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

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

data_AF046_a
_database_code_depnum_ccdc_archive 'CCDC 1562701'
_audit_update_record             
;
2017-07-17 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;

_audit_creation_date             2016-07-01
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_formula_moiety         'C15 H13 Mo N5 O2'
_chemical_formula_sum            'C15 H13 Mo N5 O2'
_chemical_formula_weight         391.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

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

_cell_length_a                   16.961(11)
_cell_length_b                   13.755(6)
_cell_length_c                   6.589(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1537.3(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2517
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      31.11
_cell_special_details            
;
To simulate systematic errors the final estimation of uncertainties
in unit cell parameters was based on 32 Monte-Carlo simulations.
;


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Bruker Kryoflex2).
;
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_F_000             784
_exptl_crystal_preparation       
'Crystal fragment soaked in perfluoro polyether oil.'
_exptl_crystal_recrystallization_method 
'recrystallised from dchloromethane and hexane by evaporation'
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.194
_exptl_absorpt_coefficient_mu    0.870
_shelx_estimated_absorpt_T_min   0.685
_shelx_estimated_absorpt_T_max   0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_T_max  0.7465
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2.00 -1.00 1.00 0.0580
2.00 -1.00 0.00 0.0960
2.00 -1.00 -1.00 0.1840
-2.00 1.00 2.00 0.0670
2.00 -2.00 1.00 0.0730
-2.00 2.00 -1.00 0.2000
-1.00 1.00 0.00 0.1320
0.00 1.00 -1.00 0.2260
-1.00 2.00 1.00 0.1180
0.00 1.00 0.00 0.1730
-1.00 -2.00 1.00 0.0790
0.00 -2.00 -1.00 0.1810
-1.00 -2.00 0.00 0.0920
1.00 -1.00 -2.00 0.1860
-1.00 0.00 1.00 0.0480
2.00 2.00 1.00 0.1130
2.00 1.00 0.00 0.1440
1.00 1.00 1.00 0.0930
-2.00 -1.00 -1.00 0.1300
-2.00 0.00 -1.00 0.1390
-1.00 0.00 0.00 0.0240
1.00 0.00 0.00 0.1130
-3.00 -1.00 -1.00 0.1120
-3.00 -2.00 -1.00 0.1110
-3.00 -2.00 0.00 0.0530
3.00 2.00 0.00 0.1550
2.00 0.00 -3.00 0.1770
-1.00 -1.00 3.00 0.0490

_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            9005
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         2.822
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1577
_reflns_number_gt                1245
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0228P)²+0.7684P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1577
_refine_ls_number_parameters     120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0596
_refine_ls_wR_factor_gt          0.0555
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.50048(2) 0.2500 0.68075(4) 0.00934(10) Uani 1 2 d S T P . .
C1 C 0.42280(14) 0.15730(17) 0.5773(4) 0.0155(5) Uani 1 1 d . . . . .
N1 N 0.44246(15) 0.2500 0.9759(4) 0.0143(6) Uani 1 2 d S T P . .
O1 O 0.37694(10) 0.10174(12) 0.5160(3) 0.0250(4) Uani 1 1 d . . . . .
C3 C 0.63036(15) -0.00149(17) 0.9593(4) 0.0198(6) Uani 1 1 d . . . . .
H3 H 0.6241 -0.0701 0.9596 0.024 Uiso 1 1 calc R U . . .
N3 N 0.30578(17) 0.2500 1.0360(5) 0.0286(8) Uani 1 2 d S T P . .
N2 N 0.37237(16) 0.2500 1.0016(4) 0.0148(6) Uani 1 2 d S T P . .
C2 C 0.57846(14) 0.05688(17) 0.8530(3) 0.0167(5) Uani 1 1 d . . . . .
H2 H 0.5369 0.0270 0.7791 0.020 Uiso 1 1 calc R U . . .
C6 C 0.64320(12) 0.19660(16) 0.9581(3) 0.0125(5) Uani 1 1 d . . . . .
C8 C 0.5936(2) 0.2500 0.4447(5) 0.0172(7) Uani 1 2 d S T P . .
H8 H 0.643(2) 0.2500 0.507(6) 0.021 Uiso 1 2 d S U P . .
C5 C 0.69804(13) 0.14138(17) 1.0650(3) 0.0154(5) Uani 1 1 d . . . . .
H5 H 0.7396 0.1722 1.1374 0.019 Uiso 1 1 calc R U . . .
N4 N 0.58441(11) 0.15392(14) 0.8499(3) 0.0113(4) Uani 1 1 d . . . . .
C4 C 0.69135(14) 0.04126(18) 1.0647(4) 0.0197(5) Uani 1 1 d . . . . .
H4 H 0.7284 0.0024 1.1363 0.024 Uiso 1 1 calc R U . . .
C7 C 0.55135(15) 0.16367(18) 0.4067(4) 0.0176(5) Uani 1 1 d . . . . .
H7A H 0.5762(15) 0.1027(19) 0.438(4) 0.021 Uiso 1 1 d . U . . .
H7B H 0.5151(14) 0.160(2) 0.292(4) 0.021 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C1 1.956(2) . ?
Mo1 C1 1.956(2) 7_565 ?
Mo1 N1 2.180(3) . ?
Mo1 C8 2.216(3) . ?
Mo1 N4 2.240(2) . ?
Mo1 N4 2.240(2) 7_565 ?
Mo1 C7 2.327(2) . ?
Mo1 C7 2.327(2) 7_565 ?
C1 O1 1.163(3) . ?
N1 N2 1.201(4) . ?
C3 C4 1.378(4) . ?
C3 C2 1.382(3) . ?
C3 H3 0.9500 . ?
N3 N2 1.152(4) . ?
C2 N4 1.339(3) . ?
C2 H2 0.9500 . ?
C6 N4 1.359(3) . ?
C6 C5 1.392(3) . ?
C6 C6 1.469(4) 7_565 ?
C8 C7 1.409(3) . ?
C8 C7 1.409(3) 7_565 ?
C8 H8 0.93(3) . ?
C5 C4 1.382(3) . ?
C5 H5 0.9500 . ?
C4 H4 0.9500 . ?
C7 H7A 0.96(3) . ?
C7 H7B 0.97(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
C1 Mo1 C1 81.36(14) . 7_565 ?
C1 Mo1 N1 90.39(9) . . ?
C1 Mo1 N1 90.39(9) 7_565 . ?
C1 Mo1 C8 103.62(10) . . ?
C1 Mo1 C8 103.62(10) 7_565 . ?
N1 Mo1 C8 161.41(11) . . ?
C1 Mo1 N4 102.53(9) . . ?
C1 Mo1 N4 170.47(8) 7_565 . ?
N1 Mo1 N4 80.96(8) . . ?
C8 Mo1 N4 84.06(9) . . ?
C1 Mo1 N4 170.47(8) . 7_565 ?
C1 Mo1 N4 102.53(9) 7_565 7_565 ?
N1 Mo1 N4 80.96(8) . 7_565 ?
C8 Mo1 N4 84.06(9) . 7_565 ?
N4 Mo1 N4 72.33(10) . 7_565 ?
C1 Mo1 C7 69.31(10) . . ?
C1 Mo1 C7 108.18(10) 7_565 . ?
N1 Mo1 C7 149.29(6) . . ?
C8 Mo1 C7 36.03(8) . . ?
N4 Mo1 C7 81.35(8) . . ?
N4 Mo1 C7 116.86(9) 7_565 . ?
C1 Mo1 C7 108.18(10) . 7_565 ?
C1 Mo1 C7 69.31(10) 7_565 7_565 ?
N1 Mo1 C7 149.29(6) . 7_565 ?
C8 Mo1 C7 36.03(8) . 7_565 ?
N4 Mo1 C7 116.86(9) . 7_565 ?
N4 Mo1 C7 81.35(8) 7_565 7_565 ?
C7 Mo1 C7 61.36(13) . 7_565 ?
O1 C1 Mo1 179.6(2) . . ?
N2 N1 Mo1 124.9(2) . . ?
C4 C3 C2 119.1(2) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
N3 N2 N1 176.7(4) . . ?
N4 C2 C3 122.6(2) . . ?
N4 C2 H2 118.7 . . ?
C3 C2 H2 118.7 . . ?
N4 C6 C5 121.3(2) . . ?
N4 C6 C6 115.60(12) . 7_565 ?
C5 C6 C6 123.05(14) . 7_565 ?
C7 C8 C7 114.8(3) . 7_565 ?
C7 C8 Mo1 76.27(16) . . ?
C7 C8 Mo1 76.27(16) 7_565 . ?
C7 C8 H8 122.3(2) . . ?
C7 C8 H8 122.3(2) 7_565 . ?
Mo1 C8 H8 109(2) . . ?
C4 C5 C6 119.2(2) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C2 N4 C6 118.6(2) . . ?
C2 N4 Mo1 123.21(16) . . ?
C6 N4 Mo1 118.19(15) . . ?
C3 C4 C5 119.2(2) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C8 C7 Mo1 67.70(16) . . ?
C8 C7 H7A 118.3(15) . . ?
Mo1 C7 H7A 116.2(16) . . ?
C8 C7 H7B 120.2(17) . . ?
Mo1 C7 H7B 113.1(15) . . ?
H7A C7 H7B 113(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
C4 C3 C2 N4 -0.8(4) . . . . ?
N4 C6 C5 C4 -1.5(3) . . . . ?
C6 C6 C5 C4 176.83(15) 7_565 . . . ?
C3 C2 N4 C6 -0.9(3) . . . . ?
C3 C2 N4 Mo1 -179.52(17) . . . . ?
C5 C6 N4 C2 2.1(3) . . . . ?
C6 C6 N4 C2 -176.35(15) 7_565 . . . ?
C5 C6 N4 Mo1 -179.27(16) . . . . ?
C6 C6 N4 Mo1 2.31(16) 7_565 . . . ?
C2 C3 C4 C5 1.4(4) . . . . ?
C6 C5 C4 C3 -0.3(3) . . . . ?
C7 C8 C7 Mo1 -67.5(2) 7_565 . . . ?

_refine_diff_density_max         0.512
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.073


_chemical_name_common            '[Mo(allyl)(N3)(bpy)(CO)2]'
####################################################################### 
# 
# 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_FSPF11121_a
_database_code_depnum_ccdc_archive 'CCDC 1562704'
_audit_update_record             
;
2017-07-17 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;

_audit_creation_date             2017-07-07
_shelx_SHELXL_version_number     2014/7
_chemical_formula_moiety         'C21 H19 Mo N5 O6'
_chemical_formula_sum            'C21 H19 Mo N5 O6'
_chemical_formula_weight         533.35

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   11.815(8)
_cell_length_b                   9.369(6)
_cell_length_c                   20.131(14)
_cell_angle_alpha                90
_cell_angle_beta                 103.280(11)
_cell_angle_gamma                90
_cell_volume                     2169(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3928
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      25.99
_cell_special_details            
;
To simulate systematic errors the final estimation of uncertainties
in unit cell parameters was based on 32 Monte-Carlo simulations.
;


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
glass fiber and transferred to stream of cold nitrogen.
;
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_F_000             1080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.654
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5979
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker SMART-APEX'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex1)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            17803
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.771
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4262
_reflns_number_gt                3900
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Smart NT ver. 5.63 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.37A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.37A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0286P)²+1.0565P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4262
_refine_ls_number_parameters     300
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0260
_refine_ls_wR_factor_ref         0.0676
_refine_ls_wR_factor_gt          0.0656
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.35873(2) 0.33517(2) 0.31338(2) 0.01871(7) Uani 1 1 d . . . . .
C1 C 0.47639(18) 0.2084(2) 0.36992(10) 0.0248(4) Uani 1 1 d . . . . .
O1 O 0.54288(15) 0.13126(18) 0.40271(8) 0.0392(4) Uani 1 1 d . . . . .
N1 N 0.24042(15) 0.40872(19) 0.43769(8) 0.0244(4) Uani 1 1 d . . . . .
O2 O 0.25564(15) 0.03856(17) 0.25921(8) 0.0355(4) Uani 1 1 d . . . . .
C2 C 0.29497(18) 0.1487(2) 0.27821(10) 0.0239(4) Uani 1 1 d . . . . .
N2 N 0.26199(15) 0.30738(18) 0.39495(8) 0.0214(4) Uani 1 1 d . . . . .
N3 N 0.23756(15) 0.17483(17) 0.41404(9) 0.0228(4) Uani 1 1 d . . . . .
C3 C 0.19594(17) 0.1929(2) 0.47083(10) 0.0221(4) Uani 1 1 d . . . . .
O3 O 0.14337(18) 0.0819(2) 0.56544(8) 0.0482(5) Uani 1 1 d . . . . .
N4 N 0.39496(14) 0.55140(17) 0.36285(8) 0.0203(3) Uani 1 1 d . . . . .
C4 C 0.19814(18) 0.3392(2) 0.48542(10) 0.0228(4) Uani 1 1 d . . . . .
O4 O 0.17661(16) -0.05341(17) 0.47987(8) 0.0392(4) Uani 1 1 d . . . . .
N5 N 0.20901(14) 0.47901(18) 0.26524(8) 0.0223(4) Uani 1 1 d . . . . .
C5 C 0.48585(18) 0.5794(2) 0.41579(10) 0.0250(4) Uani 1 1 d . . . . .
H5 H 0.5438 0.5083 0.4293 0.030 Uiso 1 1 calc R U . . .
O5 O 0.23524(15) 0.50938(19) 0.57580(9) 0.0435(4) Uani 1 1 d . . . . .
C9 C 0.31315(18) 0.6547(2) 0.34388(10) 0.0219(4) Uani 1 1 d . . . . .
C8 C 0.3215(2) 0.7859(2) 0.37697(11) 0.0291(5) Uani 1 1 d . . . . .
H8 H 0.2638 0.8569 0.3624 0.035 Uiso 1 1 calc R U . . .
C7 C 0.4149(2) 0.8124(2) 0.43145(11) 0.0317(5) Uani 1 1 d . . . . .
H7 H 0.4216 0.9012 0.4548 0.038 Uiso 1 1 calc R U . . .
O6 O 0.06809(14) 0.38698(19) 0.55482(8) 0.0380(4) Uani 1 1 d . . . . .
C6 C 0.49788(19) 0.7077(3) 0.45106(11) 0.0308(5) Uani 1 1 d . . . . .
H6 H 0.5625 0.7233 0.4883 0.037 Uiso 1 1 calc R U . . .
C10 C 0.21286(17) 0.6164(2) 0.28712(10) 0.0215(4) Uani 1 1 d . . . . .
C11 C 0.12628(19) 0.7141(2) 0.25795(11) 0.0307(5) Uani 1 1 d . . . . .
H11 H 0.1314 0.8105 0.2730 0.037 Uiso 1 1 calc R U . . .
C12 C 0.0326(2) 0.6694(2) 0.20679(12) 0.0336(5) Uani 1 1 d . . . . .
H12 H -0.0273 0.7345 0.1869 0.040 Uiso 1 1 calc R U . . .
C13 C 0.02780(19) 0.5289(2) 0.18533(11) 0.0304(5) Uani 1 1 d . . . . .
H13 H -0.0358 0.4954 0.1509 0.036 Uiso 1 1 calc R U . . .
C14 C 0.11769(19) 0.4380(2) 0.21503(10) 0.0281(5) Uani 1 1 d . . . . .
H14 H 0.1151 0.3422 0.1994 0.034 Uiso 1 1 calc R U . . .
C15 C 0.5390(2) 0.3700(3) 0.28790(12) 0.0332(5) Uani 1 1 d . . . . .
H15A H 0.5897 0.4443 0.3143 0.040 Uiso 1 1 calc R U . . .
H15B H 0.5813 0.2835 0.2790 0.040 Uiso 1 1 calc R U . . .
C16 C 0.4476(2) 0.4174(2) 0.23460(11) 0.0331(5) Uani 1 1 d . . . . .
H16 H 0.4407 0.5193 0.2195 0.040 Uiso 1 1 calc R U . . .
C17 C 0.3732(2) 0.3106(3) 0.19931(11) 0.0347(5) Uani 1 1 d . . . . .
H17A H 0.4104 0.2225 0.1874 0.042 Uiso 1 1 calc R U . . .
H17B H 0.3058 0.3428 0.1635 0.042 Uiso 1 1 calc R U . . .
C18 C 0.16831(18) 0.0704(2) 0.51075(11) 0.0268(5) Uani 1 1 d . . . . .
C19 C 0.1621(3) -0.1812(3) 0.51821(15) 0.0480(7) Uani 1 1 d . . . . .
H19A H 0.1835 -0.2654 0.4949 0.072 Uiso 1 1 calc R U . . .
H19B H 0.0808 -0.1892 0.5213 0.072 Uiso 1 1 calc R U . . .
H19C H 0.2123 -0.1751 0.5642 0.072 Uiso 1 1 calc R U . . .
C20 C 0.17191(18) 0.4212(2) 0.54391(10) 0.0253(4) Uani 1 1 d . . . . .
C21 C 0.0372(2) 0.4589(3) 0.61219(12) 0.0466(7) Uani 1 1 d . . . . .
H21A H -0.0395 0.4264 0.6166 0.070 Uiso 1 1 calc R U . . .
H21B H 0.0353 0.5623 0.6045 0.070 Uiso 1 1 calc R U . . .
H21C H 0.0952 0.4366 0.6542 0.070 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C2 1.969(2) . ?
Mo1 C1 1.978(2) . ?
Mo1 N2 2.221(2) . ?
Mo1 C16 2.230(2) . ?
Mo1 N4 2.255(2) . ?
Mo1 N5 2.2576(19) . ?
Mo1 C15 2.325(3) . ?
Mo1 C17 2.353(3) . ?
C1 O1 1.156(3) . ?
N1 N2 1.344(2) . ?
N1 C4 1.348(3) . ?
O2 C2 1.160(3) . ?
N2 N3 1.351(2) . ?
N3 C3 1.355(3) . ?
C3 C4 1.401(3) . ?
C3 C18 1.481(3) . ?
O3 C18 1.208(3) . ?
N4 C5 1.354(3) . ?
N4 C9 1.359(3) . ?
C4 C20 1.497(3) . ?
O4 C18 1.330(3) . ?
O4 C19 1.456(3) . ?
N5 C14 1.353(3) . ?
N5 C10 1.357(3) . ?
C5 C6 1.386(3) . ?
C5 H5 0.9500 . ?
O5 C20 1.197(3) . ?
C9 C8 1.391(3) . ?
C9 C10 1.489(3) . ?
C8 C7 1.388(3) . ?
C8 H8 0.9500 . ?
C7 C6 1.379(3) . ?
C7 H7 0.9500 . ?
O6 C20 1.334(3) . ?
O6 C21 1.454(3) . ?
C6 H6 0.9500 . ?
C10 C11 1.398(3) . ?
C11 C12 1.392(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.382(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.385(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.408(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.411(3) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Mo1 C1 80.47(9) . . ?
C2 Mo1 N2 86.70(8) . . ?
C1 Mo1 N2 85.25(9) . . ?
C2 Mo1 C16 104.74(9) . . ?
C1 Mo1 C16 103.48(10) . . ?
N2 Mo1 C16 166.50(7) . . ?
C2 Mo1 N4 166.99(7) . . ?
C1 Mo1 N4 104.38(8) . . ?
N2 Mo1 N4 81.75(6) . . ?
C16 Mo1 N4 86.06(8) . . ?
C2 Mo1 N5 100.25(8) . . ?
C1 Mo1 N5 169.52(7) . . ?
N2 Mo1 N5 84.36(7) . . ?
C16 Mo1 N5 86.51(9) . . ?
N4 Mo1 N5 72.77(7) . . ?
C2 Mo1 C15 109.84(9) . . ?
C1 Mo1 C15 69.69(9) . . ?
N2 Mo1 C15 146.36(7) . . ?
C16 Mo1 C15 35.92(9) . . ?
N4 Mo1 C15 83.15(7) . . ?
N5 Mo1 C15 119.25(8) . . ?
C2 Mo1 C17 70.71(9) . . ?
C1 Mo1 C17 107.69(9) . . ?
N2 Mo1 C17 151.07(8) . . ?
C16 Mo1 C17 35.73(9) . . ?
N4 Mo1 C17 118.04(7) . . ?
N5 Mo1 C17 82.24(8) . . ?
C15 Mo1 C17 61.50(9) . . ?
O1 C1 Mo1 178.07(19) . . ?
N2 N1 C4 105.71(17) . . ?
O2 C2 Mo1 177.81(19) . . ?
N1 N2 N3 112.52(16) . . ?
N1 N2 Mo1 126.57(13) . . ?
N3 N2 Mo1 119.87(13) . . ?
N2 N3 C3 105.52(16) . . ?
N3 C3 C4 107.85(17) . . ?
N3 C3 C18 121.93(19) . . ?
C4 C3 C18 129.87(19) . . ?
C5 N4 C9 117.86(18) . . ?
C5 N4 Mo1 123.92(14) . . ?
C9 N4 Mo1 117.72(13) . . ?
N1 C4 C3 108.38(18) . . ?
N1 C4 C20 119.36(18) . . ?
C3 C4 C20 132.06(19) . . ?
C18 O4 C19 116.04(19) . . ?
C14 N5 C10 118.21(18) . . ?
C14 N5 Mo1 124.25(15) . . ?
C10 N5 Mo1 117.52(13) . . ?
N4 C5 C6 122.75(19) . . ?
N4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
N4 C9 C8 121.81(19) . . ?
N4 C9 C10 115.65(17) . . ?
C8 C9 C10 122.52(19) . . ?
C7 C8 C9 119.5(2) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C6 C7 C8 118.9(2) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C20 O6 C21 115.27(19) . . ?
C7 C6 C5 119.2(2) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
N5 C10 C11 121.20(19) . . ?
N5 C10 C9 116.06(17) . . ?
C11 C10 C9 122.74(19) . . ?
C12 C11 C10 119.6(2) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C13 C12 C11 119.1(2) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 118.6(2) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
N5 C14 C13 123.3(2) . . ?
N5 C14 H14 118.4 . . ?
C13 C14 H14 118.4 . . ?
C16 C15 Mo1 68.36(13) . . ?
C16 C15 H15A 116.8 . . ?
Mo1 C15 H15A 116.8 . . ?
C16 C15 H15B 116.8 . . ?
Mo1 C15 H15B 116.8 . . ?
H15A C15 H15B 113.9 . . ?
C15 C16 C17 116.1(2) . . ?
C15 C16 Mo1 75.71(13) . . ?
C17 C16 Mo1 76.87(13) . . ?
C15 C16 H16 121.8 . . ?
C17 C16 H16 121.8 . . ?
Mo1 C16 H16 121.8 . . ?
C16 C17 Mo1 67.40(12) . . ?
C16 C17 H17A 117.0 . . ?
Mo1 C17 H17A 117.0 . . ?
C16 C17 H17B 117.0 . . ?
Mo1 C17 H17B 117.0 . . ?
H17A C17 H17B 114.0 . . ?
O3 C18 O4 124.3(2) . . ?
O3 C18 C3 123.8(2) . . ?
O4 C18 C3 111.93(18) . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O5 C20 O6 124.2(2) . . ?
O5 C20 C4 124.0(2) . . ?
O6 C20 C4 111.74(18) . . ?
O6 C21 H21A 109.5 . . ?
O6 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O6 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 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
C4 N1 N2 N3 -1.3(2) . . . . ?
C4 N1 N2 Mo1 -169.48(13) . . . . ?
N1 N2 N3 C3 1.4(2) . . . . ?
Mo1 N2 N3 C3 170.47(12) . . . . ?
N2 N3 C3 C4 -0.9(2) . . . . ?
N2 N3 C3 C18 -174.78(17) . . . . ?
N2 N1 C4 C3 0.7(2) . . . . ?
N2 N1 C4 C20 176.19(17) . . . . ?
N3 C3 C4 N1 0.2(2) . . . . ?
C18 C3 C4 N1 173.4(2) . . . . ?
N3 C3 C4 C20 -174.6(2) . . . . ?
C18 C3 C4 C20 -1.4(4) . . . . ?
C9 N4 C5 C6 0.4(3) . . . . ?
Mo1 N4 C5 C6 -171.32(16) . . . . ?
C5 N4 C9 C8 0.4(3) . . . . ?
Mo1 N4 C9 C8 172.57(16) . . . . ?
C5 N4 C9 C10 -177.80(17) . . . . ?
Mo1 N4 C9 C10 -5.6(2) . . . . ?
N4 C9 C8 C7 -0.8(3) . . . . ?
C10 C9 C8 C7 177.2(2) . . . . ?
C9 C8 C7 C6 0.5(3) . . . . ?
C8 C7 C6 C5 0.2(3) . . . . ?
N4 C5 C6 C7 -0.6(3) . . . . ?
C14 N5 C10 C11 -1.2(3) . . . . ?
Mo1 N5 C10 C11 177.21(16) . . . . ?
C14 N5 C10 C9 178.17(18) . . . . ?
Mo1 N5 C10 C9 -3.5(2) . . . . ?
N4 C9 C10 N5 6.0(3) . . . . ?
C8 C9 C10 N5 -172.19(19) . . . . ?
N4 C9 C10 C11 -174.73(19) . . . . ?
C8 C9 C10 C11 7.1(3) . . . . ?
N5 C10 C11 C12 1.8(3) . . . . ?
C9 C10 C11 C12 -177.5(2) . . . . ?
C10 C11 C12 C13 -0.7(3) . . . . ?
C11 C12 C13 C14 -0.9(3) . . . . ?
C10 N5 C14 C13 -0.5(3) . . . . ?
Mo1 N5 C14 C13 -178.74(16) . . . . ?
C12 C13 C14 N5 1.5(3) . . . . ?
Mo1 C15 C16 C17 -67.30(18) . . . . ?
C15 C16 C17 Mo1 66.64(17) . . . . ?
C19 O4 C18 O3 -4.5(3) . . . . ?
C19 O4 C18 C3 174.3(2) . . . . ?
N3 C3 C18 O3 171.6(2) . . . . ?
C4 C3 C18 O3 -0.8(4) . . . . ?
N3 C3 C18 O4 -7.2(3) . . . . ?
C4 C3 C18 O4 -179.5(2) . . . . ?
C21 O6 C20 O5 -3.5(3) . . . . ?
C21 O6 C20 C4 178.25(18) . . . . ?
N1 C4 C20 O5 -44.7(3) . . . . ?
C3 C4 C20 O5 129.6(3) . . . . ?
N1 C4 C20 O6 133.5(2) . . . . ?
C3 C4 C20 O6 -52.2(3) . . . . ?

_refine_diff_density_max         0.330
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.063


_chemical_name_common            
'[Mo(allyl)(triazolateCOOCH3,COOCH3)(bpy)(CO)2]'
####################################################################### 
# 
# 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_12s039_pl
_database_code_depnum_ccdc_archive 'CCDC 1562700'
_audit_update_record             
;
2017-07-17 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;


_audit_creation_date             2012-12-14
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            '[Mo(allyl)(triazolateCF3,COOEt)(bpy)(CO)2]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H18 F3 Mo N5 O4'
_chemical_formula_sum            'C21 H18 F3 Mo N5 O4'
_chemical_formula_weight         557.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

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

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

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

_cell_length_a                   10.545(2)
_cell_length_b                   10.8506(19)
_cell_length_c                   11.320(2)
_cell_angle_alpha                82.745(7)
_cell_angle_beta                 63.061(8)
_cell_angle_gamma                75.89(2)
_cell_volume                     1119.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    4160
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      22.67
_cell_special_details            
;
To simulate systematic errors the final estimation of uncertainties
in unit cell parameters was based on 16 Monte-Carlo simulations.
;


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Bruker Kryoflex2).
;
_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_F_000             560
_exptl_crystal_preparation       'prepared dry'
_exptl_crystal_recrystallization_method 
'by precipitation with hexane from a DCM solution'
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.454
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.085
_exptl_absorpt_coefficient_mu    0.649
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.8842
_exptl_absorpt_correction_T_max  0.9764
_exptl_absorpt_process_details   'SadAbs 2008/1 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            15715
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.216
_diffrn_reflns_theta_max         26.843
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4788
_reflns_number_gt                3932
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_cell_refinement       'Saint+ ver. V8.18C (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.18C (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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.The distances between atoms XXX and YYY 
were restrained to the value of ???.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0278P)²+0.2457P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4788
_refine_ls_number_parameters     323
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0679
_refine_ls_wR_factor_gt          0.0634
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.13611(2) -0.21681(2) 0.18121(2) 0.02537(7) Uani 1 1 d . . . . .
F1 F 0.3231(3) -0.0687(3) 0.5308(3) 0.1128(10) Uani 1 1 d . . . . .
F2 F 0.5469(2) -0.1520(2) 0.4471(2) 0.0782(6) Uani 1 1 d . . . . .
F3 F 0.3981(3) -0.2561(3) 0.5852(2) 0.1041(9) Uani 1 1 d . . . . .
O1 O 0.1504(2) -0.50644(18) 0.2395(2) 0.0542(6) Uani 1 1 d . . . . .
O2 O -0.0895(2) -0.2094(2) 0.4781(2) 0.0655(7) Uani 1 1 d . . . . .
O3 O 0.7112(2) -0.4632(2) 0.1588(2) 0.0633(7) Uani 1 1 d . . . . .
O4 O 0.6594(2) -0.41927(19) 0.36542(19) 0.0453(5) Uani 1 1 d . . . . .
N1 N 0.4278(2) -0.3259(2) 0.2065(2) 0.0316(5) Uani 1 1 d . . . . .
N2 N 0.3050(2) -0.2383(2) 0.2513(2) 0.0304(5) Uani 1 1 d . . . . .
N3 N 0.2851(2) -0.1747(2) 0.3545(2) 0.0365(5) Uani 1 1 d . . . . .
N4 N 0.3289(2) -0.2141(2) -0.0126(2) 0.0328(5) Uani 1 1 d . . . . .
N5 N 0.1699(2) -0.0175(2) 0.1443(2) 0.0332(5) Uani 1 1 d . . . . .
C1 C 0.1450(3) -0.3990(3) 0.2156(3) 0.0361(6) Uani 1 1 d . . . . .
C2 C -0.0077(3) -0.2103(3) 0.3680(3) 0.0392(7) Uani 1 1 d . . . . .
C3 C 0.4025(3) -0.2256(3) 0.3759(3) 0.0338(6) Uani 1 1 d . . . . .
C4 C 0.4917(3) -0.3198(2) 0.2841(3) 0.0305(6) Uani 1 1 d . . . . .
C5 C 0.4119(3) -0.3193(3) -0.0838(3) 0.0456(8) Uani 1 1 d . . . . .
H5 H 0.3864 -0.3970 -0.0503 0.055 Uiso 1 1 calc R U . . .
C6 C 0.5310(4) -0.3175(4) -0.2020(3) 0.0639(10) Uani 1 1 d . . . . .
H6 H 0.5851 -0.3920 -0.2483 0.077 Uiso 1 1 calc R U . . .
C7 C 0.5689(4) -0.2043(5) -0.2509(3) 0.0710(12) Uani 1 1 d . . . . .
H7 H 0.6489 -0.2004 -0.3323 0.085 Uiso 1 1 calc R U . . .
C8 C 0.4890(4) -0.0952(4) -0.1801(3) 0.0590(10) Uani 1 1 d . . . . .
H8 H 0.5155 -0.0177 -0.2129 0.071 Uiso 1 1 calc R U . . .
C9 C 0.3680(3) -0.1015(3) -0.0591(3) 0.0371(7) Uani 1 1 d . . . . .
C10 C 0.2790(3) 0.0077(3) 0.0277(3) 0.0366(7) Uani 1 1 d . . . . .
C11 C 0.3066(4) 0.1284(3) -0.0051(4) 0.0572(9) Uani 1 1 d . . . . .
H11 H 0.3815 0.1440 -0.0862 0.069 Uiso 1 1 calc R U . . .
C12 C 0.2234(5) 0.2251(3) 0.0819(4) 0.0676(11) Uani 1 1 d . . . . .
H12 H 0.2394 0.3072 0.0595 0.081 Uiso 1 1 calc R U . . .
C13 C 0.1168(4) 0.1997(3) 0.2017(4) 0.0612(10) Uani 1 1 d . . . . .
H13 H 0.0615 0.2637 0.2633 0.073 Uiso 1 1 calc R U . . .
C14 C 0.0918(3) 0.0775(3) 0.2310(3) 0.0466(8) Uani 1 1 d . . . . .
H14 H 0.0188 0.0605 0.3129 0.056 Uiso 1 1 calc R U . . .
C15 C 0.0524(3) -0.2956(3) 0.0535(3) 0.0425(7) Uani 1 1 d D . . . .
H15A H 0.130(2) -0.335(2) -0.0242(16) 0.051 Uiso 1 1 d D U . . .
H15B H -0.018(2) -0.344(2) 0.108(2) 0.051 Uiso 1 1 d D U . . .
C16 C 0.0062(3) -0.1636(3) 0.0673(3) 0.0374(7) Uani 1 1 d D . . . .
H16 H 0.049(3) -0.106(2) -0.0026(19) 0.045 Uiso 1 1 d D U . . .
C17 C -0.0926(3) -0.1198(3) 0.1941(3) 0.0428(7) Uani 1 1 d D . . . .
H17A H -0.163(2) -0.168(2) 0.249(2) 0.051 Uiso 1 1 d D U . . .
H17B H -0.117(3) -0.0326(9) 0.215(3) 0.051 Uiso 1 1 d D U . . .
C18 C 0.4175(4) -0.1749(3) 0.4836(3) 0.0541(8) Uani 1 1 d . . . . .
C19 C 0.6321(3) -0.4079(3) 0.2600(3) 0.0376(6) Uani 1 1 d . . . . .
C20 C 0.7922(3) -0.5085(3) 0.3536(3) 0.0524(8) Uani 1 1 d . . . . .
H20A H 0.8760 -0.4831 0.2804 0.063 Uiso 1 1 calc R U . . .
H20B H 0.7894 -0.5930 0.3369 0.063 Uiso 1 1 calc R U . . .
C21 C 0.8027(3) -0.5081(3) 0.4791(3) 0.0547(9) Uani 1 1 d . . . . .
H21A H 0.8061 -0.4241 0.4943 0.082 Uiso 1 1 calc R U . . .
H21B H 0.8895 -0.5665 0.4739 0.082 Uiso 1 1 calc R U . . .
H21C H 0.7193 -0.5333 0.5508 0.082 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C1 1.954(3) . ?
Mo1 C2 1.964(3) . ?
Mo1 N2 2.210(2) . ?
Mo1 C16 2.214(3) . ?
Mo1 N4 2.218(2) . ?
Mo1 N5 2.234(2) . ?
Mo1 C17 2.330(3) . ?
Mo1 C15 2.332(3) . ?
F1 C18 1.312(4) . ?
F2 C18 1.314(4) . ?
F3 C18 1.327(4) . ?
O1 C1 1.156(3) . ?
O2 C2 1.150(3) . ?
O3 C19 1.197(3) . ?
O4 C19 1.333(3) . ?
O4 C20 1.455(3) . ?
N1 N2 1.328(3) . ?
N1 C4 1.343(3) . ?
N2 N3 1.340(3) . ?
N3 C3 1.342(3) . ?
N4 C5 1.351(3) . ?
N4 C9 1.351(3) . ?
N5 C14 1.346(3) . ?
N5 C10 1.351(3) . ?
C3 C4 1.387(4) . ?
C3 C18 1.482(4) . ?
C4 C19 1.480(4) . ?
C5 C6 1.361(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.357(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.377(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.395(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.472(4) . ?
C10 C11 1.379(4) . ?
C11 C12 1.367(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.362(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.385(4) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.400(4) . ?
C15 H15A 0.947(5) . ?
C15 H15B 0.950(5) . ?
C16 C17 1.396(4) . ?
C16 H16 0.950(5) . ?
C17 H17A 0.949(5) . ?
C17 H17B 0.950(5) . ?
C20 C21 1.475(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Mo1 C2 81.42(12) . . ?
C1 Mo1 N2 87.20(9) . . ?
C2 Mo1 N2 87.59(10) . . ?
C1 Mo1 C16 103.97(11) . . ?
C2 Mo1 C16 105.05(11) . . ?
N2 Mo1 C16 164.09(9) . . ?
C1 Mo1 N4 101.81(10) . . ?
C2 Mo1 N4 167.56(10) . . ?
N2 Mo1 N4 80.62(8) . . ?
C16 Mo1 N4 85.96(9) . . ?
C1 Mo1 N5 168.13(9) . . ?
C2 Mo1 N5 101.35(10) . . ?
N2 Mo1 N5 81.42(8) . . ?
C16 Mo1 N5 86.56(9) . . ?
N4 Mo1 N5 73.11(8) . . ?
C1 Mo1 C17 108.79(11) . . ?
C2 Mo1 C17 71.09(11) . . ?
N2 Mo1 C17 150.42(10) . . ?
C16 Mo1 C17 35.66(10) . . ?
N4 Mo1 C17 118.29(10) . . ?
N5 Mo1 C17 82.94(10) . . ?
C1 Mo1 C15 70.09(11) . . ?
C2 Mo1 C15 110.07(12) . . ?
N2 Mo1 C15 147.94(10) . . ?
C16 Mo1 C15 35.75(10) . . ?
N4 Mo1 C15 82.23(10) . . ?
N5 Mo1 C15 118.85(9) . . ?
C17 Mo1 C15 61.30(11) . . ?
C19 O4 C20 115.9(2) . . ?
N2 N1 C4 105.7(2) . . ?
N1 N2 N3 113.3(2) . . ?
N1 N2 Mo1 123.39(16) . . ?
N3 N2 Mo1 122.84(16) . . ?
N2 N3 C3 104.5(2) . . ?
C5 N4 C9 118.5(2) . . ?
C5 N4 Mo1 123.6(2) . . ?
C9 N4 Mo1 117.91(18) . . ?
C14 N5 C10 118.2(2) . . ?
C14 N5 Mo1 124.60(19) . . ?
C10 N5 Mo1 117.16(18) . . ?
O1 C1 Mo1 177.9(2) . . ?
O2 C2 Mo1 178.1(3) . . ?
N3 C3 C4 108.9(2) . . ?
N3 C3 C18 119.0(3) . . ?
C4 C3 C18 132.1(3) . . ?
N1 C4 C3 107.6(2) . . ?
N1 C4 C19 118.9(2) . . ?
C3 C4 C19 133.5(2) . . ?
N4 C5 C6 123.4(3) . . ?
N4 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
C7 C6 C5 118.4(3) . . ?
C7 C6 H6 120.8 . . ?
C5 C6 H6 120.8 . . ?
C6 C7 C8 120.0(3) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C9 119.6(3) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
N4 C9 C8 120.0(3) . . ?
N4 C9 C10 115.7(2) . . ?
C8 C9 C10 124.2(3) . . ?
N5 C10 C11 121.4(3) . . ?
N5 C10 C9 116.0(2) . . ?
C11 C10 C9 122.6(3) . . ?
C12 C11 C10 119.8(3) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C13 C12 C11 119.2(3) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 119.3(3) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
N5 C14 C13 121.9(3) . . ?
N5 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
C16 C15 Mo1 67.53(16) . . ?
C16 C15 H15A 123.1(18) . . ?
Mo1 C15 H15A 111.9(18) . . ?
C16 C15 H15B 116.1(18) . . ?
Mo1 C15 H15B 110.1(18) . . ?
H15A C15 H15B 116(3) . . ?
C17 C16 C15 116.4(3) . . ?
C17 C16 Mo1 76.70(17) . . ?
C15 C16 Mo1 76.71(16) . . ?
C17 C16 H16 121.0(17) . . ?
C15 C16 H16 122.1(17) . . ?
Mo1 C16 H16 109.2(17) . . ?
C16 C17 Mo1 67.63(16) . . ?
C16 C17 H17A 118.6(18) . . ?
Mo1 C17 H17A 110.7(17) . . ?
C16 C17 H17B 121.7(18) . . ?
Mo1 C17 H17B 111.1(18) . . ?
H17A C17 H17B 116(3) . . ?
F1 C18 F2 106.7(3) . . ?
F1 C18 F3 106.8(3) . . ?
F2 C18 F3 104.9(3) . . ?
F1 C18 C3 112.4(3) . . ?
F2 C18 C3 113.5(3) . . ?
F3 C18 C3 112.0(3) . . ?
O3 C19 O4 124.0(3) . . ?
O3 C19 C4 124.3(3) . . ?
O4 C19 C4 111.8(2) . . ?
O4 C20 C21 107.8(2) . . ?
O4 C20 H20A 110.1 . . ?
C21 C20 H20A 110.1 . . ?
O4 C20 H20B 110.1 . . ?
C21 C20 H20B 110.1 . . ?
H20A C20 H20B 108.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

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
C4 N1 N2 N3 0.1(3) . . . . ?
C4 N1 N2 Mo1 -172.04(16) . . . . ?
N1 N2 N3 C3 -0.1(3) . . . . ?
Mo1 N2 N3 C3 172.13(16) . . . . ?
N2 N3 C3 C4 0.0(3) . . . . ?
N2 N3 C3 C18 178.9(2) . . . . ?
N2 N1 C4 C3 -0.1(3) . . . . ?
N2 N1 C4 C19 179.4(2) . . . . ?
N3 C3 C4 N1 0.1(3) . . . . ?
C18 C3 C4 N1 -178.6(3) . . . . ?
N3 C3 C4 C19 -179.3(3) . . . . ?
C18 C3 C4 C19 2.1(5) . . . . ?
C9 N4 C5 C6 -1.8(4) . . . . ?
Mo1 N4 C5 C6 -179.3(2) . . . . ?
N4 C5 C6 C7 0.3(5) . . . . ?
C5 C6 C7 C8 1.1(5) . . . . ?
C6 C7 C8 C9 -0.9(5) . . . . ?
C5 N4 C9 C8 2.0(4) . . . . ?
Mo1 N4 C9 C8 179.64(19) . . . . ?
C5 N4 C9 C10 -175.9(2) . . . . ?
Mo1 N4 C9 C10 1.8(3) . . . . ?
C7 C8 C9 N4 -0.7(4) . . . . ?
C7 C8 C9 C10 177.0(3) . . . . ?
C14 N5 C10 C11 -2.8(4) . . . . ?
Mo1 N5 C10 C11 178.8(2) . . . . ?
C14 N5 C10 C9 175.5(2) . . . . ?
Mo1 N5 C10 C9 -2.9(3) . . . . ?
N4 C9 C10 N5 0.7(3) . . . . ?
C8 C9 C10 N5 -177.0(2) . . . . ?
N4 C9 C10 C11 179.1(2) . . . . ?
C8 C9 C10 C11 1.3(4) . . . . ?
N5 C10 C11 C12 0.7(4) . . . . ?
C9 C10 C11 C12 -177.5(3) . . . . ?
C10 C11 C12 C13 1.8(5) . . . . ?
C11 C12 C13 C14 -2.2(5) . . . . ?
C10 N5 C14 C13 2.4(4) . . . . ?
Mo1 N5 C14 C13 -179.3(2) . . . . ?
C12 C13 C14 N5 0.1(5) . . . . ?
Mo1 C15 C16 C17 -67.6(2) . . . . ?
C15 C16 C17 Mo1 67.6(2) . . . . ?
N3 C3 C18 F1 -11.4(4) . . . . ?
C4 C3 C18 F1 167.1(3) . . . . ?
N3 C3 C18 F2 -132.7(3) . . . . ?
C4 C3 C18 F2 45.9(5) . . . . ?
N3 C3 C18 F3 108.8(3) . . . . ?
C4 C3 C18 F3 -72.6(4) . . . . ?
C20 O4 C19 O3 -2.0(4) . . . . ?
C20 O4 C19 C4 177.3(2) . . . . ?
N1 C4 C19 O3 18.8(4) . . . . ?
C3 C4 C19 O3 -161.9(3) . . . . ?
N1 C4 C19 O4 -160.5(2) . . . . ?
C3 C4 C19 O4 18.8(4) . . . . ?
C19 O4 C20 C21 -179.7(2) . . . . ?

_refine_diff_density_max         0.368
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.069

####################################################################### 
# 
# 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_af051_final
_database_code_depnum_ccdc_archive 'CCDC 1562703'
_audit_update_record             
;
2017-07-17 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;

_audit_creation_date             2016-07-08
_shelx_SHELXL_version_number     2014/7
_chemical_formula_moiety         'C15 H13 N5 O2 W'
_chemical_formula_sum            'C15 H13 N5 O2 W'
_chemical_formula_weight         479.15

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

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

_cell_length_a                   16.83(3)
_cell_length_b                   13.769(17)
_cell_length_c                   6.602(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1530(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3245
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      31.47
_cell_special_details            
;
To simulate systematic errors the final estimation of uncertainties
in unit cell parameters was based on 32 Monte-Carlo simulations.
;


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Bruker Kryoflex2).
;
_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.080
_exptl_crystal_F_000             912
_exptl_crystal_preparation       
'Crystal fragment soaked in perfluoro polyether oil.'
_exptl_crystal_recrystallization_method 
'recrystallised from acetone and methanol by evaporation'
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.321
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    7.566
_shelx_estimated_absorpt_T_min   0.161
_shelx_estimated_absorpt_T_max   0.583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5011
_exptl_absorpt_correction_T_max  0.7471
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 0.00 0.0530
-1.00 -2.00 -1.00 0.0830
1.00 2.00 1.00 0.1640
0.00 2.00 1.00 0.1220
-1.00 2.00 1.00 0.0920
-2.00 1.00 0.00 0.0600
2.00 -2.00 -1.00 0.2000
1.00 2.00 2.00 0.1480
-2.00 2.00 1.00 0.0750
0.00 -1.00 -1.00 0.1360
0.00 1.00 1.00 0.0930
-2.00 -1.00 -2.00 0.0720
2.00 1.00 2.00 0.1450
1.00 -2.00 -2.00 0.1790
0.00 1.00 2.00 0.0660
1.00 1.00 3.00 0.1180
0.00 0.00 1.00 0.0200
0.00 -3.00 -1.00 0.1500

_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            9425
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.837
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1979
_reflns_number_gt                1427
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 ver. 2014.11-0 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0109P)²+1.3487P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1979
_refine_ls_number_parameters     120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0220
_refine_ls_wR_factor_ref         0.0501
_refine_ls_wR_factor_gt          0.0452
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.49947(2) 0.2500 0.32134(2) 0.01032(6) Uani 1 2 d S T P . .
C1 C 0.5773(2) 0.1565(2) 0.4248(5) 0.0165(7) Uani 1 1 d . . . . .
N1 N 0.5558(3) 0.2500 0.0260(6) 0.0154(8) Uani 1 2 d S T P . .
O1 O 0.62320(17) 0.10061(18) 0.4852(4) 0.0257(6) Uani 1 1 d . . . . .
C3 C 0.3701(2) -0.0019(2) 0.0433(5) 0.0206(8) Uani 1 1 d . . . . .
H3 H 0.3761 -0.0705 0.0436 0.025 Uiso 1 1 calc R U . . .
N3 N 0.6935(3) 0.2500 -0.0399(8) 0.0303(11) Uani 1 2 d S T P . .
N4 N 0.41598(17) 0.15437(19) 0.1520(4) 0.0108(6) Uani 1 1 d . . . . .
C4 C 0.3093(2) 0.0413(3) -0.0622(5) 0.0211(8) Uani 1 1 d . . . . .
H4 H 0.2722 0.0027 -0.1347 0.025 Uiso 1 1 calc R U . . .
N2 N 0.6263(3) 0.2500 -0.0005(6) 0.0175(9) Uani 1 2 d S T P . .
C2 C 0.4222(2) 0.0567(2) 0.1489(5) 0.0158(7) Uani 1 1 d . . . . .
H2 H 0.4642 0.0270 0.2225 0.019 Uiso 1 1 calc R U . . .
C7 C 0.4477(2) 0.1637(3) 0.5923(5) 0.0193(8) Uani 1 1 d . . . . .
H7A H 0.487(2) 0.160(3) 0.707(6) 0.023 Uiso 1 1 d . U . . .
H7B H 0.426(3) 0.105(3) 0.557(6) 0.023 Uiso 1 1 d . U . . .
C6 C 0.3571(2) 0.1961(2) 0.0437(5) 0.0111(6) Uani 1 1 d . . . . .
C8 C 0.4050(3) 0.2500 0.5527(7) 0.0181(10) Uani 1 2 d S T P . .
H8 H 0.358(4) 0.2500 0.502(8) 0.022 Uiso 1 2 d S U P . .
C5 C 0.3026(2) 0.1412(2) -0.0623(5) 0.0168(7) Uani 1 1 d . . . . .
H5 H 0.2608 0.1719 -0.1346 0.020 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C1 1.959(4) . ?
W1 C1 1.960(4) 8_565 ?
W1 N1 2.169(5) . ?
W1 C8 2.205(5) . ?
W1 N4 2.227(3) . ?
W1 N4 2.227(3) 8_565 ?
W1 C7 2.318(4) . ?
W1 C7 2.318(4) 8_565 ?
C1 O1 1.161(4) . ?
N1 N2 1.199(6) . ?
C3 C4 1.372(6) . ?
C3 C2 1.381(5) . ?
C3 H3 0.9500 . ?
N3 N2 1.160(7) . ?
N4 C2 1.349(4) . ?
N4 C6 1.350(4) . ?
C4 C5 1.380(5) . ?
C4 H4 0.9500 . ?
C2 H2 0.9500 . ?
C7 C8 1.413(5) . ?
C7 H7A 1.01(4) . ?
C7 H7B 0.91(4) . ?
C6 C5 1.380(5) . ?
C6 C6 1.484(6) 8_565 ?
C8 C7 1.413(5) 8_565 ?
C8 H8 0.86(6) . ?
C5 H5 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W1 C1 82.2(2) . 8_565 ?
C1 W1 N1 91.20(15) . . ?
C1 W1 N1 91.20(15) 8_565 . ?
C1 W1 C8 103.92(17) . . ?
C1 W1 C8 103.92(17) 8_565 . ?
N1 W1 C8 159.79(18) . . ?
C1 W1 N4 102.02(15) . . ?
C1 W1 N4 170.17(11) 8_565 . ?
N1 W1 N4 79.90(14) . . ?
C8 W1 N4 83.84(16) . . ?
C1 W1 N4 170.17(11) . 8_565 ?
C1 W1 N4 102.02(15) 8_565 8_565 ?
N1 W1 N4 79.90(14) . 8_565 ?
C8 W1 N4 83.84(16) . 8_565 ?
N4 W1 N4 72.49(17) . 8_565 ?
C1 W1 C7 69.22(16) . . ?
C1 W1 C7 108.62(15) 8_565 . ?
N1 W1 C7 149.15(10) . . ?
C8 W1 C7 36.32(13) . . ?
N4 W1 C7 81.21(14) . . ?
N4 W1 C7 116.97(15) 8_565 . ?
C1 W1 C7 108.62(15) . 8_565 ?
C1 W1 C7 69.22(16) 8_565 8_565 ?
N1 W1 C7 149.15(10) . 8_565 ?
C8 W1 C7 36.32(13) . 8_565 ?
N4 W1 C7 116.97(15) . 8_565 ?
N4 W1 C7 81.21(14) 8_565 8_565 ?
C7 W1 C7 61.7(2) . 8_565 ?
O1 C1 W1 179.6(3) . . ?
N2 N1 W1 124.3(3) . . ?
C4 C3 C2 118.5(3) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C2 N4 C6 118.3(3) . . ?
C2 N4 W1 123.2(2) . . ?
C6 N4 W1 118.5(2) . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N3 N2 N1 175.4(5) . . ?
N4 C2 C3 122.7(3) . . ?
N4 C2 H2 118.6 . . ?
C3 C2 H2 118.6 . . ?
C8 C7 W1 67.5(2) . . ?
C8 C7 H7A 121(3) . . ?
W1 C7 H7A 111(2) . . ?
C8 C7 H7B 120(3) . . ?
W1 C7 H7B 114(2) . . ?
H7A C7 H7B 114(4) . . ?
N4 C6 C5 121.6(3) . . ?
N4 C6 C6 115.19(18) . 8_565 ?
C5 C6 C6 123.23(19) . 8_565 ?
C7 C8 C7 114.5(5) . 8_565 ?
C7 C8 W1 76.2(3) . . ?
C7 C8 W1 76.2(3) 8_565 . ?
C7 C8 H8 122.7(3) . . ?
C7 C8 H8 122.7(3) 8_565 . ?
W1 C8 H8 113(4) . . ?
C6 C5 C4 119.4(3) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?

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
C2 C3 C4 C5 0.9(5) . . . . ?
C6 N4 C2 C3 -1.3(5) . . . . ?
W1 N4 C2 C3 -180.0(3) . . . . ?
C4 C3 C2 N4 -0.2(5) . . . . ?
C2 N4 C6 C5 2.3(5) . . . . ?
W1 N4 C6 C5 -179.0(2) . . . . ?
C2 N4 C6 C6 -176.2(2) . . . 8_565 ?
W1 N4 C6 C6 2.5(2) . . . 8_565 ?
W1 C7 C8 C7 -67.6(4) . . . 8_565 ?
N4 C6 C5 C4 -1.7(5) . . . . ?
C6 C6 C5 C4 176.7(2) 8_565 . . . ?
C3 C4 C5 C6 0.0(5) . . . . ?

_refine_diff_density_max         1.380
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.129


_chemical_name_common            '[W(allyl)(N3)(bpy)(CO)2]'
####################################################################### 
# 
# 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_AF048
_database_code_depnum_ccdc_archive 'CCDC 1562705'
_audit_update_record             
;
2017-07-17 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;

_audit_creation_date             2016-07-01
_shelx_SHELXL_version_number     2014/7
_chemical_formula_moiety         'C21 H18 F3 N5 O4 W'
_chemical_formula_sum            'C21 H18 F3 N5 O4 W'
_chemical_formula_weight         645.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   11.078(5)
_cell_length_b                   9.984(5)
_cell_length_c                   19.167(11)
_cell_angle_alpha                90
_cell_angle_beta                 91.10(2)
_cell_angle_gamma                90
_cell_volume                     2119.5(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9392
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      36.34
_cell_special_details            
;
To simulate systematic errors the final estimation of uncertainties
in unit cell parameters was based on 32 Monte-Carlo simulations.
;


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Bruker Kryoflex2).
;
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.022
_exptl_crystal_F_000             1248
_exptl_crystal_preparation       
'Crystal fragment soaked in perfluoro polyether oil.'
_exptl_crystal_recrystallization_method 
'recrystallised from dichloromethane and hexane by evaporation'
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.588
_exptl_crystal_size_mid          0.472
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    5.517
_shelx_estimated_absorpt_T_min   0.140
_shelx_estimated_absorpt_T_max   0.405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5169
_exptl_absorpt_correction_T_max  0.7471
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 2.00 0.0920
1.00 0.00 -2.00 0.1000
0.00 0.00 1.00 0.1760
0.00 0.00 -1.00 0.2080
1.00 1.00 2.00 0.3320
-1.00 -2.00 2.00 0.1090
0.00 -1.00 2.00 0.1240
0.00 1.00 -2.00 0.2390
0.00 1.00 -1.00 0.2310
-1.00 -2.00 -1.00 0.1880
0.00 -2.00 1.00 0.1370
1.00 -1.00 2.00 0.1840
-1.00 1.00 -2.00 0.2710
0.00 -1.00 0.00 0.1360
0.00 1.00 0.00 0.2940
-1.00 -2.00 -2.00 0.2010
-2.00 1.00 -2.00 0.2530
0.00 -2.00 -1.00 0.1500
2.00 -2.00 1.00 0.1660
-2.00 2.00 -1.00 0.2750
-1.00 2.00 0.00 0.2800
1.00 0.00 1.00 0.2270
-1.00 0.00 -1.00 0.2180
2.00 -1.00 1.00 0.1920
1.00 -1.00 0.00 0.1550
1.00 -2.00 -1.00 0.1280
0.00 1.00 1.00 0.3090
2.00 -2.00 -1.00 0.1450
-1.00 2.00 2.00 0.2890
-2.00 -1.00 -2.00 0.2250
1.00 -1.00 -2.00 0.1150
2.00 0.00 -1.00 0.1380
0.00 -1.00 -2.00 0.1890
1.00 0.00 0.00 0.1710
3.00 -1.00 -3.00 0.1120

_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            24833
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.839
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4178
_reflns_number_gt                3932
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 ver. 2014.11-0 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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.The C-H distances between the atoms of 
the allyl moiety were kept during refinement at the value of 0.950(5) using 
DFIX restraint. 

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0072P)²+2.9018P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4178
_refine_ls_number_parameters     323
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0155
_refine_ls_wR_factor_ref         0.0351
_refine_ls_wR_factor_gt          0.0345
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.15695(2) 0.31237(2) 0.66651(2) 0.00971(4) Uani 1 1 d . . . . .
C1 C 0.0641(2) 0.1911(2) 0.60580(12) 0.0158(5) Uani 1 1 d . . . . .
O1 O 0.01350(17) 0.11375(18) 0.57061(9) 0.0237(4) Uani 1 1 d . . . . .
N1 N 0.27192(18) 0.4138(2) 0.52651(10) 0.0158(4) Uani 1 1 d . . . . .
F1 F 0.32952(17) 0.37188(19) 0.36179(8) 0.0377(4) Uani 1 1 d . . . . .
F2 F 0.47956(14) 0.48650(16) 0.39853(8) 0.0263(4) Uani 1 1 d . . . . .
O2 O 0.26539(16) 0.03212(17) 0.70379(9) 0.0205(4) Uani 1 1 d . . . . .
C2 C 0.2279(2) 0.1375(2) 0.69031(12) 0.0147(5) Uani 1 1 d . . . . .
N2 N 0.28671(18) 0.32995(19) 0.58113(10) 0.0111(4) Uani 1 1 d . . . . .
F3 F 0.30084(17) 0.56105(19) 0.41207(9) 0.0424(5) Uani 1 1 d . . . . .
C3 C 0.4283(2) 0.2786(2) 0.51294(12) 0.0154(5) Uani 1 1 d . . . . .
O3 O 0.56111(17) 0.21535(19) 0.42441(9) 0.0244(4) Uani 1 1 d . . . . .
N3 N 0.37968(19) 0.2484(2) 0.57465(10) 0.0162(4) Uani 1 1 d . . . . .
N4 N 0.10799(17) 0.51636(19) 0.63080(9) 0.0106(4) Uani 1 1 d . . . . .
C4 C 0.3603(2) 0.3813(2) 0.48300(12) 0.0151(5) Uani 1 1 d . . . . .
O4 O 0.58781(16) 0.12918(18) 0.53167(9) 0.0209(4) Uani 1 1 d . . . . .
C8 C 0.1589(2) 0.7484(2) 0.62853(12) 0.0127(5) Uani 1 1 d . . . . .
H8 H 0.2104 0.8191 0.6437 0.015 Uiso 1 1 calc R U . . .
C7 C 0.0644(2) 0.7738(2) 0.58222(12) 0.0140(5) Uani 1 1 d . . . . .
H7 H 0.0495 0.8621 0.5657 0.017 Uiso 1 1 calc R U . . .
C9 C 0.1779(2) 0.6192(2) 0.65257(11) 0.0112(5) Uani 1 1 d . . . . .
C6 C -0.0081(2) 0.6685(2) 0.56035(12) 0.0134(5) Uani 1 1 d . . . . .
H6 H -0.0738 0.6832 0.5287 0.016 Uiso 1 1 calc R U . . .
C10 C 0.2749(2) 0.5849(2) 0.70356(11) 0.0129(5) Uani 1 1 d . . . . .
N5 N 0.28686(17) 0.45295(19) 0.71757(10) 0.0119(4) Uani 1 1 d . . . . .
C5 C 0.0168(2) 0.5417(2) 0.58531(11) 0.0123(5) Uani 1 1 d . . . . .
H5 H -0.0325 0.4693 0.5698 0.015 Uiso 1 1 calc R U . . .
C11 C 0.3464(2) 0.6800(3) 0.73713(13) 0.0180(5) Uani 1 1 d . . . . .
H11 H 0.3361 0.7724 0.7269 0.022 Uiso 1 1 calc R U . . .
C21 C 0.3683(2) 0.4506(3) 0.41452(13) 0.0194(5) Uani 1 1 d . . . . .
C12 C 0.4327(2) 0.6393(3) 0.78553(13) 0.0205(5) Uani 1 1 d . . . . .
H12 H 0.4805 0.7034 0.8101 0.025 Uiso 1 1 calc R U . . .
C13 C 0.4484(2) 0.5041(3) 0.79774(12) 0.0184(5) Uani 1 1 d . . . . .
H13 H 0.5094 0.4736 0.8294 0.022 Uiso 1 1 calc R U . . .
C18 C 0.5324(2) 0.2064(2) 0.48367(13) 0.0178(5) Uani 1 1 d . . . . .
C17 C 0.1158(2) 0.2613(3) 0.78136(12) 0.0167(5) Uani 1 1 d D . . . .
H17A H 0.1750(19) 0.289(3) 0.8148(11) 0.020 Uiso 1 1 d D U . . .
H17B H 0.088(2) 0.1715(11) 0.7861(14) 0.020 Uiso 1 1 d D U . . .
C16 C 0.0346(2) 0.3571(3) 0.75324(13) 0.0165(5) Uani 1 1 d D . . . .
H16 H 0.038(3) 0.4487(9) 0.7665(13) 0.020 Uiso 1 1 d D U . . .
C15 C -0.0432(2) 0.3093(3) 0.69941(13) 0.0187(5) Uani 1 1 d D . . . .
H15A H -0.094(2) 0.371(2) 0.6757(13) 0.022 Uiso 1 1 d D U . . .
H15B H -0.075(2) 0.2210(12) 0.7031(15) 0.022 Uiso 1 1 d D U . . .
C14 C 0.3743(2) 0.4144(3) 0.76324(12) 0.0158(5) Uani 1 1 d . . . . .
H14 H 0.3851 0.3215 0.7719 0.019 Uiso 1 1 calc R U . . .
C19 C 0.6937(2) 0.0591(3) 0.50677(15) 0.0248(6) Uani 1 1 d . . . . .
H19A H 0.7547 0.1244 0.4912 0.030 Uiso 1 1 calc R U . . .
H19B H 0.6710 0.0012 0.4667 0.030 Uiso 1 1 calc R U . . .
C20 C 0.7447(2) -0.0244(3) 0.56506(14) 0.0246(6) Uani 1 1 d . . . . .
H20A H 0.7703 0.0340 0.6037 0.037 Uiso 1 1 calc R U . . .
H20B H 0.8144 -0.0749 0.5485 0.037 Uiso 1 1 calc R U . . .
H20C H 0.6830 -0.0869 0.5812 0.037 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C1 1.957(3) . ?
W1 C2 1.965(3) . ?
W1 N2 2.206(2) . ?
W1 C16 2.211(3) . ?
W1 N4 2.213(2) . ?
W1 N5 2.224(2) . ?
W1 C17 2.314(3) . ?
W1 C15 2.317(3) . ?
C1 O1 1.163(3) . ?
N1 C4 1.338(3) . ?
N1 N2 1.348(3) . ?
F1 C21 1.344(3) . ?
F2 C21 1.325(3) . ?
O2 C2 1.158(3) . ?
N2 N3 1.321(3) . ?
F3 C21 1.333(3) . ?
C3 N3 1.343(3) . ?
C3 C4 1.390(3) . ?
C3 C18 1.479(4) . ?
O3 C18 1.189(3) . ?
N4 C5 1.346(3) . ?
N4 C9 1.348(3) . ?
C4 C21 1.488(3) . ?
O4 C18 1.340(3) . ?
O4 C19 1.454(3) . ?
C8 C7 1.383(3) . ?
C8 C9 1.385(3) . ?
C8 H8 0.9500 . ?
C7 C6 1.383(3) . ?
C7 H7 0.9500 . ?
C9 C10 1.478(3) . ?
C6 C5 1.379(3) . ?
C6 H6 0.9500 . ?
C10 N5 1.350(3) . ?
C10 C11 1.387(3) . ?
N5 C14 1.349(3) . ?
C5 H5 0.9500 . ?
C11 C12 1.380(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.380(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.376(3) . ?
C13 H13 0.9500 . ?
C17 C16 1.413(4) . ?
C17 H17A 0.950(5) . ?
C17 H17B 0.951(5) . ?
C16 C15 1.415(4) . ?
C16 H16 0.950(5) . ?
C15 H15A 0.950(5) . ?
C15 H15B 0.951(5) . ?
C14 H14 0.9500 . ?
C19 C20 1.496(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W1 C2 77.98(10) . . ?
C1 W1 N2 87.17(9) . . ?
C2 W1 N2 88.82(9) . . ?
C1 W1 C16 104.44(11) . . ?
C2 W1 C16 104.68(10) . . ?
N2 W1 C16 163.64(9) . . ?
C1 W1 N4 105.22(9) . . ?
C2 W1 N4 169.83(9) . . ?
N2 W1 N4 81.76(7) . . ?
C16 W1 N4 84.05(8) . . ?
C1 W1 N5 168.58(9) . . ?
C2 W1 N5 101.89(9) . . ?
N2 W1 N5 81.42(8) . . ?
C16 W1 N5 86.70(9) . . ?
N4 W1 N5 73.02(7) . . ?
C1 W1 C17 108.57(10) . . ?
C2 W1 C17 70.64(10) . . ?
N2 W1 C17 150.07(8) . . ?
C16 W1 C17 36.30(9) . . ?
N4 W1 C17 116.46(8) . . ?
N5 W1 C17 81.85(9) . . ?
C1 W1 C15 70.06(10) . . ?
C2 W1 C15 107.80(10) . . ?
N2 W1 C15 147.52(8) . . ?
C16 W1 C15 36.32(9) . . ?
N4 W1 C15 82.31(8) . . ?
N5 W1 C15 120.21(9) . . ?
C17 W1 C15 62.03(9) . . ?
O1 C1 W1 176.3(2) . . ?
C4 N1 N2 104.7(2) . . ?
O2 C2 W1 177.3(2) . . ?
N3 N2 N1 113.15(19) . . ?
N3 N2 W1 122.77(15) . . ?
N1 N2 W1 123.67(15) . . ?
N3 C3 C4 107.8(2) . . ?
N3 C3 C18 123.6(2) . . ?
C4 C3 C18 128.5(2) . . ?
N2 N3 C3 105.74(19) . . ?
C5 N4 C9 118.5(2) . . ?
C5 N4 W1 123.37(15) . . ?
C9 N4 W1 118.00(15) . . ?
N1 C4 C3 108.6(2) . . ?
N1 C4 C21 119.6(2) . . ?
C3 C4 C21 131.8(2) . . ?
C18 O4 C19 114.4(2) . . ?
C7 C8 C9 119.5(2) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C8 C7 C6 118.9(2) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
N4 C9 C8 121.6(2) . . ?
N4 C9 C10 115.7(2) . . ?
C8 C9 C10 122.7(2) . . ?
C5 C6 C7 118.8(2) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
N5 C10 C11 121.5(2) . . ?
N5 C10 C9 115.2(2) . . ?
C11 C10 C9 123.3(2) . . ?
C14 N5 C10 118.3(2) . . ?
C14 N5 W1 123.77(16) . . ?
C10 N5 W1 117.89(15) . . ?
N4 C5 C6 122.7(2) . . ?
N4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C12 C11 C10 119.5(2) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
F2 C21 F3 106.9(2) . . ?
F2 C21 F1 105.7(2) . . ?
F3 C21 F1 106.6(2) . . ?
F2 C21 C4 113.7(2) . . ?
F3 C21 C4 111.9(2) . . ?
F1 C21 C4 111.6(2) . . ?
C11 C12 C13 119.0(2) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
C14 C13 C12 118.9(2) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
O3 C18 O4 124.9(2) . . ?
O3 C18 C3 123.4(2) . . ?
O4 C18 C3 111.7(2) . . ?
C16 C17 W1 67.88(14) . . ?
C16 C17 H17A 119.1(17) . . ?
W1 C17 H17A 115.6(18) . . ?
C16 C17 H17B 118.2(17) . . ?
W1 C17 H17B 111.6(17) . . ?
H17A C17 H17B 115(2) . . ?
C17 C16 C15 115.1(2) . . ?
C17 C16 W1 75.81(15) . . ?
C15 C16 W1 75.95(15) . . ?
C17 C16 H16 121.9(17) . . ?
C15 C16 H16 122.8(16) . . ?
W1 C16 H16 111.9(17) . . ?
C16 C15 W1 67.73(15) . . ?
C16 C15 H15A 118.6(17) . . ?
W1 C15 H15A 115.3(18) . . ?
C16 C15 H15B 118.5(17) . . ?
W1 C15 H15B 112.7(18) . . ?
H15A C15 H15B 115(2) . . ?
N5 C14 C13 122.7(2) . . ?
N5 C14 H14 118.6 . . ?
C13 C14 H14 118.6 . . ?
O4 C19 C20 108.6(2) . . ?
O4 C19 H19A 110.0 . . ?
C20 C19 H19A 110.0 . . ?
O4 C19 H19B 110.0 . . ?
C20 C19 H19B 110.0 . . ?
H19A C19 H19B 108.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

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
C4 N1 N2 N3 0.8(2) . . . . ?
C4 N1 N2 W1 -172.06(15) . . . . ?
N1 N2 N3 C3 -0.4(3) . . . . ?
W1 N2 N3 C3 172.49(15) . . . . ?
C4 C3 N3 N2 -0.1(3) . . . . ?
C18 C3 N3 N2 -177.4(2) . . . . ?
N2 N1 C4 C3 -0.8(2) . . . . ?
N2 N1 C4 C21 177.2(2) . . . . ?
N3 C3 C4 N1 0.6(3) . . . . ?
C18 C3 C4 N1 177.7(2) . . . . ?
N3 C3 C4 C21 -177.1(2) . . . . ?
C18 C3 C4 C21 0.0(4) . . . . ?
C9 C8 C7 C6 -0.8(3) . . . . ?
C5 N4 C9 C8 -0.9(3) . . . . ?
W1 N4 C9 C8 175.12(17) . . . . ?
C5 N4 C9 C10 178.8(2) . . . . ?
W1 N4 C9 C10 -5.2(3) . . . . ?
C7 C8 C9 N4 1.4(3) . . . . ?
C7 C8 C9 C10 -178.3(2) . . . . ?
C8 C7 C6 C5 -0.2(3) . . . . ?
N4 C9 C10 N5 5.0(3) . . . . ?
C8 C9 C10 N5 -175.2(2) . . . . ?
N4 C9 C10 C11 -172.7(2) . . . . ?
C8 C9 C10 C11 7.0(4) . . . . ?
C11 C10 N5 C14 -2.8(3) . . . . ?
C9 C10 N5 C14 179.5(2) . . . . ?
C11 C10 N5 W1 175.20(18) . . . . ?
C9 C10 N5 W1 -2.6(3) . . . . ?
C9 N4 C5 C6 -0.2(3) . . . . ?
W1 N4 C5 C6 -176.01(17) . . . . ?
C7 C6 C5 N4 0.8(4) . . . . ?
N5 C10 C11 C12 0.6(4) . . . . ?
C9 C10 C11 C12 178.1(2) . . . . ?
N1 C4 C21 F2 136.2(2) . . . . ?
C3 C4 C21 F2 -46.4(4) . . . . ?
N1 C4 C21 F3 14.9(3) . . . . ?
C3 C4 C21 F3 -167.6(2) . . . . ?
N1 C4 C21 F1 -104.4(3) . . . . ?
C3 C4 C21 F1 73.0(3) . . . . ?
C10 C11 C12 C13 2.1(4) . . . . ?
C11 C12 C13 C14 -2.5(4) . . . . ?
C19 O4 C18 O3 3.1(4) . . . . ?
C19 O4 C18 C3 -177.9(2) . . . . ?
N3 C3 C18 O3 165.3(2) . . . . ?
C4 C3 C18 O3 -11.3(4) . . . . ?
N3 C3 C18 O4 -13.6(3) . . . . ?
C4 C3 C18 O4 169.7(2) . . . . ?
W1 C17 C16 C15 66.7(2) . . . . ?
C17 C16 C15 W1 -66.7(2) . . . . ?
C10 N5 C14 C13 2.3(3) . . . . ?
W1 N5 C14 C13 -175.51(18) . . . . ?
C12 C13 C14 N5 0.3(4) . . . . ?
C18 O4 C19 C20 -179.1(2) . . . . ?

_refine_diff_density_max         0.873
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.078


_chemical_name_common            '[W(allyl)(triazolateCF3,COOEt)(bpy)(CO)2]'
####################################################################### 
# 
# 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_AF047_a
_database_code_depnum_ccdc_archive 'CCDC 1562702'
_audit_update_record             
;
2017-07-17 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;

_audit_creation_date             2016-07-01
_shelx_SHELXL_version_number     2014/7
_chemical_formula_moiety         'C21 H19 N5 O6 W'
_chemical_formula_sum            'C21 H19 N5 O6 W'
_chemical_formula_weight         621.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   11.697(6)
_cell_length_b                   9.262(6)
_cell_length_c                   19.887(11)
_cell_angle_alpha                90
_cell_angle_beta                 103.39(2)
_cell_angle_gamma                90
_cell_volume                     2096(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6036
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      32.91
_cell_special_details            
;
To simulate systematic errors the final estimation of uncertainties
in unit cell parameters was based on 32 Monte-Carlo simulations.
;


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Bruker Kryoflex2).
;
_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      .
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_F_000             1208
_exptl_crystal_preparation       
'Crystal fragment soaked in perfluoro polyether oil.'
_exptl_crystal_recrystallization_method 
'recrystallised from dchloromethane and hexane by evaporation'
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.784
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    5.563
_shelx_estimated_absorpt_T_min   0.097
_shelx_estimated_absorpt_T_max   0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4438
_exptl_absorpt_correction_T_max  0.7465
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 -2.00 0.0510
0.00 0.00 1.00 0.1140
1.00 0.00 3.00 0.0990
2.00 -3.00 2.00 0.2650
-1.00 0.00 -2.00 0.0530
1.00 0.00 2.00 0.0900
0.00 -3.00 -2.00 0.2630
0.00 3.00 2.00 0.3700
-2.00 3.00 -1.00 0.3330
0.00 -2.00 -1.00 0.2650
-3.00 0.00 -2.00 0.0330
1.00 3.00 1.00 0.3690
-3.00 0.00 -1.00 0.0260
3.00 0.00 1.00 0.0480
1.00 0.00 0.00 0.0450
-2.00 0.00 1.00 0.0340

_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            15002
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.438
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4133
_reflns_number_gt                3528
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 ver. 2014.11-0 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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.The C-H distances between the atoms of 
the allyl moiety were kept during refinement at the value of 0.950(5) using 
DFIX restraint.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0105P)²+0.6969P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4133
_refine_ls_number_parameters     315
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0227
_refine_ls_wR_factor_ref         0.0511
_refine_ls_wR_factor_gt          0.0487
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.63975(2) 0.66513(2) 0.68668(2) 0.00948(5) Uani 1 1 d . . . . .
O1 O 0.7461(2) 0.9631(3) 0.74166(13) 0.0180(6) Uani 1 1 d . . . . .
C1 C 0.7049(3) 0.8523(4) 0.72190(18) 0.0133(8) Uani 1 1 d . . . . .
N1 N 0.7600(3) 0.5905(3) 0.56267(15) 0.0136(7) Uani 1 1 d . . . . .
O2 O 0.4530(3) 0.8690(3) 0.59596(14) 0.0195(6) Uani 1 1 d . . . . .
C2 C 0.5216(3) 0.7915(4) 0.62956(19) 0.0131(8) Uani 1 1 d . . . . .
N2 N 0.7376(3) 0.6912(3) 0.60573(15) 0.0120(6) Uani 1 1 d . . . . .
O3 O 0.8605(3) 0.9203(3) 0.43578(14) 0.0257(7) Uani 1 1 d . . . . .
C3 C 0.8051(3) 0.8069(4) 0.53022(18) 0.0130(8) Uani 1 1 d . . . . .
N3 N 0.7622(3) 0.8249(3) 0.58689(15) 0.0134(6) Uani 1 1 d . . . . .
N4 N 0.7894(3) 0.5227(3) 0.73500(14) 0.0113(6) Uani 1 1 d . . . . .
O4 O 0.8221(3) 1.0558(3) 0.52158(14) 0.0218(6) Uani 1 1 d . . . . .
C4 C 0.8031(3) 0.6595(4) 0.51509(18) 0.0130(7) Uani 1 1 d . . . . .
N5 N 0.6036(3) 0.4489(3) 0.63687(15) 0.0104(6) Uani 1 1 d . . . . .
C5 C 0.8816(3) 0.5645(4) 0.78464(19) 0.0154(8) Uani 1 1 d . . . . .
H5 H 0.8846 0.6620 0.7997 0.018 Uiso 1 1 calc R U . . .
O5 O 0.7659(2) 0.4883(3) 0.42423(14) 0.0229(6) Uani 1 1 d . . . . .
C9 C 0.7857(3) 0.3826(4) 0.71283(18) 0.0114(7) Uani 1 1 d . . . . .
C8 C 0.8741(3) 0.2859(4) 0.7429(2) 0.0169(8) Uani 1 1 d . . . . .
H8 H 0.8696 0.1881 0.7282 0.020 Uiso 1 1 calc R U . . .
C7 C 0.9681(3) 0.3318(4) 0.79382(19) 0.0177(8) Uani 1 1 d . . . . .
H7 H 1.0291 0.2666 0.8141 0.021 Uiso 1 1 calc R U . . .
C6 C 0.9721(3) 0.4745(4) 0.81491(18) 0.0159(8) Uani 1 1 d . . . . .
H6 H 1.0361 0.5093 0.8496 0.019 Uiso 1 1 calc R U . . .
O6 O 0.9338(2) 0.6129(3) 0.44540(14) 0.0215(6) Uani 1 1 d . . . . .
C10 C 0.6858(3) 0.3449(4) 0.65642(18) 0.0118(7) Uani 1 1 d . . . . .
C11 C 0.6761(4) 0.2115(4) 0.62377(18) 0.0147(8) Uani 1 1 d . . . . .
H11 H 0.7332 0.1385 0.6394 0.018 Uiso 1 1 calc R U . . .
C21 C 0.9637(4) 0.5411(4) 0.3873(2) 0.0260(10) Uani 1 1 d . . . . .
H21A H 0.9728 0.4374 0.3968 0.039 Uiso 1 1 calc R U . . .
H21B H 1.0376 0.5805 0.3800 0.039 Uiso 1 1 calc R U . . .
H21C H 0.9010 0.5568 0.3458 0.039 Uiso 1 1 calc R U . . .
C20 C 0.8289(3) 0.5778(4) 0.45595(19) 0.0125(8) Uani 1 1 d . . . . .
C12 C 0.5831(4) 0.1861(4) 0.56865(19) 0.0177(8) Uani 1 1 d . . . . .
H12 H 0.5763 0.0963 0.5450 0.021 Uiso 1 1 calc R U . . .
C13 C 0.4999(3) 0.2924(4) 0.54808(19) 0.0154(8) Uani 1 1 d . . . . .
H13 H 0.4351 0.2767 0.5101 0.018 Uiso 1 1 calc R U . . .
C18 C 0.8339(3) 0.9311(4) 0.49046(19) 0.0155(8) Uani 1 1 d . . . . .
C17 C 0.4594(4) 0.6294(4) 0.7122(2) 0.0167(8) Uani 1 1 d D . . . .
H17A H 0.408(3) 0.562(3) 0.6842(16) 0.020 Uiso 1 1 d D U . . .
H17B H 0.428(3) 0.722(2) 0.719(2) 0.020 Uiso 1 1 d D U . . .
C16 C 0.5520(4) 0.5812(4) 0.7658(2) 0.0158(8) Uani 1 1 d D . . . .
H16 H 0.567(3) 0.4811(11) 0.772(2) 0.019 Uiso 1 1 d D U . . .
C15 C 0.6269(4) 0.6888(4) 0.8009(2) 0.0191(9) Uani 1 1 d D . . . .
H15A H 0.696(2) 0.662(4) 0.8342(16) 0.023 Uiso 1 1 d D U . . .
H15B H 0.594(3) 0.779(2) 0.809(2) 0.023 Uiso 1 1 d D U . . .
C14 C 0.5119(3) 0.4227(4) 0.58356(18) 0.0129(8) Uani 1 1 d . . . . .
H14 H 0.4539 0.4953 0.5698 0.016 Uiso 1 1 calc R U . . .
C19 C 0.8363(4) 1.1841(4) 0.4826(2) 0.0267(10) Uani 1 1 d . . . . .
H19A H 0.9181 1.1915 0.4787 0.040 Uiso 1 1 calc R U . . .
H19B H 0.8159 1.2696 0.5064 0.040 Uiso 1 1 calc R U . . .
H19C H 0.7844 1.1781 0.4363 0.040 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C1 1.957(4) . ?
W1 C2 1.960(4) . ?
W1 N2 2.194(3) . ?
W1 C16 2.209(4) . ?
W1 N4 2.224(3) . ?
W1 N5 2.231(3) . ?
W1 C17 2.305(4) . ?
W1 C15 2.321(4) . ?
O1 C1 1.163(4) . ?
N1 N2 1.332(4) . ?
N1 C4 1.333(5) . ?
O2 C2 1.165(5) . ?
N2 N3 1.344(4) . ?
O3 C18 1.202(5) . ?
C3 N3 1.346(5) . ?
C3 C4 1.397(5) . ?
C3 C18 1.478(5) . ?
N4 C5 1.340(5) . ?
N4 C9 1.368(4) . ?
O4 C18 1.332(4) . ?
O4 C19 1.450(4) . ?
C4 C20 1.487(5) . ?
N5 C14 1.344(5) . ?
N5 C10 1.353(5) . ?
C5 C6 1.372(5) . ?
C5 H5 0.9500 . ?
O5 C20 1.189(4) . ?
C9 C8 1.394(5) . ?
C9 C10 1.462(5) . ?
C8 C7 1.378(5) . ?
C8 H8 0.9500 . ?
C7 C6 1.384(5) . ?
C7 H7 0.9500 . ?
C6 H6 0.9500 . ?
O6 C20 1.332(5) . ?
O6 C21 1.444(5) . ?
C10 C11 1.389(5) . ?
C11 C12 1.374(5) . ?
C11 H11 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C12 C13 1.379(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.388(5) . ?
C13 H13 0.9500 . ?
C17 C16 1.404(6) . ?
C17 H17A 0.949(5) . ?
C17 H17B 0.950(5) . ?
C16 C15 1.402(6) . ?
C16 H16 0.948(5) . ?
C15 H15A 0.950(5) . ?
C15 H15B 0.950(5) . ?
C14 H14 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W1 C2 80.93(15) . . ?
C1 W1 N2 86.50(13) . . ?
C2 W1 N2 85.79(13) . . ?
C1 W1 C16 105.28(14) . . ?
C2 W1 C16 103.96(15) . . ?
N2 W1 C16 165.61(12) . . ?
C1 W1 N4 99.68(13) . . ?
C2 W1 N4 169.40(13) . . ?
N2 W1 N4 83.69(11) . . ?
C16 W1 N4 86.15(13) . . ?
C1 W1 N5 166.47(14) . . ?
C2 W1 N5 104.07(13) . . ?
N2 W1 N5 81.40(11) . . ?
C16 W1 N5 85.91(13) . . ?
N4 W1 N5 73.07(11) . . ?
C1 W1 C17 110.41(14) . . ?
C2 W1 C17 69.83(15) . . ?
N2 W1 C17 146.83(13) . . ?
C16 W1 C17 36.16(14) . . ?
N4 W1 C17 119.24(13) . . ?
N5 W1 C17 83.11(12) . . ?
C1 W1 C15 70.99(14) . . ?
C2 W1 C15 108.30(15) . . ?
N2 W1 C15 150.54(14) . . ?
C16 W1 C15 35.94(14) . . ?
N4 W1 C15 81.72(13) . . ?
N5 W1 C15 118.07(12) . . ?
C17 W1 C15 61.83(15) . . ?
O1 C1 W1 177.9(3) . . ?
N2 N1 C4 106.5(3) . . ?
O2 C2 W1 178.6(3) . . ?
N1 N2 N3 112.3(3) . . ?
N1 N2 W1 127.5(2) . . ?
N3 N2 W1 119.2(2) . . ?
N3 C3 C4 108.1(3) . . ?
N3 C3 C18 121.8(3) . . ?
C4 C3 C18 129.8(3) . . ?
N2 N3 C3 105.3(3) . . ?
C5 N4 C9 118.1(3) . . ?
C5 N4 W1 124.5(2) . . ?
C9 N4 W1 117.4(2) . . ?
C18 O4 C19 115.2(3) . . ?
N1 C4 C3 107.8(3) . . ?
N1 C4 C20 119.8(3) . . ?
C3 C4 C20 132.1(3) . . ?
C14 N5 C10 118.9(3) . . ?
C14 N5 W1 123.1(2) . . ?
C10 N5 W1 117.5(2) . . ?
N4 C5 C6 123.7(3) . . ?
N4 C5 H5 118.1 . . ?
C6 C5 H5 118.1 . . ?
N4 C9 C8 120.4(3) . . ?
N4 C9 C10 115.7(3) . . ?
C8 C9 C10 123.9(3) . . ?
C7 C8 C9 120.2(3) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C8 C7 C6 118.8(4) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C5 C6 C7 118.6(4) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
C20 O6 C21 114.6(3) . . ?
N5 C10 C11 121.6(3) . . ?
N5 C10 C9 116.0(3) . . ?
C11 C10 C9 122.4(3) . . ?
C12 C11 C10 119.3(4) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
O6 C21 H21A 109.5 . . ?
O6 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O6 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C20 O6 124.6(3) . . ?
O5 C20 C4 124.0(3) . . ?
O6 C20 C4 111.3(3) . . ?
C11 C12 C13 119.2(3) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C12 C13 C14 119.3(4) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
O3 C18 O4 124.6(3) . . ?
O3 C18 C3 123.9(3) . . ?
O4 C18 C3 111.4(3) . . ?
C16 C17 W1 68.2(2) . . ?
C16 C17 H17A 120(2) . . ?
W1 C17 H17A 117(2) . . ?
C16 C17 H17B 116(2) . . ?
W1 C17 H17B 107(3) . . ?
H17A C17 H17B 117(4) . . ?
C15 C16 C17 115.8(3) . . ?
C15 C16 W1 76.4(2) . . ?
C17 C16 W1 75.7(2) . . ?
C15 C16 H16 123(3) . . ?
C17 C16 H16 120(2) . . ?
W1 C16 H16 110(2) . . ?
C16 C15 W1 67.7(2) . . ?
C16 C15 H15A 120(2) . . ?
W1 C15 H15A 115(3) . . ?
C16 C15 H15B 119(3) . . ?
W1 C15 H15B 111(3) . . ?
H15A C15 H15B 115(4) . . ?
N5 C14 C13 121.7(3) . . ?
N5 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
C4 N1 N2 N3 1.4(4) . . . . ?
C4 N1 N2 W1 169.3(2) . . . . ?
N1 N2 N3 C3 -1.7(4) . . . . ?
W1 N2 N3 C3 -170.7(2) . . . . ?
C4 C3 N3 N2 1.2(4) . . . . ?
C18 C3 N3 N2 175.0(3) . . . . ?
N2 N1 C4 C3 -0.6(4) . . . . ?
N2 N1 C4 C20 -175.5(3) . . . . ?
N3 C3 C4 N1 -0.4(4) . . . . ?
C18 C3 C4 N1 -173.6(4) . . . . ?
N3 C3 C4 C20 173.6(4) . . . . ?
C18 C3 C4 C20 0.5(7) . . . . ?
C9 N4 C5 C6 -0.6(5) . . . . ?
W1 N4 C5 C6 178.6(3) . . . . ?
C5 N4 C9 C8 1.9(5) . . . . ?
W1 N4 C9 C8 -177.3(3) . . . . ?
C5 N4 C9 C10 -177.3(3) . . . . ?
W1 N4 C9 C10 3.5(4) . . . . ?
N4 C9 C8 C7 -2.0(5) . . . . ?
C10 C9 C8 C7 177.1(4) . . . . ?
C9 C8 C7 C6 0.8(6) . . . . ?
N4 C5 C6 C7 -0.6(6) . . . . ?
C8 C7 C6 C5 0.5(6) . . . . ?
C14 N5 C10 C11 -1.5(5) . . . . ?
W1 N5 C10 C11 -173.9(3) . . . . ?
C14 N5 C10 C9 177.5(3) . . . . ?
W1 N5 C10 C9 5.0(4) . . . . ?
N4 C9 C10 N5 -5.6(5) . . . . ?
C8 C9 C10 N5 175.3(3) . . . . ?
N4 C9 C10 C11 173.4(3) . . . . ?
C8 C9 C10 C11 -5.8(6) . . . . ?
N5 C10 C11 C12 2.4(5) . . . . ?
C9 C10 C11 C12 -176.5(3) . . . . ?
C21 O6 C20 O5 4.8(5) . . . . ?
C21 O6 C20 C4 -178.2(3) . . . . ?
N1 C4 C20 O5 43.1(5) . . . . ?
C3 C4 C20 O5 -130.3(5) . . . . ?
N1 C4 C20 O6 -134.0(4) . . . . ?
C3 C4 C20 O6 52.6(5) . . . . ?
C10 C11 C12 C13 -1.6(6) . . . . ?
C11 C12 C13 C14 0.0(6) . . . . ?
C19 O4 C18 O3 3.9(6) . . . . ?
C19 O4 C18 C3 -173.6(3) . . . . ?
N3 C3 C18 O3 -171.8(4) . . . . ?
C4 C3 C18 O3 0.5(7) . . . . ?
N3 C3 C18 O4 5.8(5) . . . . ?
C4 C3 C18 O4 178.1(4) . . . . ?
W1 C17 C16 C15 66.9(3) . . . . ?
C17 C16 C15 W1 -66.4(3) . . . . ?
C10 N5 C14 C13 -0.3(5) . . . . ?
W1 N5 C14 C13 171.8(3) . . . . ?
C12 C13 C14 N5 1.0(5) . . . . ?

_refine_diff_density_max         0.787
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.119


_chemical_name_common            '[W(allyl)(triazolateCOOCH3,COOCH3)(bpy)(CO)2]'
