# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_aj1-bpy0p5HxWO3
_database_code_depnum_ccdc_archive 'CCDC 2282208'
loop_
_audit_author_name
_audit_author_address
'Adam Jaffe'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2023-07-18 deposited with the CCDC.	2023-09-13 downloaded from the CCDC.
;
_audit_creation_method           
;FinalCif V123 by Daniel Kratzert, Freiburg 2023, 
https://dkratzert.de/finalcif.html
;
_audit_creation_date             2023-07-14
_diffrn_source_power             1.75
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: O2(0.25) C1(0.25) H1(0.25) C2(0.25) H2(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C5 H4 N O3 W'
_chemical_formula_moiety         'C5 H4 N O3 W'
_chemical_formula_weight         309.94
_chemical_melting_point          ?
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
_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.
;
_vrf_PLAT430_aj1-bpy0p5HxWO3     
;PROBLEM: Short Inter D...A Contact  O2       ..O2       .       2.20 Ang.  
RESPONSE: These oxygen atoms are disordered by symmetry which erroneously leads 
to a short contact distance error.
;

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

_cell_length_a                   5.2532(3)
_cell_length_b                   5.2532(3)
_cell_length_c                   22.6462(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     624.95(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    120.02
_cell_measurement_reflns_used    5596
_cell_measurement_theta_min      3.599
_cell_measurement_theta_max      28.262
_exptl_crystal_description       plate
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_recrystallization_method 
'Hydrothermal reaction at 170C for 6 h followed by cooling at 1 degree per minute to 70C.'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.294
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.016
_exptl_absorpt_coefficient_mu    18.419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4277
_exptl_absorpt_correction_T_max  0.6035
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1050 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.7087.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   0.304
_shelx_estimated_absorpt_T_max   0.757
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           
;
X-ray diffraction analyses were performed on single crystals coated with
 Paratone-N oil and mounted on MiTeGen loops. Crystals were frozen at a
 temperature of 120 K by an Oxford Cryosystems Cryostream using N₂ during
 the experiments. Data was collected at the Molecular Structure Facility
 at the University of Notre Dame using Mo k-alpha
 radiation (lamda = 0.71073 angstrom) on a Bruker Duo equipped with a
 Bruker PHOTON II detector.
;
_diffrn_ambient_temperature      120.02
_diffrn_ambient_environment      ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Bruker TRIUMPH curved-graphite'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryosteam 700'
_diffrn_radiation_probe          ?
_diffrn_source                   X-ray
_diffrn_source_type              ?
_diffrn_source_voltage           50.0
_diffrn_source_current           35.0
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_type            'Bruker PHOTON-II'
_diffrn_detector_area_resol_mean 7.41
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       'combination of ω and φ-scans'
_diffrn_measurement_specimen_support ?
_diffrn_reflns_number            7816
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_theta_min         1.798
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_standards_number         0
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             272
_reflns_number_gt                251
_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 APEX-4 (Bruker, 2021)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2021)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2021)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2015b)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2020)'
_computing_publication_material  
'FinalCIF (Kratzert, 2023)/CIFTAB (Sheldrick, 2008)'
_refine_special_details          
;
Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the 
riding model. The structure features inorganic layers comprised of WO5N 
octahedra. These layers are pillared by 4,4'-bipy molecules. The inorganic 
layers have been chemically reduced in situ with W metal with protons 
providing charge balance. These protons were not located or refined.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0161P)²+2.5070P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         272
_refine_ls_number_parameters     30
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0160
_refine_ls_R_factor_gt           0.0128
_refine_ls_wR_factor_ref         0.0327
_refine_ls_wR_factor_gt          0.0323
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_restrained_S_all      1.229
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.258
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

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'

_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_
_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 0.500000 0.500000 0.23618(2) 0.00677(12) Uani 1 8 d S T P . .
O1 O 0.500000 0.500000 0.1610(3) 0.0084(12) Uani 1 8 d S T P . .
O2 O 0.7090(6) 0.7910(6) 0.250000 0.0081(16) Uani 0.5 2 d S T P . .
C3 C 0.500000 0.500000 0.4667(4) 0.0103(18) Uani 1 8 d S T P . .
N1 N 0.500000 0.500000 0.3425(3) 0.0112(15) Uani 1 8 d S T P . .
C1 C 0.2793(15) 0.500000 0.3735(4) 0.0097(16) Uani 0.5 2 d S T P . .
H1 H 0.122831 0.500000 0.352449 0.012 Uiso 0.5 2 calc R U P . .
C2 C 0.2731(17) 0.500000 0.4345(4) 0.0140(18) Uani 0.5 2 d S T P . .
H2 H 0.114318 0.500000 0.454636 0.017 Uiso 0.5 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.00737(13) 0.00737(13) 0.00559(17) 0.000 0.000 0.000
O1 0.0082(17) 0.0082(17) 0.009(3) 0.000 0.000 0.000
O2 0.010(3) 0.010(3) 0.005(2) 0.0010(13) 0.0010(13) -0.003(3)
C3 0.014(3) 0.014(3) 0.002(4) 0.000 0.000 0.000
N1 0.013(2) 0.013(2) 0.008(4) 0.000 0.000 0.000
C1 0.008(4) 0.017(4) 0.004(4) 0.000 -0.002(3) 0.000
C2 0.008(4) 0.024(4) 0.010(4) 0.000 0.003(3) 0.000

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 O1 1.702(6) . ?
W1 O2 1.9079(8) 2_665 ?
W1 O2 1.9079(8) 28_645 ?
W1 O2 1.9079(8) 24 ?
W1 O2 1.9079(8) 27_465 ?
W1 O2 1.9079(8) . ?
W1 O2 1.9079(8) 3_655 ?
W1 O2 1.9079(8) 26_445 ?
W1 O2 1.9079(8) 4_565 ?
W1 N1 2.407(7) . ?
C3 C3 1.510(17) 17_666 ?
C3 C2 1.397(9) 4_565 ?
C3 C2 1.397(9) 3_655 ?
C3 C2 1.397(9) 2_665 ?
C3 C2 1.397(9) . ?
C3 C2 1.397(9) 23_665 ?
C3 C2 1.397(9) 24 ?
N1 C1 1.355(9) 2_665 ?
N1 C1 1.355(9) 3_655 ?
N1 C1 1.355(9) . ?
N1 C1 1.355(9) 23_665 ?
N1 C1 1.355(9) 4_565 ?
N1 C1 1.355(9) 24 ?
C1 H1 0.9500 . ?
C1 C2 1.383(11) . ?
C2 H2 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
O1 W1 O2 99.441(11) . 24 ?
O1 W1 O2 99.441(11) . 4_565 ?
O1 W1 O2 99.441(11) . 28_645 ?
O1 W1 O2 99.441(11) . . ?
O1 W1 O2 99.441(11) . 3_655 ?
O1 W1 O2 99.441(11) . 26_445 ?
O1 W1 O2 99.441(11) . 2_665 ?
O1 W1 O2 99.441(11) . 27_465 ?
O1 W1 N1 180.0 . . ?
O2 W1 O2 88.459(4) . 3_655 ?
O2 W1 O2 161.12(2) 27_465 28_645 ?
O2 W1 O2 161.12(2) 4_565 3_655 ?
O2 W1 O2 88.458(3) 26_445 28_645 ?
O2 W1 O2 18.4(3) 27_465 3_655 ?
O2 W1 O2 18.4(3) 24 . ?
O2 W1 O2 70.3(3) 24 4_565 ?
O2 W1 O2 161.12(2) 24 26_445 ?
O2 W1 O2 106.5(3) 26_445 4_565 ?
O2 W1 O2 70.3(3) 2_665 28_645 ?
O2 W1 O2 153.5(2) 27_465 4_565 ?
O2 W1 O2 153.55(19) 24 2_665 ?
O2 W1 O2 153.5(2) . 26_445 ?
O2 W1 O2 88.458(3) . 4_565 ?
O2 W1 O2 88.458(4) 24 27_465 ?
O2 W1 O2 88.458(4) 2_665 4_565 ?
O2 W1 O2 70.3(3) . 27_465 ?
O2 W1 O2 18.4(3) 28_645 4_565 ?
O2 W1 O2 88.458(4) 26_445 27_465 ?
O2 W1 O2 106.5(3) 24 3_655 ?
O2 W1 O2 106.5(3) 2_665 27_465 ?
O2 W1 O2 70.3(3) 26_445 3_655 ?
O2 W1 O2 161.12(2) . 2_665 ?
O2 W1 O2 153.5(2) 28_645 3_655 ?
O2 W1 O2 88.459(4) 24 28_645 ?
O2 W1 O2 18.4(3) 26_445 2_665 ?
O2 W1 O2 106.5(3) . 28_645 ?
O2 W1 O2 88.458(3) 2_665 3_655 ?
O2 W1 N1 80.559(11) 24 . ?
O2 W1 N1 80.559(11) 27_465 . ?
O2 W1 N1 80.559(11) 3_655 . ?
O2 W1 N1 80.559(11) . . ?
O2 W1 N1 80.559(11) 28_645 . ?
O2 W1 N1 80.559(11) 26_445 . ?
O2 W1 N1 80.559(11) 2_665 . ?
O2 W1 N1 80.559(11) 4_565 . ?
W1 O2 W1 161.6(3) 25_665 . ?
C2 C3 C3 121.4(4) . 17_666 ?
C2 C3 C3 121.4(4) 3_655 17_666 ?
C2 C3 C3 121.4(4) 23_665 17_666 ?
C2 C3 C3 121.4(4) 24 17_666 ?
C2 C3 C3 121.4(4) 2_665 17_666 ?
C2 C3 C3 121.4(4) 4_565 17_666 ?
C2 C3 C2 74.3(4) . 4_565 ?
C2 C3 C2 117.2(9) 3_655 23_665 ?
C2 C3 C2 74.3(4) 23_665 2_665 ?
C2 C3 C2 117.2(9) 24 4_565 ?
C2 C3 C2 0.0(7) 3_655 24 ?
C2 C3 C2 0.0(7) 23_665 4_565 ?
C2 C3 C2 74.3(4) 4_565 2_665 ?
C2 C3 C2 74.3(4) 3_655 2_665 ?
C2 C3 C2 74.3(4) . 23_665 ?
C2 C3 C2 117.2(9) . 2_665 ?
C2 C3 C2 74.3(4) . 24 ?
C2 C3 C2 74.3(4) 24 2_665 ?
C2 C3 C2 117.2(9) 24 23_665 ?
C2 C3 C2 117.2(9) 3_655 4_565 ?
C2 C3 C2 74.3(4) 3_655 . ?
C1 N1 W1 121.2(4) 4_565 . ?
C1 N1 W1 121.2(4) 3_655 . ?
C1 N1 W1 121.2(4) . . ?
C1 N1 W1 121.2(4) 24 . ?
C1 N1 W1 121.2(4) 2_665 . ?
C1 N1 W1 121.2(4) 23_665 . ?
C1 N1 C1 74.4(4) 2_665 24 ?
C1 N1 C1 74.4(4) 2_665 4_565 ?
C1 N1 C1 117.6(9) 4_565 3_655 ?
C1 N1 C1 0.0(6) 23_665 4_565 ?
C1 N1 C1 117.6(9) 23_665 3_655 ?
C1 N1 C1 117.6(9) 2_665 . ?
C1 N1 C1 0.0(7) 24 3_655 ?
C1 N1 C1 74.4(4) 2_665 23_665 ?
C1 N1 C1 74.4(4) 2_665 3_655 ?
C1 N1 C1 117.6(9) 23_665 24 ?
C1 N1 C1 74.4(4) 23_665 . ?
C1 N1 C1 117.6(9) 4_565 24 ?
C1 N1 C1 74.4(4) 4_565 . ?
C1 N1 C1 74.4(4) . 24 ?
C1 N1 C1 74.4(4) . 3_655 ?
N1 C1 H1 118.7 . . ?
N1 C1 C2 122.6(7) . . ?
C2 C1 H1 118.7 . . ?
C3 C2 H2 120.0 . . ?
C1 C2 C3 120.0(7) . . ?
C1 C2 H2 120.0 . . ?

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 C1 C2 180.000(3) . . . . ?
C3 C3 C2 C1 180.000(2) 17_666 . . . ?
N1 C1 C2 C3 0.000(3) . . . . ?
C1 N1 C1 C2 0.000(3) 2_665 . . . ?
C1 N1 C1 C2 -62.6(3) 23_665 . . . ?
C1 N1 C1 C2 -62.6(3) 4_565 . . . ?
C1 N1 C1 C2 62.6(3) 24 . . . ?
C1 N1 C1 C2 62.6(3) 3_655 . . . ?
C2 C3 C2 C1 -62.5(3) 24 . . . ?
C2 C3 C2 C1 62.5(3) 4_565 . . . ?
C2 C3 C2 C1 0.000(3) 2_665 . . . ?
C2 C3 C2 C1 -62.5(3) 3_655 . . . ?
C2 C3 C2 C1 62.5(3) 23_665 . . . ?

_shelx_res_file                  
;
TITL aj1_a.res in I4/mmm
    aj1.res
    created by SHELXL-2018/3 at 17:20:52 on 14-Jul-2023
REM Old TITL AJ1 in I4/mmm
REM SHELXT solution in I4/mmm: R1 0.099, Rweak 0.011, Alpha 0.013
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C2 N O W
CELL 0.71073 5.2532 5.2532 22.6462 90 90 90
ZERR 4 0.0003 0.0003 0.0016 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SFAC C H N O W
UNIT 20 16 4 12 4
EQIV $1 +Y,+X,+Z
EQIV $2 +Y,1-X,+Z
EQIV $3 1-Y,+X,+Z
EQIV $4 1-Y,1-X,+Z
EQIV $5 -0.5+X,0.5+Y,0.5-Z

L.S. 20
PLAN  5
SIZE 0.016 0.074 0.085
TEMP -153.13
CONF
FREE C2 C2_$1
FREE C2 C2_$2
FREE C2 C2_$3
FREE C2 C2_$4
FREE C1 C1_$1
FREE C1 C1_$2
FREE C1 C1_$3
FREE C1 C1_$4
FREE O2 O2_$1
FREE O2 O2_$5
BOND
LIST 4
MORE -1
BOND $H
fmap 2
acta
OMIT 1 4 1
REM <olex2.extras>
REM <HklSrc "%.\\AJ1.hkl">
REM </olex2.extras>

WGHT    0.016100    2.507000
FVAR       0.29489
W1    5    0.500000    0.500000    0.236181    10.12500    0.00737    0.00737 =
         0.00559    0.00000    0.00000    0.00000
O1    4    0.500000    0.500000    0.161013    10.12500    0.00816    0.00816 =
         0.00900    0.00000    0.00000    0.00000
O2    4    0.709042    0.790958    0.250000    10.25000    0.00965    0.00965 =
         0.00490    0.00100    0.00100   -0.00250
C3    1    0.500000    0.500000    0.466658    10.12500    0.01438    0.01438 =
         0.00216    0.00000    0.00000    0.00000
N1    3    0.500000    0.500000    0.342457    10.12500    0.01286    0.01286 =
         0.00782    0.00000    0.00000    0.00000
C1    1    0.279324    0.500000    0.373472    10.25000    0.00846    0.01705 =
         0.00372    0.00000   -0.00248    0.00000
AFIX  43
H1    2    0.122831    0.500000    0.352449    10.25000   -1.20000
AFIX   0
C2    1    0.273057    0.500000    0.434540    10.25000    0.00791    0.02397 =
         0.00999    0.00000    0.00284    0.00000
AFIX  43
H2    2    0.114318    0.500000    0.454636    10.25000   -1.20000
AFIX   0
HKLF 4




REM  aj1_a.res in I4/mmm
REM wR2 = 0.032654, GooF = S = 1.22938, Restrained GooF = 1.22938 for all data
REM R1 = 0.012840 for 251 Fo > 4sig(Fo) and 0.015993 for all 272 data
REM 30 parameters refined using 0 restraints

END

WGHT      0.0161      2.5070

REM Highest difference peak  1.258,  deepest hole -1.290,  1-sigma level  0.150
Q1    1   0.0000  0.0000  0.4704  10.12500  0.05    1.26
Q2    1   0.5000  0.5000  0.1998  10.12500  0.05    0.93
Q3    1   0.5000  0.5000  0.5000  10.06250  0.05    0.63
Q4    1   0.5000  0.5000  0.1198  10.12500  0.05    0.46
Q5    1   0.5000  0.4365  0.1543  10.50000  0.05    0.40
;
_shelx_res_checksum              20174
####################################################################### 
# 
# 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_aj1-pyz0p5HxMoO3
_database_code_depnum_ccdc_archive 'CCDC 2282218'
loop_
_audit_author_name
_audit_author_address
'Adam Jaffe'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2023-07-18 deposited with the CCDC.	2023-09-13 downloaded from the CCDC.
;
_audit_creation_method           
;FinalCif V123 by Daniel Kratzert, Freiburg 2023, 
https://dkratzert.de/finalcif.html
;
_audit_creation_date             2023-07-15
_diffrn_source_power             1.75
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: O1(0.25) C1(0.25) H1(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C2 H2 Mo N O3'
_chemical_formula_moiety         'C2 H2 Mo N O3'
_chemical_formula_weight         183.99
_chemical_melting_point          ?
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_vrf_PLAT430_aj1-pyz0p5HxMoO3    
;PROBLEM: Short Inter D...A Contact  O1       ..O1       .       2.10 Ang.  
RESPONSE: These oxygen atoms are disordered by symmetry which erroneously
leads to a short contact distance error.
;
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
_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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   5.2479(7)
_cell_length_b                   5.2479(7)
_cell_length_c                   14.143(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     389.50(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    120.00
_cell_measurement_reflns_used    2620
_cell_measurement_theta_min      2.881
_cell_measurement_theta_max      28.236
_exptl_crystal_description       block
_exptl_crystal_colour            'dark black'
_exptl_crystal_recrystallization_method 
'Hydrothermal reaction at 170C for 3 days'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.138
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.059
_exptl_absorpt_coefficient_mu    3.226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7985
_exptl_absorpt_correction_T_max  0.8372
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0300 before and 0.0207 after correction.
The Ratio of minimum to maximum transmission is 0.9538.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   0.724
_shelx_estimated_absorpt_T_max   0.832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           
;
X-ray diffraction analyses were performed on single crystals coated with
 Paratone-N oil and mounted on MiTeGen loops. Crystals were frozen at a
 temperature of 120 K by an Oxford Cryosystems Cryostream using N₂ during
 the experiments. Data was collected at the Molecular Structure Facility
 at the University of Notre Dame using Mo k-alpha
 radiation (lamda = 0.71073 angstrom) on a Bruker APEX equipped with a
 Bruker PHOTON II detector.
;
_diffrn_ambient_temperature      120.0
_diffrn_ambient_environment      ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Bruker TRIUMPH curved-graphite'
_diffrn_radiation_probe          ?
_diffrn_source                   ?
_diffrn_source_type              ?
_diffrn_source_voltage           50.0
_diffrn_source_current           35.0
_diffrn_detector                 'CCD Area Detector'
_diffrn_detector_type            'Bruker APEX-II'
_diffrn_detector_area_resol_mean 8.33
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       'combination of ω and φ-scans'
_diffrn_measurement_specimen_support ?
_diffrn_reflns_number            2961
_diffrn_reflns_av_unetI/netI     0.0058
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_theta_min         2.881
_diffrn_reflns_theta_max         28.236
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_standards_number         0
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             173
_reflns_number_gt                171
_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 APEX-4 (Bruker, 2021)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2021)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2021)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2015b)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2020)'
_computing_publication_material  
'FinalCIF (Kratzert, 2023)/CIFTAB (Sheldrick, 2008)'
_refine_special_details          
;
Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding
model. The structure features inorganic layers comprised of MoO5N octahedra.
These layers are pillared by pyrazine molecules. The inorganic 
layers have been chemically reduced in situ with Mo metal with protons 
providing charge balance. These protons were not located or refined.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0264P)²+2.3084P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         173
_refine_ls_number_parameters     21
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0181
_refine_ls_wR_factor_ref         0.0559
_refine_ls_wR_factor_gt          0.0556
_refine_ls_goodness_of_fit_ref   1.390
_refine_ls_restrained_S_all      1.390
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.595
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

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'

_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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 -1.00 -1.00 0.0210
-1.00 0.00 1.00 0.0110
0.00 -1.00 1.00 0.0080
0.00 1.00 -1.00 0.0420
1.00 1.00 1.00 0.0280
1.00 0.00 -1.00 0.0480

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 0.5000 0.5000 0.22688(4) 0.0085(2) Uani 1 8 d S T P . .
O2 O 0.5000 0.5000 0.1079(4) 0.0080(10) Uani 1 8 d S T P . .
N1 N 0.5000 0.5000 0.4014(4) 0.0104(13) Uani 1 8 d S T P . .
O1 O 0.6998(6) 0.8002(6) 0.2500 0.0089(11) Uani 0.5 2 d S T P . .
C1 C 0.2813(13) 0.5000 0.4508(4) 0.0080(13) Uani 0.5 2 d S T P . .
H1 H 0.1235 0.5000 0.4179 0.010 Uiso 0.5 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0109(3) 0.0109(3) 0.0038(3) 0.000 0.000 0.000
O2 0.0071(15) 0.0071(15) 0.010(2) 0.000 0.000 0.000
N1 0.0131(19) 0.0131(19) 0.005(3) 0.000 0.000 0.000
O1 0.0090(17) 0.0090(17) 0.0088(16) -0.0007(15) -0.0007(15) 0.0005(19)
C1 0.009(4) 0.008(3) 0.007(3) 0.000 -0.001(2) 0.000

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 O2 1.682(5) . ?
Mo1 N1 2.469(6) . ?
Mo1 O1 1.9205(9) 24 ?
Mo1 O1 1.9205(9) 3_655 ?
Mo1 O1 1.9205(9) 26_445 ?
Mo1 O1 1.9205(9) 27_465 ?
Mo1 O1 1.9205(9) . ?
Mo1 O1 1.9205(9) 2_665 ?
Mo1 O1 1.9205(9) 4_565 ?
Mo1 O1 1.9205(9) 28_645 ?
N1 C1 1.343(7) 4_565 ?
N1 C1 1.343(7) . ?
N1 C1 1.343(7) 23_665 ?
N1 C1 1.343(7) 2_665 ?
N1 C1 1.343(7) 3_655 ?
N1 C1 1.343(7) 24 ?
O1 Mo1 1.9205(9) 25_665 ?
C1 C1 1.392(12) 18_556 ?
C1 H1 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
O2 Mo1 N1 180.0 . . ?
O2 Mo1 O1 99.801(16) . 28_645 ?
O2 Mo1 O1 99.801(16) . . ?
O2 Mo1 O1 99.801(16) . 4_565 ?
O2 Mo1 O1 99.801(16) . 3_655 ?
O2 Mo1 O1 99.801(16) . 2_665 ?
O2 Mo1 O1 99.801(16) . 27_465 ?
O2 Mo1 O1 99.801(16) . 26_445 ?
O2 Mo1 O1 99.801(16) . 24 ?
O1 Mo1 N1 80.199(16) 26_445 . ?
O1 Mo1 N1 80.199(16) . . ?
O1 Mo1 N1 80.199(16) 4_565 . ?
O1 Mo1 N1 80.199(16) 3_655 . ?
O1 Mo1 N1 80.199(16) 24 . ?
O1 Mo1 N1 80.199(16) 2_665 . ?
O1 Mo1 N1 80.199(16) 28_645 . ?
O1 Mo1 N1 80.199(16) 27_465 . ?
O1 Mo1 O1 110.3(3) 26_445 4_565 ?
O1 Mo1 O1 150.1(2) 28_645 3_655 ?
O1 Mo1 O1 66.2(3) 26_445 3_655 ?
O1 Mo1 O1 66.2(3) 24 4_565 ?
O1 Mo1 O1 22.4(3) 2_665 26_445 ?
O1 Mo1 O1 110.3(3) 2_665 27_465 ?
O1 Mo1 O1 110.3(3) 24 3_655 ?
O1 Mo1 O1 150.1(2) 4_565 27_465 ?
O1 Mo1 O1 160.40(3) 26_445 24 ?
O1 Mo1 O1 88.339(5) 2_665 4_565 ?
O1 Mo1 O1 66.2(3) 2_665 28_645 ?
O1 Mo1 O1 88.339(5) 24 27_465 ?
O1 Mo1 O1 88.339(5) 26_445 28_645 ?
O1 Mo1 O1 160.40(3) 2_665 . ?
O1 Mo1 O1 110.3(3) . 28_645 ?
O1 Mo1 O1 150.1(2) 2_665 24 ?
O1 Mo1 O1 150.1(2) 26_445 . ?
O1 Mo1 O1 22.4(3) 4_565 28_645 ?
O1 Mo1 O1 88.339(6) 26_445 27_465 ?
O1 Mo1 O1 160.40(3) 27_465 28_645 ?
O1 Mo1 O1 160.40(3) 4_565 3_655 ?
O1 Mo1 O1 22.4(3) . 24 ?
O1 Mo1 O1 88.339(5) 2_665 3_655 ?
O1 Mo1 O1 88.339(5) . 3_655 ?
O1 Mo1 O1 66.2(3) . 27_465 ?
O1 Mo1 O1 22.4(3) 27_465 3_655 ?
O1 Mo1 O1 88.339(5) . 4_565 ?
O1 Mo1 O1 88.339(6) 24 28_645 ?
C1 N1 Mo1 121.3(4) 24 . ?
C1 N1 Mo1 121.3(4) 4_565 . ?
C1 N1 Mo1 121.3(4) 3_655 . ?
C1 N1 Mo1 121.3(4) 2_665 . ?
C1 N1 Mo1 121.3(4) . . ?
C1 N1 Mo1 121.3(4) 23_665 . ?
C1 N1 C1 0.0(4) 4_565 23_665 ?
C1 N1 C1 74.3(3) 23_665 2_665 ?
C1 N1 C1 74.3(3) . 3_655 ?
C1 N1 C1 117.4(7) 23_665 3_655 ?
C1 N1 C1 74.3(3) 4_565 . ?
C1 N1 C1 0.0(5) 24 3_655 ?
C1 N1 C1 74.3(3) 4_565 2_665 ?
C1 N1 C1 117.4(7) 4_565 3_655 ?
C1 N1 C1 74.3(3) 23_665 . ?
C1 N1 C1 117.4(7) 4_565 24 ?
C1 N1 C1 74.3(3) 24 . ?
C1 N1 C1 117.4(7) . 2_665 ?
C1 N1 C1 74.3(3) 24 2_665 ?
C1 N1 C1 117.4(7) 23_665 24 ?
C1 N1 C1 74.3(3) 3_655 2_665 ?
Mo1 O1 Mo1 157.6(3) 25_665 . ?
N1 C1 C1 121.3(4) . 18_556 ?
N1 C1 H1 119.3 . . ?
C1 C1 H1 119.3 18_556 . ?

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 C1 C1 180.000(2) . . . 18_556 ?
C1 N1 C1 C1 -62.5(2) 23_665 . . 18_556 ?
C1 N1 C1 C1 0.000(1) 2_665 . . 18_556 ?
C1 N1 C1 C1 -62.5(2) 4_565 . . 18_556 ?
C1 N1 C1 C1 62.5(2) 24 . . 18_556 ?
C1 N1 C1 C1 62.5(2) 3_655 . . 18_556 ?

_shelx_res_file                  
;
    aj1.res created by SHELXL-2014/7

TITL aj1_b.res in I4/mmm
REM Old TITL aj1 in I4/mmm
REM SHELXT solution in I4/mmm: R1 0.133, Rweak 0.021, Alpha 0.037
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C2 N O Mo
CELL 0.71073 5.2479 5.2479 14.1428 90 90 90
ZERR 4 0.0007 0.0007 0.0026 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SFAC C H Mo N O
UNIT 8 8 4 4 12
EQIV $1 1-Y,1-X,+Z
EQIV $2 +Y,1-X,+Z
EQIV $3 1-Y,+X,+Z
EQIV $4 +Y,+X,+Z
EQIV $5 0.5+X,-0.5+Y,1.5-Z

L.S. 20
PLAN  5
SIZE 0.059 0.09 0.107
TEMP -153.15
CONF
FREE C1 C1_$1
FREE C1 C1_$2
FREE C1 C1_$3
FREE C1 C1_$4
FREE O1 O1_$4
FREE O1 O1_$5
BOND
LIST 4
MORE -1
BOND $H
fmap 2
acta
OMIT 1 4 1
OMIT 1 2 1
REM <olex2.extras>
REM <HklSrc "%.\\aj1.hkl">
REM </olex2.extras>

WGHT    0.026400    2.308400
FVAR       0.56900
MO1   3    0.500000    0.500000    0.226883    10.12500    0.01086    0.01086 =
         0.00378    0.00000    0.00000    0.00000
O2    5    0.500000    0.500000    0.107939    10.12500    0.00709    0.00709 =
         0.00980    0.00000    0.00000    0.00000
N1    4    0.500000    0.500000    0.401434    10.12500    0.01313    0.01313 =
         0.00485    0.00000    0.00000    0.00000
O1    5    0.699759    0.800241    0.250000    10.25000    0.00896    0.00896 =
         0.00882   -0.00068   -0.00068    0.00052
C1    1    0.281302    0.500000    0.450779    10.25000    0.00884    0.00776 =
         0.00727    0.00000   -0.00119    0.00000
AFIX  43
H1    2    0.123511    0.500000    0.417857    10.25000   -1.20000
AFIX   0
HKLF 4

REM  aj1_b.res in I4/mmm
REM R1 =  0.0181 for     171 Fo > 4sig(Fo)  and  0.0185 for all     173 data
REM     21 parameters refined using      0 restraints

END

WGHT      0.0264      2.3085

REM Highest difference peak  0.595,  deepest hole -1.619,  1-sigma level  0.172
Q1    1   0.5000  0.5000  0.1870  10.12500  0.05    0.59
Q2    1   0.5000  0.8969  0.2849  10.50000  0.05    0.57
Q3    1   0.0000  0.3267  0.4607  10.50000  0.05    0.33
Q4    1   0.2596  0.5000  0.5000  10.25000  0.05    0.30
Q5    1   0.3524  0.3523  0.0384  10.50000  0.05    0.27
;
_shelx_res_checksum              4787
####################################################################### 
# 
# 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_aj1-azp0p5MoO3
_database_code_depnum_ccdc_archive 'CCDC 2282209'
loop_
_audit_author_name
_audit_author_address
'Adam Jaffe'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2023-07-18 deposited with the CCDC.	2023-09-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_aj1-azp0p5MoO3      
;
PROBLEM: Atom O2              has ADP max/min Ratio .....        5.2 prolat
RESPONSE: O2 is modelled as prolate rather than disordered to prevent refinement  instability and overparameterization. Data quality is limited by synthetic challenges.
;
_vrf_PLAT971_aj1-azp0p5MoO3      
;
PROBLEM: Check Calcd Resid. Dens.  0.75Ang From O1              3.90 eA-3
RESPONSE: O1 could not be modeled anisotropically which likely accounts for some  uncompensated electron density. Data quality is limited by synthetic challenges.
;
_vrf_PLAT972_aj1-azp0p5MoO3      
;
PROBLEM: Check Calcd Resid. Dens.  0.70Ang From O1             -4.41 eA-3
RESPONSE: O1 could not be modeled anisotropically which likely accounts for some  uncompensated electron density. Data quality is limited by synthetic challenges.
;
_vrf_PLAT976_aj1-azp0p5MoO3      
;
PROBLEM: Check Calcd Resid. Dens.  0.70Ang From O1      .      -4.41 eA-3
RESPONSE: O1 could not be modeled anisotropically which likely accounts for some  uncompensated electron density. Data quality is limited by synthetic challenges.
;
_vrf_PLAT097_aj1-azp0p5MoO3      
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       4.36 eA-3
RESPONSE: Residual density is likely due to a disordered oxygen position that was not modeled to avoid overparameterization and instability of the refinement.  Data quality is limited by synthetic challenges.
;
_vrf_PLAT201_aj1-azp0p5MoO3      
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          1 Report
RESPONSE: Atom could not be modelled anisotropically
;
_vrf_PLAT430_aj1-azp0p5MoO3      
;
PROBLEM: Short Inter D...A Contact  O1       ..O2       .       2.70 Ang.
RESPONSE: O1 likely has some disorder and O2 is modelled as prolate rather than disordered to prevent refinement instability and overparameterization. These erroneously lead to a short contact distance error.
;
_vrf_PLAT972_aj1-azp0p5MoO3_2    
;
PROBLEM: Check Calcd Resid. Dens.  1.06Ang From Mo1            -3.24 eA-3
RESPONSE: O1 could not be modeled anisotropically which likely accounts for some  uncompensated electron density. Data quality is limited by synthetic challenges.
;
_vrf_PLAT975_aj1-azp0p5MoO3      
;
PROBLEM: Check Calcd Resid. Dens.  0.93Ang From O1      .       1.60 eA-3
RESPONSE: O1 could not be modeled anisotropically which likely accounts for some  uncompensated electron density. Data quality is limited by synthetic challenges.
;
_vrf_DIFMN02_aj1-azp0p5MoO3      
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*0.75
RESPONSE: O1 could not be modeled anisotropically which likely accounts for some  uncompensated electron density. Data quality is limited by synthetic challenges.
;
_vrf_DIFMN03_aj1-azp0p5MoO3      
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*0.75
RESPONSE: O1 could not be modeled anisotropically which likely accounts for some  uncompensated electron density. Data quality is limited by synthetic challenges.
;
_vrf_DIFMX02_aj1-azp0p5MoO3      
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: O1 could not be modeled anisotropically which likely accounts for some  uncompensated electron density. Data quality is limited by synthetic challenges.
;
_vrf_PLAT098_aj1-azp0p5MoO3      
;
PROBLEM: Large Reported Min.  (Negative) Residual Density      -4.04 eA-3
RESPONSE: Residual density is likely due to a disordered oxygen position that was not modeled to avoid overparameterization and instability of the refinement
;
_vrf_PLAT213_aj1-azp0p5MoO3_2    
;
PROBLEM: Atom O3              has ADP max/min Ratio .....        3.1 oblate
RESPONSE: O2 is modelled as prolate rather than disordered to prevent refinement  instability and overparameterization. Data quality is limited by synthetic challenges.
;
_vrf_PLAT971_aj1-azp0p5MoO3_2    
;
PROBLEM: Check Calcd Resid. Dens.  1.20Ang From Mo1             1.88 eA-3
RESPONSE: O1 could not be modeled anisotropically which likely accounts for some  uncompensated electron density. Data quality is limited by synthetic challenges.
;
_vrf_PLAT972_aj1-azp0p5MoO3_3    
;
PROBLEM: Check Calcd Resid. Dens.  0.53Ang From O1             -1.76 eA-3
RESPONSE: O1 could not be modeled anisotropically which likely accounts for some  uncompensated electron density. Data quality is limited by synthetic challenges.
;
_vrf_PLAT975_aj1-azp0p5MoO3_2    
;
PROBLEM: Check Calcd Resid. Dens.  0.80Ang From O2      .       1.38 eA-3
RESPONSE: O1 could not be modeled anisotropically which likely accounts for some  uncompensated electron density. Data quality is limited by synthetic challenges.
;
_audit_creation_method           
;FinalCif V123 by Daniel Kratzert, Freiburg 2023, 
https://dkratzert.de/finalcif.html
;
_audit_creation_date             2023-07-14
_diffrn_source_power             1.75
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Mo1 \\sim O3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O1 \\sim Mo1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C6(H6), C5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C5 H4 Mo N2 O3'
_chemical_formula_moiety         'C5 H4 Mo N2 O3'
_chemical_formula_weight         236.04
_chemical_melting_point          ?
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.522(3)
_cell_length_b                   7.375(3)
_cell_length_c                   25.795(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1431.0(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    120.01
_cell_measurement_reflns_used    3004
_cell_measurement_theta_min      3.159
_cell_measurement_theta_max      26.360
_exptl_crystal_description       plate
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_recrystallization_method 
'Hydrothermal reaction at 95C for 24 h followed by 80C for 3 days'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.191
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.021
_exptl_absorpt_coefficient_mu    1.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8076
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0670 before and 0.0569 after correction.
The Ratio of minimum to maximum transmission is 0.8427.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   0.853
_shelx_estimated_absorpt_T_max   0.963
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           
;
X-ray diffraction analyses were performed on single crystals coated with
 Paratone-N oil and mounted on MiTeGen loops. Crystals were frozen at a
 temperature of 120 K by an Oxford Cryosystems Cryostream using N₂ during
 the experiments. Data was collected at the Molecular Structure Facility
 at the University of Notre Dame using Mo k-alpha
 radiation (lamda = 0.71073 angstrom) on a Bruker APEX equipped with a
 Bruker PHOTON II detector.
;
_diffrn_ambient_temperature      120.01
_diffrn_ambient_environment      ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Bruker TRIUMPH curved-graphite'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 700'
_diffrn_radiation_probe          ?
_diffrn_source                   ?
_diffrn_source_type              ?
_diffrn_source_voltage           50.0
_diffrn_source_current           35.0
_diffrn_detector                 'CCD Area Detector'
_diffrn_detector_type            'Bruker APEX-II'
_diffrn_detector_area_resol_mean 8.33
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       'combination of ω and φ-scans'
_diffrn_measurement_specimen_support ?
_diffrn_reflns_number            15450
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_theta_min         1.579
_diffrn_reflns_theta_max         26.017
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_standards_number         0
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1402
_reflns_number_gt                1160
_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 APEX-4 (Bruker, 2021)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2021)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2021)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2015b)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2020)'
_computing_publication_material  
'FinalCIF (Kratzert, 2023)/CIFTAB (Sheldrick, 2008)'
_refine_special_details          
;
Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding 
model. The structure features inorganic layers comprised of MoO5N octahedra. 
These layers are pillared by 4,4'-azopyridine molecules.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+102.6131P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         1402
_refine_ls_number_parameters     95
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0814
_refine_ls_wR_factor_ref         0.1753
_refine_ls_wR_factor_gt          0.1693
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_restrained_S_all      1.206
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         4.363
_refine_diff_density_min         -4.043
_refine_diff_density_rms         0.318
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

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'

_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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 1.00 0.0350
1.00 0.00 -1.00 0.0360
-1.00 0.00 1.00 0.0430
0.00 0.00 -1.00 0.0080
0.00 0.00 1.00 0.0090
0.00 1.00 -1.00 0.0230

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 0.53272(13) 0.32071(14) 0.76204(4) 0.0062(3) Uani 1 1 d . U . . .
O3 O 0.5117(11) 0.3286(13) 0.8273(3) 0.0102(18) Uani 1 1 d . U . . .
O1 O 0.4791(14) 0.0910(13) 0.7479(4) 0.023(2) Uiso 1 1 d . U . . .
N1 N 0.5242(15) 0.3454(14) 0.6686(4) 0.012(2) Uani 1 1 d . . . . .
N2 N 0.464(2) 0.4304(17) 0.5087(5) 0.027(3) Uani 1 1 d . . . . .
C4 C 0.4922(18) 0.4073(19) 0.5634(5) 0.017(3) Uani 1 1 d . . . . .
C3 C 0.616(2) 0.5019(19) 0.5925(6) 0.019(3) Uani 1 1 d . . . . .
H3 H 0.690396 0.590058 0.576837 0.023 Uiso 1 1 calc R U . . .
C2 C 0.6275(18) 0.4650(19) 0.6448(5) 0.015(3) Uani 1 1 d . . . . .
H2 H 0.713761 0.528308 0.664714 0.018 Uiso 1 1 calc R U . . .
C6 C 0.4065(18) 0.249(2) 0.6401(5) 0.016(3) Uani 1 1 d . . . . .
H6 H 0.334019 0.161461 0.656830 0.019 Uiso 1 1 calc R U . . .
O2 O 0.7608(14) 0.339(3) 0.7530(4) 0.058(5) Uani 1 1 d . . . . .
C5 C 0.389(2) 0.276(2) 0.5872(6) 0.022(3) Uani 1 1 d . . . . .
H5 H 0.307669 0.205349 0.567524 0.026 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0046(5) 0.0043(5) 0.0098(5) -0.0001(4) -0.0013(4) -0.0001(4)
O3 0.005(4) 0.009(4) 0.017(4) -0.001(4) -0.003(3) -0.004(4)
N1 0.018(6) 0.008(5) 0.010(5) 0.001(4) 0.003(5) 0.004(5)
N2 0.038(8) 0.021(6) 0.023(7) 0.005(5) -0.004(6) -0.007(6)
C4 0.016(8) 0.018(7) 0.018(7) 0.004(6) 0.002(5) -0.003(6)
C3 0.020(7) 0.016(7) 0.022(8) 0.005(6) 0.004(6) -0.004(6)
C2 0.014(7) 0.016(7) 0.016(7) -0.004(6) 0.000(5) 0.012(6)
C6 0.017(7) 0.016(6) 0.015(7) -0.001(6) 0.004(5) -0.009(6)
O2 0.006(5) 0.155(15) 0.013(5) 0.003(8) 0.001(4) -0.001(8)
C5 0.021(7) 0.021(8) 0.022(8) 0.000(6) -0.006(6) -0.007(6)

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 O3 1.692(9) . ?
Mo1 O1 2.012(10) 3_656 ?
Mo1 O1 1.779(10) . ?
Mo1 N1 2.419(10) . ?
Mo1 O2 2.086(11) 6_557 ?
Mo1 O2 1.737(11) . ?
N1 C2 1.326(18) . ?
N1 C6 1.351(17) . ?
N2 N2 1.25(3) 5_666 ?
N2 C4 1.439(18) . ?
C4 C3 1.38(2) . ?
C4 C5 1.38(2) . ?
C3 H3 0.9500 . ?
C3 C2 1.379(19) . ?
C2 H2 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.387(19) . ?
C5 H5 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mo1 O1 95.1(5) . 3_656 ?
O3 Mo1 O1 102.5(5) . . ?
O3 Mo1 N1 170.7(4) . . ?
O3 Mo1 O2 102.9(4) . . ?
O3 Mo1 O2 95.2(4) . 6_557 ?
O1 Mo1 O1 155.13(9) . 3_656 ?
O1 Mo1 N1 82.0(4) . . ?
O1 Mo1 N1 78.3(4) 3_656 . ?
O1 Mo1 O2 82.4(6) 3_656 6_557 ?
O1 Mo1 O2 78.6(6) . 6_557 ?
O2 Mo1 O1 87.0(7) . 3_656 ?
O2 Mo1 O1 105.8(7) . . ?
O2 Mo1 N1 83.4(4) . . ?
O2 Mo1 N1 77.5(4) 6_557 . ?
O2 Mo1 O2 159.7(5) . 6_557 ?
Mo1 O1 Mo1 168.4(6) . 3_646 ?
C2 N1 Mo1 119.7(9) . . ?
C2 N1 C6 118.8(11) . . ?
C6 N1 Mo1 121.3(9) . . ?
N2 N2 C4 112.6(16) 5_666 . ?
C3 C4 N2 125.0(13) . . ?
C3 C4 C5 119.3(13) . . ?
C5 C4 N2 115.7(13) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 C4 118.4(13) . . ?
C2 C3 H3 120.8 . . ?
N1 C2 C3 123.1(13) . . ?
N1 C2 H2 118.5 . . ?
C3 C2 H2 118.5 . . ?
N1 C6 H6 119.2 . . ?
N1 C6 C5 121.5(13) . . ?
C5 C6 H6 119.2 . . ?
Mo1 O2 Mo1 171.2(11) . 6_657 ?
C4 C5 C6 118.8(13) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?

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 C2 C3 -172.3(10) . . . . ?
Mo1 N1 C6 C5 173.6(11) . . . . ?
O3 Mo1 O1 Mo1 -74(3) . . . 3_646 ?
O1 Mo1 O1 Mo1 152(3) 3_656 . . 3_646 ?
N1 Mo1 O1 Mo1 114(3) . . . 3_646 ?
N1 C6 C5 C4 -2(2) . . . . ?
N2 N2 C4 C3 -13(3) 5_666 . . . ?
N2 N2 C4 C5 168.4(17) 5_666 . . . ?
N2 C4 C3 C2 179.9(13) . . . . ?
N2 C4 C5 C6 -178.5(13) . . . . ?
C4 C3 C2 N1 -1(2) . . . . ?
C3 C4 C5 C6 3(2) . . . . ?
C2 N1 C6 C5 -1(2) . . . . ?
C6 N1 C2 C3 3(2) . . . . ?
O2 Mo1 O1 Mo1 33(3) . . . 3_646 ?
O2 Mo1 O1 Mo1 -167(3) 6_557 . . 3_646 ?
C5 C4 C3 C2 -2(2) . . . . ?

_shelx_res_file                  
;
TITL aj1_a.res in Pbca
    aj1.res
    created by SHELXL-2018/3 at 18:21:00 on 14-Jul-2023
REM Old TITL aj1 in Pbca
REM SHELXT solution in Pbca: R1 0.140, Rweak 0.007, Alpha 0.057
REM <I/s> 1.320 for 276 systematic absences, Orientation as input
REM Formula found by SHELXT: C7 N2 O Mo
CELL 0.71073 7.522 7.3754 25.7947 90 90 90
ZERR 8 0.0032 0.0031 0.0107 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Mo N O
UNIT 40 32 8 16 24
SIMU Mo1 O3
SIMU O1 Mo1

L.S. 20
PLAN  2
SIZE 0.021 0.079 0.092
TEMP -153.14
CONF
BOND
LIST 4
MORE -1
BOND $H
fmap 2
acta
OMIT 8 3 2
REM <olex2.extras>
REM <HklSrc "%.\\aj1.hkl">
REM </olex2.extras>

WGHT    0.000100  102.613098
FVAR       0.23632
MO1   3    0.532718    0.320708    0.762043    11.00000    0.00461    0.00430 =
         0.00976   -0.00006   -0.00128   -0.00008
O3    5    0.511742    0.328624    0.827306    11.00000    0.00454    0.00930 =
         0.01687   -0.00126   -0.00332   -0.00406
O1    5    0.479067    0.091005    0.747907    11.00000    0.02342
N1    4    0.524231    0.345431    0.668573    11.00000    0.01838    0.00752 =
         0.01009    0.00081    0.00311    0.00437
N2    4    0.463597    0.430429    0.508650    11.00000    0.03821    0.02055 =
         0.02291    0.00498   -0.00432   -0.00707
C4    1    0.492203    0.407251    0.563415    11.00000    0.01621    0.01777 =
         0.01769    0.00445    0.00204   -0.00252
C3    1    0.615635    0.501864    0.592496    11.00000    0.02020    0.01580 =
         0.02227    0.00460    0.00430   -0.00351
AFIX  43
H3    2    0.690396    0.590058    0.576837    11.00000   -1.20000
AFIX   0
C2    1    0.627532    0.465036    0.644794    11.00000    0.01358    0.01561 =
         0.01626   -0.00429    0.00048    0.01203
AFIX  43
H2    2    0.713761    0.528308    0.664714    11.00000   -1.20000
AFIX   0
C6    1    0.406516    0.249330    0.640150    11.00000    0.01659    0.01611 =
         0.01488   -0.00071    0.00363   -0.00922
AFIX  43
H6    2    0.334019    0.161461    0.656830    11.00000   -1.20000
AFIX   0
O2    5    0.760813    0.339388    0.752968    11.00000    0.00637    0.15453 =
         0.01297    0.00297    0.00054   -0.00108
C5    1    0.389031    0.275973    0.587164    11.00000    0.02136    0.02113 =
         0.02204   -0.00004   -0.00649   -0.00701
AFIX  43
H5    2    0.307669    0.205349    0.567524    11.00000   -1.20000
AFIX   0
HKLF 4




REM  aj1_a.res in Pbca
REM wR2 = 0.175310, GooF = S = 1.21140, Restrained GooF = 1.20613 for all data
REM R1 = 0.081381 for 1160 Fo > 4sig(Fo) and 0.096942 for all 1402 data
REM 95 parameters refined using 12 restraints

END

WGHT      0.0000    102.6281

REM Highest difference peak  4.363,  deepest hole -4.043,  1-sigma level  0.318
Q1    1   0.5808  0.0910  0.7513  11.00000  0.05    4.36
Q2    1   0.4604  0.4282  0.7361  11.00000  0.05    1.69
;
_shelx_res_checksum              69512
