# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_MCU_LML_Np_1027_a
_database_code_depnum_ccdc_archive 'CCDC 2335543'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2024-02-26 deposited with the CCDC.	2024-05-01 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H20 Cl4 N4 Np'
_chemical_formula_weight         695.20

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   19.2449(8)
_cell_length_b                   9.5303(4)
_cell_length_c                   15.6081(11)
_cell_angle_alpha                90
_cell_angle_beta                 127.5220(10)
_cell_angle_gamma                90
_cell_volume                     2270.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    61182
_cell_measurement_theta_min      2.5196
_cell_measurement_theta_max      33.1838

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_F_000             1316
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.243
_exptl_absorpt_coefficient_mu    5.062
_shelx_estimated_absorpt_T_min   0.314
_shelx_estimated_absorpt_T_max   0.373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6470
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_process_details   
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D. (2015). J. Appl. Cryst. 48, 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_measurement_device       'three circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS D8 Quest'
_diffrn_detector_type            
'PhotonII charge-integrating pixel array (CPAD)'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            35651
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.669
_diffrn_reflns_theta_max         33.192
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4351
_reflns_number_gt                4231
_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      ' Apex4 v2022.10-1 (Bruker, 2022) '
_computing_cell_refinement       ' SAINT V8.40B (Bruker, 2020)'
_computing_data_reduction        ' SAINT V8.40B (Bruker, 2020)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0165P)²+3.0428P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   none
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.00027(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4351
_refine_ls_number_parameters     133
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0170
_refine_ls_R_factor_gt           0.0162
_refine_ls_wR_factor_ref         0.0403
_refine_ls_wR_factor_gt          0.0399
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_restrained_S_all      1.180
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Np1 Np 0.500000 0.64151(2) 0.250000 0.01418(3) Uani 1 2 d S T P . .
Cl1 Cl 0.64173(2) 0.72708(4) 0.27650(3) 0.02232(7) Uani 1 1 d . . . . .
Cl2 Cl 0.41527(3) 0.55581(4) 0.05018(3) 0.02462(8) Uani 1 1 d . . . . .
N1 N 0.55375(9) 0.87143(14) 0.37510(11) 0.0187(2) Uani 1 1 d . . . . .
N2 N 0.41344(9) 0.41349(15) 0.24030(11) 0.0189(2) Uani 1 1 d . . . . .
C1 C 0.49975(10) 0.97673(17) 0.35676(13) 0.0205(3) Uani 1 1 d . . . . .
H1 H 0.441263 0.974928 0.292050 0.025 Uiso 1 1 calc R U . . .
C2 C 0.52508(11) 1.08782(18) 0.42746(15) 0.0235(3) Uani 1 1 d . . . . .
H2 H 0.484700 1.160228 0.410928 0.028 Uiso 1 1 calc R U . . .
C3 C 0.61013(12) 1.09205(19) 0.52271(14) 0.0248(3) Uani 1 1 d . . . . .
H3 H 0.628682 1.165604 0.573503 0.030 Uiso 1 1 calc R U . . .
C4 C 0.66730(11) 0.98587(19) 0.54168(13) 0.0240(3) Uani 1 1 d . . . . .
H4 H 0.726391 0.986499 0.605177 0.029 Uiso 1 1 calc R U . . .
C5 C 0.63687(11) 0.87889(17) 0.46656(14) 0.0214(3) Uani 1 1 d . . . . .
H5 H 0.676654 0.806992 0.480191 0.026 Uiso 1 1 calc R U . . .
C6 C 0.38717(10) 0.40907(18) 0.30306(13) 0.0196(3) Uani 1 1 d . . . . .
H6 H 0.408571 0.478743 0.357301 0.024 Uiso 1 1 calc R U . . .
C7 C 0.33052(11) 0.30804(19) 0.29244(14) 0.0224(3) Uani 1 1 d . . . . .
H7 H 0.313017 0.309971 0.337685 0.027 Uiso 1 1 calc R U . . .
C8 C 0.29978(11) 0.20417(19) 0.21492(15) 0.0245(3) Uani 1 1 d . . . . .
H8 H 0.260400 0.134265 0.205338 0.029 Uiso 1 1 calc R U . . .
C9 C 0.32800(12) 0.20509(18) 0.15191(15) 0.0250(3) Uani 1 1 d . . . . .
H9 H 0.309181 0.134290 0.099092 0.030 Uiso 1 1 calc R U . . .
C10 C 0.38411(11) 0.31059(18) 0.16668(14) 0.0218(3) Uani 1 1 d . . . . .
H10 H 0.402744 0.310116 0.122595 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
Np1 Cl2 2.6188(4) . ?
Np1 Cl2 2.6188(4) 2_655 ?
Np1 Cl1 2.6269(4) 2_655 ?
Np1 Cl1 2.6270(4) . ?
Np1 N2 2.6857(14) 2_655 ?
Np1 N2 2.6857(14) . ?
Np1 N1 2.6877(14) . ?
Np1 N1 2.6877(14) 2_655 ?
N1 C1 1.344(2) . ?
N1 C5 1.349(2) . ?
N2 C10 1.346(2) . ?
N2 C6 1.349(2) . ?
C1 C2 1.386(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.388(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(2) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.387(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.386(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.388(2) . ?
C9 H9 0.9500 . ?
C10 H10 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
Cl2 Np1 Cl2 143.656(19) . 2_655 ?
Cl2 Np1 Cl1 94.338(13) . 2_655 ?
Cl2 Np1 Cl1 96.775(14) 2_655 2_655 ?
Cl2 Np1 Cl1 96.776(14) . . ?
Cl2 Np1 Cl1 94.340(13) 2_655 . ?
Cl1 Np1 Cl1 143.829(18) 2_655 . ?
Cl2 Np1 N2 74.32(3) . 2_655 ?
Cl2 Np1 N2 76.44(3) 2_655 2_655 ?
Cl1 Np1 N2 143.99(3) 2_655 2_655 ?
Cl1 Np1 N2 72.15(3) . 2_655 ?
Cl2 Np1 N2 76.44(3) . . ?
Cl2 Np1 N2 74.32(3) 2_655 . ?
Cl1 Np1 N2 72.15(3) 2_655 . ?
Cl1 Np1 N2 143.99(3) . . ?
N2 Np1 N2 71.97(6) 2_655 . ?
Cl2 Np1 N1 143.56(3) . . ?
Cl2 Np1 N1 72.79(3) 2_655 . ?
Cl1 Np1 N1 76.39(3) 2_655 . ?
Cl1 Np1 N1 74.29(3) . . ?
N2 Np1 N1 131.89(4) 2_655 . ?
N2 Np1 N1 130.67(4) . . ?
Cl2 Np1 N1 72.79(3) . 2_655 ?
Cl2 Np1 N1 143.56(3) 2_655 2_655 ?
Cl1 Np1 N1 74.29(3) 2_655 2_655 ?
Cl1 Np1 N1 76.39(3) . 2_655 ?
N2 Np1 N1 130.67(4) 2_655 2_655 ?
N2 Np1 N1 131.89(4) . 2_655 ?
N1 Np1 N1 70.77(6) . 2_655 ?
C1 N1 C5 116.79(14) . . ?
C1 N1 Np1 123.26(10) . . ?
C5 N1 Np1 119.69(10) . . ?
C10 N2 C6 116.71(14) . . ?
C10 N2 Np1 124.13(11) . . ?
C6 N2 Np1 118.56(10) . . ?
N1 C1 C2 123.32(15) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 119.24(16) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C4 C3 C2 118.15(16) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C5 C4 C3 118.97(15) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
N1 C5 C4 123.48(15) . . ?
N1 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
N2 C6 C7 123.35(15) . . ?
N2 C6 H6 118.3 . . ?
C7 C6 H6 118.3 . . ?
C8 C7 C6 119.13(16) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C7 118.19(16) . . ?
C9 C8 H8 120.9 . . ?
C7 C8 H8 120.9 . . ?
C8 C9 C10 119.29(16) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N2 C10 C9 123.29(16) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?

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
C5 N1 C1 C2 -1.4(3) . . . . ?
Np1 N1 C1 C2 172.67(13) . . . . ?
N1 C1 C2 C3 -0.3(3) . . . . ?
C1 C2 C3 C4 1.8(3) . . . . ?
C2 C3 C4 C5 -1.5(3) . . . . ?
C1 N1 C5 C4 1.8(3) . . . . ?
Np1 N1 C5 C4 -172.57(14) . . . . ?
C3 C4 C5 N1 -0.3(3) . . . . ?
C10 N2 C6 C7 -2.1(2) . . . . ?
Np1 N2 C6 C7 169.42(13) . . . . ?
N2 C6 C7 C8 1.1(3) . . . . ?
C6 C7 C8 C9 0.7(3) . . . . ?
C7 C8 C9 C10 -1.3(3) . . . . ?
C6 N2 C10 C9 1.4(2) . . . . ?
Np1 N2 C10 C9 -169.58(13) . . . . ?
C8 C9 C10 N2 0.3(3) . . . . ?

_refine_diff_density_max         1.537
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.106



_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_MCU_Np_1025_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2335544'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2024-02-26 deposited with the CCDC.	2024-05-01 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H12 Cl4 N4 Np'
_chemical_formula_sum            'C8 H12 Cl4 N4 Np'
_chemical_formula_weight         543.02

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   14.6308(5)
_cell_length_b                   8.4327(3)
_cell_length_c                   13.7095(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.6870(10)
_cell_angle_gamma                90
_cell_volume                     1690.71(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9757
_cell_measurement_theta_min      2.7857
_cell_measurement_theta_max      33.1300

_exptl_crystal_description       plate
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.133
_exptl_crystal_F_000             996
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.566
_exptl_crystal_size_mid          0.446
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    6.764
_shelx_estimated_absorpt_T_min   0.114
_shelx_estimated_absorpt_T_max   0.430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3794
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_measurement_device       'three circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS D8 Quest'
_diffrn_detector_type            
'PhotonII charge-integrating pixel array (CPAD)'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            10988
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.786
_diffrn_reflns_theta_max         33.153
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3213
_reflns_number_gt                3174
_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       ' Apex4 v2022.10-1 (Bruker, 2022) '
_computing_cell_refinement       ' SAINT V8.40B (Bruker, 2020)'
_computing_data_reduction        ' SAINT V8.40B (Bruker, 2020)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1.9835P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   none
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.00323(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3213
_refine_ls_number_parameters     81
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0161
_refine_ls_R_factor_gt           0.0157
_refine_ls_wR_factor_ref         0.0376
_refine_ls_wR_factor_gt          0.0375
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_restrained_S_all      1.261
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Np1 Np 0.500000 0.32138(2) 0.250000 0.01820(4) Uani 1 2 d S T P . .
Cl1 Cl 0.65172(3) 0.41011(6) 0.33983(4) 0.03088(9) Uani 1 1 d . . . . .
Cl2 Cl 0.57753(3) 0.23198(6) 0.09030(3) 0.02938(9) Uani 1 1 d . . . . .
N1 N 0.45230(13) 0.5731(2) 0.33858(12) 0.0307(3) Uani 1 1 d . . . . .
N2 N 0.41321(12) 0.06796(19) 0.19915(12) 0.0293(3) Uani 1 1 d . . . . .
C1 C 0.42313(14) 0.6780(2) 0.37946(14) 0.0256(3) Uani 1 1 d . . . . .
C2 C 0.38414(17) 0.8113(2) 0.43038(15) 0.0326(4) Uani 1 1 d . . . . .
H2A H 0.421311 0.906043 0.419823 0.049 Uiso 1 1 calc R U . . .
H2B H 0.383104 0.787869 0.500363 0.049 Uiso 1 1 calc R U . . .
H2C H 0.321617 0.829976 0.405408 0.049 Uiso 1 1 calc R U . . .
C3 C 0.36894(13) -0.0351(2) 0.17244(13) 0.0262(3) Uani 1 1 d . . . . .
C4 C 0.31199(17) -0.1654(3) 0.13830(19) 0.0403(5) Uani 1 1 d . . . . .
H4A H 0.289163 -0.143210 0.071773 0.060 Uiso 1 1 calc R U . . .
H4B H 0.260216 -0.177719 0.181417 0.060 Uiso 1 1 calc R U . . .
H4C H 0.348045 -0.263314 0.138610 0.060 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
Np1 N1 2.5526(17) 2_655 ?
Np1 N1 2.5526(17) . ?
Np1 N2 2.5716(16) 2_655 ?
Np1 N2 2.5716(16) . ?
Np1 Cl2 2.6067(4) . ?
Np1 Cl2 2.6067(4) 2_655 ?
Np1 Cl1 2.6159(4) 2_655 ?
Np1 Cl1 2.6159(4) . ?
N1 C1 1.137(2) . ?
N2 C3 1.138(2) . ?
C1 C2 1.449(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.448(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Np1 N1 67.51(8) 2_655 . ?
N1 Np1 N2 132.86(6) 2_655 2_655 ?
N1 Np1 N2 134.56(5) . 2_655 ?
N1 Np1 N2 134.56(5) 2_655 . ?
N1 Np1 N2 132.86(6) . . ?
N2 Np1 N2 67.60(8) 2_655 . ?
N1 Np1 Cl2 73.09(4) 2_655 . ?
N1 Np1 Cl2 140.52(4) . . ?
N2 Np1 Cl2 76.33(4) 2_655 . ?
N2 Np1 Cl2 75.85(4) . . ?
N1 Np1 Cl2 140.52(4) 2_655 2_655 ?
N1 Np1 Cl2 73.09(4) . 2_655 ?
N2 Np1 Cl2 75.85(4) 2_655 2_655 ?
N2 Np1 Cl2 76.33(4) . 2_655 ?
Cl2 Np1 Cl2 146.38(2) . 2_655 ?
N1 Np1 Cl1 77.19(4) 2_655 2_655 ?
N1 Np1 Cl1 75.29(4) . 2_655 ?
N2 Np1 Cl1 140.42(4) 2_655 2_655 ?
N2 Np1 Cl1 72.82(4) . 2_655 ?
Cl2 Np1 Cl1 94.100(16) . 2_655 ?
Cl2 Np1 Cl1 95.392(16) 2_655 2_655 ?
N1 Np1 Cl1 75.29(4) 2_655 . ?
N1 Np1 Cl1 77.19(4) . . ?
N2 Np1 Cl1 72.82(4) 2_655 . ?
N2 Np1 Cl1 140.42(4) . . ?
Cl2 Np1 Cl1 95.392(16) . . ?
Cl2 Np1 Cl1 94.098(16) 2_655 . ?
Cl1 Np1 Cl1 146.76(2) 2_655 . ?
C1 N1 Np1 173.30(17) . . ?
C3 N2 Np1 173.58(16) . . ?
N1 C1 C2 178.8(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 C4 179.5(2) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?


_refine_diff_density_max         0.968
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.124



####################################################################### 
# 
# 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_NP_1038_0m_b_xle
_database_code_depnum_ccdc_archive 'CCDC 2345808'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2024-04-04 deposited with the CCDC.	2024-05-01 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 Cl4 Np O2 P2'
_chemical_formula_sum            'C36 H30 Cl4 Np O2 P2'
_chemical_formula_weight         935.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -4.5053 13.9666 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   9.9552(5)
_cell_length_b                   15.3552(8)
_cell_length_c                   11.9194(6)
_cell_angle_alpha                90
_cell_angle_beta                 98.955(2)
_cell_angle_gamma                90
_cell_volume                     1799.84(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9110
_cell_measurement_theta_min      5.3934
_cell_measurement_theta_max      79.9919

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_F_000             906
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.052
_exptl_absorpt_coefficient_mu    17.733
_shelx_estimated_absorpt_T_min   0.176
_shelx_estimated_absorpt_T_max   0.459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5272
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_process_details   
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D. (2015). J. Appl. Cryst. 48, 3-10.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'I-mu-S 3.0 microsource X-ray tube'
_diffrn_source_current           '1.1 mA'
_diffrn_source_voltage           '50 kV'
_diffrn_radiation_monochromator  'HELIOS multilayer Montel optics'
_diffrn_measurement_device       'four circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS D8 Quest'
_diffrn_detector_type            
'PhotonIII_C14 charge-integrating and photon counting pixel array'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            63868
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.754
_diffrn_reflns_theta_max         80.612
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             7672
_reflns_number_gt                7496
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_max     0.943
_reflns_Friedel_fraction_full    0.985

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ' Apex4 v2022.10-1 (Bruker, 2022) '
_computing_cell_refinement       ' SAINT V8.40B (Bruker, 2020)'
_computing_data_reduction        ' SAINT V8.40B (Bruker, 2020)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0249P)²+1.8101P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   none
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.00020(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.324(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7672
_refine_ls_number_parameters     408
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0207
_refine_ls_wR_factor_ref         0.0519
_refine_ls_wR_factor_gt          0.0517
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Np1 Np 0.74122(2) 0.41575(3) 0.74150(2) 0.01864(6) Uani 1 1 d . . . . .
Cl1 Cl 0.89653(18) 0.55061(12) 0.75951(15) 0.0365(3) Uani 1 1 d . . . . .
Cl2 Cl 0.89971(16) 0.33265(11) 0.62295(14) 0.0340(3) Uani 1 1 d . . . . .
Cl3 Cl 0.56411(16) 0.49989(10) 0.84052(13) 0.0309(3) Uani 1 1 d . . . . .
Cl4 Cl 0.59037(17) 0.27599(11) 0.73663(14) 0.0341(3) Uani 1 1 d . . . . .
P1 P 0.55226(14) 0.52733(9) 0.49419(11) 0.0195(3) Uani 1 1 d . . . . .
P2 P 0.95517(16) 0.35839(10) 1.01642(14) 0.0234(3) Uani 1 1 d . . . . .
O1 O 0.6250(4) 0.4593(3) 0.5756(3) 0.0245(9) Uani 1 1 d . . . . .
O2 O 0.8596(4) 0.3691(3) 0.9044(4) 0.0275(9) Uani 1 1 d . . . . .
C1 C 0.5528(6) 0.4927(4) 0.3504(5) 0.0238(12) Uani 1 1 d . . . . .
C2 C 0.5828(7) 0.4062(6) 0.3294(5) 0.0342(15) Uani 1 1 d . . . . .
H2 H 0.610985 0.367252 0.390496 0.041 Uiso 1 1 calc R U . . .
C3 C 0.5708(9) 0.3777(5) 0.2177(6) 0.0399(17) Uani 1 1 d . . . . .
H3 H 0.590382 0.318663 0.202435 0.048 Uiso 1 1 calc R U . . .
C4 C 0.5312(7) 0.4336(5) 0.1293(6) 0.0354(18) Uani 1 1 d . . . . .
H4 H 0.521602 0.412939 0.053345 0.043 Uiso 1 1 calc R U . . .
C5 C 0.5053(7) 0.5195(5) 0.1501(6) 0.0367(15) Uani 1 1 d . . . . .
H5 H 0.480529 0.558424 0.088383 0.044 Uiso 1 1 calc R U . . .
C6 C 0.5151(7) 0.5496(5) 0.2607(5) 0.0321(14) Uani 1 1 d . . . . .
H6 H 0.496179 0.608888 0.275003 0.039 Uiso 1 1 calc R U . . .
C7 C 0.6336(6) 0.6307(4) 0.5156(5) 0.0254(12) Uani 1 1 d . . . . .
C8 C 0.7346(7) 0.6541(5) 0.4537(6) 0.0364(15) Uani 1 1 d . . . . .
H8 H 0.754231 0.617896 0.393617 0.044 Uiso 1 1 calc R U . . .
C9 C 0.8072(9) 0.7305(6) 0.4797(9) 0.048(2) Uani 1 1 d . . . . .
H9 H 0.875749 0.747103 0.436597 0.057 Uiso 1 1 calc R U . . .
C10 C 0.7802(8) 0.7823(5) 0.5676(8) 0.047(2) Uani 1 1 d . . . . .
H10 H 0.830778 0.834351 0.585151 0.056 Uiso 1 1 calc R U . . .
C11 C 0.6802(9) 0.7595(5) 0.6306(7) 0.0426(18) Uani 1 1 d . . . . .
H11 H 0.662672 0.795307 0.691713 0.051 Uiso 1 1 calc R U . . .
C12 C 0.6055(8) 0.6836(4) 0.6038(6) 0.0345(15) Uani 1 1 d . . . . .
H12 H 0.535383 0.668036 0.645728 0.041 Uiso 1 1 calc R U . . .
C13 C 0.8784(7) 0.2865(5) 1.1060(7) 0.0273(15) Uani 1 1 d . . . . .
C14 C 0.9051(8) 0.2939(5) 1.2234(6) 0.0369(16) Uani 1 1 d . . . . .
H14 H 0.961844 0.339348 1.257863 0.044 Uiso 1 1 calc R U . . .
C15 C 0.8485(9) 0.2346(6) 1.2900(6) 0.0451(19) Uani 1 1 d . . . . .
H15 H 0.868498 0.238422 1.370403 0.054 Uiso 1 1 calc R U . . .
C16 C 0.7628(7) 0.1697(5) 1.2398(6) 0.0367(16) Uani 1 1 d . . . . .
H16 H 0.723694 0.129531 1.286046 0.044 Uiso 1 1 calc R U . . .
C17 C 0.7342(8) 0.1630(5) 1.1242(6) 0.0383(16) Uani 1 1 d . . . . .
H17 H 0.674961 0.118429 1.090593 0.046 Uiso 1 1 calc R U . . .
C18 C 0.7918(8) 0.2215(5) 1.0550(6) 0.0354(15) Uani 1 1 d . . . . .
H18 H 0.772255 0.216900 0.974654 0.042 Uiso 1 1 calc R U . . .
C19 C 0.3781(6) 0.5354(4) 0.5150(5) 0.0218(11) Uani 1 1 d . . . . .
C20 C 0.2958(7) 0.6019(4) 0.4661(5) 0.0290(13) Uani 1 1 d . . . . .
H20 H 0.332716 0.647767 0.426875 0.035 Uiso 1 1 calc R U . . .
C21 C 0.1579(8) 0.6010(5) 0.4749(6) 0.0324(17) Uani 1 1 d . . . . .
H21 H 0.100241 0.645854 0.439974 0.039 Uiso 1 1 calc R U . . .
C22 C 0.1045(7) 0.5358(5) 0.5337(6) 0.0344(15) Uani 1 1 d . . . . .
H22 H 0.010104 0.535563 0.538356 0.041 Uiso 1 1 calc R U . . .
C23 C 0.1874(7) 0.4707(5) 0.5859(6) 0.0339(15) Uani 1 1 d . . . . .
H23 H 0.150769 0.426836 0.628519 0.041 Uiso 1 1 calc R U . . .
C24 C 0.3246(7) 0.4696(4) 0.5759(5) 0.0271(13) Uani 1 1 d . . . . .
H24 H 0.381718 0.424360 0.610376 0.033 Uiso 1 1 calc R U . . .
C25 C 1.1153(7) 0.3148(4) 0.9929(5) 0.0271(13) Uani 1 1 d . . . . .
C26 C 1.1747(7) 0.3487(5) 0.9038(6) 0.0315(14) Uani 1 1 d . . . . .
H26 H 1.128241 0.391711 0.855195 0.038 Uiso 1 1 calc R U . . .
C27 C 1.3017(7) 0.3195(5) 0.8862(6) 0.0372(16) Uani 1 1 d . . . . .
H27 H 1.342484 0.342690 0.825754 0.045 Uiso 1 1 calc R U . . .
C28 C 1.3686(7) 0.2567(5) 0.9566(7) 0.0394(17) Uani 1 1 d . . . . .
H28 H 1.455962 0.237247 0.944879 0.047 Uiso 1 1 calc R U . . .
C29 C 1.3093(8) 0.2218(5) 1.0443(6) 0.0379(16) Uani 1 1 d . . . . .
H29 H 1.355883 0.178291 1.091871 0.046 Uiso 1 1 calc R U . . .
C30 C 1.1828(7) 0.2500(4) 1.0630(6) 0.0313(14) Uani 1 1 d . . . . .
H30 H 1.141928 0.225667 1.122747 0.038 Uiso 1 1 calc R U . . .
C31 C 0.9860(7) 0.4616(5) 1.0864(6) 0.0277(13) Uani 1 1 d . . . . .
C32 C 0.8744(9) 0.5126(6) 1.1004(7) 0.0365(18) Uani 1 1 d . . . . .
H32 H 0.784900 0.492381 1.073633 0.044 Uiso 1 1 calc R U . . .
C33 C 0.8938(9) 0.5929(5) 1.1535(7) 0.0442(18) Uani 1 1 d . . . . .
H33 H 0.817656 0.626824 1.165914 0.053 Uiso 1 1 calc R U . . .
C34 C 1.0236(9) 0.6234(5) 1.1884(6) 0.0462(19) Uani 1 1 d . . . . .
H34 H 1.036688 0.679194 1.222900 0.055 Uiso 1 1 calc R U . . .
C35 C 1.1345(9) 0.5739(5) 1.1735(7) 0.0469(19) Uani 1 1 d . . . . .
H35 H 1.223627 0.595515 1.198120 0.056 Uiso 1 1 calc R U . . .
C36 C 1.1171(8) 0.4926(5) 1.1229(6) 0.0380(16) Uani 1 1 d . . . . .
H36 H 1.193856 0.458315 1.113231 0.046 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
Np1 O2 2.227(4) . ?
Np1 O1 2.233(4) . ?
Np1 Cl1 2.5732(17) . ?
Np1 Cl2 2.6093(15) . ?
Np1 Cl3 2.6113(15) . ?
Np1 Cl4 2.6148(17) . ?
P1 O1 1.528(4) . ?
P1 C7 1.782(6) . ?
P1 C19 1.794(6) . ?
P1 C1 1.795(6) . ?
P2 O2 1.523(4) . ?
P2 C13 1.788(7) . ?
P2 C25 1.791(7) . ?
P2 C31 1.794(7) . ?
C1 C6 1.387(9) . ?
C1 C2 1.393(10) . ?
C2 C3 1.389(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.369(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(9) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.384(10) . ?
C7 C12 1.392(10) . ?
C8 C9 1.388(12) . ?
C8 H8 0.9500 . ?
C9 C10 1.375(14) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(10) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.388(10) . ?
C13 C18 1.395(11) . ?
C14 C15 1.383(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(11) . ?
C15 H15 0.9500 . ?
C16 C17 1.367(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.401(10) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.381(9) . ?
C19 C24 1.397(9) . ?
C20 C21 1.393(10) . ?
C20 H20 0.9500 . ?
C21 C22 1.375(11) . ?
C21 H21 0.9500 . ?
C22 C23 1.382(11) . ?
C22 H22 0.9500 . ?
C23 C24 1.389(9) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.394(9) . ?
C25 C30 1.401(9) . ?
C26 C27 1.388(10) . ?
C26 H26 0.9500 . ?
C27 C28 1.379(11) . ?
C27 H27 0.9500 . ?
C28 C29 1.386(12) . ?
C28 H28 0.9500 . ?
C29 C30 1.382(10) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.391(11) . ?
C31 C36 1.394(10) . ?
C32 C33 1.386(11) . ?
C32 H32 0.9500 . ?
C33 C34 1.377(12) . ?
C33 H33 0.9500 . ?
C34 C35 1.374(12) . ?
C34 H34 0.9500 . ?
C35 C36 1.385(11) . ?
C35 H35 0.9500 . ?
C36 H36 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 Np1 O1 178.34(18) . . ?
O2 Np1 Cl1 87.52(13) . . ?
O1 Np1 Cl1 93.12(13) . . ?
O2 Np1 Cl2 91.85(13) . . ?
O1 Np1 Cl2 86.59(12) . . ?
Cl1 Np1 Cl2 91.87(5) . . ?
O2 Np1 Cl3 93.90(12) . . ?
O1 Np1 Cl3 87.64(12) . . ?
Cl1 Np1 Cl3 90.19(6) . . ?
Cl2 Np1 Cl3 173.97(5) . . ?
O2 Np1 Cl4 88.82(13) . . ?
O1 Np1 Cl4 90.56(12) . . ?
Cl1 Np1 Cl4 176.28(6) . . ?
Cl2 Np1 Cl4 88.87(6) . . ?
Cl3 Np1 Cl4 89.44(5) . . ?
O1 P1 C7 111.0(3) . . ?
O1 P1 C19 109.4(3) . . ?
C7 P1 C19 110.2(3) . . ?
O1 P1 C1 109.4(3) . . ?
C7 P1 C1 109.4(3) . . ?
C19 P1 C1 107.4(3) . . ?
O2 P2 C13 108.9(3) . . ?
O2 P2 C25 110.7(3) . . ?
C13 P2 C25 109.6(3) . . ?
O2 P2 C31 110.5(3) . . ?
C13 P2 C31 109.0(3) . . ?
C25 P2 C31 108.1(3) . . ?
P1 O1 Np1 153.6(3) . . ?
P2 O2 Np1 166.6(3) . . ?
C6 C1 C2 120.1(6) . . ?
C6 C1 P1 120.6(5) . . ?
C2 C1 P1 119.2(5) . . ?
C3 C2 C1 119.0(7) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C4 C3 C2 120.8(7) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 120.2(6) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 120.3(7) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 119.6(6) . . ?
C5 C6 H6 120.2 . . ?
C1 C6 H6 120.2 . . ?
C8 C7 C12 120.0(6) . . ?
C8 C7 P1 120.4(5) . . ?
C12 C7 P1 119.2(5) . . ?
C7 C8 C9 119.8(8) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 120.2(8) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 120.7(7) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C10 C11 C12 119.4(8) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C7 C12 C11 119.9(7) . . ?
C7 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C14 C13 C18 120.4(7) . . ?
C14 C13 P2 121.2(6) . . ?
C18 C13 P2 118.3(6) . . ?
C15 C14 C13 119.5(7) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 120.3(7) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C17 C16 C15 120.5(7) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 120.3(7) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C13 C18 C17 119.0(7) . . ?
C13 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C20 C19 C24 120.3(6) . . ?
C20 C19 P1 121.0(5) . . ?
C24 C19 P1 118.5(5) . . ?
C19 C20 C21 119.2(6) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
C22 C21 C20 120.6(7) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 120.3(6) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C22 C23 C24 119.8(6) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C23 C24 C19 119.7(6) . . ?
C23 C24 H24 120.2 . . ?
C19 C24 H24 120.2 . . ?
C26 C25 C30 119.9(6) . . ?
C26 C25 P2 118.2(5) . . ?
C30 C25 P2 121.8(5) . . ?
C27 C26 C25 119.9(6) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C28 C27 C26 119.9(7) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.4(7) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C30 C29 C28 120.5(7) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C29 C30 C25 119.3(7) . . ?
C29 C30 H30 120.3 . . ?
C25 C30 H30 120.3 . . ?
C32 C31 C36 119.8(7) . . ?
C32 C31 P2 118.1(6) . . ?
C36 C31 P2 122.1(6) . . ?
C33 C32 C31 119.9(8) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C34 C33 C32 119.9(8) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C35 C34 C33 120.5(8) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C34 C35 C36 120.4(8) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C35 C36 C31 119.5(7) . . ?
C35 C36 H36 120.3 . . ?
C31 C36 H36 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 P1 O1 Np1 34.6(7) . . . . ?
C19 P1 O1 Np1 -87.2(6) . . . . ?
C1 P1 O1 Np1 155.4(6) . . . . ?
C13 P2 O2 Np1 148.5(12) . . . . ?
C25 P2 O2 Np1 -91.0(13) . . . . ?
C31 P2 O2 Np1 28.8(13) . . . . ?
O1 P1 C1 C6 -168.4(5) . . . . ?
C7 P1 C1 C6 -46.6(6) . . . . ?
C19 P1 C1 C6 73.0(6) . . . . ?
O1 P1 C1 C2 15.8(6) . . . . ?
C7 P1 C1 C2 137.6(5) . . . . ?
C19 P1 C1 C2 -102.8(5) . . . . ?
C6 C1 C2 C3 -1.7(10) . . . . ?
P1 C1 C2 C3 174.1(6) . . . . ?
C1 C2 C3 C4 0.5(12) . . . . ?
C2 C3 C4 C5 1.3(12) . . . . ?
C3 C4 C5 C6 -1.9(12) . . . . ?
C4 C5 C6 C1 0.7(11) . . . . ?
C2 C1 C6 C5 1.1(10) . . . . ?
P1 C1 C6 C5 -174.6(5) . . . . ?
O1 P1 C7 C8 91.6(6) . . . . ?
C19 P1 C7 C8 -147.1(5) . . . . ?
C1 P1 C7 C8 -29.2(6) . . . . ?
O1 P1 C7 C12 -81.2(6) . . . . ?
C19 P1 C7 C12 40.1(6) . . . . ?
C1 P1 C7 C12 158.0(5) . . . . ?
C12 C7 C8 C9 -0.2(11) . . . . ?
P1 C7 C8 C9 -173.1(6) . . . . ?
C7 C8 C9 C10 0.9(13) . . . . ?
C8 C9 C10 C11 -0.4(13) . . . . ?
C9 C10 C11 C12 -0.6(12) . . . . ?
C8 C7 C12 C11 -0.8(10) . . . . ?
P1 C7 C12 C11 172.1(5) . . . . ?
C10 C11 C12 C7 1.2(11) . . . . ?
O2 P2 C13 C14 -150.3(6) . . . . ?
C25 P2 C13 C14 88.5(7) . . . . ?
C31 P2 C13 C14 -29.7(7) . . . . ?
O2 P2 C13 C18 30.5(7) . . . . ?
C25 P2 C13 C18 -90.6(6) . . . . ?
C31 P2 C13 C18 151.2(6) . . . . ?
C18 C13 C14 C15 2.0(12) . . . . ?
P2 C13 C14 C15 -177.1(6) . . . . ?
C13 C14 C15 C16 -1.7(13) . . . . ?
C14 C15 C16 C17 0.6(13) . . . . ?
C15 C16 C17 C18 0.3(12) . . . . ?
C14 C13 C18 C17 -1.1(11) . . . . ?
P2 C13 C18 C17 178.1(6) . . . . ?
C16 C17 C18 C13 -0.1(12) . . . . ?
O1 P1 C19 C20 169.1(5) . . . . ?
C7 P1 C19 C20 46.8(6) . . . . ?
C1 P1 C19 C20 -72.3(6) . . . . ?
O1 P1 C19 C24 -15.0(5) . . . . ?
C7 P1 C19 C24 -137.3(5) . . . . ?
C1 P1 C19 C24 103.6(5) . . . . ?
C24 C19 C20 C21 -2.2(9) . . . . ?
P1 C19 C20 C21 173.6(5) . . . . ?
C19 C20 C21 C22 1.4(10) . . . . ?
C20 C21 C22 C23 0.7(11) . . . . ?
C21 C22 C23 C24 -2.0(10) . . . . ?
C22 C23 C24 C19 1.3(9) . . . . ?
C20 C19 C24 C23 0.8(9) . . . . ?
P1 C19 C24 C23 -175.1(5) . . . . ?
O2 P2 C25 C26 43.9(6) . . . . ?
C13 P2 C25 C26 164.0(5) . . . . ?
C31 P2 C25 C26 -77.2(6) . . . . ?
O2 P2 C25 C30 -137.8(5) . . . . ?
C13 P2 C25 C30 -17.8(7) . . . . ?
C31 P2 C25 C30 101.0(6) . . . . ?
C30 C25 C26 C27 -1.3(10) . . . . ?
P2 C25 C26 C27 176.9(6) . . . . ?
C25 C26 C27 C28 0.3(11) . . . . ?
C26 C27 C28 C29 0.6(11) . . . . ?
C27 C28 C29 C30 -0.5(11) . . . . ?
C28 C29 C30 C25 -0.5(11) . . . . ?
C26 C25 C30 C29 1.4(10) . . . . ?
P2 C25 C30 C29 -176.8(5) . . . . ?
O2 P2 C31 C32 50.8(6) . . . . ?
C13 P2 C31 C32 -68.8(7) . . . . ?
C25 P2 C31 C32 172.0(6) . . . . ?
O2 P2 C31 C36 -127.0(6) . . . . ?
C13 P2 C31 C36 113.4(6) . . . . ?
C25 P2 C31 C36 -5.7(7) . . . . ?
C36 C31 C32 C33 -1.9(11) . . . . ?
P2 C31 C32 C33 -179.7(6) . . . . ?
C31 C32 C33 C34 2.5(12) . . . . ?
C32 C33 C34 C35 -1.7(13) . . . . ?
C33 C34 C35 C36 0.2(13) . . . . ?
C34 C35 C36 C31 0.4(12) . . . . ?
C32 C31 C36 C35 0.4(11) . . . . ?
P2 C31 C36 C35 178.1(6) . . . . ?

_refine_diff_density_max         1.018
_refine_diff_density_min         -1.493
_refine_diff_density_rms         0.098



####################################################################### 
# 
# 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_Np_19_0m
_database_code_depnum_ccdc_archive 'CCDC 2335545'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2024-02-26 deposited with the CCDC.	2024-05-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H48 Cl4 N4 Np, 2.441(C4 H8 O)'
_chemical_formula_sum            'C45.76 H67.53 Cl4 N4 Np O2.44'
_chemical_formula_weight         1091.64

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   16.6555(6)
_cell_length_b                   11.5350(4)
_cell_length_c                   25.7510(9)
_cell_angle_alpha                90
_cell_angle_beta                 94.5345(14)
_cell_angle_gamma                90
_cell_volume                     4931.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9992
_cell_measurement_theta_min      2.4535
_cell_measurement_theta_max      30.4897

_exptl_crystal_description       plate
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_F_000             2202.6
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.037
_exptl_absorpt_coefficient_mu    2.363
_shelx_estimated_absorpt_T_min   0.601
_shelx_estimated_absorpt_T_max   0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5783
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_measurement_device_type  
;
Bruker AXS D8 Quest diffractometer with PhotonII charge-integrating pixel 
array detector (CPAD)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            89329
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.374
_diffrn_reflns_theta_max         30.549
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             15071
_reflns_number_gt                12148
_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       'Apex4 v2021.4-0 (Bruker, 2021)'
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
;  
SHELXL-2019/3 (Sheldrick, 2015, 2019), 
SHELXLE Rev1275(Hübschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
5 reflections were ommitted from refinement due to partial obstruction 
by the beamstop and due to a non-integratable minor twin domain.

#---

A THF molecule was found to be disordered about two positions, which has
close contact with H27 of one of the di-tert-butylbipyridine ligands. The
Uij components of the ADPs of atoms closer to each other than 2.0 Angstrom
were restrained to be similar with an esd of 0.01 Angstrom squared. 
Geometries were restrained to be similar to each other. Subject to these 
conditions, this resulted in the most well defined THF molecule in the 
structure solution, with an occupancy ratio refining to 0.533(11):0.467(11).

#---

Another 4 THF molecules were found to be disordered over 10 positions 
in the volume between metal complexes. 5 of the positions are unique, the 
others are created by inversion symmetry. Two distinct THF moieties partially 
overlap with their symmetry-related positions through the inversion center 
(THFs O2 and O6, respectively) while the other moieties are generally 
disordered (THFs O3, O4, O5). 

The Uij components of the ADPs of atoms closer to each other than 2.0 
Angstrom were restrained to be similar with an esd of 0.01 Angstrom
squared. Atom  positions were restrained to be similar to the well-defined 
THF O1. Subject to these conditions the occupancy ratio associated
with these THF molecule positions refined to:
THF O2 = 0.280(13)
THF O3 = 0.367(10)
THF O4 = 0.229(9)
THF O5 = 0.141(4)
THF O6 = 0.330(13)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0421P)²+10.2109P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.00166(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         15071
_refine_ls_number_parameters     740
_refine_ls_number_restraints     828
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0937
_refine_ls_wR_factor_gt          0.0869
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Np1 Np 0.60439(2) 0.60012(2) 0.34221(2) 0.02121(5) Uani 1 1 d . . . . .
Cl1 Cl 0.72760(6) 0.73629(8) 0.36777(4) 0.0379(2) Uani 1 1 d . . . . .
Cl2 Cl 0.70379(6) 0.42595(8) 0.34244(4) 0.0392(2) Uani 1 1 d . . . . .
Cl3 Cl 0.50081(6) 0.69930(9) 0.39996(4) 0.0385(2) Uani 1 1 d . . . . .
Cl4 Cl 0.48809(6) 0.56869(9) 0.26847(4) 0.0397(2) Uani 1 1 d . . . . .
N1 N 0.66372(17) 0.6197(2) 0.25105(10) 0.0237(5) Uani 1 1 d . . . . .
N2 N 0.58521(17) 0.7982(2) 0.29385(10) 0.0251(5) Uani 1 1 d . . . . .
N3 N 0.64216(19) 0.5345(3) 0.43971(11) 0.0298(6) Uani 1 1 d . . . . .
N4 N 0.52614(18) 0.4218(2) 0.37778(11) 0.0257(5) Uani 1 1 d . . . . .
C1 C 0.7000(2) 0.5305(3) 0.22857(13) 0.0283(7) Uani 1 1 d . . . . .
H1 H 0.712631 0.463697 0.249207 0.034 Uiso 1 1 calc R U . . .
C2 C 0.7200(2) 0.5295(3) 0.17762(13) 0.0300(7) Uani 1 1 d . . . . .
H2 H 0.746393 0.464139 0.164358 0.036 Uiso 1 1 calc R U . . .
C3 C 0.7014(2) 0.6245(3) 0.14579(13) 0.0270(6) Uani 1 1 d . . . . .
C4 C 0.6635(2) 0.7165(3) 0.16852(13) 0.0267(6) Uani 1 1 d . . . . .
H4 H 0.649108 0.783153 0.148195 0.032 Uiso 1 1 calc R U . . .
C5 C 0.64596(19) 0.7131(3) 0.22094(12) 0.0225(6) Uani 1 1 d . . . . .
C6 C 0.60845(18) 0.8134(3) 0.24542(12) 0.0220(6) Uani 1 1 d . . . . .
C7 C 0.5993(2) 0.9205(3) 0.22006(12) 0.0250(6) Uani 1 1 d . . . . .
H7 H 0.616633 0.928481 0.185958 0.030 Uiso 1 1 calc R U . . .
C8 C 0.56575(19) 1.0153(3) 0.24337(13) 0.0245(6) Uani 1 1 d . . . . .
C9 C 0.5455(2) 0.9985(3) 0.29426(14) 0.0315(7) Uani 1 1 d . . . . .
H9 H 0.524286 1.061038 0.312941 0.038 Uiso 1 1 calc R U . . .
C10 C 0.5562(2) 0.8907(3) 0.31778(13) 0.0312(7) Uani 1 1 d . . . . .
H10 H 0.542219 0.881959 0.352624 0.037 Uiso 1 1 calc R U . . .
C11 C 0.7244(3) 0.6262(3) 0.08937(14) 0.0356(8) Uani 1 1 d . . . . .
C12 C 0.6889(3) 0.7310(4) 0.05945(15) 0.0450(10) Uani 1 1 d . . . . .
H12A H 0.702795 0.727149 0.023211 0.067 Uiso 1 1 calc R U . . .
H12B H 0.710983 0.802350 0.075586 0.067 Uiso 1 1 calc R U . . .
H12C H 0.630198 0.730853 0.060345 0.067 Uiso 1 1 calc R U . . .
C13 C 0.8164(3) 0.6306(4) 0.09018(17) 0.0445(10) Uani 1 1 d . . . . .
H13A H 0.838974 0.556315 0.102736 0.067 Uiso 1 1 calc R U . . .
H13B H 0.836972 0.692911 0.113433 0.067 Uiso 1 1 calc R U . . .
H13C H 0.832122 0.645272 0.054901 0.067 Uiso 1 1 calc R U . . .
C14 C 0.6929(3) 0.5170(4) 0.06076(17) 0.0534(12) Uani 1 1 d . . . . .
H14A H 0.708380 0.518496 0.024839 0.080 Uiso 1 1 calc R U . . .
H14B H 0.634048 0.514222 0.060555 0.080 Uiso 1 1 calc R U . . .
H14C H 0.716067 0.448220 0.078586 0.080 Uiso 1 1 calc R U . . .
C15 C 0.5529(2) 1.1327(3) 0.21707(14) 0.0298(7) Uani 1 1 d . . . . .
C16 C 0.6094(3) 1.2219(3) 0.2447(2) 0.0473(11) Uani 1 1 d . . . . .
H16A H 0.665325 1.202094 0.239222 0.071 Uiso 1 1 calc R U . . .
H16B H 0.602059 1.221462 0.282062 0.071 Uiso 1 1 calc R U . . .
H16C H 0.596956 1.299169 0.230423 0.071 Uiso 1 1 calc R U . . .
C17 C 0.4650(3) 1.1693(4) 0.22082(18) 0.0420(9) Uani 1 1 d . . . . .
H17A H 0.456786 1.247277 0.206243 0.063 Uiso 1 1 calc R U . . .
H17B H 0.452767 1.169475 0.257427 0.063 Uiso 1 1 calc R U . . .
H17C H 0.429316 1.114542 0.201200 0.063 Uiso 1 1 calc R U . . .
C18 C 0.5682(3) 1.1262(4) 0.15901(17) 0.0489(11) Uani 1 1 d . . . . .
H18A H 0.531531 1.069336 0.141587 0.073 Uiso 1 1 calc R U . . .
H18B H 0.624010 1.102576 0.155537 0.073 Uiso 1 1 calc R U . . .
H18C H 0.558679 1.202456 0.142921 0.073 Uiso 1 1 calc R U . . .
C19 C 0.7033(3) 0.5825(4) 0.46886(16) 0.0454(11) Uani 1 1 d . . . . .
H19 H 0.725867 0.652051 0.456663 0.054 Uiso 1 1 calc R U . . .
C20 C 0.7359(3) 0.5373(4) 0.51569(16) 0.0453(10) Uani 1 1 d . . . . .
H20 H 0.779851 0.575255 0.534367 0.054 Uiso 1 1 calc R U . . .
C21 C 0.7045(2) 0.4369(3) 0.53519(13) 0.0314(7) Uani 1 1 d . . . . .
C22 C 0.6382(2) 0.3915(3) 0.50679(11) 0.0248(6) Uani 1 1 d . . . . .
H22 H 0.612425 0.325080 0.519666 0.030 Uiso 1 1 calc R U . . .
C23 C 0.6076(2) 0.4406(3) 0.45941(12) 0.0248(6) Uani 1 1 d . . . . .
C24 C 0.53899(19) 0.3868(3) 0.42805(12) 0.0237(6) Uani 1 1 d . . . . .
C25 C 0.4924(2) 0.2996(3) 0.44840(13) 0.0290(7) Uani 1 1 d . . . . .
H25 H 0.500526 0.281135 0.484378 0.035 Uiso 1 1 calc R U . . .
C26 C 0.4348(2) 0.2398(3) 0.41769(14) 0.0292(7) Uani 1 1 d . . . . .
C27 C 0.4246(2) 0.2742(3) 0.36575(15) 0.0339(7) Uani 1 1 d . . . . .
H27 H 0.386480 0.235606 0.342420 0.041 Uiso 1 1 calc R U . . .
C28 C 0.4697(2) 0.3643(3) 0.34809(14) 0.0324(7) Uani 1 1 d . . . . .
H28 H 0.460102 0.386847 0.312663 0.039 Uiso 1 1 calc R U . . .
C29 C 0.7411(3) 0.3824(4) 0.58554(15) 0.0411(9) Uani 1 1 d . . . . .
C30 C 0.7104(4) 0.4490(5) 0.63164(17) 0.0671(16) Uani 1 1 d . . . . .
H30A H 0.731574 0.528324 0.631997 0.101 Uiso 1 1 calc R U . . .
H30B H 0.728704 0.410036 0.664273 0.101 Uiso 1 1 calc R U . . .
H30C H 0.651428 0.451254 0.628091 0.101 Uiso 1 1 calc R U . . .
C31 C 0.8340(3) 0.3897(6) 0.5876(2) 0.0696(17) Uani 1 1 d . . . . .
H31A H 0.852606 0.358742 0.555230 0.104 Uiso 1 1 calc R U . . .
H31B H 0.857424 0.344253 0.617205 0.104 Uiso 1 1 calc R U . . .
H31C H 0.850855 0.470808 0.591759 0.104 Uiso 1 1 calc R U . . .
C32 C 0.7180(3) 0.2546(4) 0.59036(16) 0.0424(9) Uani 1 1 d . . . . .
H32A H 0.659632 0.248234 0.592372 0.064 Uiso 1 1 calc R U . . .
H32B H 0.745824 0.221818 0.621953 0.064 Uiso 1 1 calc R U . . .
H32C H 0.733677 0.211979 0.559839 0.064 Uiso 1 1 calc R U . . .
C33 C 0.3868(3) 0.1378(4) 0.43708(16) 0.0376(8) Uani 1 1 d . . . . .
C34 C 0.4173(4) 0.0279(4) 0.4116(2) 0.0605(14) Uani 1 1 d . . . . .
H34A H 0.406606 0.033269 0.373705 0.091 Uiso 1 1 calc R U . . .
H34B H 0.389477 -0.039900 0.424462 0.091 Uiso 1 1 calc R U . . .
H34C H 0.475409 0.019993 0.420337 0.091 Uiso 1 1 calc R U . . .
C35 C 0.4000(4) 0.1228(5) 0.49631(19) 0.0587(14) Uani 1 1 d . . . . .
H35A H 0.368899 0.056111 0.507118 0.088 Uiso 1 1 calc R U . . .
H35B H 0.382290 0.192893 0.513591 0.088 Uiso 1 1 calc R U . . .
H35C H 0.457387 0.109694 0.506084 0.088 Uiso 1 1 calc R U . . .
C36 C 0.2981(3) 0.1523(6) 0.4224(3) 0.0706(17) Uani 1 1 d . . . . .
H36A H 0.289259 0.165805 0.384851 0.106 Uiso 1 1 calc R U . . .
H36B H 0.277806 0.218647 0.441251 0.106 Uiso 1 1 calc R U . . .
H36C H 0.269518 0.081939 0.431684 0.106 Uiso 1 1 calc R U . . .
O1 O 0.2750(5) 0.2505(8) 0.2542(5) 0.072(2) Uani 0.533(11) 1 d D U P A 1
C37 C 0.1993(7) 0.2343(12) 0.2780(6) 0.081(2) Uani 0.533(11) 1 d D U P A 1
H37A H 0.210920 0.217446 0.315588 0.098 Uiso 0.533(11) 1 calc R U P A 1
H37B H 0.170688 0.166538 0.261849 0.098 Uiso 0.533(11) 1 calc R U P A 1
C38 C 0.1469(6) 0.3370(12) 0.2720(6) 0.077(2) Uani 0.533(11) 1 d D U P A 1
H38A H 0.144114 0.378236 0.305555 0.092 Uiso 0.533(11) 1 calc R U P A 1
H38B H 0.091736 0.315611 0.258164 0.092 Uiso 0.533(11) 1 calc R U P A 1
C39 C 0.1886(8) 0.4099(14) 0.2334(8) 0.075(2) Uani 0.533(11) 1 d D U P A 1
H39A H 0.183499 0.493590 0.240895 0.091 Uiso 0.533(11) 1 calc R U P A 1
H39B H 0.166375 0.394474 0.197224 0.091 Uiso 0.533(11) 1 calc R U P A 1
C40 C 0.2759(8) 0.3701(15) 0.2418(11) 0.069(2) Uani 0.533(11) 1 d D U P A 1
H40A H 0.303980 0.382801 0.209782 0.083 Uiso 0.533(11) 1 calc R U P A 1
H40B H 0.304312 0.414426 0.270578 0.083 Uiso 0.533(11) 1 calc R U P A 1
O1B O 0.2720(7) 0.2659(11) 0.2788(5) 0.081(2) Uani 0.467(11) 1 d D U P A 2
C37B C 0.1925(8) 0.2285(13) 0.2611(7) 0.079(3) Uani 0.467(11) 1 d D U P A 2
H37C H 0.164065 0.199664 0.290838 0.094 Uiso 0.467(11) 1 calc R U P A 2
H37D H 0.195535 0.164630 0.235636 0.094 Uiso 0.467(11) 1 calc R U P A 2
C38B C 0.1475(7) 0.3292(12) 0.2360(6) 0.072(2) Uani 0.467(11) 1 d D U P A 2
H38C H 0.108046 0.360216 0.259187 0.087 Uiso 0.467(11) 1 calc R U P A 2
H38D H 0.118420 0.305336 0.202643 0.087 Uiso 0.467(11) 1 calc R U P A 2
C39B C 0.2108(9) 0.4190(14) 0.2266(9) 0.071(2) Uani 0.467(11) 1 d D U P A 2
H39C H 0.209325 0.440228 0.189326 0.085 Uiso 0.467(11) 1 calc R U P A 2
H39D H 0.203236 0.489792 0.247435 0.085 Uiso 0.467(11) 1 calc R U P A 2
C40B C 0.2887(9) 0.3587(19) 0.2443(13) 0.070(2) Uani 0.467(11) 1 d D U P A 2
H40C H 0.314227 0.327727 0.213709 0.084 Uiso 0.467(11) 1 calc R U P A 2
H40D H 0.326408 0.414568 0.262386 0.084 Uiso 0.467(11) 1 calc R U P A 2
O2 O 0.397(2) 0.791(3) 0.0623(12) 0.138(4) Uani 0.280(13) 1 d D U P B -1
C41 C 0.408(3) 0.761(3) 0.0083(13) 0.139(4) Uani 0.280(13) 1 d D U P B -1
H41A H 0.355416 0.750347 -0.011475 0.167 Uiso 0.280(13) 1 calc R U P B -1
H41B H 0.439579 0.688622 0.006605 0.167 Uiso 0.280(13) 1 calc R U P B -1
C42 C 0.453(3) 0.860(4) -0.0139(11) 0.140(4) Uani 0.280(13) 1 d D U P B -1
H42A H 0.415302 0.917967 -0.030537 0.168 Uiso 0.280(13) 1 calc R U P B -1
H42B H 0.489556 0.832407 -0.039710 0.168 Uiso 0.280(13) 1 calc R U P B -1
C43 C 0.499(2) 0.909(4) 0.0340(14) 0.139(4) Uani 0.280(13) 1 d D U P B -1
H43A H 0.483801 0.990601 0.039793 0.167 Uiso 0.280(13) 1 calc R U P B -1
H43B H 0.558017 0.905465 0.030541 0.167 Uiso 0.280(13) 1 calc R U P B -1
C44 C 0.476(2) 0.832(4) 0.0785(12) 0.139(4) Uani 0.280(13) 1 d D U P B -1
H44A H 0.513855 0.766137 0.083961 0.167 Uiso 0.280(13) 1 calc R U P B -1
H44B H 0.475468 0.876462 0.111257 0.167 Uiso 0.280(13) 1 calc R U P B -1
O3 O 0.4497(15) 0.3919(17) 0.1033(9) 0.152(5) Uani 0.367(10) 1 d D U P C 2
C45 C 0.4916(18) 0.480(2) 0.1345(10) 0.145(5) Uani 0.367(10) 1 d D U P C 2
H45A H 0.549196 0.482874 0.127564 0.174 Uiso 0.367(10) 1 calc R U P C 2
H45B H 0.487488 0.465607 0.172047 0.174 Uiso 0.367(10) 1 calc R U P C 2
C46 C 0.450(3) 0.591(2) 0.1180(13) 0.143(4) Uani 0.367(10) 1 d D U P C 2
H46A H 0.483396 0.659899 0.127969 0.172 Uiso 0.367(10) 1 calc R U P C 2
H46B H 0.396920 0.598531 0.132525 0.172 Uiso 0.367(10) 1 calc R U P C 2
C47 C 0.442(4) 0.573(2) 0.0594(12) 0.145(4) Uani 0.367(10) 1 d D U P C 2
H47A H 0.486568 0.610415 0.042662 0.174 Uiso 0.367(10) 1 calc R U P C 2
H47B H 0.389985 0.605507 0.043838 0.174 Uiso 0.367(10) 1 calc R U P C 2
C48 C 0.444(2) 0.441(2) 0.0534(9) 0.149(5) Uani 0.367(10) 1 d D U P C 2
H48A H 0.394311 0.413501 0.033346 0.178 Uiso 0.367(10) 1 calc R U P C 2
H48B H 0.490815 0.417885 0.034435 0.178 Uiso 0.367(10) 1 calc R U P C 2
O4 O 0.381(2) 0.441(3) 0.0862(13) 0.149(5) Uani 0.229(9) 1 d D U P D 3
C49 C 0.415(3) 0.494(4) 0.1335(12) 0.143(4) Uani 0.229(9) 1 d D U P D 3
H49A H 0.447655 0.436946 0.154858 0.172 Uiso 0.229(9) 1 calc R U P D 3
H49B H 0.372053 0.523795 0.154181 0.172 Uiso 0.229(9) 1 calc R U P D 3
C50 C 0.468(3) 0.592(4) 0.1177(19) 0.144(4) Uani 0.229(9) 1 d D U P D 3
H50A H 0.523805 0.565774 0.115430 0.172 Uiso 0.229(9) 1 calc R U P D 3
H50B H 0.466827 0.657227 0.142492 0.172 Uiso 0.229(9) 1 calc R U P D 3
C51 C 0.428(3) 0.625(4) 0.0646(17) 0.143(4) Uani 0.229(9) 1 d D U P D 3
H51A H 0.465436 0.611017 0.036941 0.171 Uiso 0.229(9) 1 calc R U P D 3
H51B H 0.411822 0.707213 0.063723 0.171 Uiso 0.229(9) 1 calc R U P D 3
C52 C 0.355(2) 0.544(4) 0.0582(15) 0.149(5) Uani 0.229(9) 1 d D U P D 3
H52A H 0.307696 0.578750 0.073379 0.178 Uiso 0.229(9) 1 calc R U P D 3
H52B H 0.340268 0.526188 0.020965 0.178 Uiso 0.229(9) 1 calc R U P D 3
O5 O 0.4436(19) 0.765(3) 0.1157(11) 0.141(4) Uani 0.235(10) 1 d D U P E 4
C53 C 0.437(4) 0.640(3) 0.1148(15) 0.143(4) Uani 0.235(10) 1 d D U P E 4
H53A H 0.385363 0.615176 0.127159 0.171 Uiso 0.235(10) 1 calc R U P E 4
H53B H 0.481574 0.605174 0.137603 0.171 Uiso 0.235(10) 1 calc R U P E 4
C54 C 0.443(6) 0.604(4) 0.0598(18) 0.144(4) Uani 0.235(10) 1 d D U P E 4
H54A H 0.407721 0.536388 0.050879 0.173 Uiso 0.235(10) 1 calc R U P E 4
H54B H 0.499281 0.582671 0.053405 0.173 Uiso 0.235(10) 1 calc R U P E 4
C55 C 0.416(3) 0.709(4) 0.0287(12) 0.140(4) Uani 0.235(10) 1 d D U P E 4
H55A H 0.367205 0.691766 0.005336 0.168 Uiso 0.235(10) 1 calc R U P E 4
H55B H 0.458786 0.737599 0.007533 0.168 Uiso 0.235(10) 1 calc R U P E 4
C56 C 0.397(4) 0.798(4) 0.0698(15) 0.138(4) Uani 0.235(10) 1 d D U P E 4
H56A H 0.411889 0.877268 0.058828 0.165 Uiso 0.235(10) 1 calc R U P E 4
H56B H 0.338873 0.797539 0.075463 0.165 Uiso 0.235(10) 1 calc R U P E 4
O6 O 0.4131(15) 0.831(2) 0.0371(10) 0.139(4) Uani 0.330(13) 1 d D U P F -5
C57 C 0.479(2) 0.894(3) 0.0641(11) 0.138(4) Uani 0.330(13) 1 d D U P F -5
H57A H 0.522324 0.838831 0.075874 0.165 Uiso 0.330(13) 1 calc R U P F -5
H57B H 0.459909 0.932298 0.095138 0.165 Uiso 0.330(13) 1 calc R U P F -5
C58 C 0.511(2) 0.982(3) 0.0289(13) 0.138(5) Uani 0.330(13) 1 d D U P F -5
H58A H 0.568770 0.969529 0.024897 0.166 Uiso 0.330(13) 1 calc R U P F -5
H58B H 0.502487 1.061348 0.041780 0.166 Uiso 0.330(13) 1 calc R U P F -5
C59 C 0.460(2) 0.960(3) -0.0219(12) 0.139(5) Uani 0.330(13) 1 d D U P F -5
H59A H 0.493278 0.967444 -0.052138 0.166 Uiso 0.330(13) 1 calc R U P F -5
H59B H 0.414291 1.013724 -0.026196 0.166 Uiso 0.330(13) 1 calc R U P F -5
C60 C 0.432(3) 0.834(3) -0.0160(10) 0.140(4) Uani 0.330(13) 1 d D U P F -5
H60A H 0.383531 0.817374 -0.039840 0.169 Uiso 0.330(13) 1 calc R U P F -5
H60B H 0.474709 0.777844 -0.022588 0.169 Uiso 0.330(13) 1 calc R U P F -5


_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
Np1 Cl2 2.6031(9) . ?
Np1 N2 2.610(3) . ?
Np1 Cl1 2.6264(9) . ?
Np1 Cl3 2.6271(8) . ?
Np1 N1 2.628(3) . ?
Np1 Cl4 2.6282(9) . ?
Np1 N4 2.637(3) . ?
Np1 N3 2.650(3) . ?
N1 C1 1.347(4) . ?
N1 C5 1.347(4) . ?
N2 C10 1.341(4) . ?
N2 C6 1.346(4) . ?
N3 C19 1.336(5) . ?
N3 C23 1.345(4) . ?
N4 C28 1.340(5) . ?
N4 C24 1.357(4) . ?
C1 C2 1.379(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.389(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(4) . ?
C3 C11 1.531(5) . ?
C4 C5 1.404(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.479(4) . ?
C6 C7 1.400(4) . ?
C7 C8 1.386(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.392(5) . ?
C8 C15 1.522(5) . ?
C9 C10 1.389(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.527(6) . ?
C11 C14 1.532(6) . ?
C11 C13 1.532(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.530(6) . ?
C15 C17 1.534(5) . ?
C15 C18 1.538(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.385(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.381(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.380(5) . ?
C21 C29 1.524(5) . ?
C22 C23 1.404(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.482(5) . ?
C24 C25 1.397(4) . ?
C25 C26 1.378(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.393(5) . ?
C26 C33 1.529(5) . ?
C27 C28 1.379(5) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C32 1.531(6) . ?
C29 C30 1.535(7) . ?
C29 C31 1.547(7) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C36 1.505(7) . ?
C33 C34 1.533(6) . ?
C33 C35 1.534(6) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
O1 C40 1.417(14) . ?
O1 C37 1.456(13) . ?
C37 C38 1.473(14) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.513(15) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.523(13) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
O1B C37B 1.433(13) . ?
O1B C40B 1.433(15) . ?
C37B C38B 1.500(14) . ?
C37B H37C 0.9900 . ?
C37B H37D 0.9900 . ?
C38B C39B 1.511(15) . ?
C38B H38C 0.9900 . ?
C38B H38D 0.9900 . ?
C39B C40B 1.510(14) . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
C40B H40C 0.9900 . ?
C40B H40D 0.9900 . ?
O2 C44 1.418(18) . ?
O2 C41 1.458(18) . ?
C41 C42 1.496(18) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.513(18) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.527(18) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
O3 C48 1.402(17) . ?
O3 C45 1.442(17) . ?
C45 C46 1.501(18) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.520(18) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.537(18) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
O4 C52 1.436(18) . ?
O4 C49 1.438(18) . ?
C49 C50 1.498(19) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.517(19) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.541(19) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
O5 C56 1.415(18) . ?
O5 C53 1.447(18) . ?
C53 C54 1.489(19) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.509(19) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.525(19) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
O6 C60 1.426(18) . ?
O6 C57 1.445(17) . ?
C57 C58 1.488(18) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.518(17) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C60 1.538(18) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?

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
Cl2 Np1 N2 136.94(6) . . ?
Cl2 Np1 Cl1 88.67(3) . . ?
N2 Np1 Cl1 70.11(7) . . ?
Cl2 Np1 Cl3 141.33(3) . . ?
N2 Np1 Cl3 80.08(6) . . ?
Cl1 Np1 Cl3 97.63(3) . . ?
Cl2 Np1 N1 77.54(6) . . ?
N2 Np1 N1 62.55(8) . . ?
Cl1 Np1 N1 80.26(7) . . ?
Cl3 Np1 N1 141.12(6) . . ?
Cl2 Np1 Cl4 109.12(4) . . ?
N2 Np1 Cl4 73.77(7) . . ?
Cl1 Np1 Cl4 141.28(3) . . ?
Cl3 Np1 Cl4 89.40(4) . . ?
N1 Np1 Cl4 70.99(7) . . ?
Cl2 Np1 N4 74.28(7) . . ?
N2 Np1 N4 143.44(9) . . ?
Cl1 Np1 N4 140.99(6) . . ?
Cl3 Np1 N4 77.19(7) . . ?
N1 Np1 N4 127.47(8) . . ?
Cl4 Np1 N4 77.71(6) . . ?
Cl2 Np1 N3 70.98(7) . . ?
N2 Np1 N3 135.48(9) . . ?
Cl1 Np1 N3 79.11(7) . . ?
Cl3 Np1 N3 72.86(7) . . ?
N1 Np1 N3 142.47(9) . . ?
Cl4 Np1 N3 138.71(7) . . ?
N4 Np1 N3 62.30(9) . . ?
C1 N1 C5 116.7(3) . . ?
C1 N1 Np1 122.1(2) . . ?
C5 N1 Np1 120.1(2) . . ?
C10 N2 C6 117.5(3) . . ?
C10 N2 Np1 120.8(2) . . ?
C6 N2 Np1 121.5(2) . . ?
C19 N3 C23 116.8(3) . . ?
C19 N3 Np1 121.8(2) . . ?
C23 N3 Np1 120.7(2) . . ?
C28 N4 C24 116.6(3) . . ?
C28 N4 Np1 122.1(2) . . ?
C24 N4 Np1 121.2(2) . . ?
N1 C1 C2 124.4(3) . . ?
N1 C1 H1 117.8 . . ?
C2 C1 H1 117.8 . . ?
C1 C2 C3 119.7(3) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 116.2(3) . . ?
C4 C3 C11 123.1(3) . . ?
C2 C3 C11 120.6(3) . . ?
C3 C4 C5 121.4(3) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
N1 C5 C4 121.5(3) . . ?
N1 C5 C6 117.5(3) . . ?
C4 C5 C6 121.0(3) . . ?
N2 C6 C7 121.2(3) . . ?
N2 C6 C5 117.1(3) . . ?
C7 C6 C5 121.7(3) . . ?
C8 C7 C6 121.8(3) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C7 C8 C9 115.8(3) . . ?
C7 C8 C15 123.8(3) . . ?
C9 C8 C15 120.4(3) . . ?
C10 C9 C8 120.1(3) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
N2 C10 C9 123.4(3) . . ?
N2 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
C12 C11 C3 111.9(3) . . ?
C12 C11 C14 107.7(4) . . ?
C3 C11 C14 110.1(3) . . ?
C12 C11 C13 109.1(4) . . ?
C3 C11 C13 108.2(3) . . ?
C14 C11 C13 109.7(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C8 C15 C16 109.4(3) . . ?
C8 C15 C17 108.5(3) . . ?
C16 C15 C17 109.9(3) . . ?
C8 C15 C18 111.1(3) . . ?
C16 C15 C18 110.0(4) . . ?
C17 C15 C18 107.9(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 C20 124.2(4) . . ?
N3 C19 H19 117.9 . . ?
C20 C19 H19 117.9 . . ?
C21 C20 C19 119.9(4) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C22 C21 C20 115.9(3) . . ?
C22 C21 C29 122.9(3) . . ?
C20 C21 C29 121.2(4) . . ?
C21 C22 C23 121.8(3) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
N3 C23 C22 121.1(3) . . ?
N3 C23 C24 117.8(3) . . ?
C22 C23 C24 121.0(3) . . ?
N4 C24 C25 121.4(3) . . ?
N4 C24 C23 116.9(3) . . ?
C25 C24 C23 121.6(3) . . ?
C26 C25 C24 121.8(3) . . ?
C26 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
C25 C26 C27 115.8(3) . . ?
C25 C26 C33 123.8(3) . . ?
C27 C26 C33 120.4(3) . . ?
C28 C27 C26 120.2(3) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
N4 C28 C27 124.1(3) . . ?
N4 C28 H28 118.0 . . ?
C27 C28 H28 118.0 . . ?
C21 C29 C32 112.4(3) . . ?
C21 C29 C30 108.4(4) . . ?
C32 C29 C30 108.6(4) . . ?
C21 C29 C31 109.8(4) . . ?
C32 C29 C31 107.9(4) . . ?
C30 C29 C31 109.8(5) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C36 C33 C26 111.2(4) . . ?
C36 C33 C34 109.7(4) . . ?
C26 C33 C34 107.3(3) . . ?
C36 C33 C35 108.8(4) . . ?
C26 C33 C35 112.0(3) . . ?
C34 C33 C35 107.8(4) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C40 O1 C37 104.2(10) . . ?
O1 C37 C38 112.2(10) . . ?
O1 C37 H37A 109.2 . . ?
C38 C37 H37A 109.2 . . ?
O1 C37 H37B 109.2 . . ?
C38 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
C37 C38 C39 102.5(10) . . ?
C37 C38 H38A 111.3 . . ?
C39 C38 H38A 111.3 . . ?
C37 C38 H38B 111.3 . . ?
C39 C38 H38B 111.3 . . ?
H38A C38 H38B 109.2 . . ?
C38 C39 C40 102.8(10) . . ?
C38 C39 H39A 111.2 . . ?
C40 C39 H39A 111.2 . . ?
C38 C39 H39B 111.2 . . ?
C40 C39 H39B 111.2 . . ?
H39A C39 H39B 109.1 . . ?
O1 C40 C39 107.3(10) . . ?
O1 C40 H40A 110.2 . . ?
C39 C40 H40A 110.2 . . ?
O1 C40 H40B 110.2 . . ?
C39 C40 H40B 110.2 . . ?
H40A C40 H40B 108.5 . . ?
C37B O1B C40B 104.3(11) . . ?
O1B C37B C38B 108.8(10) . . ?
O1B C37B H37C 109.9 . . ?
C38B C37B H37C 109.9 . . ?
O1B C37B H37D 109.9 . . ?
C38B C37B H37D 109.9 . . ?
H37C C37B H37D 108.3 . . ?
C37B C38B C39B 105.5(9) . . ?
C37B C38B H38C 110.6 . . ?
C39B C38B H38C 110.6 . . ?
C37B C38B H38D 110.6 . . ?
C39B C38B H38D 110.6 . . ?
H38C C38B H38D 108.8 . . ?
C40B C39B C38B 103.3(10) . . ?
C40B C39B H39C 111.1 . . ?
C38B C39B H39C 111.1 . . ?
C40B C39B H39D 111.1 . . ?
C38B C39B H39D 111.1 . . ?
H39C C39B H39D 109.1 . . ?
O1B C40B C39B 109.0(12) . . ?
O1B C40B H40C 109.9 . . ?
C39B C40B H40C 109.9 . . ?
O1B C40B H40D 109.9 . . ?
C39B C40B H40D 109.9 . . ?
H40C C40B H40D 108.3 . . ?
C44 O2 C41 100.2(17) . . ?
O2 C41 C42 106.7(18) . . ?
O2 C41 H41A 110.4 . . ?
C42 C41 H41A 110.4 . . ?
O2 C41 H41B 110.4 . . ?
C42 C41 H41B 110.4 . . ?
H41A C41 H41B 108.6 . . ?
C41 C42 C43 102.1(15) . . ?
C41 C42 H42A 111.3 . . ?
C43 C42 H42A 111.3 . . ?
C41 C42 H42B 111.3 . . ?
C43 C42 H42B 111.3 . . ?
H42A C42 H42B 109.2 . . ?
C42 C43 C44 104.4(15) . . ?
C42 C43 H43A 110.9 . . ?
C44 C43 H43A 110.9 . . ?
C42 C43 H43B 110.9 . . ?
C44 C43 H43B 110.9 . . ?
H43A C43 H43B 108.9 . . ?
O2 C44 C43 104.9(17) . . ?
O2 C44 H44A 110.8 . . ?
C43 C44 H44A 110.8 . . ?
O2 C44 H44B 110.8 . . ?
C43 C44 H44B 110.8 . . ?
H44A C44 H44B 108.8 . . ?
C48 O3 C45 102.7(16) . . ?
O3 C45 C46 104.7(16) . . ?
O3 C45 H45A 110.8 . . ?
C46 C45 H45A 110.8 . . ?
O3 C45 H45B 110.8 . . ?
C46 C45 H45B 110.8 . . ?
H45A C45 H45B 108.9 . . ?
C45 C46 C47 99.8(16) . . ?
C45 C46 H46A 111.8 . . ?
C47 C46 H46A 111.8 . . ?
C45 C46 H46B 111.8 . . ?
C47 C46 H46B 111.8 . . ?
H46A C46 H46B 109.5 . . ?
C46 C47 C48 103.5(15) . . ?
C46 C47 H47A 111.1 . . ?
C48 C47 H47A 111.1 . . ?
C46 C47 H47B 111.1 . . ?
C48 C47 H47B 111.1 . . ?
H47A C47 H47B 109.0 . . ?
O3 C48 C47 108.0(15) . . ?
O3 C48 H48A 110.1 . . ?
C47 C48 H48A 110.1 . . ?
O3 C48 H48B 110.1 . . ?
C47 C48 H48B 110.1 . . ?
H48A C48 H48B 108.4 . . ?
C52 O4 C49 99.3(18) . . ?
O4 C49 C50 106.6(19) . . ?
O4 C49 H49A 110.4 . . ?
C50 C49 H49A 110.4 . . ?
O4 C49 H49B 110.4 . . ?
C50 C49 H49B 110.4 . . ?
H49A C49 H49B 108.6 . . ?
C49 C50 C51 102.6(16) . . ?
C49 C50 H50A 111.3 . . ?
C51 C50 H50A 111.3 . . ?
C49 C50 H50B 111.3 . . ?
C51 C50 H50B 111.3 . . ?
H50A C50 H50B 109.2 . . ?
C50 C51 C52 103.0(16) . . ?
C50 C51 H51A 111.2 . . ?
C52 C51 H51A 111.2 . . ?
C50 C51 H51B 111.2 . . ?
C52 C51 H51B 111.2 . . ?
H51A C51 H51B 109.1 . . ?
O4 C52 C51 103.5(19) . . ?
O4 C52 H52A 111.1 . . ?
C51 C52 H52A 111.1 . . ?
O4 C52 H52B 111.1 . . ?
C51 C52 H52B 111.1 . . ?
H52A C52 H52B 109.0 . . ?
C56 O5 C53 102.8(19) . . ?
O5 C53 C54 107(2) . . ?
O5 C53 H53A 110.4 . . ?
C54 C53 H53A 110.4 . . ?
O5 C53 H53B 110.4 . . ?
C54 C53 H53B 110.4 . . ?
H53A C53 H53B 108.6 . . ?
C53 C54 C55 103.6(16) . . ?
C53 C54 H54A 111.0 . . ?
C55 C54 H54A 111.0 . . ?
C53 C54 H54B 111.0 . . ?
C55 C54 H54B 111.0 . . ?
H54A C54 H54B 109.0 . . ?
C54 C55 C56 104.4(16) . . ?
C54 C55 H55A 110.9 . . ?
C56 C55 H55A 110.9 . . ?
C54 C55 H55B 110.9 . . ?
C56 C55 H55B 110.9 . . ?
H55A C55 H55B 108.9 . . ?
O5 C56 C55 105.5(18) . . ?
O5 C56 H56A 110.6 . . ?
C55 C56 H56A 110.6 . . ?
O5 C56 H56B 110.6 . . ?
C55 C56 H56B 110.6 . . ?
H56A C56 H56B 108.8 . . ?
C60 O6 C57 103.5(16) . . ?
O6 C57 C58 110.1(16) . . ?
O6 C57 H57A 109.6 . . ?
C58 C57 H57A 109.6 . . ?
O6 C57 H57B 109.6 . . ?
C58 C57 H57B 109.6 . . ?
H57A C57 H57B 108.1 . . ?
C57 C58 C59 102.2(15) . . ?
C57 C58 H58A 111.3 . . ?
C59 C58 H58A 111.3 . . ?
C57 C58 H58B 111.3 . . ?
C59 C58 H58B 111.3 . . ?
H58A C58 H58B 109.2 . . ?
C58 C59 C60 103.2(15) . . ?
C58 C59 H59A 111.1 . . ?
C60 C59 H59A 111.1 . . ?
C58 C59 H59B 111.1 . . ?
C60 C59 H59B 111.1 . . ?
H59A C59 H59B 109.1 . . ?
O6 C60 C59 102.3(16) . . ?
O6 C60 H60A 111.3 . . ?
C59 C60 H60A 111.3 . . ?
O6 C60 H60B 111.3 . . ?
C59 C60 H60B 111.3 . . ?
H60A C60 H60B 109.2 . . ?

_refine_diff_density_max         2.291
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.124




