0032(7) -0.0075(9) -0.0016(8)
O1 0.0614(12) 0.0153(7) 0.0242(8) 0.0028(6) -0.0162(8) 0.0010(7)
C10 0.0329(11) 0.0161(9) 0.0179(10) -0.0001(8) -0.0048(8) 0.0019(8)
O2 0.0624(12) 0.0231(8) 0.0281(8) -0.0107(7) -0.0118(8) -0.0001(8)
C11 0.0277(11) 0.0215(9) 0.0138(8) 0.0000(7) -0.0032(8) -0.0080(8)
O3 0.0299(9) 0.0500(10) 0.0284(8) -0.0044(8) 0.0080(7) -0.0166(8)
C12 0.0236(10) 0.0173(9) 0.0153(9) -0.0032(7) -0.0050(8) 0.0079(8)
O4 0.0202(8) 0.0388(9) 0.0296(8) -0.0051(7) 0.0005(6) 0.0084(7)
P1 0.0114(2) 0.01038(19) 0.01027(19) -0.00069(16) -0.00057(16) -0.00042(16)
C21 0.0134(8) 0.0123(8) 0.0131(7) -0.0005(6) 0.0019(6) 0.0010(7)
C22 0.0129(8) 0.0138(8) 0.0146(8) -0.0007(6) 0.0007(7) 0.0013(7)
C23 0.0160(9) 0.0222(9) 0.0183(9) -0.0039(7) -0.0035(7) 0.0027(7)
C24 0.0176(9) 0.0249(10) 0.0230(10) -0.0024(8) -0.0031(8) 0.0078(8)
C25 0.0189(9) 0.0182(8) 0.0198(10) -0.0037(7) 0.0015(7) 0.0059(7)
C26 0.0186(9) 0.0144(8) 0.0168(8) -0.0032(7) 0.0012(7) 0.0014(7)
C31 0.0122(8) 0.0169(8) 0.0111(7) 0.0013(7) -0.0022(6) -0.0009(7)
C32 0.0157(9) 0.0184(9) 0.0168(9) 0.0009(7) 0.0002(7) 0.0014(7)
C33 0.0176(10) 0.0346(12) 0.0178(9) -0.0011(8) 0.0042(8) 0.0027(8)
C34 0.0199(10) 0.0355(12) 0.0236(10) 0.0063(9) 0.0033(8) -0.0075(9)
C35 0.0262(11) 0.0221(10) 0.0253(10) 0.0051(8) 0.0012(8) -0.0085(8)
C36 0.0193(9) 0.0159(9) 0.0211(9) -0.0001(7) -0.0003(8) -0.0018(7)
C41 0.0144(8) 0.0130(8) 0.0121(8) -0.0028(6) -0.0013(6) 0.0003(6)
C42 0.0184(9) 0.0220(9) 0.0129(8) 0.0016(7) -0.0009(7) -0.0039(7)
C43 0.0179(9) 0.0245(10) 0.0204(9) -0.0005(8) -0.0023(7) -0.0071(8)
C44 0.0181(9) 0.0234(10) 0.0169(9) -0.0024(7) -0.0074(7) 0.0001(8)
C45 0.0235(10) 0.0207(9) 0.0139(9) 0.0039(8) -0.0046(7) 0.0013(8)
C46 0.0182(9) 0.0146(9) 0.0154(9) 0.0015(7) -0.0015(7) -0.0009(7)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo C9 1.973(2) . ?
Mo C10 2.011(2) . ?
Mo C12 2.039(2) . ?
Mo C11 2.050(2) . ?
Mo P3 2.4219(5) . ?
Mo P1 2.5442(5) . ?
N1 C2 1.369(2) . ?
N1 C7A 1.381(2) . ?
C2 C21 1.464(2) . ?
C2 P3 1.7173(17) . ?
P3 C3A 1.7574(18) . ?
C3A C4 1.407(2) . ?
C3A C7A 1.412(2) . ?
C4 C5 1.383(3) . ?
C5 C6 1.419(3) . ?
C5 C8 1.501(3) . ?
C6 C7 1.376(3) . ?
C7 C7A 1.399(2) . ?
C9 O1 1.160(2) . ?
C10 O2 1.148(2) . ?
C11 O3 1.141(3) . ?
C12 O4 1.140(3) . ?
P1 C31 1.8284(18) . ?
P1 C41 1.8340(18) . ?
P1 C22 1.8496(18) . ?
C21 C26 1.404(2) . ?
C21 C22 1.417(2) . ?
C22 C23 1.398(3) . ?
C23 C24 1.387(3) . ?
C24 C25 1.386(3) . ?
C25 C26 1.386(3) . ?
C31 C36 1.393(3) . ?
C31 C32 1.396(3) . ?
C32 C33 1.390(3) . ?
C33 C34 1.387(3) . ?
C34 C35 1.385(3) . ?
C35 C36 1.391(3) . ?
C41 C42 1.396(3) . ?
C41 C46 1.396(3) . ?
C42 C43 1.386(3) . ?
C43 C44 1.383(3) . ?
C44 C45 1.387(3) . ?
C45 C46 1.387(2) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 Mo C10 91.33(7) . . ?
C9 Mo C12 87.31(9) . . ?
C10 Mo C12 90.70(9) . . ?
C9 Mo C11 88.32(9) . . ?
C10 Mo C11 93.81(9) . . ?
C12 Mo C11 173.79(8) . . ?
C9 Mo P3 94.45(6) . . ?
C10 Mo P3 171.81(7) . . ?
C12 Mo P3 83.80(5) . . ?
C11 Mo P3 92.15(6) . . ?
C9 Mo P1 174.05(6) . . ?
C10 Mo P1 94.61(6) . . ?
C12 Mo P1 92.23(5) . . ?
C11 Mo P1 91.66(6) . . ?
P3 Mo P1 79.598(13) . . ?
C2 N1 C7A 115.17(15) . . ?
N1 C2 C21 122.29(15) . . ?
N1 C2 P3 110.84(13) . . ?
C21 C2 P3 126.38(13) . . ?
C2 P3 C3A 92.17(8) . . ?
C2 P3 Mo 126.51(6) . . ?
C3A P3 Mo 136.83(6) . . ?
C4 C3A C7A 119.56(16) . . ?
C4 C3A P3 131.09(14) . . ?
C7A C3A P3 109.31(13) . . ?
C5 C4 C3A 120.06(17) . . ?
C4 C5 C6 119.00(17) . . ?
C4 C5 C8 120.64(18) . . ?
C6 C5 C8 120.34(17) . . ?
C7 C6 C5 122.17(18) . . ?
C6 C7 C7A 118.40(17) . . ?
N1 C7A C7 126.76(16) . . ?
N1 C7A C3A 112.43(16) . . ?
C7 C7A C3A 120.79(17) . . ?
O1 C9 Mo 179.34(18) . . ?
O2 C10 Mo 177.2(2) . . ?
O3 C11 Mo 176.06(18) . . ?
O4 C12 Mo 175.24(17) . . ?
C31 P1 C41 100.79(8) . . ?
C31 P1 C22 102.68(8) . . ?
C41 P1 C22 102.73(8) . . ?
C31 P1 Mo 116.00(6) . . ?
C41 P1 Mo 115.26(6) . . ?
C22 P1 Mo 117.09(6) . . ?
C26 C21 C22 118.64(16) . . ?
C26 C21 C2 118.59(16) . . ?
C22 C21 C2 122.76(15) . . ?
C23 C22 C21 118.66(16) . . ?
C23 C22 P1 119.07(14) . . ?
C21 C22 P1 122.24(13) . . ?
C24 C23 C22 121.67(17) . . ?
C25 C24 C23 119.79(18) . . ?
C26 C25 C24 119.63(17) . . ?
C25 C26 C21 121.59(17) . . ?
C36 C31 C32 118.95(17) . . ?
C36 C31 P1 123.83(14) . . ?
C32 C31 P1 117.06(14) . . ?
C33 C32 C31 120.73(18) . . ?
C34 C33 C32 119.91(19) . . ?
C35 C34 C33 119.70(19) . . ?
C34 C35 C36 120.61(19) . . ?
C35 C36 C31 120.09(19) . . ?
C42 C41 C46 118.67(16) . . ?
C42 C41 P1 118.28(14) . . ?
C46 C41 P1 123.04(14) . . ?
C43 C42 C41 120.53(17) . . ?
C44 C43 C42 120.34(18) . . ?
C43 C44 C45 119.73(17) . . ?
C44 C45 C46 120.18(16) . . ?
C45 C46 C41 120.54(16) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H01 O1 0.808(16) 2.167(17) 2.959(2) 167(2) 1_565
C42 H42 O4 0.95 2.50 3.151(2) 126.2 3_455
C43 H43 O4 0.95 2.67 3.234(3) 118.8 3_455
_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.064
_iucr_refine_instructions_details 
;
TITL greme in Pna2(1)
CELL 0.71073 15.579552 9.448430 19.008628 90.0000 90.0000 90.0000
ZERR 4.00 0.0004 0.0002 0.0004 0.0000 0.0000 0.0000
LATT -1
SYMM -x,-y, z+1/2
SYMM x+1/2,-y+1/2, z
SYMM -x+1/2, y+1/2, z+1/2
SFAC C H N O P Mo
UNIT 120.00 84.00 4.00 16.00 8.00 4.00
TEMP -173
SIZE 0.4 0.25 0.1
FMAP 2
PLAN 10
L.S. 4
OMIT 0 0 2
TWIN
SHEL 999 0.7
ACTA
DFIX 0.85 0.02 N1 H01
EQIV $1 x,1+y,z
HTAB N1 O1_$1
EQIV $2 -0.5+x,0.5-y,z
HTAB C42 O4_$2
HTAB C43 O4_$2
WGHT 0.019700 1.011200
BASF 0.39151
FVAR 3.84041
MO 6 0.641807 0.309642 0.220358 11.00000 0.01798 0.00882 =
0.01053 -0.00039 -0.00270 -0.00094
N1 3 0.709293 0.770838 0.316816 11.00000 0.01697 0.00825 =
0.01854 -0.00192 -0.00408 -0.00066
H01 2 0.706576 0.855937 0.313316 11.00000 0.02709
C2 1 0.655842 0.682815 0.279987 11.00000 0.01339 0.01204 =
0.01022 -0.00205 0.00174 -0.00023
P3 5 0.683486 0.508803 0.292929 11.00000 0.01333 0.01060 =
0.01215 -0.00132 -0.00182 -0.00019
C3A 1 0.771716 0.555415 0.345671 11.00000 0.01383 0.01450 =
0.01092 -0.00060 0.00012 -0.00031
C4 1 0.833072 0.471310 0.380388 11.00000 0.01453 0.01574 =
0.01286 -0.00046 0.00063 0.00161
AFIX 43
H4 2 0.831322 0.371229 0.375807 11.00000 -1.20000
AFIX 0
C5 1 0.895899 0.534220 0.421161 11.00000 0.01516 0.02184 =
0.01529 0.00032 -0.00096 0.00027
C6 1 0.896232 0.683661 0.428410 11.00000 0.01646 0.02307 =
0.01911 -0.00060 -0.00685 -0.00265
AFIX 43
H6 2 0.938793 0.726609 0.457135 11.00000 -1.20000
AFIX 0
C7 1 0.836948 0.768442 0.395209 11.00000 0.02104 0.01415 =
0.02207 -0.00295 -0.00525 -0.00260
AFIX 43
H7 2 0.838464 0.868361 0.400643 11.00000 -1.20000
AFIX 0
C7A 1 0.774399 0.703988 0.353270 11.00000 0.01413 0.01545 =
0.01306 -0.00051 -0.00022 -0.00055
C8 1 0.963780 0.446264 0.456251 11.00000 0.01935 0.02629 =
0.02441 0.00030 -0.00645 0.00345
AFIX 137
H8A 2 0.936496 0.376148 0.486964 11.00000 -1.50000
H8B 2 1.001180 0.507618 0.484328 11.00000 -1.50000
H8C 2 0.997973 0.397611 0.420366 11.00000 -1.50000
AFIX 0
C9 1 0.678935 0.165977 0.289292 11.00000 0.03529 0.01404 =
0.01704 -0.00318 -0.00750 -0.00159
O1 4 0.701023 0.082570 0.330236 11.00000 0.06142 0.01534 =
0.02419 0.00275 -0.01621 0.00099
C10 1 0.615361 0.159185 0.148767 11.00000 0.03288 0.01611 =
0.01792 -0.00006 -0.00481 0.00192
O2 4 0.603724 0.072020 0.107804 11.00000 0.06236 0.02308 =
0.02805 -0.01073 -0.01176 -0.00014
C11 1 0.521919 0.302107 0.264605 11.00000 0.02769 0.02150 =
0.01383 -0.00005 -0.00321 -0.00804
O3 4 0.457368 0.295603 0.292771 11.00000 0.02990 0.04999 =
0.02838 -0.00441 0.00799 -0.01656
C12 1 0.766194 0.317843 0.187167 11.00000 0.02360 0.01729 =
0.01526 -0.00324 -0.00505 0.00790
O4 4 0.837327 0.324047 0.173353 11.00000 0.02022 0.03878 =
0.02962 -0.00513 0.00052 0.00839
P1 5 0.598561 0.514131 0.140818 11.00000 0.01140 0.01038 =
0.01027 -0.00069 -0.00057 -0.00042
C21 1 0.579513 0.734794 0.243205 11.00000 0.01343 0.01234 =
0.01310 -0.00054 0.00187 0.00097
C22 1 0.545241 0.667155 0.182924 11.00000 0.01286 0.01379 =
0.01459 -0.00067 0.00066 0.00125
C23 1 0.470000 0.721039 0.153120 11.00000 0.01598 0.02225 =
0.01830 -0.00390 -0.00353 0.00275
AFIX 43
H23 2 0.445852 0.674909 0.113368 11.00000 -1.20000
AFIX 0
C24 1 0.429699 0.840187 0.180127 11.00000 0.01765 0.02491 =
0.02304 -0.00244 -0.00310 0.00782
AFIX 43
H24 2 0.378888 0.875274 0.158697 11.00000 -1.20000
AFIX 0
C25 1 0.463801 0.907846 0.238458 11.00000 0.01889 0.01817 =
0.01977 -0.00373 0.00154 0.00591
AFIX 43
H25 2 0.436781 0.989949 0.256946 11.00000 -1.20000
AFIX 0
C26 1 0.537535 0.855070 0.269667 11.00000 0.01857 0.01437 =
0.01680 -0.00322 0.00120 0.00141
AFIX 43
H26 2 0.560237 0.901373 0.309939 11.00000 -1.20000
AFIX 0
C31 1 0.685377 0.597425 0.091069 11.00000 0.01224 0.01688 =
0.01114 0.00130 -0.00216 -0.00093
C32 1 0.735150 0.509476 0.048457 11.00000 0.01574 0.01840 =
0.01679 0.00091 0.00022 0.00141
AFIX 43
H32 2 0.726094 0.410066 0.049466 11.00000 -1.20000
AFIX 0
C33 1 0.797824 0.565727 0.004559 11.00000 0.01761 0.03463 =
0.01781 -0.00109 0.00424 0.00271
AFIX 43
H33 2 0.830946 0.504993 -0.024586 11.00000 -1.20000
AFIX 0
C34 1 0.811933 0.710619 0.003366 11.00000 0.01990 0.03555 =
0.02362 0.00626 0.00332 -0.00747
AFIX 43
H34 2 0.854475 0.749509 -0.026772 11.00000 -1.20000
AFIX 0
C35 1 0.763729 0.798349 0.046304 11.00000 0.02618 0.02206 =
0.02528 0.00513 0.00120 -0.00850
AFIX 43
H35 2 0.774094 0.897431 0.046104 11.00000 -1.20000
AFIX 0
C36 1 0.700248 0.742728 0.089743 11.00000 0.01934 0.01588 =
0.02108 -0.00008 -0.00032 -0.00176
AFIX 43
H36 2 0.667007 0.803963 0.118536 11.00000 -1.20000
AFIX 0
C41 1 0.524184 0.468297 0.069587 11.00000 0.01443 0.01302 =
0.01213 -0.00279 -0.00134 0.00033
C42 1 0.461001 0.367056 0.082875 11.00000 0.01841 0.02201 =
0.01290 0.00160 -0.00088 -0.00387
AFIX 43
H42 2 0.458272 0.322735 0.127679 11.00000 -1.20000
AFIX 0
C43 1 0.402208 0.330655 0.031237 11.00000 0.01789 0.02451 =
0.02038 -0.00050 -0.00233 -0.00709
AFIX 43
H43 2 0.359082 0.262350 0.041016 11.00000 -1.20000
AFIX 0
C44 1 0.406003 0.393279 -0.034474 11.00000 0.01809 0.02335 =
0.01689 -0.00238 -0.00740 0.00013
AFIX 43
H44 2 0.365874 0.367584 -0.069870 11.00000 -1.20000
AFIX 0
C45 1 0.468621 0.493714 -0.048464 11.00000 0.02351 0.02069 =
0.01386 0.00392 -0.00461 0.00132
AFIX 43
H45 2 0.471331 0.536983 -0.093523 11.00000 -1.20000
AFIX 0
C46 1 0.527309 0.531169 0.003152 11.00000 0.01815 0.01455 =
0.01545 0.00151 -0.00151 -0.00088
AFIX 43
H46 2 0.569981 0.600161 -0.006772 11.00000 -1.20000
HKLF 4
;