# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_lv194_moco3pyz2_e_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 2063156'
loop_
_audit_author_name
_audit_author_address
'Mariusz Kubus'
;Technical University of Denmark
Denmark
;
_audit_update_record             
;
2021-03-18 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_audit_creation_date             2021-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H6 Mo N3 O3, C2 H2 N'
_chemical_formula_sum            'C11 H8 Mo N4 O3'
_chemical_formula_weight         340.15
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22 H16 Mo2 N8 O8'
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'

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

_cell_length_a                   6.8571(8)
_cell_length_b                   9.7204(11)
_cell_length_c                   10.0406(10)
_cell_angle_alpha                64.131(10)
_cell_angle_beta                 88.185(9)
_cell_angle_gamma                86.345(10)
_cell_volume                     600.95(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1262
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.0670
_cell_measurement_theta_min      4.7810
_shelx_estimated_absorpt_T_max   0.978
_shelx_estimated_absorpt_T_min   0.978
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.1047
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4212
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.679
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     13.00  39.00   1.00  110.00    --   10.87 -99.00 120.00   26
  2  ω    -57.00  34.00   1.00  110.00    --   10.87 -57.00 120.00   91
  3  ω    -15.00  77.00   1.00  110.00    --   10.87  77.00  30.00   92
  4  ω    -16.00  83.00   1.00  110.00    --   10.87  57.00 -90.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0878018000
_diffrn_orient_matrix_UB_12      -0.0467549000
_diffrn_orient_matrix_UB_13      0.0211321000
_diffrn_orient_matrix_UB_21      0.0531043000
_diffrn_orient_matrix_UB_22      0.0655437000
_diffrn_orient_matrix_UB_23      -0.0151634000
_diffrn_orient_matrix_UB_31      -0.0146481000
_diffrn_orient_matrix_UB_32      -0.0107264000
_diffrn_orient_matrix_UB_33      0.0740777000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3081
_reflns_number_total             4212
_reflns_special_details          
;
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0361
_refine_ls_restrained_S_all      0.868
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0249P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0672
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.6022(9)
 0.3978(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C7(H7), C9(H9), C11(H11)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.33092(6) 0.65555(5) 0.17640(4) 0.00945(11) Uani 1 1 d . . . . .
N1 N 0.1204(6) 0.8639(4) 0.0709(4) 0.0100(9) Uani 1 1 d . . . . .
O1 O 0.5743(4) 0.8308(4) 0.3034(3) 0.0202(7) Uani 1 1 d . . . . .
N3 N 0.1263(6) 0.5635(4) 0.3760(4) 0.0101(9) Uani 1 1 d . . . . .
N4 N 0.1306(5) 0.5532(4) 0.0711(4) 0.0093(8) Uani 1 1 d . . . . .
O2 O 0.5941(5) 0.7658(4) -0.1065(3) 0.0213(8) Uani 1 1 d . . . . .
C1 C 0.4831(6) 0.7625(5) 0.2579(5) 0.0152(10) Uani 1 1 d . . . . .
C2 C 0.4956(8) 0.7261(5) -0.0002(5) 0.0133(12) Uani 1 1 d . . . . .
O3 O 0.6410(6) 0.3838(4) 0.3230(4) 0.0290(9) Uani 1 1 d . . . . .
C3 C 0.5194(8) 0.4825(6) 0.2677(5) 0.0149(11) Uani 1 1 d . . . . .
C4 C 0.0447(8) 0.4193(5) 0.1419(5) 0.0149(11) Uani 1 1 d . . . . .
H4 H 0.072492 0.359460 0.241496 0.018 Uiso 1 1 calc R U . . .
C5 C 0.0828(7) 0.6329(5) -0.0729(5) 0.0134(11) Uani 1 1 d . . . . .
H5 H 0.137721 0.726461 -0.127636 0.016 Uiso 1 1 calc R U . . .
C6 C -0.0723(6) 0.8627(5) 0.0551(4) 0.0115(10) Uani 1 1 d . . . . .
H6 H -0.129709 0.768875 0.092394 0.014 Uiso 1 1 calc R U . . .
C8 C 0.1381(7) 0.4132(5) 0.4731(4) 0.0128(10) Uani 1 1 d . . . . .
H8 H 0.233334 0.348516 0.458510 0.015 Uiso 1 1 calc R U . . .
C7 C 0.1903(7) 1.0046(5) 0.0146(4) 0.0108(10) Uani 1 1 d . . . . .
H7 H 0.323158 1.013192 0.022915 0.013 Uiso 1 1 calc R U . . .
C9 C -0.0126(7) 0.6473(5) 0.4066(4) 0.0134(11) Uani 1 1 d . . . . .
H9 H -0.026407 0.751567 0.344358 0.016 Uiso 1 1 calc R U . . .
N5 N 0.0208(7) 0.9805(5) -0.3547(4) 0.0265(11) Uani 1 1 d . . . . .
C10 C -0.1518(8) 1.0024(6) -0.4180(6) 0.0257(12) Uani 1 1 d . . . . .
C11 C 0.1720(7) 0.9786(5) -0.4387(5) 0.0264(12) Uani 1 1 d . . . . .
H11 H 0.296963 0.963960 -0.399714 0.032 Uiso 1 1 calc R U . . .
H10 H -0.263(8) 0.997(6) -0.357(6) 0.038(16) Uiso 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
Mo1 N1 2.271(4) . ?
Mo1 N3 2.281(4) . ?
Mo1 N4 2.276(3) . ?
Mo1 C1 1.943(5) . ?
Mo1 C2 1.949(5) . ?
Mo1 C3 1.948(5) . ?
N1 C6 1.337(6) . ?
N1 C7 1.346(6) . ?
O1 C1 1.173(5) . ?
N3 C8 1.356(5) . ?
N3 C9 1.330(6) . ?
N4 C4 1.345(6) . ?
N4 C5 1.349(5) . ?
O2 C2 1.172(6) . ?
O3 C3 1.177(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.380(6) 2_565 ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C6 C7 1.387(6) 2_575 ?
C8 H8 0.9300 . ?
C8 C9 1.387(6) 2_566 ?
C7 H7 0.9300 . ?
C9 H9 0.9300 . ?
N5 C10 1.321(6) . ?
N5 C11 1.320(6) . ?
C10 C11 1.379(7) 2_574 ?
C10 H10 0.95(6) . ?
C11 H11 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Mo1 N3 88.55(12) . . ?
N1 Mo1 N4 83.07(13) . . ?
N4 Mo1 N3 85.90(13) . . ?
C1 Mo1 N1 90.78(16) . . ?
C1 Mo1 N3 93.73(16) . . ?
C1 Mo1 N4 173.85(15) . . ?
C1 Mo1 C2 90.42(19) . . ?
C1 Mo1 C3 86.93(19) . . ?
C2 Mo1 N1 91.56(18) . . ?
C2 Mo1 N3 175.84(17) . . ?
C2 Mo1 N4 89.98(16) . . ?
C3 Mo1 N1 177.59(19) . . ?
C3 Mo1 N3 92.35(18) . . ?
C3 Mo1 N4 99.22(17) . . ?
C3 Mo1 C2 87.70(18) . . ?
C6 N1 Mo1 126.3(3) . . ?
C6 N1 C7 114.5(4) . . ?
C7 N1 Mo1 119.2(3) . . ?
C8 N3 Mo1 120.7(3) . . ?
C9 N3 Mo1 124.6(3) . . ?
C9 N3 C8 114.7(4) . . ?
C4 N4 Mo1 125.7(3) . . ?
C4 N4 C5 114.9(4) . . ?
C5 N4 Mo1 119.3(3) . . ?
O1 C1 Mo1 178.1(4) . . ?
O2 C2 Mo1 178.6(4) . . ?
O3 C3 Mo1 176.0(5) . . ?
N4 C4 H4 118.6 . . ?
N4 C4 C5 122.7(4) . 2_565 ?
C5 C4 H4 118.6 2_565 . ?
N4 C5 C4 122.3(4) . 2_565 ?
N4 C5 H5 118.8 . . ?
C4 C5 H5 118.8 2_565 . ?
N1 C6 H6 118.6 . . ?
N1 C6 C7 122.8(4) . 2_575 ?
C7 C6 H6 118.6 2_575 . ?
N3 C8 H8 118.9 . . ?
N3 C8 C9 122.2(4) . 2_566 ?
C9 C8 H8 118.9 2_566 . ?
N1 C7 C6 122.7(4) . 2_575 ?
N1 C7 H7 118.6 . . ?
C6 C7 H7 118.6 2_575 . ?
N3 C9 C8 123.2(4) . 2_566 ?
N3 C9 H9 118.4 . . ?
C8 C9 H9 118.4 2_566 . ?
C11 N5 C10 115.2(4) . . ?
N5 C10 C11 122.3(5) . 2_574 ?
N5 C10 H10 116(3) . . ?
C11 C10 H10 121(3) 2_574 . ?
N5 C11 C10 122.5(5) . 2_574 ?
N5 C11 H11 118.7 . . ?
C10 C11 H11 118.7 2_574 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 N1 C6 C7 -178.1(3) . . . 2_575 ?
Mo1 N1 C7 C6 178.2(3) . . . 2_575 ?
Mo1 N3 C8 C9 -178.3(3) . . . 2_566 ?
Mo1 N3 C9 C8 178.3(3) . . . 2_566 ?
Mo1 N4 C4 C5 176.9(3) . . . 2_565 ?
Mo1 N4 C5 C4 -177.1(3) . . . 2_565 ?
C4 N4 C5 C4 0.1(7) . . . 2_565 ?
C5 N4 C4 C5 -0.1(7) . . . 2_565 ?
C6 N1 C7 C6 -0.6(7) . . . 2_575 ?
C8 N3 C9 C8 -0.8(7) . . . 2_566 ?
C7 N1 C6 C7 0.6(7) . . . 2_575 ?
C9 N3 C8 C9 0.8(7) . . . 2_566 ?
C10 N5 C11 C10 -0.2(8) . . . 2_574 ?
C11 N5 C10 C11 0.2(8) . . . 2_574 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.209
_oxdiff_exptl_absorpt_empirical_full_min 0.672
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.6022(9) 2924 2079 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.3978(9) 2942 2079 nmt -1.0004 0.0354 -0.0355 -0.0011 -0.0567 -0.9446 0.0020
-1.0575 0.0582

_twin_special_details            
;
Component 2 rotated by -179.9834° 
 around [0.03 0.67 -0.75] (reciprocal) or [-0.00 0.71 -0.71] (direct)
;
####################################################################### 
# 
# 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_lv195_wco3pyz2_cubic
_database_code_depnum_ccdc_archive 'CCDC 2063159'
loop_
_audit_author_name
_audit_author_address
'Laura Voigt'
;Department of Chemistry, Technical University of Denmark
Denmark
;
_audit_update_record             
;
2021-02-15 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_audit_creation_date             2020-10-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C9 H6 N3 O3 W1'
_chemical_formula_sum            'C9 H6 N3 O3 W'
_chemical_formula_weight         388.02
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W1 C9 H6 N3 O3'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y+1/4, -x+3/4, -z+1/4'
'-x, -y+1/2, z'
'-y+1/4, x+1/4, -z+3/4'
'-x+1/4, z+1/4, -y+3/4'
'x, -y, -z+1/2'
'-x+3/4, -z+1/4, y+1/4'
'-z+3/4, -y+1/4, x+1/4'
'-x+1/2, y, -z'
'z+1/4, -y+3/4, -x+1/4'
'z, x, y'
'y, z, x'
'-y, -z+1/2, x'
'z, -x, -y+1/2'
'-y+1/2, z, -x'
'-z, -x+1/2, y'
'-z+1/2, x, -y'
'y, -z, -x+1/2'
'-y+3/4, -x+1/4, z+1/4'
'y+1/4, x+1/4, z+1/4'
'x+1/4, -z+3/4, -y+1/4'
'x+1/4, z+1/4, y+1/4'
'-z+1/4, y+1/4, -x+3/4'
'z+1/4, y+1/4, x+1/4'
'x+1/2, y+1/2, z+1/2'
'y+3/4, -x+5/4, -z+3/4'
'-x+1/2, -y+1, z+1/2'
'-y+3/4, x+3/4, -z+5/4'
'-x+3/4, z+3/4, -y+5/4'
'x+1/2, -y+1/2, -z+1'
'-x+5/4, -z+3/4, y+3/4'
'-z+5/4, -y+3/4, x+3/4'
'-x+1, y+1/2, -z+1/2'
'z+3/4, -y+5/4, -x+3/4'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1, x+1/2'
'z+1/2, -x+1/2, -y+1'
'-y+1, z+1/2, -x+1/2'
'-z+1/2, -x+1, y+1/2'
'-z+1, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1'
'-y+5/4, -x+3/4, z+3/4'
'y+3/4, x+3/4, z+3/4'
'x+3/4, -z+5/4, -y+3/4'
'x+3/4, z+3/4, y+3/4'
'-z+3/4, y+3/4, -x+5/4'
'z+3/4, y+3/4, x+3/4'

_cell_length_a                   16.13834(17)
_cell_length_b                   16.13834(17)
_cell_length_c                   16.13834(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4203.17(13)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    8679
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.2520
_cell_measurement_theta_min      3.9620
_shelx_estimated_absorpt_T_max   0.096
_shelx_estimated_absorpt_T_min   0.096
_exptl_absorpt_coefficient_mu    10.987
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic yellowish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.453
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18475
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.691
_diffrn_reflns_theta_min         3.571
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00  87.00   1.00    5.00    --   10.87  77.00  60.00  109
  2  ω    -58.00  15.00   1.00    5.00    --   10.87 -38.00 120.00   73
  3  ω    -17.00  52.00   1.00    5.00    --   10.87 -99.00 -90.00   69
  4  ω    -12.00  52.00   1.00    5.00    --   10.87  38.00 -90.00   64
  5  ω     -7.00  22.00   1.00    5.00    --  -11.58 -99.00 -90.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0173202000
_diffrn_orient_matrix_UB_12      -0.0321911000
_diffrn_orient_matrix_UB_13      -0.0243597000
_diffrn_orient_matrix_UB_21      -0.0404012000
_diffrn_orient_matrix_UB_22      0.0138448000
_diffrn_orient_matrix_UB_23      0.0104149000
_diffrn_orient_matrix_UB_31      0.0000604000
_diffrn_orient_matrix_UB_32      0.0265217000
_diffrn_orient_matrix_UB_33      -0.0350666000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.950
_reflns_number_gt                874
_reflns_number_total             972
_reflns_odcompleteness_completeness 99.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 
;
 Flack x determined using 374 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.031(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         972
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0170
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0041P)²+5.8686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0238
_refine_ls_wR_factor_ref         0.0252
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.97579(2) 0.47579(2) 0.02421(2) 0.01045(7) Uani 1 3 d S T P . .
C3 C 0.9953(3) 0.4657(3) -0.0941(3) 0.0189(10) Uani 1 1 d . . . . .
N4 N 0.9882(2) 0.3369(2) 0.0417(2) 0.0123(8) Uani 1 1 d . . . . .
O2 O 1.0098(2) 0.4629(3) -0.16525(19) 0.0360(10) Uani 1 1 d . . . . .
C5 C 0.9252(3) 0.2833(3) 0.0433(3) 0.0185(10) Uani 1 1 d . . . . .
H5 H 0.871421 0.303913 0.044037 0.022 Uiso 1 1 calc R U . . .
C6 C 1.0635(3) 0.3011(3) 0.0438(3) 0.0201(10) Uani 1 1 d . . . . .
H6 H 1.109984 0.335031 0.045736 0.024 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C3 1.942(4) . ?
W1 C3 1.942(4) 41_545 ?
W1 C3 1.942(4) 42 ?
W1 N4 2.269(3) 42 ?
W1 N4 2.269(3) 41_545 ?
W1 N4 2.269(3) . ?
C3 O2 1.172(5) . ?
N4 C5 1.335(5) . ?
N4 C6 1.346(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.373(6) 3_755 ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 W1 C3 86.3(2) . 41_545 ?
C3 W1 C3 86.3(2) . 42 ?
C3 W1 C3 86.3(2) 41_545 42 ?
C3 W1 N4 93.63(17) . 42 ?
C3 W1 N4 177.80(15) 42 . ?
C3 W1 N4 177.80(15) 41_545 42 ?
C3 W1 N4 91.46(18) . . ?
C3 W1 N4 177.80(16) . 41_545 ?
C3 W1 N4 91.46(18) 42 42 ?
C3 W1 N4 93.63(17) 41_545 . ?
C3 W1 N4 93.63(17) 42 41_545 ?
C3 W1 N4 91.46(18) 41_545 41_545 ?
N4 W1 N4 88.57(13) 42 41_545 ?
N4 W1 N4 88.57(13) 41_545 . ?
N4 W1 N4 88.57(13) 42 . ?
O2 C3 W1 176.7(5) . . ?
C5 N4 W1 125.1(3) . . ?
C5 N4 C6 114.1(4) . . ?
C6 N4 W1 120.5(3) . . ?
N4 C5 H5 118.6 . . ?
N4 C5 C6 122.8(4) . 3_755 ?
C6 C5 H5 118.6 3_755 . ?
N4 C6 C5 123.0(4) . 3_755 ?
N4 C6 H6 118.5 . . ?
C5 C6 H6 118.5 3_755 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W1 N4 C5 C6 171.8(4) . . . 3_755 ?
W1 N4 C6 C5 -171.2(4) . . . 3_755 ?
C5 N4 C6 C5 3.2(6) . . . 3_755 ?
C6 N4 C5 C6 -2.3(5) . . . 3_755 ?

_olex2_date_sample_data_collection 2019-03-06
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.460
_oxdiff_exptl_absorpt_empirical_full_min 0.744
####################################################################### 
# 
# 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_lv194_moco3pyz2_b
_database_code_depnum_ccdc_archive 'CCDC 2063160'
loop_
_audit_author_name
_audit_author_address
'Laura Voigt'
;Department of Chemistry, Technical University of Denmark
Denmark
;
_audit_update_record             
;
2021-02-15 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_audit_creation_date             2020-10-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H6 Mo1 N3 O3'
_chemical_formula_sum            'C9 H6 Mo N3 O3'
_chemical_formula_weight         300.11
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mo C15 O3 H12 N6'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y+1/4, -x+3/4, -z+1/4'
'-x, -y+1/2, z'
'-y+1/4, x+1/4, -z+3/4'
'-x+1/4, z+1/4, -y+3/4'
'x, -y, -z+1/2'
'-x+3/4, -z+1/4, y+1/4'
'-z+3/4, -y+1/4, x+1/4'
'-x+1/2, y, -z'
'z+1/4, -y+3/4, -x+1/4'
'z, x, y'
'y, z, x'
'-y, -z+1/2, x'
'z, -x, -y+1/2'
'-y+1/2, z, -x'
'-z, -x+1/2, y'
'-z+1/2, x, -y'
'y, -z, -x+1/2'
'-y+3/4, -x+1/4, z+1/4'
'y+1/4, x+1/4, z+1/4'
'x+1/4, -z+3/4, -y+1/4'
'x+1/4, z+1/4, y+1/4'
'-z+1/4, y+1/4, -x+3/4'
'z+1/4, y+1/4, x+1/4'
'x+1/2, y+1/2, z+1/2'
'y+3/4, -x+5/4, -z+3/4'
'-x+1/2, -y+1, z+1/2'
'-y+3/4, x+3/4, -z+5/4'
'-x+3/4, z+3/4, -y+5/4'
'x+1/2, -y+1/2, -z+1'
'-x+5/4, -z+3/4, y+3/4'
'-z+5/4, -y+3/4, x+3/4'
'-x+1, y+1/2, -z+1/2'
'z+3/4, -y+5/4, -x+3/4'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1, x+1/2'
'z+1/2, -x+1/2, -y+1'
'-y+1, z+1/2, -x+1/2'
'-z+1/2, -x+1, y+1/2'
'-z+1, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1'
'-y+5/4, -x+3/4, z+3/4'
'y+3/4, x+3/4, z+3/4'
'x+3/4, -z+5/4, -y+3/4'
'x+3/4, z+3/4, y+3/4'
'-z+3/4, y+3/4, -x+5/4'
'z+3/4, y+3/4, x+3/4'

_cell_length_a                   16.2253(5)
_cell_length_b                   16.2253(5)
_cell_length_c                   16.2253(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4271.5(4)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    848
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.8410
_cell_measurement_theta_min      3.9570
_shelx_estimated_absorpt_T_max   0.711
_shelx_estimated_absorpt_T_min   0.711
_exptl_absorpt_coefficient_mu    1.222
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic yellowish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2352
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2128
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.079
_diffrn_reflns_theta_min         3.552
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00 -22.00   1.00   12.50    --  -11.58 -57.00 150.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0047128000
_diffrn_orient_matrix_UB_12      -0.0418993000
_diffrn_orient_matrix_UB_13      -0.0114934000
_diffrn_orient_matrix_UB_21      -0.0186584000
_diffrn_orient_matrix_UB_22      0.0084939000
_diffrn_orient_matrix_UB_23      -0.0386209000
_diffrn_orient_matrix_UB_31      0.0392404000
_diffrn_orient_matrix_UB_32      0.0090717000
_diffrn_orient_matrix_UB_33      -0.0170095000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.675
_reflns_Friedel_fraction_full    0.856
_reflns_Friedel_fraction_max     0.832
_reflns_number_gt                622
_reflns_number_total             727
_reflns_odcompleteness_completeness 99.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 
;
 Flack x determined using 229 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         727
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0305
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0074P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0546
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.97640(3) 0.47640(3) 0.02360(3) 0.0110(2) Uani 1 3 d S T P . .
C3 C 0.9679(4) 0.5940(3) 0.0039(4) 0.0182(14) Uani 1 1 d . . . . .
O2 O 0.9665(3) 0.6642(3) -0.0107(3) 0.0338(13) Uani 1 1 d . . . . .
N4 N 0.9600(3) 0.4888(3) 0.1635(3) 0.0115(11) Uani 1 1 d . . . . .
C5 C 0.9589(4) 0.4260(4) 0.2167(4) 0.0187(14) Uani 1 1 d . . . . .
H5 H 0.958346 0.372488 0.196077 0.022 Uiso 1 1 calc R U . . .
C6 C 0.9587(4) 0.5629(4) 0.1993(4) 0.0217(16) Uani 1 1 d . . . . .
H6 H 0.957477 0.609278 0.165724 0.026 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C3 1.939(5) 42 ?
Mo1 C3 1.939(5) 41_545 ?
Mo1 C3 1.939(5) . ?
Mo1 N4 2.295(4) . ?
Mo1 N4 2.295(4) 41_545 ?
Mo1 N4 2.295(4) 42 ?
C3 O2 1.164(6) . ?
N4 C5 1.335(8) . ?
N4 C6 1.335(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.374(8) 6_565 ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Mo1 C3 85.4(3) 42 41_545 ?
C3 Mo1 C3 85.4(3) 42 . ?
C3 Mo1 C3 85.4(3) 41_545 . ?
C3 Mo1 N4 91.7(2) 42 . ?
C3 Mo1 N4 177.0(2) . 42 ?
C3 Mo1 N4 177.0(2) 41_545 . ?
C3 Mo1 N4 93.9(2) 42 42 ?
C3 Mo1 N4 177.0(2) 42 41_545 ?
C3 Mo1 N4 93.9(2) . . ?
C3 Mo1 N4 91.7(2) 41_545 42 ?
C3 Mo1 N4 91.7(2) . 41_545 ?
C3 Mo1 N4 93.9(2) 41_545 41_545 ?
N4 Mo1 N4 88.97(18) . 41_545 ?
N4 Mo1 N4 88.97(18) 41_545 42 ?
N4 Mo1 N4 88.97(18) . 42 ?
O2 C3 Mo1 176.3(6) . . ?
C5 N4 Mo1 125.0(4) . . ?
C5 N4 C6 114.0(5) . . ?
C6 N4 Mo1 120.7(4) . . ?
N4 C5 H5 118.7 . . ?
N4 C5 C6 122.7(5) . 6_565 ?
C6 C5 H5 118.7 6_565 . ?
N4 C6 C5 123.4(6) . 6_565 ?
N4 C6 H6 118.3 . . ?
C5 C6 H6 118.3 6_565 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 N4 C5 C6 172.1(6) . . . 6_565 ?
Mo1 N4 C6 C5 -172.0(5) . . . 6_565 ?
C5 N4 C6 C5 2.1(9) . . . 6_565 ?
C6 N4 C5 C6 -1.6(7) . . . 6_565 ?

_olex2_date_sample_data_collection 2019-03-04
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.063
_oxdiff_exptl_absorpt_empirical_full_min 0.954
####################################################################### 
# 
# 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_lv382_crco3pyz_cubic_b
_database_code_depnum_ccdc_archive 'CCDC 2063157'
loop_
_audit_author_name
_audit_author_address
'Laura Voigt'
;Department of Chemistry, Technical University of Denmark
Denmark
;
_audit_update_record             
;
2021-02-15 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_audit_creation_date             2020-10-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H6 Cr1 N3 O3'
_chemical_formula_sum            'C9 H6 Cr N3 O3'
_chemical_formula_weight         256.17
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cr C9 H6 O3 N3'
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'
Cr Cr 0.3209 0.6236 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y+1/4, -x+3/4, -z+1/4'
'-x, -y+1/2, z'
'-y+1/4, x+1/4, -z+3/4'
'-x+1/4, z+1/4, -y+3/4'
'x, -y, -z+1/2'
'-x+3/4, -z+1/4, y+1/4'
'-z+3/4, -y+1/4, x+1/4'
'-x+1/2, y, -z'
'z+1/4, -y+3/4, -x+1/4'
'z, x, y'
'y, z, x'
'-y, -z+1/2, x'
'z, -x, -y+1/2'
'-y+1/2, z, -x'
'-z, -x+1/2, y'
'-z+1/2, x, -y'
'y, -z, -x+1/2'
'-y+3/4, -x+1/4, z+1/4'
'y+1/4, x+1/4, z+1/4'
'x+1/4, -z+3/4, -y+1/4'
'x+1/4, z+1/4, y+1/4'
'-z+1/4, y+1/4, -x+3/4'
'z+1/4, y+1/4, x+1/4'
'x+1/2, y+1/2, z+1/2'
'y+3/4, -x+5/4, -z+3/4'
'-x+1/2, -y+1, z+1/2'
'-y+3/4, x+3/4, -z+5/4'
'-x+3/4, z+3/4, -y+5/4'
'x+1/2, -y+1/2, -z+1'
'-x+5/4, -z+3/4, y+3/4'
'-z+5/4, -y+3/4, x+3/4'
'-x+1, y+1/2, -z+1/2'
'z+3/4, -y+5/4, -x+3/4'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1, x+1/2'
'z+1/2, -x+1/2, -y+1'
'-y+1, z+1/2, -x+1/2'
'-z+1/2, -x+1, y+1/2'
'-z+1, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1'
'-y+5/4, -x+3/4, z+3/4'
'y+3/4, x+3/4, z+3/4'
'x+3/4, -z+5/4, -y+3/4'
'x+3/4, z+3/4, y+3/4'
'-z+3/4, y+3/4, -x+5/4'
'z+3/4, y+3/4, x+3/4'

_cell_length_a                   15.8757(6)
_cell_length_b                   15.8757(6)
_cell_length_c                   15.8757(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4001.3(5)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    852
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      27.1330
_cell_measurement_theta_min      4.0530
_shelx_estimated_absorpt_T_max   0.727
_shelx_estimated_absorpt_T_min   0.727
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic yellowish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1916
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.211
_diffrn_reflns_theta_min         3.630
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -34.00   5.00   1.00   35.00    --   10.87 -77.00-150.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0085667000
_diffrn_orient_matrix_UB_12      0.0314339000
_diffrn_orient_matrix_UB_13      0.0305782000
_diffrn_orient_matrix_UB_21      -0.0193433000
_diffrn_orient_matrix_UB_22      0.0252534000
_diffrn_orient_matrix_UB_23      -0.0313864000
_diffrn_orient_matrix_UB_31      -0.0393221000
_diffrn_orient_matrix_UB_32      -0.0192445000
_diffrn_orient_matrix_UB_33      0.0088549000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.646
_reflns_Friedel_fraction_full    0.852
_reflns_Friedel_fraction_max     0.775
_reflns_number_gt                669
_reflns_number_total             739
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 
;
 Flack x determined using 238 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         739
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0359
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0274P)²+3.7015P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0766
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.97362(4) 0.47362(4) 0.02638(4) 0.0113(3) Uani 1 3 d S T P . .
N2 N 0.83857(19) 0.4597(2) 0.0127(2) 0.0131(7) Uani 1 1 d . . . . .
C6 C 0.9657(3) 0.5868(2) 0.0065(3) 0.0166(8) Uani 1 1 d . . . . .
O5 O 0.9666(2) 0.65789(18) -0.0104(2) 0.0304(8) Uani 1 1 d . . . . .
C3 C 0.7835(3) 0.4590(3) 0.0757(3) 0.0192(9) Uani 1 1 d . . . . .
H3 H 0.805(3) 0.458(3) 0.127(3) 0.023 Uiso 1 1 d . U . . .
C4 C 0.8028(3) 0.4584(3) -0.0641(3) 0.0210(10) Uani 1 1 d . . . . .
H4 H 0.843(3) 0.456(3) -0.111(3) 0.025 Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 N2 2.166(3) . ?
Cr1 N2 2.166(3) 42 ?
Cr1 N2 2.166(3) 41_545 ?
Cr1 C6 1.828(4) 42 ?
Cr1 C6 1.828(4) . ?
Cr1 C6 1.828(4) 41_545 ?
N2 C3 1.327(5) . ?
N2 C4 1.346(5) . ?
C6 O5 1.160(5) . ?
C3 H3 0.88(5) . ?
C3 C4 1.382(6) 9_655 ?
C4 H4 0.99(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cr1 N2 90.47(13) 42 41_545 ?
N2 Cr1 N2 90.47(13) . 42 ?
N2 Cr1 N2 90.47(13) . 41_545 ?
C6 Cr1 N2 90.87(17) . . ?
C6 Cr1 N2 175.56(17) . 41_545 ?
C6 Cr1 N2 175.56(17) 41_545 42 ?
C6 Cr1 N2 175.56(17) 42 . ?
C6 Cr1 N2 90.87(17) 42 42 ?
C6 Cr1 N2 93.76(16) . 42 ?
C6 Cr1 N2 93.76(16) 42 41_545 ?
C6 Cr1 N2 93.76(16) 41_545 . ?
C6 Cr1 N2 90.87(17) 41_545 41_545 ?
C6 Cr1 C6 84.8(2) 41_545 . ?
C6 Cr1 C6 84.8(2) 42 . ?
C6 Cr1 C6 84.8(2) 42 41_545 ?
C3 N2 Cr1 125.3(3) . . ?
C3 N2 C4 113.8(3) . . ?
C4 N2 Cr1 120.6(3) . . ?
O5 C6 Cr1 174.3(4) . . ?
N2 C3 H3 116(3) . . ?
N2 C3 C4 123.6(4) . 9_655 ?
C4 C3 H3 121(3) 9_655 . ?
N2 C4 C3 122.6(4) . 9_655 ?
N2 C4 H4 115(3) . . ?
C3 C4 H4 123(3) 9_655 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr1 N2 C3 C4 173.3(4) . . . 9_655 ?
Cr1 N2 C4 C3 -172.7(3) . . . 9_655 ?
C3 N2 C4 C3 1.9(6) . . . 9_655 ?
C4 N2 C3 C4 -0.9(5) . . . 9_655 ?

_olex2_date_sample_data_collection 2020-10-05
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.028
_oxdiff_exptl_absorpt_empirical_full_min 0.972
####################################################################### 
# 
# 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_lv_wco3pyz_aferrevacat150degrees_120k
_database_code_depnum_ccdc_archive 'CCDC 2063161'
loop_
_audit_author_name
_audit_author_address
'Laura Voigt'
;Department of Chemistry, Technical University of Denmark
Denmark
;
_audit_update_record             
;
2021-02-15 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_audit_creation_date             2021-01-26
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H6 N3 O3 W'
_chemical_formula_sum            'C9 H6 N3 O3 W'
_chemical_formula_weight         388.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         'W C9 N3 H6 O3'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   17.8974(7)
_cell_length_b                   9.9861(5)
_cell_length_c                   6.7067(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.482(4)
_cell_angle_gamma                90
_cell_volume                     1198.61(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3812
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.7990
_cell_measurement_theta_min      4.5440
_shelx_estimated_absorpt_T_max   0.644
_shelx_estimated_absorpt_T_min   0.249
_exptl_absorpt_coefficient_mu    9.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.150
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5042
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         3.781
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  82.00   1.00   20.00    --   10.87  38.00 150.00   96
  2  ω    -69.00  31.00   1.00   20.00    --   10.87 -19.00 -30.00  100
  3  ω      3.00  52.00   1.00   20.00    --   10.87 -99.00-120.00   49
  4  ω      3.00  30.00   1.00   20.00    --   10.87 -38.00-120.00   27
  5  ω    -20.00  28.00   1.00   20.00    --  -11.58 -99.00 -60.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0022860000
_diffrn_orient_matrix_UB_12      0.0643413000
_diffrn_orient_matrix_UB_13      -0.0444418000
_diffrn_orient_matrix_UB_21      0.0070011000
_diffrn_orient_matrix_UB_22      0.0288264000
_diffrn_orient_matrix_UB_23      0.0950104000
_diffrn_orient_matrix_UB_31      0.0389378000
_diffrn_orient_matrix_UB_32      -0.0090077000
_diffrn_orient_matrix_UB_33      -0.0135394000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1385
_reflns_number_total             1392
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.287
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1392
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0215
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0199P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0422
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N1-C4
 1.345 with sigma of 0.02
 N2-C8
 1.345 with sigma of 0.02
 N2-C10
 1.345 with sigma of 0.02
 N1-C3
 1.345 with sigma of 0.02
 C7-N2 \\sim N2-C9
 with sigma of 0.02
 C9-N2 \\sim N2-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N2 \\sim C8 \\sim C10: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
N2 \\sim C7 \\sim C9: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4A) \\sim Ueq, Uanis(C3A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Sof(C4A)=Sof(H4A)=Sof(C3A)=Sof(H3A)=1-FVAR(1)
 Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=FVAR(1)
 Fixed Sof: C7(0.16667) H7(0.16667) C8(0.33333) C9(0.16667) H9(0.16667)
 C10(0.33333) H8(0.33333) H10(0.33333)
 Fixed Uiso: H8(0.024) H10(0.024)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C9(H9), C4A(H4A), C3A(H3A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.33485(2) 1.000000 0.67255(2) 0.01504(8) Uani 1 2 d S T P A .
O1 O 0.40592(15) 1.2213(3) 0.4070(5) 0.0410(8) Uani 1 1 d . . . . .
C1 C 0.37943(18) 1.1373(4) 0.5048(5) 0.0205(8) Uani 1 1 d . . . . .
C2 C 0.2470(3) 1.000000 0.4995(8) 0.0271(13) Uani 1 2 d S T P . .
O2 O 0.1942(2) 1.000000 0.3959(8) 0.0606(15) Uani 1 2 d S T P . .
N1 N 0.28364(15) 1.1527(3) 0.8769(4) 0.0219(7) Uani 1 1 d D . . . .
C3 C 0.3208(3) 1.2530(8) 0.9570(11) 0.047(2) Uani 0.660(6) 1 d D . P A 1
H3 H 0.371349 1.261299 0.928779 0.056 Uiso 0.660(6) 1 calc R U P A 1
C4 C 0.2114(3) 1.1534(8) 0.9195(11) 0.051(2) Uani 0.660(6) 1 d D . P A 1
H4 H 0.181023 1.087675 0.863386 0.061 Uiso 0.660(6) 1 calc R U P A 1
N2 N 0.4348(2) 1.000000 0.8788(6) 0.0196(9) Uani 1 2 d DS TU P . .
C7 C 0.5037(7) 1.000000 0.804(2) 0.020(3) Uani 0.3333 2 d DS TU P A 1
H7 H 0.509037 1.000000 0.665704 0.024 Uiso 0.3333 2 calc R U P A 1
C8 C 0.4832(6) 1.1054(12) 0.8870(17) 0.023(2) Uani 0.3333 1 d D U P A 2
C9 C 0.4337(8) 1.000000 1.0809(18) 0.020(3) Uani 0.3333 2 d DS TU P A 1
H9 H 0.387517 1.000000 1.143593 0.024 Uiso 0.3333 2 calc R U P A 1
C10 C 0.4544(6) 0.8966(12) 0.9939(17) 0.023(2) Uani 0.3333 1 d D U P A 2
C4A C 0.2825(6) 1.1439(12) 1.0779(16) 0.026(3) Uani 0.340(6) 1 d . U P A 2
H4A H 0.305911 1.071301 1.138823 0.031 Uiso 0.340(6) 1 calc R U P A 2
C3A C 0.2518(6) 1.2626(12) 0.8038(16) 0.026(3) Uani 0.340(6) 1 d . U P A 2
H3A H 0.252836 1.276782 0.666778 0.032 Uiso 0.340(6) 1 calc R U P A 2
H8 H 0.479(6) 1.180(13) 0.809(17) 0.024 Uiso 0.3333 1 d . U P . .
H10 H 0.419(6) 0.817(13) 1.003(17) 0.024 Uiso 0.3333 1 d . U 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
W1 C1 1.949(4) 6_575 ?
W1 C1 1.949(4) . ?
W1 C2 1.947(5) . ?
W1 N1 2.251(3) . ?
W1 N1 2.251(3) 6_575 ?
W1 N2 2.253(4) . ?
O1 C1 1.167(4) . ?
C2 O2 1.169(7) . ?
N1 C3 1.314(7) . ?
N1 C4 1.327(6) . ?
N1 C4A 1.352(11) . ?
N1 C3A 1.328(12) . ?
C3 H3 0.9300 . ?
C3 C4 1.378(9) 7_577 ?
C4 H4 0.9300 . ?
N2 C7 1.337(12) . ?
N2 C8 1.364(10) . ?
N2 C8 1.364(10) 6_575 ?
N2 C9 1.355(12) . ?
N2 C10 1.334(11) . ?
N2 C10 1.334(11) 6_575 ?
C7 H7 0.9300 . ?
C7 C9 1.36(2) 5_677 ?
C8 C10 1.368(14) 5_677 ?
C8 C10 0.887(13) 6_575 ?
C8 H8 0.91(12) . ?
C9 H9 0.9300 . ?
C10 H10 1.01(12) . ?
C4A H4A 0.9300 . ?
C4A C3A 1.374(15) 7_577 ?
C3A H3A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W1 C1 89.4(2) . 6_575 ?
C1 W1 N1 177.65(12) 6_575 . ?
C1 W1 N1 92.61(14) 6_575 6_575 ?
C1 W1 N1 92.61(14) . . ?
C1 W1 N1 177.65(13) . 6_575 ?
C1 W1 N2 91.58(12) . . ?
C1 W1 N2 91.58(12) 6_575 . ?
C2 W1 C1 89.33(15) . . ?
C2 W1 C1 89.33(15) . 6_575 ?
C2 W1 N1 91.83(13) . 6_575 ?
C2 W1 N1 91.84(13) . . ?
C2 W1 N2 178.72(16) . . ?
N1 W1 N1 85.31(16) . 6_575 ?
N1 W1 N2 87.22(10) . . ?
N1 W1 N2 87.22(10) 6_575 . ?
O1 C1 W1 178.8(3) . . ?
O2 C2 W1 179.9(5) . . ?
C3 N1 W1 123.9(3) . . ?
C3 N1 C4 113.5(4) . . ?
C4 N1 W1 122.5(3) . . ?
C4A N1 W1 125.0(5) . . ?
C3A N1 W1 120.7(5) . . ?
C3A N1 C4A 114.3(7) . . ?
N1 C3 H3 118.3 . . ?
N1 C3 C4 123.4(5) . 7_577 ?
C4 C3 H3 118.3 7_577 . ?
N1 C4 C3 123.1(5) . 7_577 ?
N1 C4 H4 118.4 . . ?
C3 C4 H4 118.4 7_577 . ?
C7 N2 W1 119.9(6) . . ?
C7 N2 C8 55.1(6) . 6_575 ?
C7 N2 C9 113.6(9) . . ?
C8 N2 W1 121.7(5) . . ?
C8 N2 W1 121.7(5) 6_575 . ?
C9 N2 W1 126.5(6) . . ?
C9 N2 C8 88.6(7) . 6_575 ?
C10 N2 W1 124.0(5) 6_575 . ?
C10 N2 W1 124.0(5) . . ?
C10 N2 C8 38.4(6) 6_575 . ?
C10 N2 C8 114.3(7) . . ?
C10 N2 C10 101.4(11) 6_575 . ?
N2 C7 H7 118.5 . . ?
N2 C7 C9 123.0(11) . 5_677 ?
C9 C7 H7 118.5 5_677 . ?
N2 C8 C10 121.8(10) . 5_677 ?
N2 C8 H8 124(7) . . ?
C10 C8 N2 69.0(10) 6_575 . ?
C10 C8 H8 114(7) 5_677 . ?
C10 C8 H8 116(7) 6_575 . ?
N2 C9 C7 123.5(11) . 5_677 ?
N2 C9 H9 118.3 . . ?
C7 C9 H9 118.3 5_677 . ?
N2 C10 C8 123.9(10) . 5_677 ?
N2 C10 H10 119(7) . . ?
C8 C10 H10 117(7) 5_677 . ?
N1 C4A H4A 118.6 . . ?
N1 C4A C3A 122.8(10) . 7_577 ?
C3A C4A H4A 118.6 7_577 . ?
N1 C3A C4A 122.7(10) . 7_577 ?
N1 C3A H3A 118.6 . . ?
C4A C3A H3A 118.6 7_577 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W1 N1 C3 C4 179.4(6) . . . 7_577 ?
W1 N1 C4 C3 -179.5(6) . . . 7_577 ?
W1 N1 C4A C3A -177.6(8) . . . 7_577 ?
W1 N1 C3A C4A 177.6(8) . . . 7_577 ?
W1 N2 C7 C9 180.000(2) . . . 5_677 ?
W1 N2 C8 C10 -177.3(10) . . . 5_677 ?
W1 N2 C8 C10 106.1(10) . . . 6_575 ?
W1 N2 C9 C7 180.000(3) . . . 5_677 ?
W1 N2 C10 C8 177.2(11) . . . 5_677 ?
C3 N1 C4 C3 -2.7(12) . . . 7_577 ?
C4 N1 C3 C4 2.7(12) . . . 7_577 ?
C7 N2 C9 C7 0.000(4) . . . 5_677 ?
C8 N2 C8 C10 -38.7(19) 6_575 . . 5_677 ?
C8 N2 C8 C10 -115.3(12) 6_575 . . 6_575 ?
C8 N2 C10 C8 77.5(14) 6_575 . . 5_677 ?
C8 N2 C10 C8 1(2) . . . 5_677 ?
C9 N2 C7 C9 0.000(3) . . . 5_677 ?
C10 N2 C8 C10 -1(2) . . . 5_677 ?
C10 N2 C8 C10 76.6(14) 6_575 . . 5_677 ?
C10 N2 C8 C10 -77.3(15) . . . 6_575 ?
C10 N2 C10 C8 -37.4(19) 6_575 . . 5_677 ?
C4A N1 C3A C4A -3.0(16) . . . 7_577 ?
C3A N1 C4A C3A 3.0(16) . . . 7_577 ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 78 electrons were 
found in a volume of 216 A³ in 1 void per unit cell. 
This is consistent with the presence of 
0.25[C4H4N2] per Asymmetric Unit 
which account for 84 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.325 107.8 38.9 '1 C4H4N2'
2 0.500 0.500 -0.630 107.8 38.9 '1 C4H4N2'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.152
_oxdiff_exptl_absorpt_empirical_full_min 0.906
