# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_exp_2516
_database_code_depnum_ccdc_archive 'CCDC 2056050'
loop_
_audit_author_name
_audit_author_address
'Eduard Bernhardt'
;Bergische Universitat Wuppertal
Germany
;
_audit_update_record             
;
2021-01-14 deposited with the CCDC.	2021-02-09 downloaded from the CCDC.
;
_audit_creation_date             2020-03-09
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C3 N3 O3 P'
_chemical_formula_sum            'C3 N3 O3 P'
_chemical_formula_weight         157.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C3 N3 O3 P1'
_chemical_oxdiff_usercomment     'P(NCO)3 100K'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   7.2574(4)
_cell_length_b                   11.2605(6)
_cell_length_c                   7.1530(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     584.56(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3606
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.6692
_cell_measurement_theta_min      3.3328
_shelx_estimated_absorpt_T_max   0.920
_shelx_estimated_absorpt_T_min   0.800
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.5673
_exptl_crystal_size_mid          0.4878
_exptl_crystal_size_min          0.207
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5868
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.746
_diffrn_reflns_theta_min         3.374
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   25.00   67.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.2288  -99.0000  -90.0000 168

#__ type_ start__ end____ width___ exp.time_
  2 omega   22.00   68.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.2288  -99.0000   30.0000 184

#__ type_ start__ end____ width___ exp.time_
  3 omega    7.00   66.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.2288  -99.0000  150.0000 236

#__ type_ start__ end____ width___ exp.time_
  4 omega  -82.00  -54.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.7913 -178.0000    0.0000 112

#__ type_ start__ end____ width___ exp.time_
  5 omega  -34.00   34.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.7913   57.0000   60.0000 272

#__ type_ start__ end____ width___ exp.time_
  6 omega  -97.00   -6.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.7913  -57.0000 -180.0000 364

#__ type_ start__ end____ width___ exp.time_
  7 omega -101.00   16.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.7913  -19.0000 -120.0000 468
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0724617000
_diffrn_orient_matrix_UB_12      0.0398548000
_diffrn_orient_matrix_UB_13      -0.0224646000
_diffrn_orient_matrix_UB_21      -0.0419810000
_diffrn_orient_matrix_UB_22      0.0116885000
_diffrn_orient_matrix_UB_23      -0.0875806000
_diffrn_orient_matrix_UB_31      -0.0504103000
_diffrn_orient_matrix_UB_32      0.0474136000
_diffrn_orient_matrix_UB_33      0.0405213000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                981
_reflns_number_total             1050
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         1050
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0265
_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)+(0.0351P)²+0.1721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0736
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
P001 P 0.30987(5) 0.250000 0.53291(5) 0.01502(11) Uani 1 2 d S T P . .
O002 O 0.31359(16) 0.250000 0.00642(17) 0.0315(3) Uani 1 2 d S T P . .
N003 N 0.43319(11) 0.36463(7) 0.62606(12) 0.01912(17) Uani 1 1 d . . . . .
O004 O 0.36191(14) 0.52396(8) 0.82822(15) 0.0425(3) Uani 1 1 d . . . . .
N005 N 0.41291(16) 0.250000 0.32055(17) 0.0201(2) Uani 1 2 d S T P . .
C006 C 0.35484(18) 0.250000 0.16348(19) 0.0187(2) Uani 1 2 d S T P . .
C007 C 0.39059(15) 0.44387(9) 0.72901(15) 0.0234(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P001 N003 1.7062(8) 7_565 ?
P001 N003 1.7062(8) . ?
P001 N005 1.6931(12) . ?
O002 C006 1.1626(18) . ?
N003 C007 1.1975(13) . ?
O004 C007 1.1663(13) . ?
N005 C006 1.1999(18) . ?

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
N003 P001 N003 98.32(6) . 7_565 ?
N005 P001 N003 96.82(4) . . ?
N005 P001 N003 96.82(4) . 7_565 ?
C007 N003 P001 131.94(8) . . ?
C006 N005 P001 133.23(11) . . ?
O002 C006 N005 174.36(15) . . ?
O004 C007 N003 175.14(12) . . ?

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
N003 P001 N003 C007 -119.49(10) 7_565 . . . ?
N003 P001 N005 C006 130.37(3) 7_565 . . . ?
N003 P001 N005 C006 -130.37(3) . . . . ?
N005 P001 N003 C007 142.56(11) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 -1 0 0.0862 -1.0000 -1.0000 -0.0000 -0.1123 0.0303 0.0030
1 1 0 0.1208 1.0000 1.0000 0.0000 0.1123 -0.0303 -0.0030
0 0 -1 0.1888 -0.0000 0.0000 -1.0000 0.0225 0.0876 -0.0405
-1 3 0 0.2271 -1.0000 3.0000 -0.0000 0.0471 0.0770 0.1927
5 -13 -3 0.3068 5.0001 -13.0000 -2.9999 -0.0884 -0.0991 -0.9900
6 -4 8 0.1871 6.0002 -4.0001 8.0002 0.0956 -0.9993 -0.1680
-1 -5 9 0.2552 -0.9999 -5.0001 9.0000 -0.4739 -0.8047 0.1780
0 -9 8 0.2256 0.0001 -9.0001 8.0000 -0.5384 -0.8059 -0.1026
3 -1 -10 0.1967 2.9999 -0.9999 -10.0000 0.4022 0.7382 -0.6038
-10 6 1 0.2128 -10.0002 5.9999 0.9998 -0.5080 0.4024 0.8291
3 12 5 0.2873 3.0002 12.0000 5.0001 0.5833 -0.4236 0.6203
9 5 3 0.1472 9.0003 5.0000 3.0002 0.7841 -0.5822 -0.0951
9 5 -4 0.1349 9.0002 5.0001 -3.9998 0.9413 0.0309 -0.3787
-7 -10 3 0.1247 -7.0001 -10.0001 2.9999 -0.9732 -0.0857 0.0003
-8 5 5 0.2909 -8.0001 4.9999 4.9999 -0.4928 -0.0436 0.8430
1 3 10 0.3143 1.0002 2.9999 10.0001 -0.0326 -0.8827 0.4970
-5 6 -8 0.2607 -5.0002 6.0001 -8.0001 0.0565 0.9807 0.2124
2 -9 -8 0.2752 1.9999 -8.9999 -8.0000 -0.0341 0.5115 -0.8517
8 2 6 0.1584 8.0003 2.0000 6.0002 0.5246 -0.8380 -0.0653
-10 1 1 0.1719 -10.0002 0.9999 0.9998 -0.7072 0.3439 0.5920
-8 -9 1 0.0869 -8.0002 -9.0001 0.9998 -0.9609 0.1431 0.0171
-5 -2 9 0.2663 -5.0000 -2.0002 9.0000 -0.6442 -0.6017 0.5219

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_2547
_database_code_depnum_ccdc_archive 'CCDC 2056051'
loop_
_audit_author_name
_audit_author_address
'Eduard Bernhardt'
;Bergische Universitat Wuppertal
Germany
;
_audit_update_record             
;
2021-01-14 deposited with the CCDC.	2021-02-09 downloaded from the CCDC.
;
_audit_creation_date             2020-01-07
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C2 Cl N2 O2 P'
_chemical_formula_sum            'C2 Cl N2 O2 P'
_chemical_formula_weight         150.46
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C2 N2 O2 P1 Cl1'
_chemical_oxdiff_usercomment     PCl(NCO)2
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   7.2241(17)
_cell_length_b                   12.227(3)
_cell_length_c                   6.3593(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     561.7(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1660
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1363
_cell_measurement_theta_min      3.2688
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.4715
_exptl_crystal_size_mid          0.3683
_exptl_crystal_size_min          0.3333
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2888
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.840
_diffrn_reflns_theta_min         3.332
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -4.00   22.00   0.2500   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9787   77.0000 -180.0000 104

#__ type_ start__ end____ width___ exp.time_
  2 omega   -7.00   21.00   0.2500   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9787   77.0000   60.0000 112

#__ type_ start__ end____ width___ exp.time_
  3 omega  -11.00   64.00   0.2500   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9787   77.0000 -150.0000 300

#__ type_ start__ end____ width___ exp.time_
  4 omega  -41.00   49.00   0.2500   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5412   77.0000   60.0000 360

#__ type_ start__ end____ width___ exp.time_
  5 omega  -25.00   42.00   0.2500   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5412   77.0000 -180.0000 268

#__ type_ start__ end____ width___ exp.time_
  6 omega  -48.00  -27.00   0.2500   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5412   77.0000  -60.0000 84
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0792733000
_diffrn_orient_matrix_UB_12      -0.0335013000
_diffrn_orient_matrix_UB_13      0.0130654000
_diffrn_orient_matrix_UB_21      -0.0580040000
_diffrn_orient_matrix_UB_22      -0.0442050000
_diffrn_orient_matrix_UB_23      0.0294215000
_diffrn_orient_matrix_UB_31      -0.0061975000
_diffrn_orient_matrix_UB_32      -0.0162902000
_diffrn_orient_matrix_UB_33      -0.1069139000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                599
_reflns_number_total             704
_reflns_odcompleteness_completeness 99.29
_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, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         704
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0329
_refine_ls_restrained_S_all      1.057
_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)+(0.0549P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0894
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
P001 P 0.33904(8) 0.250000 0.59366(8) 0.0215(2) Uani 1 2 d S T P . .
Cl02 Cl 0.55039(11) 0.250000 0.37515(11) 0.0453(3) Uani 1 2 d S T P . .
O003 O 0.2980(2) 0.51500(13) 0.8936(2) 0.0463(4) Uani 1 1 d . . . . .
N004 N 0.4187(2) 0.35326(13) 0.7473(2) 0.0291(4) Uani 1 1 d . . . . .
C005 C 0.3505(2) 0.43416(15) 0.8179(3) 0.0296(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P001 Cl02 2.0645(9) . ?
P001 N004 1.6969(16) 7_565 ?
P001 N004 1.6970(16) . ?
O003 C005 1.163(2) . ?
N004 C005 1.193(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N004 P001 Cl02 97.87(6) 7_565 . ?
N004 P001 Cl02 97.87(6) . . ?
N004 P001 N004 96.15(11) 7_565 . ?
C005 N004 P001 133.92(15) . . ?
O003 C005 N004 174.4(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl02 P001 N004 C005 130.5(2) . . . . ?
N004 P001 N004 C005 -130.62(17) 7_565 . . . ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
8 -3 5 0.1138 8.0548 -2.9271 5.0324 0.8023 -0.1898 -0.5403
5 14 -3 0.2000 4.9588 14.0673 -2.9965 -0.1173 -0.9976 0.0605
2 4 -8 0.1492 1.9943 4.0231 -8.0157 -0.0814 -0.5294 0.7791
-9 7 0 0.1360 -9.0819 6.9244 -0.0224 -0.9522 0.2200 -0.0541
-7 -9 -4 0.2635 -6.9910 -9.0806 -4.0265 -0.3026 0.6884 0.6217
-4 -13 -5 0.2563 -3.9551 -13.0580 -5.0215 0.0583 0.6589 0.7741
4 -8 -7 0.1729 4.0634 -7.9750 -7.0075 0.4977 -0.0893 0.8539
4 14 3 0.1853 3.9510 14.0591 3.0163 -0.1184 -0.7619 -0.5760
1 -11 7 0.1696 1.0564 -11.0049 7.0210 0.5442 0.6318 -0.5779
1 -16 -4 0.2244 1.0856 -16.0146 -4.0065 0.5702 0.5271 0.6825
-1 -2 -9 0.1884 -0.9916 -2.0144 -9.0251 -0.1290 -0.1190 1.0039
-1 16 3 0.2040 -1.0852 16.0143 3.0040 -0.5833 -0.5566 -0.5753
-1 13 -6 0.2019 -1.0666 13.0080 -6.0186 -0.5990 -0.6902 0.4382
5 2 -8 0.1218 5.0200 2.0488 -8.0083 0.2247 -0.6174 0.7917
8 9 1 0.1467 7.9975 9.0895 1.0213 0.3428 -0.8356 -0.3068
-3 -8 7 0.1869 -2.9795 -8.0387 7.0111 0.1247 0.7344 -0.6002
-10 5 0 0.1442 -10.0773 4.9120 -0.0247 -0.9637 0.3667 -0.0149
1 7 8 0.2316 0.9674 7.0214 8.0222 -0.0537 -0.1305 -0.9781

_olex2_submission_special_instructions 'No special instructions were received'
