# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_mo_jv170412mo1_vinklarek
_database_code_depnum_ccdc_archive 'CCDC 1914239'
loop_
_audit_author_name
_audit_author_address
'Ivana Cisarova'
;Charles Univerzity
Czech Republic
;
_audit_update_record             
;
2019-05-06 deposited with the CCDC.	2019-07-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H17 Mo N O2'
_chemical_formula_sum            'C23 H17 Mo N O2'
_chemical_formula_weight         435.32
_chemical_compound_source        'synthesized by the authors'

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           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   9.9777(5)
_cell_length_b                   7.6944(4)
_cell_length_c                   12.0138(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.813(2)
_cell_angle_gamma                90
_cell_volume                     921.22(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9827
_cell_measurement_theta_min      2.5919
_cell_measurement_theta_max      27.4891

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_F_000             440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.116
_exptl_absorpt_coefficient_mu    0.729
_shelx_estimated_absorpt_T_min   0.869
_shelx_estimated_absorpt_T_max   0.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS  micro-focus sealed tube'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27429
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.592
_diffrn_reflns_theta_max         27.517
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4220
_reflns_number_gt                4109
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.999

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.4'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0279P)²+0.1755P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.37(3)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         4220
_refine_ls_number_parameters     252
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0172
_refine_ls_wR_factor_ref         0.0451
_refine_ls_wR_factor_gt          0.0445
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_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 0.83638(2) 0.18333(4) 0.20869(2) 0.02028(6) Uani 1 1 d . . . . .
O1 O 0.8789(2) 0.2983(3) 0.45466(16) 0.0370(5) Uani 1 1 d . . . . .
O2 O 1.0038(2) -0.1318(3) 0.2983(2) 0.0415(5) Uani 1 1 d . . . . .
N1 N 0.3790(2) 0.1225(3) 0.3332(2) 0.0253(5) Uani 1 1 d . . . . .
C9 C 0.7241(3) 0.1224(6) -0.0631(3) 0.0572(13) Uani 1 1 d . . . . .
H9 H 0.760278 0.022358 -0.096889 0.069 Uiso 1 1 calc R U . . .
C1 C 0.6038(2) 0.2311(4) 0.2136(2) 0.0227(6) Uani 1 1 d . . . . .
C2 C 0.6315(3) 0.0515(4) 0.2299(2) 0.0282(5) Uani 1 1 d . . . . .
H2 H 0.606811 -0.018333 0.296053 0.034 Uiso 1 1 calc R U . . .
C3 C 0.6869(3) -0.0171(4) 0.1318(3) 0.0357(7) Uani 1 1 d . . . . .
H3 H 0.706614 -0.142445 0.117764 0.043 Uiso 1 1 calc R U . . .
C4 C 0.6852(3) 0.1175(5) 0.0509(2) 0.0373(7) Uani 1 1 d . . . . .
C5 C 0.6349(2) 0.2730(4) 0.0998(2) 0.0288(6) Uani 1 1 d . . . . .
C6 C 0.6200(3) 0.4283(5) 0.0358(2) 0.0395(7) Uani 1 1 d . . . . .
H6 H 0.585669 0.531202 0.067595 0.047 Uiso 1 1 calc R U . . .
C7 C 0.6566(3) 0.4255(6) -0.0729(3) 0.0557(12) Uani 1 1 d . . . . .
H7 H 0.647221 0.528012 -0.116666 0.067 Uiso 1 1 calc R U . . .
C8 C 0.7079(3) 0.2729(7) -0.1209(3) 0.0629(13) Uani 1 1 d . . . . .
H8 H 0.731821 0.275990 -0.196479 0.076 Uiso 1 1 calc R U . . .
C10 C 0.5339(2) 0.3501(3) 0.28885(19) 0.0219(5) Uani 1 1 d . . . . .
C11 C 0.5737(3) 0.5200(3) 0.3036(2) 0.0282(5) Uani 1 1 d . . . . .
H11 H 0.651694 0.559132 0.268897 0.034 Uiso 1 1 calc R U . . .
C12 C 0.5029(3) 0.6379(3) 0.3683(2) 0.0320(6) Uani 1 1 d . . . . .
H12 H 0.532724 0.754818 0.375505 0.038 Uiso 1 1 calc R U . . .
C13 C 0.3910(3) 0.5848(4) 0.4209(2) 0.0309(6) Uani 1 1 d . . . . .
H13 H 0.343391 0.664792 0.464494 0.037 Uiso 1 1 calc R U . . .
C14 C 0.3469(3) 0.4119(3) 0.4102(2) 0.0241(5) Uani 1 1 d . . . . .
C15 C 0.2328(3) 0.3494(4) 0.4646(2) 0.0298(5) Uani 1 1 d . . . . .
H15 H 0.181800 0.425995 0.507857 0.036 Uiso 1 1 calc R U . . .
C16 C 0.1976(2) 0.1799(6) 0.45419(19) 0.0312(4) Uani 1 1 d . . . . .
H16 H 0.122700 0.135669 0.490999 0.037 Uiso 1 1 calc R U . . .
C17 C 0.2741(3) 0.0699(4) 0.3877(2) 0.0289(5) Uani 1 1 d . . . . .
H17 H 0.248864 -0.048942 0.381781 0.035 Uiso 1 1 calc R U . . .
C18 C 0.4173(3) 0.2914(4) 0.3447(2) 0.0205(5) Uani 1 1 d . . . . .
C19 C 0.8649(2) 0.2576(3) 0.3617(2) 0.0244(5) Uani 1 1 d . . . . .
C20 C 0.9444(3) -0.0125(3) 0.2644(2) 0.0273(5) Uani 1 1 d . . . . .
C21A C 0.9410(4) 0.4529(5) 0.1950(3) 0.0472(8) Uani 1 1 d . . . . .
H211 H 0.881593 0.555197 0.179922 0.057 Uiso 0.634(5) 1 d R U P A 1
H221 H 1.017036 0.477382 0.248720 0.057 Uiso 0.634(5) 1 d R U P A 1
H231 H 0.860093 0.458183 0.150100 0.057 Uiso 0.366(5) 1 d R U P A 2
H241 H 0.956490 0.533326 0.254274 0.057 Uiso 0.366(5) 1 d R U P A 2
C22A C 0.9648(4) 0.3438(6) 0.1056(4) 0.0339(9) Uani 0.634(5) 1 d D . P A 1
H22A H 0.929260 0.378814 0.029621 0.041 Uiso 0.634(5) 1 d R U P A 1
C23A C 1.0366(7) 0.1842(9) 0.1169(5) 0.0360(13) Uani 0.634(5) 1 d D . P A 1
H23A H 1.106582 0.184180 0.155381 0.043 Uiso 0.634(5) 1 d R U P A 1
H24A H 1.041082 0.106978 0.056781 0.043 Uiso 0.634(5) 1 d R U P A 1
C22B C 1.0278(7) 0.3410(11) 0.1747(6) 0.0339(9) Uani 0.366(5) 1 d D . P A 2
H22B H 1.108981 0.341102 0.219525 0.041 Uiso 0.366(5) 1 calc R U P A 2
C23B C 1.0128(15) 0.2137(16) 0.0889(9) 0.0360(13) Uani 0.366(5) 1 d D . P A 2
H23B H 0.932863 0.209966 0.042583 0.043 Uiso 0.366(5) 1 calc R U P A 2
H24B H 1.082650 0.132480 0.077976 0.043 Uiso 0.366(5) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C19 1.933(3) . ?
Mo1 C20 1.952(3) . ?
Mo1 C22A 2.204(4) . ?
Mo1 C3 2.307(3) . ?
Mo1 C2 2.307(3) . ?
Mo1 C22B 2.316(7) . ?
Mo1 C23A 2.329(7) . ?
Mo1 C21A 2.332(3) . ?
Mo1 C23B 2.339(15) . ?
Mo1 C1 2.353(2) . ?
Mo1 C4 2.418(3) . ?
Mo1 C5 2.443(2) . ?
O1 C19 1.162(3) . ?
O2 C20 1.156(3) . ?
N1 C17 1.325(3) . ?
N1 C18 1.359(3) . ?
C9 C8 1.356(7) . ?
C9 C4 1.441(4) . ?
C9 H9 0.9500 . ?
C1 C2 1.421(5) . ?
C1 C5 1.453(4) . ?
C1 C10 1.485(3) . ?
C2 C3 1.427(4) . ?
C2 H2 1.0000 . ?
C3 C4 1.420(5) . ?
C3 H3 1.0000 . ?
C4 C5 1.435(4) . ?
C5 C6 1.425(4) . ?
C6 C7 1.373(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.416(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C10 C11 1.375(4) . ?
C10 C18 1.444(3) . ?
C11 C12 1.407(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.372(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.405(4) . ?
C13 H13 0.9500 . ?
C14 C18 1.423(4) . ?
C14 C15 1.424(3) . ?
C15 C16 1.355(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.413(4) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C21A C22B 1.253(9) . ?
C21A C22A 1.393(6) . ?
C21A H211 0.9968 . ?
C21A H221 0.9892 . ?
C21A H231 0.9500 . ?
C21A H241 0.9500 . ?
C22A C23A 1.425(4) . ?
C22A H22A 1.0000 . ?
C23A H23A 0.8178 . ?
C23A H24A 0.9385 . ?
C22B C23B 1.425(4) . ?
C22B H22B 0.9500 . ?
C23B H23B 0.9500 . ?
C23B H24B 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
C19 Mo1 C20 81.32(11) . . ?
C19 Mo1 C22A 107.84(15) . . ?
C20 Mo1 C22A 107.36(14) . . ?
C19 Mo1 C3 129.84(11) . . ?
C20 Mo1 C3 87.50(11) . . ?
C22A Mo1 C3 122.14(15) . . ?
C19 Mo1 C2 96.60(10) . . ?
C20 Mo1 C2 95.75(11) . . ?
C22A Mo1 C2 148.34(14) . . ?
C3 Mo1 C2 36.03(10) . . ?
C19 Mo1 C22B 85.9(2) . . ?
C20 Mo1 C22B 91.0(2) . . ?
C3 Mo1 C22B 143.4(2) . . ?
C2 Mo1 C22B 173.0(2) . . ?
C19 Mo1 C23A 111.07(16) . . ?
C20 Mo1 C23A 72.08(16) . . ?
C22A Mo1 C23A 36.50(13) . . ?
C3 Mo1 C23A 111.43(18) . . ?
C2 Mo1 C23A 147.02(18) . . ?
C19 Mo1 C21A 76.02(12) . . ?
C20 Mo1 C21A 117.98(13) . . ?
C22A Mo1 C21A 35.63(15) . . ?
C3 Mo1 C21A 148.17(14) . . ?
C2 Mo1 C21A 143.24(12) . . ?
C22B Mo1 C21A 31.3(2) . . ?
C23A Mo1 C21A 64.30(19) . . ?
C19 Mo1 C23B 118.4(2) . . ?
C20 Mo1 C23B 82.4(3) . . ?
C3 Mo1 C23B 108.2(2) . . ?
C2 Mo1 C23B 144.0(2) . . ?
C22B Mo1 C23B 35.65(17) . . ?
C21A Mo1 C23B 61.0(3) . . ?
C19 Mo1 C1 91.68(9) . . ?
C20 Mo1 C1 129.85(10) . . ?
C22A Mo1 C1 121.87(13) . . ?
C3 Mo1 C1 59.70(10) . . ?
C2 Mo1 C1 35.49(12) . . ?
C22B Mo1 C1 138.2(2) . . ?
C23A Mo1 C1 151.82(13) . . ?
C21A Mo1 C1 107.97(12) . . ?
C23B Mo1 C1 140.6(3) . . ?
C19 Mo1 C4 149.88(10) . . ?
C20 Mo1 C4 114.82(11) . . ?
C22A Mo1 C4 91.96(14) . . ?
C3 Mo1 C4 34.89(12) . . ?
C2 Mo1 C4 58.16(10) . . ?
C22B Mo1 C4 117.4(2) . . ?
C23A Mo1 C4 98.40(15) . . ?
C21A Mo1 C4 113.30(13) . . ?
C23B Mo1 C4 89.9(3) . . ?
C1 Mo1 C4 58.30(9) . . ?
C19 Mo1 C5 120.31(10) . . ?
C20 Mo1 C5 145.85(11) . . ?
C22A Mo1 C5 91.53(13) . . ?
C3 Mo1 C5 58.38(11) . . ?
C2 Mo1 C5 58.21(10) . . ?
C22B Mo1 C5 114.9(2) . . ?
C23A Mo1 C5 116.62(13) . . ?
C21A Mo1 C5 94.05(13) . . ?
C23B Mo1 C5 105.5(3) . . ?
C1 Mo1 C5 35.21(8) . . ?
C4 Mo1 C5 34.32(10) . . ?
C17 N1 C18 117.8(2) . . ?
C8 C9 C4 118.6(4) . . ?
C8 C9 H9 120.7 . . ?
C4 C9 H9 120.7 . . ?
C2 C1 C5 107.2(2) . . ?
C2 C1 C10 127.6(2) . . ?
C5 C1 C10 124.4(2) . . ?
C2 C1 Mo1 70.52(15) . . ?
C5 C1 Mo1 75.80(14) . . ?
C10 C1 Mo1 127.24(17) . . ?
C1 C2 C3 109.1(3) . . ?
C1 C2 Mo1 73.99(16) . . ?
C3 C2 Mo1 71.97(15) . . ?
C1 C2 H2 125.3 . . ?
C3 C2 H2 125.3 . . ?
Mo1 C2 H2 125.3 . . ?
C4 C3 C2 107.7(3) . . ?
C4 C3 Mo1 76.82(16) . . ?
C2 C3 Mo1 72.00(15) . . ?
C4 C3 H3 125.7 . . ?
C2 C3 H3 125.7 . . ?
Mo1 C3 H3 125.7 . . ?
C3 C4 C5 108.7(2) . . ?
C3 C4 C9 132.4(3) . . ?
C5 C4 C9 118.9(3) . . ?
C3 C4 Mo1 68.29(15) . . ?
C5 C4 Mo1 73.81(15) . . ?
C9 C4 Mo1 123.6(2) . . ?
C6 C5 C4 120.5(3) . . ?
C6 C5 C1 132.2(3) . . ?
C4 C5 C1 107.2(3) . . ?
C6 C5 Mo1 125.94(19) . . ?
C4 C5 Mo1 71.86(15) . . ?
C1 C5 Mo1 68.99(14) . . ?
C7 C6 C5 118.3(4) . . ?
C7 C6 H6 120.8 . . ?
C5 C6 H6 120.8 . . ?
C6 C7 C8 121.3(4) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C9 C8 C7 122.4(3) . . ?
C9 C8 H8 118.8 . . ?
C7 C8 H8 118.8 . . ?
C11 C10 C18 118.1(2) . . ?
C11 C10 C1 121.6(2) . . ?
C18 C10 C1 120.2(2) . . ?
C10 C11 C12 122.3(2) . . ?
C10 C11 H11 118.8 . . ?
C12 C11 H11 118.8 . . ?
C13 C12 C11 120.3(2) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 119.8(2) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C13 C14 C18 120.5(2) . . ?
C13 C14 C15 122.1(2) . . ?
C18 C14 C15 117.4(2) . . ?
C16 C15 C14 119.5(2) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 118.9(2) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
N1 C17 C16 123.9(3) . . ?
N1 C17 H17 118.0 . . ?
C16 C17 H17 118.0 . . ?
N1 C18 C14 122.4(2) . . ?
N1 C18 C10 118.7(2) . . ?
C14 C18 C10 118.9(2) . . ?
O1 C19 Mo1 177.7(2) . . ?
O2 C20 Mo1 177.3(2) . . ?
C22B C21A Mo1 73.7(4) . . ?
C22A C21A Mo1 67.2(2) . . ?
C22A C21A H211 117.3 . . ?
Mo1 C21A H211 116.8 . . ?
C22A C21A H221 117.6 . . ?
Mo1 C21A H221 117.1 . . ?
H211 C21A H221 113.5 . . ?
C22B C21A H231 119.7 . . ?
Mo1 C21A H231 72.9 . . ?
C22B C21A H241 120.3 . . ?
Mo1 C21A H241 125.7 . . ?
H231 C21A H241 120.0 . . ?
C21A C22A C23A 123.3(4) . . ?
C21A C22A Mo1 77.2(2) . . ?
C23A C22A Mo1 76.5(3) . . ?
C21A C22A H22A 118.4 . . ?
C23A C22A H22A 118.3 . . ?
Mo1 C22A H22A 118.3 . . ?
C22A C23A Mo1 67.0(3) . . ?
C22A C23A H23A 117.8 . . ?
Mo1 C23A H23A 117.4 . . ?
C22A C23A H24A 121.0 . . ?
Mo1 C23A H24A 115.9 . . ?
H23A C23A H24A 111.3 . . ?
C21A C22B C23B 124.3(9) . . ?
C21A C22B Mo1 75.0(3) . . ?
C23B C22B Mo1 73.1(7) . . ?
C21A C22B H22B 117.8 . . ?
C23B C22B H22B 117.8 . . ?
Mo1 C22B H22B 126.0 . . ?
C22B C23B Mo1 71.3(6) . . ?
C22B C23B H23B 120.0 . . ?
Mo1 C23B H23B 73.9 . . ?
C22B C23B H24B 120.0 . . ?
Mo1 C23B H24B 126.8 . . ?
H23B C23B H24B 120.0 . . ?

_refine_diff_density_max         0.430
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.048

####################################################################### 
# 
# 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_mo_jv171009w1_vinklarek
_database_code_depnum_ccdc_archive 'CCDC 1914241'
loop_
_audit_author_name
_audit_author_address
'Ivana Cisarova'
;Charles Univerzity
Czech Republic
;
_audit_update_record             
;
2019-05-06 deposited with the CCDC.	2019-07-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H18 N O2 W, B F4'
_chemical_formula_sum            'C23 H18 B F4 N O2 W'
_chemical_formula_weight         611.04
_chemical_compound_source        'synthesized by the authors'


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.4483(16)
_cell_length_b                   8.0338(4)
_cell_length_c                   21.5649(11)
_cell_angle_alpha                90
_cell_angle_beta                 123.377(2)
_cell_angle_gamma                90
_cell_volume                     4115.7(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9884
_cell_measurement_theta_min      2.6764
_cell_measurement_theta_max      27.4796

_exptl_crystal_description       prism
_exptl_crystal_colour            red-orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_F_000             2352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.053
_exptl_absorpt_coefficient_mu    5.671
_shelx_estimated_absorpt_T_min   0.492
_shelx_estimated_absorpt_T_max   0.753
_exptl_absorpt_correction_type   'Numerical Mu From Formula'
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_T_max  0.75

_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS  micro-focus sealed tube'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35020
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.676
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4726
_reflns_number_gt                4149
_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       'Bruker Instrument Service vV6.2.6'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0675P)²+91.9365P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4726
_refine_ls_number_parameters     290
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0556
_refine_ls_wR_factor_ref         0.1322
_refine_ls_wR_factor_gt          0.1279
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_restrained_S_all      1.148
_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 0.37511(2) 0.42958(4) 0.53947(2) 0.01531(12) Uani 1 1 d . . . A 1
C1 C 0.3688(3) 0.2857(10) 0.4418(4) 0.0190(15) Uani 1 1 d . . . A 1
C2 C 0.3273(3) 0.2276(10) 0.4552(4) 0.0173(15) Uani 1 1 d . . . A 1
H2 H 0.287562 0.237875 0.422953 0.021 Uiso 1 1 calc R U . A 1
C3 C 0.3581(3) 0.1508(9) 0.5275(4) 0.0175(15) Uani 1 1 d . . . A 1
H3 H 0.341803 0.104785 0.552063 0.021 Uiso 1 1 calc R U . A 1
C4 C 0.4163(4) 0.1543(10) 0.5562(4) 0.0220(16) Uani 1 1 d . . . A 1
C5 C 0.4234(3) 0.2380(10) 0.5034(4) 0.0178(15) Uani 1 1 d . . . A 1
C6 C 0.4781(3) 0.2533(11) 0.5161(5) 0.0258(18) Uani 1 1 d . . . A 1
H6 H 0.483291 0.309139 0.481421 0.031 Uiso 1 1 calc R U . A 1
C7 C 0.5222(4) 0.1862(13) 0.5787(5) 0.035(2) Uani 1 1 d . . . A 1
H7 H 0.558716 0.193998 0.587606 0.042 Uiso 1 1 calc R U . A 1
C8 C 0.5153(4) 0.1039(12) 0.6319(5) 0.031(2) Uani 1 1 d . . . A 1
H8 H 0.547440 0.059286 0.675425 0.037 Uiso 1 1 calc R U . A 1
C9 C 0.4640(4) 0.0875(11) 0.6220(5) 0.0282(19) Uani 1 1 d . . . A 1
H9 H 0.460087 0.032923 0.657988 0.034 Uiso 1 1 calc R U . A 1
C10 C 0.3577(3) 0.3908(10) 0.3796(4) 0.0176(15) Uani 1 1 d . . . A 1
C11 C 0.3380(3) 0.5499(10) 0.3788(4) 0.0185(15) Uani 1 1 d . . . A 1
C12 C 0.3089(3) 0.7409(10) 0.4319(5) 0.0223(17) Uani 1 1 d . . . A 1
H12 H 0.302460 0.768941 0.469374 0.027 Uiso 1 1 calc R U . A 1
C13 C 0.2907(4) 0.8522(11) 0.3731(5) 0.0260(18) Uani 1 1 d . . . A 1
H13 H 0.272772 0.953326 0.371534 0.031 Uiso 1 1 calc R U . A 1
C14 C 0.2989(4) 0.8144(11) 0.3172(5) 0.0274(18) Uani 1 1 d . . . A 1
H14 H 0.288805 0.892026 0.278514 0.033 Uiso 1 1 calc R U . A 1
C15 C 0.3224(3) 0.6593(11) 0.3182(4) 0.0221(17) Uani 1 1 d . . . A 1
C16 C 0.3291(4) 0.6036(12) 0.2617(5) 0.0267(19) Uani 1 1 d . . . A 1
H16 H 0.320162 0.675588 0.221645 0.032 Uiso 1 1 calc R U . A 1
C17 C 0.3484(4) 0.4467(12) 0.2640(5) 0.029(2) Uani 1 1 d . . . A 1
H17 H 0.352602 0.410332 0.225397 0.035 Uiso 1 1 calc R U . A 1
C18 C 0.3621(3) 0.3388(12) 0.3226(4) 0.0238(17) Uani 1 1 d . . . A 1
H18 H 0.374599 0.228969 0.322841 0.029 Uiso 1 1 calc R U . A 1
C19 C 0.3088(3) 0.4773(10) 0.5452(4) 0.0173(15) Uani 1 1 d . . . A 1
C20 C 0.4103(3) 0.3719(10) 0.6488(5) 0.0207(16) Uani 1 1 d . . . A 1
C21 C 0.4048(4) 0.6824(10) 0.5971(5) 0.0254(18) Uani 1 1 d . . . A 1
H21A H 0.414556 0.674104 0.644880 0.030 Uiso 1 1 d R U . A 1
H21B H 0.372324 0.741493 0.568912 0.030 Uiso 1 1 d R U . A 1
C22 C 0.4432(3) 0.6280(11) 0.5795(5) 0.0245(17) Uani 1 1 d . . . A 1
H22 H 0.431517 0.616801 0.529122 0.029 Uiso 1 1 calc R U . A 1
C23 C 0.5027(4) 0.5877(13) 0.6408(6) 0.035(2) Uani 1 1 d . . . A 1
H23A H 0.525261 0.689773 0.656883 0.052 Uiso 1 1 calc R U . A 1
H23B H 0.518525 0.507896 0.622650 0.052 Uiso 1 1 calc R U . A 1
H23C H 0.503094 0.539096 0.682746 0.052 Uiso 1 1 calc R U . A 1
B1 B 0.1757(5) 0.5241(14) 0.3410(5) 0.028(2) Uani 1 1 d . . . B 1
F1 F 0.1966(5) 0.5568(8) 0.2981(5) 0.076(3) Uani 1 1 d . . . B 1
F2 F 0.1183(3) 0.5312(11) 0.3002(5) 0.080(3) Uani 1 1 d . . . B 1
F3 F 0.1945(3) 0.3712(7) 0.3731(3) 0.0353(12) Uani 1 1 d . . . B 1
F4 F 0.1943(2) 0.6443(7) 0.3954(3) 0.0380(13) Uani 1 1 d . . . B 1
N1 N 0.3347(3) 0.5986(8) 0.4382(4) 0.0176(13) Uani 1 1 d . . . A 1
O1 O 0.2711(3) 0.4896(8) 0.5498(3) 0.0248(12) Uani 1 1 d . . . A 1
O2 O 0.4274(3) 0.3424(8) 0.7087(3) 0.0294(14) Uani 1 1 d . . . A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C19 1.995(8) . ?
W1 C20 2.045(8) . ?
W1 C2 2.251(7) . ?
W1 N1 2.274(7) . ?
W1 C3 2.276(7) . ?
W1 C22 2.280(8) . ?
W1 C21 2.286(8) . ?
W1 C1 2.321(8) . ?
W1 C4 2.435(8) . ?
W1 C5 2.457(7) . ?
C1 C5 1.432(11) . ?
C1 C2 1.441(10) . ?
C1 C10 1.466(11) . ?
C2 C3 1.440(11) . ?
C2 H2 0.9500 . ?
C3 C4 1.413(12) . ?
C3 H3 0.9500 . ?
C4 C9 1.423(12) . ?
C4 C5 1.429(11) . ?
C5 C6 1.429(11) . ?
C6 C7 1.350(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.428(14) . ?
C7 H7 0.9500 . ?
C8 C9 1.360(14) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C18 1.367(11) . ?
C10 C11 1.392(11) . ?
C11 N1 1.393(10) . ?
C11 C15 1.428(11) . ?
C12 N1 1.323(10) . ?
C12 C13 1.398(12) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(13) . ?
C13 H13 0.9500 . ?
C14 C15 1.408(13) . ?
C14 H14 0.9500 . ?
C15 C16 1.407(12) . ?
C16 C17 1.364(13) . ?
C16 H16 0.9500 . ?
C17 C18 1.399(12) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 O1 1.133(10) . ?
C20 O2 1.126(10) . ?
C21 C22 1.409(12) . ?
C21 H21A 0.9106 . ?
C21 H21B 0.9106 . ?
C22 C23 1.501(12) . ?
C22 H22 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
B1 F2 1.365(13) . ?
B1 F3 1.367(12) . ?
B1 F1 1.372(13) . ?
B1 F4 1.380(12) . ?

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
C19 W1 C20 81.5(3) . . ?
C19 W1 C2 90.9(3) . . ?
C20 W1 C2 117.6(3) . . ?
C19 W1 N1 87.0(3) . . ?
C20 W1 N1 155.6(3) . . ?
C2 W1 N1 83.9(3) . . ?
C19 W1 C3 92.7(3) . . ?
C20 W1 C3 81.2(3) . . ?
C2 W1 C3 37.1(3) . . ?
N1 W1 C3 121.0(3) . . ?
C19 W1 C22 118.5(3) . . ?
C20 W1 C22 86.9(3) . . ?
C2 W1 C22 145.1(3) . . ?
N1 W1 C22 79.8(3) . . ?
C3 W1 C22 144.5(3) . . ?
C19 W1 C21 82.8(3) . . ?
C20 W1 C21 77.0(3) . . ?
C2 W1 C21 163.3(3) . . ?
N1 W1 C21 80.3(3) . . ?
C3 W1 C21 158.1(3) . . ?
C22 W1 C21 36.0(3) . . ?
C19 W1 C1 123.3(3) . . ?
C20 W1 C1 132.7(3) . . ?
C2 W1 C1 36.7(3) . . ?
N1 W1 C1 71.4(3) . . ?
C3 W1 C1 60.1(3) . . ?
C22 W1 C1 108.5(3) . . ?
C21 W1 C1 139.2(3) . . ?
C19 W1 C4 124.1(3) . . ?
C20 W1 C4 74.5(3) . . ?
C2 W1 C4 59.5(3) . . ?
N1 W1 C4 129.2(2) . . ?
C3 W1 C4 34.7(3) . . ?
C22 W1 C4 109.9(3) . . ?
C21 W1 C4 136.3(3) . . ?
C1 W1 C4 58.2(3) . . ?
C19 W1 C5 148.5(3) . . ?
C20 W1 C5 102.7(3) . . ?
C2 W1 C5 59.2(3) . . ?
N1 W1 C5 98.4(3) . . ?
C3 W1 C5 57.9(3) . . ?
C22 W1 C5 92.9(3) . . ?
C21 W1 C5 128.7(3) . . ?
C1 W1 C5 34.7(3) . . ?
C4 W1 C5 34.0(3) . . ?
C5 C1 C2 108.6(7) . . ?
C5 C1 C10 125.5(7) . . ?
C2 C1 C10 125.6(7) . . ?
C5 C1 W1 77.8(4) . . ?
C2 C1 W1 69.0(4) . . ?
C10 C1 W1 114.4(6) . . ?
C3 C2 C1 106.1(6) . . ?
C3 C2 W1 72.4(4) . . ?
C1 C2 W1 74.3(4) . . ?
C3 C2 H2 126.9 . . ?
C1 C2 H2 126.9 . . ?
W1 C2 H2 118.4 . . ?
C4 C3 C2 109.5(6) . . ?
C4 C3 W1 78.8(5) . . ?
C2 C3 W1 70.5(4) . . ?
C4 C3 H3 125.2 . . ?
C2 C3 H3 125.2 . . ?
W1 C3 H3 117.2 . . ?
C3 C4 C9 132.4(8) . . ?
C3 C4 C5 107.8(7) . . ?
C9 C4 C5 119.8(8) . . ?
C3 C4 W1 66.5(4) . . ?
C9 C4 W1 127.4(6) . . ?
C5 C4 W1 73.9(5) . . ?
C6 C5 C4 120.3(7) . . ?
C6 C5 C1 131.7(7) . . ?
C4 C5 C1 107.9(7) . . ?
C6 C5 W1 128.7(6) . . ?
C4 C5 W1 72.2(4) . . ?
C1 C5 W1 67.4(4) . . ?
C7 C6 C5 118.1(8) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?
C6 C7 C8 121.7(9) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C9 C8 C7 121.9(8) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C8 C9 C4 118.2(8) . . ?
C8 C9 H9 120.9 . . ?
C4 C9 H9 120.9 . . ?
C18 C10 C11 120.3(8) . . ?
C18 C10 C1 124.5(8) . . ?
C11 C10 C1 115.0(7) . . ?
C10 C11 N1 118.5(7) . . ?
C10 C11 C15 119.8(7) . . ?
N1 C11 C15 121.6(7) . . ?
N1 C12 C13 123.7(8) . . ?
N1 C12 H12 118.1 . . ?
C13 C12 H12 118.1 . . ?
C14 C13 C12 119.6(8) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 119.1(8) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C16 C15 C14 123.9(8) . . ?
C16 C15 C11 118.3(8) . . ?
C14 C15 C11 117.8(8) . . ?
C17 C16 C15 120.4(8) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 120.8(8) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C10 C18 C17 120.3(8) . . ?
C10 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
O1 C19 W1 173.8(7) . . ?
O2 C20 W1 176.8(7) . . ?
C22 C21 W1 71.8(5) . . ?
C22 C21 H21A 118.8 . . ?
W1 C21 H21A 110.0 . . ?
C22 C21 H21B 129.4 . . ?
W1 C21 H21B 99.5 . . ?
H21A C21 H21B 111.1 . . ?
C21 C22 C23 119.8(8) . . ?
C21 C22 W1 72.3(5) . . ?
C23 C22 W1 119.6(6) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
W1 C22 H22 79.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
F2 B1 F3 111.1(9) . . ?
F2 B1 F1 111.4(9) . . ?
F3 B1 F1 108.7(8) . . ?
F2 B1 F4 106.4(8) . . ?
F3 B1 F4 109.7(8) . . ?
F1 B1 F4 109.5(9) . . ?
C12 N1 C11 117.5(7) . . ?
C12 N1 W1 125.1(5) . . ?
C11 N1 W1 117.5(5) . . ?

_refine_diff_density_max         10.956
_refine_diff_density_min         -2.027
_refine_diff_density_rms         0.261

_vrf_PLAT971_mo_jv171009w1_vinklarek 
;
PROBLEM: ALERT_2_A Check Calcd Resid.Dens. 1.25A From C21  10.23 eA-3
RESPONSE: This residual peaks is in close vicinity of W atom (1.21A) and
 has no chemical meaning. It could be caused by the real structure of
 the crysal, either by second twinning or disorder of the whole complex,   
 from which only second position of W atom could be recognized. 
;
_vrf_PLAT094_mo_jv171009w1_vinklarek 
;
PROBLEM:ALERT_2_B Ratio of Maximum / Minimum Residual Density  5.41 Report
RESPONSE: see above
;
_vrf_PLAT097_mo_jv171009w1_vinklarek 
;
PROBLEM: ALERT_2_B Large Reported Max.(Positive) Residual Density  10.96 eA-3
RESPONSE: see above
;
####################################################################### 
# 
# 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_jv190116w1_vinklarek
_database_code_depnum_ccdc_archive 'CCDC 1914240'
loop_
_audit_author_name
_audit_author_address
'Ivana Cisarova'
;Charles Univerzity
Czech Republic
;
_audit_update_record             
;
2019-05-06 deposited with the CCDC.	2019-07-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H17 N O2 W'
_chemical_formula_sum            'C23 H17 N O2 W'
_chemical_formula_weight         523.22
_chemical_compound_source        'synthesized by the authors'

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           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   9.9642(5)
_cell_length_b                   7.6797(4)
_cell_length_c                   12.0078(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.6570(10)
_cell_angle_gamma                90
_cell_volume                     917.87(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9797
_cell_measurement_theta_min      3.7138
_cell_measurement_theta_max      27.5140

_exptl_crystal_description       prism
_exptl_crystal_colour            green-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_F_000             504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.066
_exptl_absorpt_coefficient_mu    6.310
_shelx_estimated_absorpt_T_min   0.299
_shelx_estimated_absorpt_T_max   0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'NoniusKappa+Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16531
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.598
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_full        25.242
_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 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4131
_reflns_number_gt                4044
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_max     0.964
_reflns_Friedel_fraction_full    0.991

_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       'Bruker Instrument Service vV6.2.10'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0269P)²+0.7148P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1809 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         4131
_refine_ls_number_parameters     248
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0173
_refine_ls_wR_factor_ref         0.0435
_refine_ls_wR_factor_gt          0.0430
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.085
_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 0.83593(2) 0.61154(5) 0.70844(2) 0.01642(6) Uani 1 1 d . . . . .
C1 C 0.6036(5) 0.5629(7) 0.7138(4) 0.0200(11) Uani 1 1 d . . . . .
C2 C 0.6309(5) 0.7439(8) 0.7291(5) 0.0236(11) Uani 1 1 d . . . . .
H2 H 0.614810 0.808863 0.794505 0.028 Uiso 1 1 calc R U . . .
C3 C 0.6863(5) 0.8121(8) 0.6302(5) 0.0300(12) Uani 1 1 d . . . . .
H3 H 0.718113 0.927326 0.619858 0.036 Uiso 1 1 calc R U . . .
C4 C 0.6849(5) 0.6751(8) 0.5500(5) 0.0307(12) Uani 1 1 d . . . . .
C5 C 0.7240(6) 0.6694(10) 0.4361(6) 0.046(2) Uani 1 1 d . . . . .
H5 H 0.759346 0.769924 0.401929 0.056 Uiso 1 1 calc R U . . .
C6 C 0.7095(6) 0.5182(12) 0.3783(5) 0.053(2) Uani 1 1 d . . . . .
H6 H 0.735322 0.514204 0.303190 0.064 Uiso 1 1 calc R U . . .
C7 C 0.6567(6) 0.3655(11) 0.4273(5) 0.0464(18) Uani 1 1 d . . . . .
H7 H 0.646270 0.262610 0.383848 0.056 Uiso 1 1 calc R U . . .
C8 C 0.6207(5) 0.3645(9) 0.5362(5) 0.0325(12) Uani 1 1 d . . . . .
H8 H 0.587057 0.261517 0.568684 0.039 Uiso 1 1 calc R U . . .
C9 C 0.6348(5) 0.5205(7) 0.5995(4) 0.0240(10) Uani 1 1 d . . . . .
C10 C 0.5344(5) 0.4438(6) 0.7892(4) 0.0188(9) Uani 1 1 d . . . . .
C11 C 0.4169(5) 0.5020(7) 0.8440(4) 0.0170(10) Uani 1 1 d . . . . .
C12 C 0.2721(5) 0.7240(7) 0.8870(4) 0.0242(10) Uani 1 1 d . . . . .
H12 H 0.246333 0.842741 0.880147 0.029 Uiso 1 1 calc R U . . .
C13 C 0.1952(4) 0.6156(14) 0.9541(3) 0.0261(8) Uani 1 1 d . . . . .
H13 H 0.120595 0.660494 0.991363 0.031 Uiso 1 1 calc R U . . .
C14 C 0.2307(5) 0.4437(7) 0.9641(4) 0.0242(10) Uani 1 1 d . . . . .
H14 H 0.178957 0.366691 1.006748 0.029 Uiso 1 1 calc R U . . .
C15 C 0.3452(5) 0.3814(6) 0.9105(4) 0.0203(9) Uani 1 1 d . . . . .
C16 C 0.3911(5) 0.2080(7) 0.9219(4) 0.0259(10) Uani 1 1 d . . . . .
H16 H 0.343409 0.127573 0.965307 0.031 Uiso 1 1 calc R U . . .
C17 C 0.5038(5) 0.1555(6) 0.8707(4) 0.0265(12) Uani 1 1 d . . . . .
H17 H 0.534811 0.039094 0.879430 0.032 Uiso 1 1 calc R U . . .
C18 C 0.5746(5) 0.2740(7) 0.8045(4) 0.0239(10) Uani 1 1 d . . . . .
H18 H 0.652615 0.234619 0.769485 0.029 Uiso 1 1 calc R U . . .
C19 C 1.0272(6) 0.6002(18) 0.6056(5) 0.0495(18) Uani 1 1 d . . . . .
H19A H 1.064155 0.645752 0.673669 0.059 Uiso 0.599(10) 1 d R U P A 1
H19B H 1.036690 0.664225 0.538003 0.059 Uiso 0.599(10) 1 d R U P A 1
H19C H 0.949014 0.627180 0.560638 0.059 Uiso 0.401(10) 1 d R U P A 2
H19D H 1.104765 0.671718 0.602658 0.059 Uiso 0.401(10) 1 d R U P A 2
C20A C 0.9634(8) 0.4537(12) 0.6040(7) 0.0284(15) Uani 0.599(10) 1 d . . P A 1
H20A H 0.928676 0.416988 0.532759 0.034 Uiso 0.599(10) 1 d R U P A 1
C20B C 1.0281(13) 0.4558(19) 0.6749(11) 0.0284(15) Uani 0.401(10) 1 d . . P A 2
H20B H 1.110373 0.438948 0.716664 0.034 Uiso 0.401(10) 1 d R U P A 2
C21 C 0.9380(7) 0.3419(8) 0.6932(6) 0.0401(15) Uani 1 1 d . . . . .
H21A H 0.969225 0.370234 0.766113 0.048 Uiso 0.599(10) 1 d R U P A 1
H21B H 0.888294 0.236962 0.679262 0.048 Uiso 0.599(10) 1 d R U P A 1
H21C H 0.852466 0.348430 0.655038 0.048 Uiso 0.401(10) 1 d R U P A 2
H21D H 0.956808 0.250701 0.745019 0.048 Uiso 0.401(10) 1 d R U P A 2
C22 C 0.8645(5) 0.5374(6) 0.8624(4) 0.0206(9) Uani 1 1 d . . . . .
C23 C 0.9437(5) 0.8073(6) 0.7650(4) 0.0238(10) Uani 1 1 d . . . . .
N1 N 0.3779(5) 0.6718(6) 0.8328(4) 0.0210(10) Uani 1 1 d . . . . .
O1 O 0.8776(4) 0.4949(5) 0.9545(3) 0.0299(8) Uani 1 1 d . . . . .
O2 O 1.0039(4) 0.9285(5) 0.7987(4) 0.0339(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C22 1.943(5) . ?
W1 C23 1.951(5) . ?
W1 C20A 2.192(8) . ?
W1 C2 2.306(5) . ?
W1 C20B 2.309(12) . ?
W1 C3 2.313(5) . ?
W1 C21 2.318(6) . ?
W1 C19 2.320(5) . ?
W1 C1 2.349(5) . ?
W1 C4 2.420(5) . ?
W1 C9 2.444(5) . ?
W1 H19C 2.1493 . ?
W1 H21C 2.1286 . ?
C1 C2 1.427(9) . ?
C1 C9 1.457(7) . ?
C1 C10 1.481(7) . ?
C2 C3 1.432(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.425(9) . ?
C3 H3 0.9500 . ?
C4 C9 1.429(8) . ?
C4 C5 1.440(8) . ?
C5 C6 1.356(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.424(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.372(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.422(8) . ?
C8 H8 0.9500 . ?
C10 C18 1.374(7) . ?
C10 C11 1.440(6) . ?
C11 N1 1.366(7) . ?
C11 C15 1.434(7) . ?
C12 N1 1.326(7) . ?
C12 C13 1.409(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.370(12) . ?
C13 H13 0.9500 . ?
C14 C15 1.419(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.413(7) . ?
C16 C17 1.366(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.418(7) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20A 1.292(16) . ?
C19 C20B 1.386(19) . ?
C19 H19A 0.9474 . ?
C19 H19B 0.9575 . ?
C19 H19C 0.9500 . ?
C19 H19D 0.9500 . ?
C20A C21 1.405(12) . ?
C20A H20A 0.9500 . ?
C20B C21 1.279(16) . ?
C20B H20B 0.9500 . ?
C21 H21A 0.9415 . ?
C21 H21B 0.9565 . ?
C21 H21C 0.9500 . ?
C21 H21D 0.9500 . ?
C22 O1 1.155(6) . ?
C23 O2 1.170(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22 W1 C23 80.8(2) . . ?
C22 W1 C20A 108.6(3) . . ?
C23 W1 C20A 107.5(3) . . ?
C22 W1 C2 96.80(19) . . ?
C23 W1 C2 95.7(2) . . ?
C20A W1 C2 147.7(3) . . ?
C22 W1 C20B 85.9(4) . . ?
C23 W1 C20B 90.7(4) . . ?
C2 W1 C20B 173.4(4) . . ?
C22 W1 C3 130.2(2) . . ?
C23 W1 C3 87.9(2) . . ?
C20A W1 C3 121.0(3) . . ?
C2 W1 C3 36.13(19) . . ?
C20B W1 C3 143.0(4) . . ?
C22 W1 C21 76.6(2) . . ?
C23 W1 C21 118.6(2) . . ?
C20A W1 C21 36.2(3) . . ?
C2 W1 C21 142.8(2) . . ?
C20B W1 C21 32.1(4) . . ?
C3 W1 C21 147.1(2) . . ?
C22 W1 C19 114.1(2) . . ?
C23 W1 C19 76.2(4) . . ?
C20A W1 C19 33.1(4) . . ?
C2 W1 C19 145.9(3) . . ?
C20B W1 C19 34.9(5) . . ?
C3 W1 C19 109.8(3) . . ?
C21 W1 C19 63.3(4) . . ?
C22 W1 C1 91.65(19) . . ?
C23 W1 C1 129.8(2) . . ?
C20A W1 C1 121.7(3) . . ?
C2 W1 C1 35.7(2) . . ?
C20B W1 C1 138.5(4) . . ?
C3 W1 C1 59.95(19) . . ?
C21 W1 C1 107.3(2) . . ?
C19 W1 C1 147.5(3) . . ?
C22 W1 C4 149.94(19) . . ?
C23 W1 C4 115.5(2) . . ?
C20A W1 C4 91.0(3) . . ?
C2 W1 C4 58.2(2) . . ?
C20B W1 C4 117.3(4) . . ?
C3 W1 C4 35.0(2) . . ?
C21 W1 C4 112.2(2) . . ?
C19 W1 C4 94.9(2) . . ?
C1 W1 C4 58.37(18) . . ?
C22 W1 C9 120.38(19) . . ?
C23 W1 C9 146.2(2) . . ?
C20A W1 C9 91.0(3) . . ?
C2 W1 C9 58.3(2) . . ?
C20B W1 C9 115.1(4) . . ?
C3 W1 C9 58.4(2) . . ?
C21 W1 C9 93.1(2) . . ?
C19 W1 C9 112.2(3) . . ?
C1 W1 C9 35.33(16) . . ?
C4 W1 C9 34.16(18) . . ?
C22 W1 H19C 138.0 . . ?
C23 W1 H19C 86.7 . . ?
C2 W1 H19C 124.4 . . ?
C20B W1 H19C 54.1 . . ?
C3 W1 H19C 88.9 . . ?
C21 W1 H19C 74.7 . . ?
C19 W1 H19C 24.2 . . ?
C1 W1 H19C 125.9 . . ?
C4 W1 H19C 70.8 . . ?
C9 W1 H19C 91.3 . . ?
C22 W1 H21C 89.9 . . ?
C23 W1 H21C 141.9 . . ?
C2 W1 H21C 122.2 . . ?
C20B W1 H21C 51.6 . . ?
C3 W1 H21C 124.6 . . ?
C21 W1 H21C 24.2 . . ?
C19 W1 H21C 74.2 . . ?
C1 W1 H21C 87.0 . . ?
C4 W1 H21C 90.5 . . ?
C9 W1 H21C 68.9 . . ?
H19C W1 H21C 75.7 . . ?
C2 C1 C9 107.0(5) . . ?
C2 C1 C10 127.9(5) . . ?
C9 C1 C10 124.3(5) . . ?
C2 C1 W1 70.5(3) . . ?
C9 C1 W1 75.9(3) . . ?
C10 C1 W1 127.0(3) . . ?
C1 C2 C3 109.1(5) . . ?
C1 C2 W1 73.8(3) . . ?
C3 C2 W1 72.2(3) . . ?
C1 C2 H2 125.4 . . ?
C3 C2 H2 125.4 . . ?
W1 C2 H2 120.3 . . ?
C4 C3 C2 107.3(5) . . ?
C4 C3 W1 76.6(3) . . ?
C2 C3 W1 71.7(3) . . ?
C4 C3 H3 126.3 . . ?
C2 C3 H3 126.3 . . ?
W1 C3 H3 117.4 . . ?
C3 C4 C9 109.0(4) . . ?
C3 C4 C5 132.0(6) . . ?
C9 C4 C5 119.0(6) . . ?
C3 C4 W1 68.4(3) . . ?
C9 C4 W1 73.8(3) . . ?
C5 C4 W1 123.7(4) . . ?
C6 C5 C4 119.0(6) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C7 121.7(5) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C8 C7 C6 121.1(7) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C7 C8 C9 118.8(6) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 H8 120.6 . . ?
C8 C9 C4 120.4(5) . . ?
C8 C9 C1 132.2(5) . . ?
C4 C9 C1 107.4(5) . . ?
C8 C9 W1 125.8(4) . . ?
C4 C9 W1 72.0(3) . . ?
C1 C9 W1 68.8(3) . . ?
C18 C10 C11 118.1(4) . . ?
C18 C10 C1 121.8(4) . . ?
C11 C10 C1 120.0(4) . . ?
N1 C11 C15 121.6(5) . . ?
N1 C11 C10 119.0(5) . . ?
C15 C11 C10 119.4(5) . . ?
N1 C12 C13 124.6(6) . . ?
N1 C12 H12 117.7 . . ?
C13 C12 H12 117.7 . . ?
C14 C13 C12 118.3(5) . . ?
C14 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C13 C14 C15 119.7(4) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C16 C15 C14 122.5(5) . . ?
C16 C15 C11 119.7(5) . . ?
C14 C15 C11 117.8(5) . . ?
C17 C16 C15 120.3(5) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 120.2(4) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C10 C18 C17 122.3(5) . . ?
C10 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?
C20A C19 W1 68.0(4) . . ?
C20B C19 W1 72.1(5) . . ?
C20A C19 H19A 120.4 . . ?
W1 C19 H19A 79.8 . . ?
C20A C19 H19B 120.1 . . ?
W1 C19 H19B 123.2 . . ?
H19A C19 H19B 119.5 . . ?
C20B C19 H19C 119.8 . . ?
W1 C19 H19C 67.8 . . ?
C20B C19 H19D 120.2 . . ?
W1 C19 H19D 133.5 . . ?
H19C C19 H19D 120.0 . . ?
C19 C20A C21 128.8(8) . . ?
C19 C20A W1 78.9(5) . . ?
C21 C20A W1 76.8(4) . . ?
C19 C20A H20A 115.5 . . ?
C21 C20A H20A 115.7 . . ?
W1 C20A H20A 118.9 . . ?
C21 C20B C19 131.7(12) . . ?
C21 C20B W1 74.4(6) . . ?
C19 C20B W1 73.0(6) . . ?
C21 C20B H20B 114.3 . . ?
C19 C20B H20B 114.0 . . ?
W1 C20B H20B 132.9 . . ?
C20B C21 W1 73.5(6) . . ?
C20A C21 W1 67.0(4) . . ?
C20A C21 H21A 120.3 . . ?
W1 C21 H21A 81.2 . . ?
C20A C21 H21B 119.5 . . ?
W1 C21 H21B 122.7 . . ?
H21A C21 H21B 120.2 . . ?
C20B C21 H21C 120.1 . . ?
W1 C21 H21C 66.6 . . ?
C20B C21 H21D 119.9 . . ?
W1 C21 H21D 132.9 . . ?
H21C C21 H21D 120.0 . . ?
O1 C22 W1 177.9(4) . . ?
O2 C23 W1 177.4(5) . . ?
C12 N1 C11 118.0(5) . . ?

_refine_diff_density_max         1.029
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.088

####################################################################### 
# 
# 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_jv190319mo1_vinklarek
_database_code_depnum_ccdc_archive 'CCDC 1914242'
loop_
_audit_author_name
_audit_author_address
'Ivana Cisarova'
;Charles Univerzity
Czech Republic
;
_audit_update_record             
;
2019-05-06 deposited with the CCDC.	2019-07-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C22 H18 Mo N O2 S),2(B F4),C H2 Cl2'
_chemical_formula_sum            'C45 H38 B2 Cl2 F8 Mo2 N2 O4 S2'
_chemical_formula_weight         1171.29
_chemical_compound_source        'synthesized by the authors'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 '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                   14.5014(7)
_cell_length_b                   11.0265(6)
_cell_length_c                   14.7195(7)
_cell_angle_alpha                90
_cell_angle_beta                 106.503(2)
_cell_angle_gamma                90
_cell_volume                     2256.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9875
_cell_measurement_theta_min      2.3574
_cell_measurement_theta_max      27.5376

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_F_000             1172
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.847
_shelx_estimated_absorpt_T_min   0.764
_shelx_estimated_absorpt_T_max   0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS  micro-focus sealed tube'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29921
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.344
_diffrn_reflns_theta_max         27.538
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5192
_reflns_number_gt                4529
_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       'Bruker Instrument Service vV6.2.10'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0284P)²+2.8869P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5192
_refine_ls_number_parameters     318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0674
_refine_ls_wR_factor_gt          0.0637
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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 0.79407(2) 0.24778(2) 0.33452(2) 0.01357(6) Uani 1 1 d . . . . .
N1 N 0.64363(11) 0.19438(16) 0.33258(11) 0.0185(3) Uani 1 1 d . . . . .
C1 C 0.79766(13) 0.04483(17) 0.37808(13) 0.0158(4) Uani 1 1 d . . . . .
C2 C 0.82333(14) 0.05545(18) 0.29141(14) 0.0178(4) Uani 1 1 d . . . . .
H2 H 0.788538 0.022811 0.231798 0.021 Uiso 1 1 calc R U . . .
C3 C 0.90966(13) 0.12315(18) 0.31014(14) 0.0168(4) Uani 1 1 d . . . . .
H3 H 0.940439 0.148908 0.264459 0.020 Uiso 1 1 calc R U . . .
C4 C 0.94299(13) 0.14637(17) 0.41141(13) 0.0155(4) Uani 1 1 d . . . . .
C5 C 0.87335(13) 0.09652(17) 0.45297(13) 0.0144(4) Uani 1 1 d . . . . .
C6 C 0.88852(13) 0.09827(18) 0.55253(13) 0.0170(4) Uani 1 1 d . . . . .
H6 H 0.842154 0.065780 0.580231 0.020 Uiso 1 1 calc R U . . .
C7 C 0.97193(14) 0.14820(19) 0.60707(14) 0.0195(4) Uani 1 1 d . . . . .
H7 H 0.984337 0.148625 0.674010 0.023 Uiso 1 1 calc R U . . .
C8 C 1.04098(13) 0.19980(19) 0.56612(14) 0.0197(4) Uani 1 1 d . . . . .
H8 H 1.097933 0.234289 0.606629 0.024 Uiso 1 1 calc R U . . .
C9 C 1.02787(13) 0.20120(19) 0.47068(14) 0.0181(4) Uani 1 1 d . . . . .
H9 H 1.073908 0.237635 0.444465 0.022 Uiso 1 1 calc R U . . .
C10 C 0.70590(13) -0.00062(19) 0.38936(13) 0.0171(4) Uani 1 1 d . . . . .
C11 C 0.62730(13) 0.08047(19) 0.36336(13) 0.0179(4) Uani 1 1 d . . . . .
C12 C 0.56920(15) 0.2695(2) 0.30573(16) 0.0263(5) Uani 1 1 d . . . . .
H12 H 0.579399 0.347620 0.283071 0.032 Uiso 1 1 calc R U . . .
C13 C 0.47589(15) 0.2391(2) 0.30920(17) 0.0302(5) Uani 1 1 d . . . . .
H13 H 0.424756 0.295587 0.288269 0.036 Uiso 1 1 calc R U . . .
C14 C 0.45925(15) 0.1286(2) 0.34264(15) 0.0280(5) Uani 1 1 d . . . . .
H14 H 0.396932 0.108121 0.346764 0.034 Uiso 1 1 calc R U . . .
C15 C 0.53583(14) 0.0446(2) 0.37120(14) 0.0223(4) Uani 1 1 d . . . . .
C16 C 0.52728(15) -0.0715(2) 0.40845(15) 0.0257(5) Uani 1 1 d . . . . .
H16 H 0.466739 -0.097331 0.414317 0.031 Uiso 1 1 calc R U . . .
C17 C 0.60439(16) -0.1469(2) 0.43604(15) 0.0262(5) Uani 1 1 d . . . . .
H17 H 0.597412 -0.224009 0.462131 0.031 Uiso 1 1 calc R U . . .
C18 C 0.69486(15) -0.11171(19) 0.42628(14) 0.0211(4) Uani 1 1 d . . . . .
H18 H 0.748131 -0.165365 0.445430 0.025 Uiso 1 1 calc R U . . .
C19 C 0.8548(2) 0.4349(3) 0.53816(17) 0.0410(7) Uani 1 1 d . . . . .
H19A H 0.910491 0.457305 0.516579 0.061 Uiso 1 1 calc R U . . .
H19B H 0.869361 0.360787 0.576366 0.061 Uiso 1 1 calc R U . . .
H19C H 0.840150 0.500724 0.576566 0.061 Uiso 1 1 calc R U . . .
C20 C 0.7416(2) 0.5576(2) 0.38558(17) 0.0355(6) Uani 1 1 d . . . . .
H20A H 0.726212 0.616082 0.429274 0.053 Uiso 1 1 calc R U . . .
H20B H 0.690016 0.557452 0.325750 0.053 Uiso 1 1 calc R U . . .
H20C H 0.802336 0.580448 0.373524 0.053 Uiso 1 1 calc R U . . .
C21 C 0.73387(14) 0.2938(2) 0.20410(15) 0.0208(4) Uani 1 1 d . . . . .
C22 C 0.88803(14) 0.38053(19) 0.32437(14) 0.0204(4) Uani 1 1 d . . . . .
S1 S 0.75282(4) 0.40872(5) 0.43728(4) 0.02170(11) Uani 1 1 d . . . . .
O1 O 0.70133(11) 0.31199(17) 0.12382(10) 0.0303(4) Uani 1 1 d . . . . .
O2 O 0.93795(11) 0.45720(15) 0.31752(12) 0.0303(4) Uani 1 1 d . . . . .
B1 B 0.78976(18) 0.7433(2) 0.17590(17) 0.0249(5) Uani 1 1 d . . . . .
F1 F 0.77023(11) 0.62224(13) 0.15407(10) 0.0377(3) Uani 1 1 d . . . . .
F2 F 0.88762(11) 0.7636(2) 0.20322(13) 0.0717(7) Uani 1 1 d . . . . .
F3 F 0.74777(15) 0.81371(16) 0.09754(11) 0.0601(5) Uani 1 1 d . . . . .
F4 F 0.75283(9) 0.77578(12) 0.24956(9) 0.0279(3) Uani 1 1 d . . . . .
C1S C 0.4441(6) -0.5006(10) 0.4701(7) 0.090(3) Uani 0.5 1 d . . P . .
H1S1 H 0.399748 -0.568906 0.445573 0.109 Uiso 0.5 1 d R U P . .
H1S2 H 0.406960 -0.436418 0.491000 0.109 Uiso 0.5 1 d R U P . .
Cl1 Cl 0.48164(14) -0.44637(15) 0.38140(15) 0.0523(4) Uani 0.5 1 d . . P . .
Cl2 Cl 0.5342(2) -0.5525(3) 0.5705(2) 0.0886(8) Uani 0.5 1 d . . P . .


_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 C21 1.937(2) . ?
Mo1 C22 2.034(2) . ?
Mo1 N1 2.2520(16) . ?
Mo1 C3 2.2735(18) . ?
Mo1 C2 2.288(2) . ?
Mo1 C1 2.3245(19) . ?
Mo1 C4 2.4097(18) . ?
Mo1 C5 2.4505(18) . ?
Mo1 S1 2.5118(5) . ?
N1 C12 1.329(3) . ?
N1 C11 1.378(3) . ?
C1 C2 1.432(3) . ?
C1 C5 1.434(3) . ?
C1 C10 1.475(3) . ?
C2 C3 1.416(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.453(3) . ?
C3 H3 0.9500 . ?
C4 C9 1.425(3) . ?
C4 C5 1.431(3) . ?
C5 C6 1.419(3) . ?
C6 C7 1.363(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.426(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.363(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C18 1.368(3) . ?
C10 C11 1.413(3) . ?
C11 C15 1.420(3) . ?
C12 C13 1.409(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.361(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.415(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.412(3) . ?
C16 C17 1.360(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.414(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 S1 1.796(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 S1 1.797(2) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 O1 1.159(3) . ?
C22 O2 1.136(3) . ?
B1 F2 1.379(3) . ?
B1 F3 1.380(3) . ?
B1 F1 1.383(3) . ?
B1 F4 1.386(3) . ?
C1S Cl2 0.951(9) 3_646 ?
C1S C1S 1.610(18) 3_646 ?
C1S Cl1 1.662(9) . ?
C1S Cl2 1.766(10) . ?
C1S Cl1 2.223(11) 3_646 ?
C1S H1S1 0.9900 . ?
C1S H1S2 0.9900 . ?
Cl1 Cl2 0.805(3) 3_646 ?
Cl2 Cl2 2.336(5) 3_646 ?

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
C21 Mo1 C22 82.04(8) . . ?
C21 Mo1 N1 83.89(7) . . ?
C22 Mo1 N1 148.65(7) . . ?
C21 Mo1 C3 98.44(8) . . ?
C22 Mo1 C3 83.34(8) . . ?
N1 Mo1 C3 126.51(7) . . ?
C21 Mo1 C2 91.99(8) . . ?
C22 Mo1 C2 117.77(7) . . ?
N1 Mo1 C2 90.54(7) . . ?
C3 Mo1 C2 36.17(7) . . ?
C21 Mo1 C1 119.60(8) . . ?
C22 Mo1 C1 138.60(7) . . ?
N1 Mo1 C1 72.39(6) . . ?
C3 Mo1 C1 60.12(7) . . ?
C2 Mo1 C1 36.16(7) . . ?
C21 Mo1 C4 132.72(7) . . ?
C22 Mo1 C4 80.72(7) . . ?
N1 Mo1 C4 128.34(6) . . ?
C3 Mo1 C4 36.01(6) . . ?
C2 Mo1 C4 59.20(7) . . ?
C1 Mo1 C4 58.45(6) . . ?
C21 Mo1 C5 150.64(8) . . ?
C22 Mo1 C5 110.69(7) . . ?
N1 Mo1 C5 95.05(6) . . ?
C3 Mo1 C5 58.86(6) . . ?
C2 Mo1 C5 58.66(7) . . ?
C1 Mo1 C5 34.83(6) . . ?
C4 Mo1 C5 34.23(6) . . ?
C21 Mo1 S1 107.12(6) . . ?
C22 Mo1 S1 79.33(6) . . ?
N1 Mo1 S1 78.27(5) . . ?
C3 Mo1 S1 146.56(5) . . ?
C2 Mo1 S1 156.44(5) . . ?
C1 Mo1 S1 120.30(5) . . ?
C4 Mo1 S1 112.33(5) . . ?
C5 Mo1 S1 101.32(5) . . ?
C12 N1 C11 117.72(18) . . ?
C12 N1 Mo1 122.88(15) . . ?
C11 N1 Mo1 119.36(12) . . ?
C2 C1 C5 108.45(16) . . ?
C2 C1 C10 126.83(17) . . ?
C5 C1 C10 124.51(17) . . ?
C2 C1 Mo1 70.52(11) . . ?
C5 C1 Mo1 77.39(11) . . ?
C10 C1 Mo1 114.08(13) . . ?
C3 C2 C1 108.00(17) . . ?
C3 C2 Mo1 71.38(11) . . ?
C1 C2 Mo1 73.32(11) . . ?
C3 C2 H2 126.0 . . ?
C1 C2 H2 126.0 . . ?
Mo1 C2 H2 121.0 . . ?
C2 C3 C4 108.10(16) . . ?
C2 C3 Mo1 72.46(11) . . ?
C4 C3 Mo1 77.11(10) . . ?
C2 C3 H3 125.9 . . ?
C4 C3 H3 125.9 . . ?
Mo1 C3 H3 116.5 . . ?
C9 C4 C5 119.53(17) . . ?
C9 C4 C3 132.87(17) . . ?
C5 C4 C3 107.54(16) . . ?
C9 C4 Mo1 126.40(14) . . ?
C5 C4 Mo1 74.45(10) . . ?
C3 C4 Mo1 66.88(10) . . ?
C6 C5 C4 121.01(17) . . ?
C6 C5 C1 131.25(17) . . ?
C4 C5 C1 107.64(16) . . ?
C6 C5 Mo1 129.00(13) . . ?
C4 C5 Mo1 71.33(10) . . ?
C1 C5 Mo1 67.77(10) . . ?
C7 C6 C5 117.71(17) . . ?
C7 C6 H6 121.1 . . ?
C5 C6 H6 121.1 . . ?
C6 C7 C8 121.62(18) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C9 C8 C7 122.08(18) . . ?
C9 C8 H8 119.0 . . ?
C7 C8 H8 119.0 . . ?
C8 C9 C4 118.00(18) . . ?
C8 C9 H9 121.0 . . ?
C4 C9 H9 121.0 . . ?
C18 C10 C11 119.86(18) . . ?
C18 C10 C1 124.07(18) . . ?
C11 C10 C1 116.02(18) . . ?
N1 C11 C10 117.71(17) . . ?
N1 C11 C15 122.15(19) . . ?
C10 C11 C15 120.13(19) . . ?
N1 C12 C13 123.2(2) . . ?
N1 C12 H12 118.4 . . ?
C13 C12 H12 118.4 . . ?
C14 C13 C12 119.8(2) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C15 119.25(19) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C16 C15 C14 124.12(19) . . ?
C16 C15 C11 118.11(19) . . ?
C14 C15 C11 117.8(2) . . ?
C17 C16 C15 121.00(19) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 120.7(2) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C10 C18 C17 120.2(2) . . ?
C10 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
S1 C19 H19A 109.5 . . ?
S1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
S1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
S1 C20 H20A 109.5 . . ?
S1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
S1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1 C21 Mo1 173.92(19) . . ?
O2 C22 Mo1 177.69(19) . . ?
C19 S1 C20 99.09(13) . . ?
C19 S1 Mo1 109.28(8) . . ?
C20 S1 Mo1 113.50(8) . . ?
F2 B1 F3 109.0(2) . . ?
F2 B1 F1 110.5(2) . . ?
F3 B1 F1 109.64(19) . . ?
F2 B1 F4 108.92(18) . . ?
F3 B1 F4 109.4(2) . . ?
F1 B1 F4 109.39(19) . . ?
Cl2 C1S C1S 83.0(7) 3_646 3_646 ?
Cl2 C1S Cl1 17.3(4) 3_646 . ?
C1S C1S Cl1 85.6(6) 3_646 . ?
Cl2 C1S Cl2 115.3(7) 3_646 . ?
C1S C1S Cl2 32.3(5) 3_646 . ?
Cl1 C1S Cl2 116.4(5) . . ?
Cl2 C1S Cl1 128.7(8) 3_646 3_646 ?
C1S C1S Cl1 48.2(6) 3_646 3_646 ?
Cl1 C1S Cl1 133.8(5) . 3_646 ?
Cl2 C1S Cl1 19.24(18) . 3_646 ?
Cl2 C1S H1S1 122.4 3_646 . ?
C1S C1S H1S1 130.9 3_646 . ?
Cl1 C1S H1S1 108.1 . . ?
Cl2 C1S H1S1 107.9 . . ?
Cl1 C1S H1S1 104.0 3_646 . ?
Cl2 C1S H1S2 93.5 3_646 . ?
C1S C1S H1S2 112.1 3_646 . ?
Cl1 C1S H1S2 108.4 . . ?
Cl2 C1S H1S2 108.1 . . ?
Cl1 C1S H1S2 92.1 3_646 . ?
H1S1 C1S H1S2 107.6 . . ?
Cl2 Cl1 C1S 20.5(5) 3_646 . ?
Cl2 Cl1 C1S 46.3(3) 3_646 3_646 ?
C1S Cl1 C1S 46.2(5) . 3_646 ?
Cl1 Cl2 C1S 142.2(8) 3_646 3_646 ?
Cl1 Cl2 C1S 114.4(5) 3_646 . ?
C1S Cl2 C1S 64.7(7) 3_646 . ?
Cl1 Cl2 Cl2 129.4(4) 3_646 3_646 ?
C1S Cl2 Cl2 43.1(6) 3_646 3_646 ?
C1S Cl2 Cl2 21.6(3) . 3_646 ?

_refine_diff_density_max         0.799
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.070

####################################################################### 
# 
# 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_jv160425w3_vinklarek_sq
_database_code_depnum_ccdc_archive 'CCDC 1914243'
loop_
_audit_author_name
_audit_author_address
'Ivana Cisarova'
;Charles Univerzity
Czech Republic
;
_audit_update_record             
;
2019-05-06 deposited with the CCDC.	2019-07-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H18 N3 O2 W, B F4'
_chemical_formula_sum            'C24 H18 B F4 N3 O2 W'
_chemical_formula_weight         651.07
_chemical_compound_source        'synthesized by the authors'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   12.2756(5)
_cell_length_b                   27.6227(11)
_cell_length_c                   15.3654(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.2560(10)
_cell_angle_gamma                90
_cell_volume                     5210.1(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9046
_cell_measurement_theta_min      2.2197
_cell_measurement_theta_max      27.5156


_exptl_crystal_description       prism
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_F_000             2512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.178
_exptl_absorpt_coefficient_mu    4.487
_shelx_estimated_absorpt_T_min   0.290
_shelx_estimated_absorpt_T_max   0.502
_exptl_absorpt_correction_type   'Numerical Mu From Formula'
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_T_max  0.50
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'NoniusKappa+Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42097
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         0.737
_diffrn_reflns_theta_max         27.546
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             23451
_reflns_number_gt                21424
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_max     0.957
_reflns_Friedel_fraction_full    0.986

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker Instrument Service v2016.1.0.1'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0552P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration unk
_refine_ls_number_reflns         23451
_refine_ls_number_parameters     1269
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0943
_refine_ls_wR_factor_gt          0.0920
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.031
_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 0.46663(3) 0.245952 0.41022(2) 0.02413(9) Uani 1 1 d . . . . .
W2 W -0.02379(4) 0.47579(2) 0.85331(3) 0.02741(10) Uani 1 1 d . . . . .
W3 W 0.39406(3) 0.46546(2) 0.34685(2) 0.01999(9) Uani 1 1 d . . . . .
W4 W 1.09761(3) 0.74959(2) 0.09136(2) 0.02493(9) Uani 1 1 d . . . . .
C1A C 0.6393(9) 0.2168(4) 0.4534(7) 0.032(2) Uani 1 1 d . . . . .
C1B C 0.1478(9) 0.5075(4) 0.8190(7) 0.032(2) Uani 1 1 d . . . . .
C1C C 0.2275(8) 0.4998(3) 0.3056(6) 0.022(2) Uani 1 1 d . . . . .
C1D C 1.2692(9) 0.7173(3) 0.0524(7) 0.026(2) Uani 1 1 d . . . . .
C2A C 0.5456(9) 0.1898(4) 0.4856(7) 0.029(2) Uani 1 1 d . . . . .
H2A H 0.517989 0.159756 0.465030 0.035 Uiso 1 1 calc R U . . .
C2B C 0.0582(9) 0.5325(4) 0.7798(7) 0.034(3) Uani 1 1 d . . . . .
H2B H 0.028561 0.562594 0.798020 0.041 Uiso 1 1 calc R U . . .
C2C C 0.3229(8) 0.5229(3) 0.2690(6) 0.023(2) Uani 1 1 d . . . . .
H2C H 0.356969 0.552123 0.287003 0.027 Uiso 1 1 calc R U . . .
C2D C 1.1731(8) 0.6925(3) 0.0146(7) 0.024(2) Uani 1 1 d . . . . .
H2D H 1.142483 0.662398 0.031830 0.029 Uiso 1 1 calc R U . . .
C3A C 0.5057(12) 0.2184(4) 0.5540(7) 0.042(3) Uani 1 1 d . . . . .
H3A H 0.433152 0.218053 0.575236 0.051 Uiso 1 1 calc R U . . .
C3B C 0.0220(10) 0.5042(4) 0.7093(7) 0.037(3) Uani 1 1 d . . . . .
H3B H -0.048884 0.504241 0.684261 0.044 Uiso 1 1 calc R U . . .
C3C C 0.3540(10) 0.4916(4) 0.1997(6) 0.030(2) Uani 1 1 d . . . . .
H3C H 0.424770 0.489090 0.175393 0.036 Uiso 1 1 calc R U . . .
C3D C 1.1361(9) 0.7241(4) -0.0542(7) 0.031(2) Uani 1 1 d . . . . .
H3D H 1.064281 0.726389 -0.077157 0.037 Uiso 1 1 calc R U . . .
C4A C 0.5915(14) 0.2480(4) 0.5863(8) 0.055(4) Uani 1 1 d . . . . .
C4B C 0.1161(10) 0.4744(4) 0.6817(7) 0.038(3) Uani 1 1 d . . . . .
C4C C 0.2570(9) 0.4637(4) 0.1720(6) 0.028(2) Uani 1 1 d . . . . .
C4D C 1.2316(10) 0.7518(4) -0.0814(6) 0.034(2) Uani 1 1 d . . . . .
C5A C 0.6770(11) 0.2470(4) 0.5254(8) 0.047(3) Uani 1 1 d . . . . .
C5B C 0.1948(9) 0.4762(4) 0.7462(7) 0.036(3) Uani 1 1 d . . . . .
C5C C 0.1781(8) 0.4695(3) 0.2363(6) 0.025(2) Uani 1 1 d . . . . .
C5D C 1.3122(9) 0.7478(4) -0.0191(7) 0.033(2) Uani 1 1 d . . . . .
C6A C 0.7687(13) 0.2735(5) 0.5412(12) 0.064(5) Uani 1 1 d . . . . .
H6A H 0.822710 0.271849 0.497242 0.077 Uiso 1 1 calc R U . . .
C6B C 0.2922(11) 0.4519(5) 0.7401(9) 0.050(3) Uani 1 1 d . . . . .
H6B H 0.346133 0.453556 0.784577 0.060 Uiso 1 1 calc R U . . .
C6C C 0.0782(9) 0.4471(4) 0.2300(7) 0.029(2) Uani 1 1 d . . . . .
H6C H 0.024544 0.450889 0.273837 0.034 Uiso 1 1 calc R U . . .
C6D C 1.4113(10) 0.7728(4) -0.0260(8) 0.039(3) Uani 1 1 d . . . . .
H6D H 1.464440 0.771682 0.019039 0.046 Uiso 1 1 calc R U . . .
C7A C 0.7935(16) 0.3012(7) 0.6092(12) 0.078(5) Uani 1 1 d . U . . .
H7A H 0.858293 0.319897 0.614111 0.093 Uiso 1 1 calc R U . . .
C7B C 0.3072(13) 0.4241(5) 0.6635(11) 0.061(5) Uani 1 1 d . . . . .
H7B H 0.372953 0.406401 0.656509 0.073 Uiso 1 1 calc R U . . .
C17C C 0.0234(10) 0.5569(4) 0.4593(8) 0.041(3) Uani 1 1 d . . . . .
H17C H -0.052046 0.564431 0.461232 0.049 Uiso 1 1 calc R U . . .
C7D C 1.4287(12) 0.7999(4) -0.1041(9) 0.050(4) Uani 1 1 d . . . . .
H7D H 1.495976 0.816175 -0.112581 0.060 Uiso 1 1 calc R U . . .
C8A C 0.7165(14) 0.2996(6) 0.6692(11) 0.063(4) Uani 1 1 d . U . . .
H8A H 0.731207 0.316089 0.722233 0.075 Uiso 1 1 calc R U . . .
C8B C 0.2310(15) 0.4221(5) 0.6002(9) 0.061(5) Uani 1 1 d . . . . .
H8B H 0.246009 0.403838 0.549287 0.074 Uiso 1 1 calc R U . . .
C8C C 0.1353(12) 0.4141(4) 0.0948(8) 0.042(3) Uani 1 1 d . . . . .
H8C H 0.119321 0.395185 0.044718 0.051 Uiso 1 1 calc R U . . .
C8D C 1.3508(14) 0.8025(4) -0.1655(8) 0.051(4) Uani 1 1 d . . . . .
H8D H 1.365426 0.820456 -0.216945 0.061 Uiso 1 1 calc R U . . .
C9A C 0.6148(14) 0.2758(6) 0.6628(11) 0.064(4) Uani 1 1 d . U . . .
H9A H 0.562893 0.278297 0.708236 0.077 Uiso 1 1 calc R U . . .
C9B C 0.1298(14) 0.4460(5) 0.6066(8) 0.055(4) Uani 1 1 d . . . . .
H9B H 0.074834 0.443178 0.563236 0.066 Uiso 1 1 calc R U . . .
C9C C 0.2397(11) 0.4364(4) 0.1001(7) 0.038(3) Uani 1 1 d . . . . .
H9C H 0.293417 0.432316 0.056388 0.045 Uiso 1 1 calc R U . . .
C9D C 1.2462(14) 0.7796(4) -0.1572(8) 0.048(4) Uani 1 1 d . . . . .
H9D H 1.190713 0.782941 -0.200072 0.058 Uiso 1 1 calc R U . . .
C10A C 0.6980(9) 0.2001(4) 0.3782(9) 0.035(3) Uani 1 1 d . . . . .
C10B C 0.2033(10) 0.5248(4) 0.8967(8) 0.034(3) Uani 1 1 d . . . . .
C10C C 0.1746(9) 0.5215(4) 0.3823(7) 0.028(2) Uani 1 1 d . . . . .
C10D C 1.3252(8) 0.6972(3) 0.1277(7) 0.027(2) Uani 1 1 d . . . . .
C11A C 0.6404(9) 0.1885(3) 0.3035(8) 0.031(2) Uani 1 1 d . . . . .
C11B C 0.1376(9) 0.5364(3) 0.9688(7) 0.028(2) Uani 1 1 d . . . . .
C11C C 0.2412(8) 0.5319(3) 0.4557(6) 0.022(2) Uani 1 1 d . . . . .
C11D C 1.2618(9) 0.6865(3) 0.2020(7) 0.027(2) Uani 1 1 d . . . . .
C12A C 0.4728(12) 0.1881(4) 0.2323(8) 0.043(3) Uani 1 1 d . . . . .
H12A H 0.396631 0.194017 0.231282 0.052 Uiso 1 1 calc R U . . .
C12B C -0.0344(11) 0.5367(4) 1.0301(8) 0.040(3) Uani 1 1 d . . . . .
H12B H -0.110217 0.530302 1.025777 0.048 Uiso 1 1 calc R U . . .
C12C C 0.4127(10) 0.5294(4) 0.5204(7) 0.030(2) Uani 1 1 d . . . . .
H12C H 0.487260 0.520324 0.517664 0.036 Uiso 1 1 calc R U . . .
C12D C 1.0934(10) 0.6890(4) 0.2670(7) 0.032(3) Uani 1 1 d . . . . .
H12D H 1.018539 0.697650 0.265355 0.039 Uiso 1 1 calc R U . . .
C13A C 0.5239(13) 0.1661(5) 0.1574(10) 0.057(4) Uani 1 1 d . U . . .
H13A H 0.480913 0.158698 0.107578 0.069 Uiso 1 1 calc R U . . .
C13B C 0.0049(13) 0.5603(4) 1.1044(8) 0.047(3) Uani 1 1 d . . . . .
H13B H -0.043916 0.568989 1.149544 0.057 Uiso 1 1 calc R U . . .
C13C C 0.3776(10) 0.5550(4) 0.5926(7) 0.033(2) Uani 1 1 d . . . . .
H13C H 0.427116 0.562516 0.638276 0.039 Uiso 1 1 calc R U . . .
C13D C 1.1304(13) 0.6638(4) 0.3403(8) 0.045(3) Uani 1 1 d . . . . .
H13D H 1.082178 0.656096 0.386487 0.054 Uiso 1 1 calc R U . . .
C14A C 0.6274(11) 0.1562(5) 0.1569(9) 0.045(3) Uani 1 1 d . U . . .
H14A H 0.659694 0.141710 0.107272 0.054 Uiso 1 1 calc R U . . .
C14B C 0.1129(13) 0.5709(4) 1.1123(8) 0.045(3) Uani 1 1 d . . . . .
H14B H 0.140545 0.586138 1.163197 0.054 Uiso 1 1 calc R U . . .
C14C C 0.2726(10) 0.5691(4) 0.5977(7) 0.033(2) Uani 1 1 d . . . . .
H14C H 0.248537 0.586830 0.646923 0.040 Uiso 1 1 calc R U . . .
C14D C 1.2332(13) 0.6511(4) 0.3437(8) 0.047(4) Uani 1 1 d . . . . .
H14D H 1.259539 0.634192 0.393342 0.057 Uiso 1 1 calc R U . . .
C15A C 0.6907(12) 0.1672(4) 0.2301(10) 0.048(4) Uani 1 1 d . . . . .
C15B C 0.1830(11) 0.5585(4) 1.0428(8) 0.041(3) Uani 1 1 d . . . . .
C15C C 0.1967(9) 0.5574(3) 0.5289(6) 0.026(2) Uani 1 1 d . . . . .
C15D C 1.3075(10) 0.6621(4) 0.2737(8) 0.033(3) Uani 1 1 d . . . . .
C16A C 0.8054(15) 0.1597(5) 0.2341(14) 0.075(6) Uani 1 1 d . . . . .
H16A H 0.841624 0.144778 0.186687 0.090 Uiso 1 1 calc R U . . .
C16B C 0.2960(12) 0.5673(4) 1.0451(9) 0.049(4) Uani 1 1 d . . . . .
H16B H 0.327899 0.582916 1.094055 0.058 Uiso 1 1 calc R U . . .
C16C C 0.0860(9) 0.5694(4) 0.5284(7) 0.034(3) Uani 1 1 d . . . . .
H16C H 0.055012 0.586105 0.576287 0.041 Uiso 1 1 calc R U . . .
C16D C 1.4175(11) 0.6505(4) 0.2710(9) 0.042(3) Uani 1 1 d . . . . .
H16D H 1.450512 0.633841 0.318390 0.050 Uiso 1 1 calc R U . . .
C17A C 0.8623(14) 0.1736(6) 0.3037(15) 0.081(7) Uani 1 1 d . . . . .
H17A H 0.939326 0.170297 0.303934 0.097 Uiso 1 1 calc R U . . .
C17B C 0.3593(11) 0.5533(5) 0.9771(10) 0.051(4) Uani 1 1 d . . . . .
H17B H 0.435930 0.557544 0.980929 0.062 Uiso 1 1 calc R U . . .
C17D C 1.4764(11) 0.6627(4) 0.2026(10) 0.051(4) Uani 1 1 d . . . . .
H17D H 1.552237 0.655859 0.203545 0.061 Uiso 1 1 calc R U . . .
C18A C 0.8107(11) 0.1928(5) 0.3758(11) 0.057(4) Uani 1 1 d . . . . .
H18A H 0.853215 0.201232 0.425371 0.068 Uiso 1 1 calc R U . . .
C18B C 0.3148(10) 0.5331(4) 0.9022(9) 0.042(3) Uani 1 1 d . . . . .
H18B H 0.360530 0.524869 0.854727 0.050 Uiso 1 1 calc R U . . .
C18C C 0.0628(9) 0.5338(4) 0.3857(8) 0.033(2) Uani 1 1 d . . . . .
H18C H 0.015535 0.526344 0.338420 0.040 Uiso 1 1 calc R U . . .
C18D C 1.4332(10) 0.6849(4) 0.1298(8) 0.041(3) Uani 1 1 d . . . . .
H18D H 1.478356 0.691745 0.081279 0.049 Uiso 1 1 calc R U . . .
C19A C 0.5705(9) 0.2985(4) 0.3928(7) 0.028(2) Uani 1 1 d . . . . .
C19B C 0.0824(10) 0.4224(4) 0.8700(6) 0.032(3) Uani 1 1 d . . . . .
C19C C 0.4378(9) 0.4151(4) 0.2635(7) 0.032(2) Uani 1 1 d . . . . .
C19D C 1.2036(10) 0.8012(4) 0.1078(7) 0.034(3) Uani 1 1 d . . . . .
C20A C 0.4107(11) 0.2931(4) 0.4969(8) 0.041(3) Uani 1 1 d . . . . .
C20B C -0.0725(11) 0.4283(5) 0.7655(8) 0.045(3) Uani 1 1 d . . . . .
C20C C 0.2814(9) 0.4166(4) 0.3681(7) 0.025(2) Uani 1 1 d . . . . .
C20D C 1.0454(10) 0.7971(4) 0.0055(8) 0.037(3) Uani 1 1 d . . . . .
C21A C 0.2529(11) 0.1739(5) 0.4284(9) 0.045(3) Uani 1 1 d . . . . .
C21B C -0.1823(10) 0.4264(4) 0.9997(9) 0.040(3) Uani 1 1 d . . . . .
C21C C 0.6256(11) 0.5271(5) 0.3294(8) 0.042(3) Uani 1 1 d . . . . .
C21D C 0.9456(13) 0.7988(5) 0.2412(9) 0.051(4) Uani 1 1 d . . . . .
C22A C 0.1506(12) 0.1489(6) 0.4392(12) 0.069(5) Uani 1 1 d . . . . .
H22A H 0.092039 0.172566 0.447128 0.103 Uiso 1 1 calc R U . . .
H22B H 0.154800 0.127784 0.490392 0.103 Uiso 1 1 calc R U . . .
H22C H 0.135412 0.129275 0.387364 0.103 Uiso 1 1 calc R U . . .
C22B C -0.2522(13) 0.4052(5) 1.0642(10) 0.060(4) Uani 1 1 d . . . . .
H22D H -0.319775 0.423922 1.068059 0.091 Uiso 1 1 calc R U . . .
H22E H -0.215168 0.405302 1.120807 0.091 Uiso 1 1 calc R U . . .
H22F H -0.269362 0.371743 1.047582 0.091 Uiso 1 1 calc R U . . .
C22C C 0.7321(13) 0.5484(6) 0.3245(10) 0.067(5) Uani 1 1 d . . . . .
H22G H 0.756113 0.558066 0.382913 0.100 Uiso 1 1 calc R U . . .
H22H H 0.729454 0.576973 0.286699 0.100 Uiso 1 1 calc R U . . .
H22I H 0.783465 0.524797 0.300592 0.100 Uiso 1 1 calc R U . . .
C22D C 0.8778(15) 0.8199(6) 0.3104(12) 0.086(6) Uani 1 1 d . . . . .
H22J H 0.800626 0.815382 0.295803 0.129 Uiso 1 1 calc R U . . .
H22K H 0.893556 0.854545 0.315596 0.129 Uiso 1 1 calc R U . . .
H22L H 0.893995 0.803774 0.365765 0.129 Uiso 1 1 calc R U . . .
C23A C 0.3093(11) 0.2928(4) 0.2600(9) 0.044(3) Uani 1 1 d . . . . .
C23B C -0.2397(12) 0.5443(5) 0.8284(8) 0.044(3) Uani 1 1 d . . . . .
C23C C 0.5450(10) 0.4175(4) 0.5007(8) 0.037(3) Uani 1 1 d . . . . .
C23D C 0.8784(10) 0.6794(5) 0.0762(8) 0.040(3) Uani 1 1 d . . . . .
C24A C 0.2368(14) 0.3138(5) 0.1924(11) 0.068(5) Uani 1 1 d . . . . .
H24A H 0.186074 0.336612 0.219666 0.102 Uiso 1 1 calc R U . . .
H24B H 0.195570 0.287893 0.163849 0.102 Uiso 1 1 calc R U . . .
H24C H 0.280744 0.330950 0.149125 0.102 Uiso 1 1 calc R U . . .
C24B C -0.3367(14) 0.5713(7) 0.8120(11) 0.080(6) Uani 1 1 d . . . . .
H24D H -0.351673 0.571769 0.749302 0.120 Uiso 1 1 calc R U . . .
H24E H -0.327363 0.604510 0.833091 0.120 Uiso 1 1 calc R U . . .
H24F H -0.397899 0.556075 0.842345 0.120 Uiso 1 1 calc R U . . .
C24C C 0.6106(14) 0.3962(5) 0.5682(9) 0.062(4) Uani 1 1 d . . . . .
H24G H 0.575105 0.366804 0.589684 0.093 Uiso 1 1 calc R U . . .
H24H H 0.619029 0.419346 0.616190 0.093 Uiso 1 1 calc R U . . .
H24I H 0.682479 0.388018 0.544959 0.093 Uiso 1 1 calc R U . . .
C24D C 0.7781(12) 0.6508(7) 0.0647(11) 0.069(5) Uani 1 1 d . . . . .
H24J H 0.717753 0.672424 0.049255 0.104 Uiso 1 1 calc R U . . .
H24K H 0.761240 0.633947 0.119093 0.104 Uiso 1 1 calc R U . . .
H24L H 0.788718 0.627066 0.018134 0.104 Uiso 1 1 calc R U . . .
C7C C 0.0586(12) 0.4181(4) 0.1553(9) 0.047(3) Uani 1 1 d . . . . .
H7C H -0.008940 0.401701 0.148466 0.057 Uiso 1 1 calc R U . . .
N1A N 0.5291(8) 0.1998(3) 0.3009(5) 0.0285(19) Uani 1 1 d . . . . .
N1B N 0.0307(8) 0.5228(3) 0.9646(6) 0.0288(19) Uani 1 1 d . . . . .
N1C N 0.3469(7) 0.5168(3) 0.4541(5) 0.0179(16) Uani 1 1 d . . . . .
N1D N 1.1521(7) 0.7016(3) 0.2013(5) 0.0270(19) Uani 1 1 d . . . . .
N2A N 0.3276(8) 0.1975(4) 0.4180(7) 0.037(2) Uani 1 1 d . . . . .
N2B N -0.1270(8) 0.4437(3) 0.9490(6) 0.036(2) Uani 1 1 d . . . . .
N2C N 0.5439(7) 0.5074(3) 0.3335(6) 0.0265(19) Uani 1 1 d . . . . .
N2D N 0.9996(8) 0.7823(3) 0.1898(6) 0.037(2) Uani 1 1 d . . . . .
N3A N 0.3667(8) 0.2773(3) 0.3116(6) 0.036(2) Uani 1 1 d . . . . .
N3B N -0.1637(8) 0.5231(4) 0.8402(6) 0.035(2) Uani 1 1 d . . . . .
N3C N 0.4899(8) 0.4317(3) 0.4483(6) 0.030(2) Uani 1 1 d . . . . .
N3D N 0.9539(9) 0.7012(4) 0.0821(6) 0.035(2) Uani 1 1 d . . . . .
O1A O 0.6290(7) 0.3313(3) 0.3873(5) 0.0399(19) Uani 1 1 d . . . . .
O1B O 0.1397(9) 0.3904(3) 0.8756(5) 0.050(3) Uani 1 1 d . . . . .
O1C O 0.4567(8) 0.3849(3) 0.2140(6) 0.048(2) Uani 1 1 d . . . . .
O1D O 1.2606(9) 0.8344(3) 0.1137(5) 0.052(3) Uani 1 1 d . . . . .
O2A O 0.3819(10) 0.3218(3) 0.5458(7) 0.061(3) Uani 1 1 d . . . . .
O2B O -0.0959(9) 0.3986(4) 0.7152(6) 0.062(3) Uani 1 1 d . . . . .
O2C O 0.2177(8) 0.3864(3) 0.3781(5) 0.045(2) Uani 1 1 d . . . . .
O2D O 1.0238(10) 0.8268(4) -0.0462(6) 0.065(3) Uani 1 1 d . . . . .
B1 B 0.1377(13) 0.1772(8) 0.1736(10) 0.053(4) Uani 1 1 d . . . . .
B2 B -0.3589(12) 0.5344(7) 1.0814(11) 0.051(4) Uani 1 1 d . . . . .
B3 B 0.796(2) 0.6835(9) 0.3170(14) 0.084(8) Uani 1 1 d . . . . .
B4 B -0.298(2) 0.5297(8) 0.5844(14) 0.086(8) Uani 1 1 d . . . . .
F11 F 0.1523(15) 0.1576(9) 0.2489(9) 0.213(11) Uani 1 1 d . . . . .
F12 F 0.0801(9) 0.2174(5) 0.1937(10) 0.119(5) Uani 1 1 d . . . . .
F13 F 0.0737(9) 0.1477(4) 0.1241(8) 0.089(3) Uani 1 1 d . . . . .
F14 F 0.2307(9) 0.1859(6) 0.1334(8) 0.122(5) Uani 1 1 d . . . . .
F21 F -0.2596(8) 0.5228(5) 1.1195(7) 0.098(4) Uani 1 1 d . . . . .
F22 F -0.4163(9) 0.5627(4) 1.1351(8) 0.097(4) Uani 1 1 d . . . . .
F23 F -0.3463(13) 0.5520(9) 1.0076(7) 0.214(12) Uani 1 1 d . . . . .
F24 F -0.4234(9) 0.4922(4) 1.0716(10) 0.118(5) Uani 1 1 d . . . . .
F31 F 0.8531(10) 0.6443(4) 0.2773(10) 0.116(5) Uani 1 1 d . . . . .
F32 F 0.8633(13) 0.7074(5) 0.3738(8) 0.120(5) Uani 1 1 d . . . . .
F33 F 0.7080(9) 0.6644(4) 0.3599(8) 0.104(4) Uani 1 1 d . . . . .
F34 F 0.7688(14) 0.7109(5) 0.2537(8) 0.135(6) Uani 1 1 d . . . . .
F41 F -0.2978(13) 0.5038(5) 0.5134(7) 0.124(5) Uani 1 1 d . . . . .
F42 F -0.2064(9) 0.5386(5) 0.6206(8) 0.104(4) Uani 1 1 d . . . . .
F43 F -0.3678(11) 0.5058(4) 0.6404(8) 0.097(4) Uani 1 1 d . . . . .
F44 F -0.3546(10) 0.5731(5) 0.5686(14) 0.169(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C19A 1.951(11) . ?
W1 C20A 1.988(12) . ?
W1 N3A 2.129(10) . ?
W1 C2A 2.163(10) . ?
W1 N2A 2.172(10) . ?
W1 N1A 2.246(9) . ?
W1 C1A 2.360(11) . ?
W1 C3A 2.384(11) . ?
W2 C20B 1.973(13) . ?
W2 C19B 1.984(12) . ?
W2 N2B 2.138(9) . ?
W2 N3B 2.167(10) . ?
W2 C2B 2.180(10) . ?
W2 N1B 2.246(9) . ?
W2 C1B 2.343(11) . ?
W2 C3B 2.417(11) . ?
W3 C20C 1.962(10) . ?
W3 C19C 1.968(10) . ?
W3 N3C 2.159(10) . ?
W3 C2C 2.168(9) . ?
W3 N2C 2.184(8) . ?
W3 N1C 2.252(7) . ?
W3 C1C 2.339(10) . ?
W3 C3C 2.423(10) . ?
W4 C19D 1.945(12) . ?
W4 C20D 1.968(12) . ?
W4 N2D 2.137(9) . ?
W4 C2D 2.179(10) . ?
W4 N3D 2.219(11) . ?
W4 N1D 2.247(9) . ?
W4 C1D 2.367(10) . ?
W4 C3D 2.394(10) . ?
C1A C10A 1.440(16) . ?
C1A C2A 1.459(16) . ?
C1A C5A 1.460(16) . ?
C1B C2B 1.429(16) . ?
C1B C10B 1.453(17) . ?
C1B C5B 1.529(15) . ?
C1C C2C 1.449(14) . ?
C1C C10C 1.475(14) . ?
C1C C5C 1.483(12) . ?
C1D C10D 1.453(15) . ?
C1D C2D 1.481(14) . ?
C1D C5D 1.484(14) . ?
C2A C3A 1.406(15) . ?
C2A H2A 0.9500 . ?
C2B C3B 1.406(16) . ?
C2B H2B 0.9500 . ?
C2C C3C 1.424(14) . ?
C2C H2C 0.9500 . ?
C2D C3D 1.442(14) . ?
C2D H2D 0.9500 . ?
C3A C4A 1.421(19) . ?
C3A H3A 0.9500 . ?
C3B C4B 1.483(16) . ?
C3B H3B 0.9500 . ?
C3C C4C 1.479(15) . ?
C3C H3C 0.9500 . ?
C3D C4D 1.464(16) . ?
C3D H3D 0.9500 . ?
C4A C5A 1.41(2) . ?
C4A C9A 1.43(2) . ?
C4B C5B 1.382(17) . ?
C4B C9B 1.404(17) . ?
C4C C9C 1.354(14) . ?
C4C C5C 1.396(14) . ?
C4D C5D 1.378(16) . ?
C4D C9D 1.407(15) . ?
C5A C6A 1.362(19) . ?
C5B C6B 1.376(17) . ?
C5C C6C 1.377(14) . ?
C5D C6D 1.402(15) . ?
C6A C7A 1.33(2) . ?
C6A H6A 0.9500 . ?
C6B C7B 1.42(2) . ?
C6B H6B 0.9500 . ?
C6C C7C 1.419(15) . ?
C6C H6C 0.9500 . ?
C6D C7D 1.432(16) . ?
C6D H6D 0.9500 . ?
C7A C8A 1.32(2) . ?
C7A H7A 0.9500 . ?
C7B C8B 1.35(2) . ?
C7B H7B 0.9500 . ?
C17C C16C 1.353(17) . ?
C17C C18C 1.387(15) . ?
C17C H17C 0.9500 . ?
C7D C8D 1.34(2) . ?
C7D H7D 0.9500 . ?
C8A C9A 1.41(2) . ?
C8A H8A 0.9500 . ?
C8B C9B 1.41(2) . ?
C8B H8B 0.9500 . ?
C8C C7C 1.33(2) . ?
C8C C9C 1.423(19) . ?
C8C H8C 0.9500 . ?
C8D C9D 1.44(2) . ?
C8D H8D 0.9500 . ?
C9A H9A 0.9500 . ?
C9B H9B 0.9500 . ?
C9C H9C 0.9500 . ?
C9D H9D 0.9500 . ?
C10A C11A 1.383(17) . ?
C10A C18A 1.399(17) . ?
C10B C18B 1.389(17) . ?
C10B C11B 1.410(16) . ?
C10C C18C 1.415(15) . ?
C10C C11C 1.420(15) . ?
C10D C18D 1.368(16) . ?
C10D C11D 1.416(15) . ?
C11A N1A 1.401(14) . ?
C11A C15A 1.416(16) . ?
C11B N1B 1.366(15) . ?
C11B C15B 1.404(16) . ?
C11C N1C 1.364(13) . ?
C11C C15C 1.437(13) . ?
C11D C15D 1.406(15) . ?
C11D N1D 1.409(14) . ?
C12A N1A 1.299(15) . ?
C12A C13A 1.447(19) . ?
C12A H12A 0.9500 . ?
C12B N1B 1.344(15) . ?
C12B C13B 1.397(17) . ?
C12B H12B 0.9500 . ?
C12C N1C 1.343(13) . ?
C12C C13C 1.385(14) . ?
C12C H12C 0.9500 . ?
C12D N1D 1.290(13) . ?
C12D C13D 1.399(17) . ?
C12D H12D 0.9500 . ?
C13A C14A 1.30(2) . ?
C13A H13A 0.9500 . ?
C13B C14B 1.36(2) . ?
C13B H13B 0.9500 . ?
C13C C14C 1.348(17) . ?
C13C H13C 0.9500 . ?
C13D C14D 1.31(2) . ?
C13D H13D 0.9500 . ?
C14A C15A 1.40(2) . ?
C14A H14A 0.9500 . ?
C14B C15B 1.42(2) . ?
C14B H14B 0.9500 . ?
C14C C15C 1.443(16) . ?
C14C H14C 0.9500 . ?
C14D C15D 1.446(19) . ?
C14D H14D 0.9500 . ?
C15A C16A 1.42(2) . ?
C15B C16B 1.408(19) . ?
C15C C16C 1.398(16) . ?
C15D C16D 1.389(18) . ?
C16A C17A 1.33(3) . ?
C16A H16A 0.9500 . ?
C16B C17B 1.36(2) . ?
C16B H16B 0.9500 . ?
C16C H16C 0.9500 . ?
C16D C17D 1.32(2) . ?
C16D H16D 0.9500 . ?
C17A C18A 1.38(2) . ?
C17A H17A 0.9500 . ?
C17B C18B 1.390(19) . ?
C17B H17B 0.9500 . ?
C17D C18D 1.379(18) . ?
C17D H17D 0.9500 . ?
C18A H18A 0.9500 . ?
C18B H18B 0.9500 . ?
C18C H18C 0.9500 . ?
C18D H18D 0.9500 . ?
C19A O1A 1.159(13) . ?
C19B O1B 1.134(14) . ?
C19C O1C 1.152(13) . ?
C19D O1D 1.157(14) . ?
C20A O2A 1.149(14) . ?
C20B O2B 1.161(15) . ?
C20C O2C 1.153(13) . ?
C20D O2D 1.169(14) . ?
C21A N2A 1.139(16) . ?
C21A C22A 1.443(19) . ?
C21B N2B 1.140(14) . ?
C21B C22B 1.439(17) . ?
C21C N2C 1.142(15) . ?
C21C C22C 1.44(2) . ?
C21D N2D 1.129(15) . ?
C21D C22D 1.474(18) . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C22C H22G 0.9800 . ?
C22C H22H 0.9800 . ?
C22C H22I 0.9800 . ?
C22D H22J 0.9800 . ?
C22D H22K 0.9800 . ?
C22D H22L 0.9800 . ?
C23A N3A 1.142(16) . ?
C23A C24A 1.484(18) . ?
C23B N3B 1.116(16) . ?
C23B C24B 1.43(2) . ?
C23C N3C 1.121(14) . ?
C23C C24C 1.437(16) . ?
C23D N3D 1.107(16) . ?
C23D C24D 1.472(18) . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C24C H24G 0.9800 . ?
C24C H24H 0.9800 . ?
C24C H24I 0.9800 . ?
C24D H24J 0.9800 . ?
C24D H24K 0.9800 . ?
C24D H24L 0.9800 . ?
C7C H7C 0.9500 . ?
B1 F11 1.29(2) . ?
B1 F14 1.323(19) . ?
B1 F12 1.35(2) . ?
B1 F13 1.36(2) . ?
B2 F23 1.24(2) . ?
B2 F22 1.340(16) . ?
B2 F21 1.39(2) . ?
B2 F24 1.42(2) . ?
B3 F34 1.28(3) . ?
B3 F32 1.37(3) . ?
B3 F33 1.37(2) . ?
B3 F31 1.43(3) . ?
B4 F42 1.28(2) . ?
B4 F41 1.30(3) . ?
B4 F43 1.38(2) . ?
B4 F44 1.40(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
C19A W1 C20A 80.3(5) . . ?
C19A W1 N3A 88.6(4) . . ?
C20A W1 N3A 90.6(5) . . ?
C19A W1 C2A 108.4(4) . . ?
C20A W1 C2A 105.5(5) . . ?
N3A W1 C2A 158.1(4) . . ?
C19A W1 N2A 168.4(4) . . ?
C20A W1 N2A 95.3(5) . . ?
N3A W1 N2A 80.8(4) . . ?
C2A W1 N2A 83.1(4) . . ?
C19A W1 N1A 95.4(4) . . ?
C20A W1 N1A 173.3(4) . . ?
N3A W1 N1A 84.0(4) . . ?
C2A W1 N1A 80.8(4) . . ?
N2A W1 N1A 87.9(4) . . ?
C19A W1 C1A 72.9(4) . . ?
C20A W1 C1A 110.4(5) . . ?
N3A W1 C1A 148.5(4) . . ?
C2A W1 C1A 37.3(4) . . ?
N2A W1 C1A 118.6(4) . . ?
N1A W1 C1A 73.0(4) . . ?
C19A W1 C3A 103.6(5) . . ?
C20A W1 C3A 69.9(4) . . ?
N3A W1 C3A 154.5(4) . . ?
C2A W1 C3A 35.6(4) . . ?
N2A W1 C3A 84.7(4) . . ?
N1A W1 C3A 116.4(4) . . ?
C1A W1 C3A 56.9(4) . . ?
C20B W2 C19B 78.0(5) . . ?
C20B W2 N2B 90.9(4) . . ?
C19B W2 N2B 89.7(4) . . ?
C20B W2 N3B 95.8(5) . . ?
C19B W2 N3B 168.7(4) . . ?
N2B W2 N3B 80.9(4) . . ?
C20B W2 C2B 105.2(5) . . ?
C19B W2 C2B 107.2(4) . . ?
N2B W2 C2B 158.6(4) . . ?
N3B W2 C2B 83.4(4) . . ?
C20B W2 N1B 173.3(4) . . ?
C19B W2 N1B 97.9(4) . . ?
N2B W2 N1B 83.8(3) . . ?
N3B W2 N1B 87.4(4) . . ?
C2B W2 N1B 80.9(4) . . ?
C20B W2 C1B 111.4(5) . . ?
C19B W2 C1B 73.5(4) . . ?
N2B W2 C1B 147.8(4) . . ?
N3B W2 C1B 117.8(4) . . ?
C2B W2 C1B 36.6(4) . . ?
N1B W2 C1B 72.0(4) . . ?
C20B W2 C3B 70.2(5) . . ?
C19B W2 C3B 101.8(4) . . ?
N2B W2 C3B 154.9(4) . . ?
N3B W2 C3B 84.6(4) . . ?
C2B W2 C3B 35.1(4) . . ?
N1B W2 C3B 116.1(4) . . ?
C1B W2 C3B 57.3(4) . . ?
C20C W3 C19C 79.4(4) . . ?
C20C W3 N3C 88.0(4) . . ?
C19C W3 N3C 90.9(4) . . ?
C20C W3 C2C 108.2(4) . . ?
C19C W3 C2C 105.6(4) . . ?
N3C W3 C2C 158.5(4) . . ?
C20C W3 N2C 167.3(4) . . ?
C19C W3 N2C 94.7(4) . . ?
N3C W3 N2C 80.8(3) . . ?
C2C W3 N2C 84.1(4) . . ?
C20C W3 N1C 97.3(4) . . ?
C19C W3 N1C 173.5(4) . . ?
N3C W3 N1C 83.3(3) . . ?
C2C W3 N1C 80.8(3) . . ?
N2C W3 N1C 87.4(3) . . ?
C20C W3 C1C 73.0(4) . . ?
C19C W3 C1C 110.6(4) . . ?
N3C W3 C1C 147.5(3) . . ?
C2C W3 C1C 37.3(3) . . ?
N2C W3 C1C 119.7(3) . . ?
N1C W3 C1C 73.5(3) . . ?
C20C W3 C3C 102.7(4) . . ?
C19C W3 C3C 70.0(4) . . ?
N3C W3 C3C 155.5(4) . . ?
C2C W3 C3C 35.6(4) . . ?
N2C W3 C3C 85.5(4) . . ?
N1C W3 C3C 116.4(3) . . ?
C1C W3 C3C 56.8(4) . . ?
C19D W4 C20D 79.3(5) . . ?
C19D W4 N2D 88.7(4) . . ?
C20D W4 N2D 90.5(4) . . ?
C19D W4 C2D 108.4(4) . . ?
C20D W4 C2D 105.0(4) . . ?
N2D W4 C2D 158.6(3) . . ?
C19D W4 N3D 168.9(4) . . ?
C20D W4 N3D 95.9(4) . . ?
N2D W4 N3D 81.4(4) . . ?
C2D W4 N3D 82.4(4) . . ?
C19D W4 N1D 97.9(4) . . ?
C20D W4 N1D 173.4(4) . . ?
N2D W4 N1D 83.4(3) . . ?
C2D W4 N1D 81.6(3) . . ?
N3D W4 N1D 85.8(3) . . ?
C19D W4 C1D 73.4(4) . . ?
C20D W4 C1D 111.7(4) . . ?
N2D W4 C1D 147.4(4) . . ?
C2D W4 C1D 37.7(4) . . ?
N3D W4 C1D 117.7(3) . . ?
N1D W4 C1D 72.8(3) . . ?
C19D W4 C3D 101.7(4) . . ?
C20D W4 C3D 68.6(4) . . ?
N2D W4 C3D 154.1(4) . . ?
C2D W4 C3D 36.4(4) . . ?
N3D W4 C3D 85.6(4) . . ?
N1D W4 C3D 118.0(3) . . ?
C1D W4 C3D 58.2(4) . . ?
C10A C1A C2A 120.4(10) . . ?
C10A C1A C5A 129.3(11) . . ?
C2A C1A C5A 106.4(10) . . ?
C10A C1A W1 109.6(8) . . ?
C2A C1A W1 64.0(6) . . ?
C5A C1A W1 107.4(7) . . ?
C2B C1B C10B 123.0(10) . . ?
C2B C1B C5B 104.9(10) . . ?
C10B C1B C5B 127.6(10) . . ?
C2B C1B W2 65.5(6) . . ?
C10B C1B W2 110.9(7) . . ?
C5B C1B W2 107.2(7) . . ?
C2C C1C C10C 119.5(9) . . ?
C2C C1C C5C 107.4(8) . . ?
C10C C1C C5C 128.5(9) . . ?
C2C C1C W3 65.0(5) . . ?
C10C C1C W3 109.6(7) . . ?
C5C C1C W3 108.6(6) . . ?
C10D C1D C2D 120.6(9) . . ?
C10D C1D C5D 129.6(10) . . ?
C2D C1D C5D 104.9(9) . . ?
C10D C1D W4 111.2(7) . . ?
C2D C1D W4 64.2(5) . . ?
C5D C1D W4 107.0(7) . . ?
C3A C2A C1A 104.1(10) . . ?
C3A C2A W1 80.8(7) . . ?
C1A C2A W1 78.7(6) . . ?
C3A C2A H2A 128.0 . . ?
C1A C2A H2A 128.0 . . ?
W1 C2A H2A 106.8 . . ?
C3B C2B C1B 107.2(11) . . ?
C3B C2B W2 81.7(7) . . ?
C1B C2B W2 77.9(6) . . ?
C3B C2B H2B 126.4 . . ?
C1B C2B H2B 126.4 . . ?
W2 C2B H2B 107.4 . . ?
C3C C2C C1C 104.1(9) . . ?
C3C C2C W3 82.0(6) . . ?
C1C C2C W3 77.8(6) . . ?
C3C C2C H2C 128.0 . . ?
C1C C2C H2C 128.0 . . ?
W3 C2C H2C 106.6 . . ?
C3D C2D C1D 104.8(9) . . ?
C3D C2D W4 79.9(6) . . ?
C1D C2D W4 78.0(6) . . ?
C3D C2D H2D 127.6 . . ?
C1D C2D H2D 127.6 . . ?
W4 C2D H2D 108.2 . . ?
C2A C3A C4A 109.0(12) . . ?
C2A C3A W1 63.6(6) . . ?
C4A C3A W1 106.6(8) . . ?
C2A C3A H3A 125.5 . . ?
C4A C3A H3A 125.5 . . ?
W1 C3A H3A 97.8 . . ?
C2B C3B C4B 106.6(11) . . ?
C2B C3B W2 63.2(6) . . ?
C4B C3B W2 105.4(7) . . ?
C2B C3B H3B 126.7 . . ?
C4B C3B H3B 126.7 . . ?
W2 C3B H3B 98.9 . . ?
C2C C3C C4C 108.3(9) . . ?
C2C C3C W3 62.4(5) . . ?
C4C C3C W3 105.8(6) . . ?
C2C C3C H3C 125.9 . . ?
C4C C3C H3C 125.9 . . ?
W3 C3C H3C 99.3 . . ?
C2D C3D C4D 106.0(10) . . ?
C2D C3D W4 63.7(5) . . ?
C4D C3D W4 105.9(7) . . ?
C2D C3D H3D 127.0 . . ?
C4D C3D H3D 127.0 . . ?
W4 C3D H3D 98.1 . . ?
C5A C4A C3A 108.0(11) . . ?
C5A C4A C9A 114.1(14) . . ?
C3A C4A C9A 137.8(16) . . ?
C5B C4B C9B 121.5(12) . . ?
C5B C4B C3B 108.5(10) . . ?
C9B C4B C3B 129.9(12) . . ?
C9C C4C C5C 122.3(11) . . ?
C9C C4C C3C 130.4(11) . . ?
C5C C4C C3C 107.3(8) . . ?
C5D C4D C9D 121.7(12) . . ?
C5D C4D C3D 109.5(9) . . ?
C9D C4D C3D 128.8(12) . . ?
C6A C5A C4A 119.2(14) . . ?
C6A C5A C1A 134.4(15) . . ?
C4A C5A C1A 106.3(11) . . ?
C6B C5B C4B 122.6(11) . . ?
C6B C5B C1B 131.1(12) . . ?
C4B C5B C1B 106.3(10) . . ?
C6C C5C C4C 121.3(9) . . ?
C6C C5C C1C 131.8(9) . . ?
C4C C5C C1C 106.9(9) . . ?
C4D C5D C6D 121.9(10) . . ?
C4D C5D C1D 107.7(9) . . ?
C6D C5D C1D 130.3(11) . . ?
C7A C6A C5A 129(2) . . ?
C7A C6A H6A 115.3 . . ?
C5A C6A H6A 115.3 . . ?
C5B C6B C7B 115.9(14) . . ?
C5B C6B H6B 122.1 . . ?
C7B C6B H6B 122.1 . . ?
C5C C6C C7C 117.3(10) . . ?
C5C C6C H6C 121.4 . . ?
C7C C6C H6C 121.4 . . ?
C5D C6D C7D 117.0(13) . . ?
C5D C6D H6D 121.5 . . ?
C7D C6D H6D 121.5 . . ?
C8A C7A C6A 111.4(19) . . ?
C8A C7A H7A 124.3 . . ?
C6A C7A H7A 124.3 . . ?
C8B C7B C6B 121.9(14) . . ?
C8B C7B H7B 119.0 . . ?
C6B C7B H7B 119.0 . . ?
C16C C17C C18C 123.9(11) . . ?
C16C C17C H17C 118.0 . . ?
C18C C17C H17C 118.0 . . ?
C8D C7D C6D 120.6(12) . . ?
C8D C7D H7D 119.7 . . ?
C6D C7D H7D 119.7 . . ?
C7A C8A C9A 126.9(17) . . ?
C7A C8A H8A 116.6 . . ?
C9A C8A H8A 116.6 . . ?
C7B C8B C9B 122.6(14) . . ?
C7B C8B H8B 118.7 . . ?
C9B C8B H8B 118.7 . . ?
C7C C8C C9C 124.3(11) . . ?
C7C C8C H8C 117.8 . . ?
C9C C8C H8C 117.8 . . ?
C7D C8D C9D 123.2(11) . . ?
C7D C8D H8D 118.4 . . ?
C9D C8D H8D 118.4 . . ?
C8A C9A C4A 118.7(16) . . ?
C8A C9A H9A 120.7 . . ?
C4A C9A H9A 120.7 . . ?
C4B C9B C8B 115.3(15) . . ?
C4B C9B H9B 122.3 . . ?
C8B C9B H9B 122.3 . . ?
C4C C9C C8C 115.2(12) . . ?
C4C C9C H9C 122.4 . . ?
C8C C9C H9C 122.4 . . ?
C4D C9D C8D 115.5(13) . . ?
C4D C9D H9D 122.2 . . ?
C8D C9D H9D 122.2 . . ?
C11A C10A C18A 116.6(13) . . ?
C11A C10A C1A 119.0(10) . . ?
C18A C10A C1A 124.4(13) . . ?
C18B C10B C11B 118.8(12) . . ?
C18B C10B C1B 124.2(11) . . ?
C11B C10B C1B 116.9(10) . . ?
C18C C10C C11C 118.5(10) . . ?
C18C C10C C1C 123.9(10) . . ?
C11C C10C C1C 117.6(9) . . ?
C18D C10D C11D 117.8(11) . . ?
C18D C10D C1D 124.6(11) . . ?
C11D C10D C1D 117.5(9) . . ?
C10A C11A N1A 117.8(10) . . ?
C10A C11A C15A 122.3(11) . . ?
N1A C11A C15A 119.9(12) . . ?
N1B C11B C15B 122.4(11) . . ?
N1B C11B C10B 117.0(10) . . ?
C15B C11B C10B 120.6(11) . . ?
N1C C11C C10C 117.9(8) . . ?
N1C C11C C15C 121.9(9) . . ?
C10C C11C C15C 120.1(9) . . ?
C15D C11D N1D 121.7(10) . . ?
C15D C11D C10D 120.8(10) . . ?
N1D C11D C10D 117.5(9) . . ?
N1A C12A C13A 121.3(14) . . ?
N1A C12A H12A 119.3 . . ?
C13A C12A H12A 119.3 . . ?
N1B C12B C13B 122.8(13) . . ?
N1B C12B H12B 118.6 . . ?
C13B C12B H12B 118.6 . . ?
N1C C12C C13C 123.4(11) . . ?
N1C C12C H12C 118.3 . . ?
C13C C12C H12C 118.3 . . ?
N1D C12D C13D 125.7(12) . . ?
N1D C12D H12D 117.1 . . ?
C13D C12D H12D 117.1 . . ?
C14A C13A C12A 121.3(15) . . ?
C14A C13A H13A 119.3 . . ?
C12A C13A H13A 119.3 . . ?
C14B C13B C12B 120.3(13) . . ?
C14B C13B H13B 119.8 . . ?
C12B C13B H13B 119.8 . . ?
C14C C13C C12C 119.7(11) . . ?
C14C C13C H13C 120.2 . . ?
C12C C13C H13C 120.2 . . ?
C14D C13D C12D 118.3(12) . . ?
C14D C13D H13D 120.9 . . ?
C12D C13D H13D 120.9 . . ?
C13A C14A C15A 119.3(13) . . ?
C13A C14A H14A 120.3 . . ?
C15A C14A H14A 120.3 . . ?
C13B C14B C15B 118.4(12) . . ?
C13B C14B H14B 120.8 . . ?
C15B C14B H14B 120.8 . . ?
C13C C14C C15C 120.5(10) . . ?
C13C C14C H14C 119.8 . . ?
C15C C14C H14C 119.8 . . ?
C13D C14D C15D 121.7(11) . . ?
C13D C14D H14D 119.2 . . ?
C15D C14D H14D 119.2 . . ?
C14A C15A C11A 119.2(13) . . ?
C14A C15A C16A 123.3(14) . . ?
C11A C15A C16A 117.4(16) . . ?
C11B C15B C16B 118.9(13) . . ?
C11B C15B C14B 118.4(12) . . ?
C16B C15B C14B 122.7(13) . . ?
C16C C15C C11C 119.0(10) . . ?
C16C C15C C14C 125.2(9) . . ?
C11C C15C C14C 115.9(10) . . ?
C16D C15D C11D 118.2(12) . . ?
C16D C15D C14D 126.2(12) . . ?
C11D C15D C14D 115.6(11) . . ?
C17A C16A C15A 120.5(16) . . ?
C17A C16A H16A 119.7 . . ?
C15A C16A H16A 119.7 . . ?
C17B C16B C15B 119.8(12) . . ?
C17B C16B H16B 120.1 . . ?
C15B C16B H16B 120.1 . . ?
C17C C16C C15C 119.5(10) . . ?
C17C C16C H16C 120.2 . . ?
C15C C16C H16C 120.2 . . ?
C17D C16D C15D 119.9(12) . . ?
C17D C16D H16D 120.0 . . ?
C15D C16D H16D 120.0 . . ?
C16A C17A C18A 120.9(16) . . ?
C16A C17A H17A 119.6 . . ?
C18A C17A H17A 119.6 . . ?
C16B C17B C18B 121.8(12) . . ?
C16B C17B H17B 119.1 . . ?
C18B C17B H17B 119.1 . . ?
C16D C17D C18D 123.3(13) . . ?
C16D C17D H17D 118.4 . . ?
C18D C17D H17D 118.4 . . ?
C17A C18A C10A 122.2(17) . . ?
C17A C18A H18A 118.9 . . ?
C10A C18A H18A 118.9 . . ?
C17B C18B C10B 120.0(12) . . ?
C17B C18B H18B 120.0 . . ?
C10B C18B H18B 120.0 . . ?
C17C C18C C10C 118.8(11) . . ?
C17C C18C H18C 120.6 . . ?
C10C C18C H18C 120.6 . . ?
C10D C18D C17D 119.9(12) . . ?
C10D C18D H18D 120.1 . . ?
C17D C18D H18D 120.1 . . ?
O1A C19A W1 175.3(9) . . ?
O1B C19B W2 175.7(11) . . ?
O1C C19C W3 175.8(10) . . ?
O1D C19D W4 174.1(11) . . ?
O2A C20A W1 176.9(12) . . ?
O2B C20B W2 175.9(13) . . ?
O2C C20C W3 176.8(10) . . ?
O2D C20D W4 174.0(12) . . ?
N2A C21A C22A 173.3(14) . . ?
N2B C21B C22B 179.4(14) . . ?
N2C C21C C22C 175.8(15) . . ?
N2D C21D C22D 178.2(18) . . ?
C21A C22A H22A 109.5 . . ?
C21A C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C21A C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C21B C22B H22D 109.5 . . ?
C21B C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C21B C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C21C C22C H22G 109.5 . . ?
C21C C22C H22H 109.5 . . ?
H22G C22C H22H 109.5 . . ?
C21C C22C H22I 109.5 . . ?
H22G C22C H22I 109.5 . . ?
H22H C22C H22I 109.5 . . ?
C21D C22D H22J 109.5 . . ?
C21D C22D H22K 109.5 . . ?
H22J C22D H22K 109.5 . . ?
C21D C22D H22L 109.5 . . ?
H22J C22D H22L 109.5 . . ?
H22K C22D H22L 109.5 . . ?
N3A C23A C24A 178.6(15) . . ?
N3B C23B C24B 179.2(16) . . ?
N3C C23C C24C 175.8(14) . . ?
N3D C23D C24D 177.8(14) . . ?
C23A C24A H24A 109.5 . . ?
C23A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C23A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C23B C24B H24D 109.5 . . ?
C23B C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C23B C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C23C C24C H24G 109.5 . . ?
C23C C24C H24H 109.5 . . ?
H24G C24C H24H 109.5 . . ?
C23C C24C H24I 109.5 . . ?
H24G C24C H24I 109.5 . . ?
H24H C24C H24I 109.5 . . ?
C23D C24D H24J 109.5 . . ?
C23D C24D H24K 109.5 . . ?
H24J C24D H24K 109.5 . . ?
C23D C24D H24L 109.5 . . ?
H24J C24D H24L 109.5 . . ?
H24K C24D H24L 109.5 . . ?
C8C C7C C6C 119.6(12) . . ?
C8C C7C H7C 120.2 . . ?
C6C C7C H7C 120.2 . . ?
C12A N1A C11A 118.8(10) . . ?
C12A N1A W1 124.5(9) . . ?
C11A N1A W1 116.2(7) . . ?
C12B N1B C11B 117.4(10) . . ?
C12B N1B W2 124.1(8) . . ?
C11B N1B W2 118.5(7) . . ?
C12C N1C C11C 118.4(8) . . ?
C12C N1C W3 124.3(7) . . ?
C11C N1C W3 117.0(6) . . ?
C12D N1D C11D 116.8(10) . . ?
C12D N1D W4 125.5(8) . . ?
C11D N1D W4 117.5(6) . . ?
C21A N2A W1 174.4(11) . . ?
C21B N2B W2 179.7(12) . . ?
C21C N2C W3 175.7(10) . . ?
C21D N2D W4 178.1(12) . . ?
C23A N3A W1 176.9(10) . . ?
C23B N3B W2 173.5(11) . . ?
C23C N3C W3 174.3(10) . . ?
C23D N3D W4 175.7(10) . . ?
F11 B1 F14 112.3(16) . . ?
F11 B1 F12 102.2(17) . . ?
F14 B1 F12 114.1(17) . . ?
F11 B1 F13 109(2) . . ?
F14 B1 F13 110.2(14) . . ?
F12 B1 F13 108.4(13) . . ?
F23 B2 F22 114(2) . . ?
F23 B2 F21 111.2(14) . . ?
F22 B2 F21 109.7(14) . . ?
F23 B2 F24 107.2(16) . . ?
F22 B2 F24 104.5(12) . . ?
F21 B2 F24 110.2(15) . . ?
F34 B3 F32 110.8(19) . . ?
F34 B3 F33 113(2) . . ?
F32 B3 F33 110.6(16) . . ?
F34 B3 F31 104.6(16) . . ?
F32 B3 F31 110(2) . . ?
F33 B3 F31 107.7(17) . . ?
F42 B4 F41 117(3) . . ?
F42 B4 F43 111.5(16) . . ?
F41 B4 F43 105.3(15) . . ?
F42 B4 F44 110.1(16) . . ?
F41 B4 F44 109.2(17) . . ?
F43 B4 F44 102(2) . . ?

_refine_diff_density_max         3.458
_refine_diff_density_min         -1.464
_refine_diff_density_rms         0.131



