# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 2287577'
loop_
_audit_author_name
_audit_author_address
'Harindu Rajapaksha'
;The University of Iowa
United States of America
;
_audit_update_record             
;
2023-08-08 deposited with the CCDC.	2024-01-17 downloaded from the CCDC.
;
_audit_creation_date             2023-04-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl2 H2 Np O3 Rb'
_chemical_formula_sum            'Cl2 H2 Np O3 Rb'
_chemical_formula_weight         443.39
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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'
Np Np -11.4937 4.1493 '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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   8.4988(4)
_cell_length_b                   11.3956(5)
_cell_length_c                   7.4459(6)
_cell_angle_alpha                90
_cell_angle_beta                 114.2050(10)
_cell_angle_gamma                90
_cell_volume                     657.73(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    137.76
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      3.18
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.873
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    4.478
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             760
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   0.4302
_exptl_transmission_factor_min   0.2836
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0079
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            12453
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.178
_diffrn_ambient_temperature      137.76
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                606
_reflns_number_total             608
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.00256(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         608
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0070
_refine_ls_R_factor_gt           0.0069
_refine_ls_restrained_S_all      1.245
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0031P)²+1.3496P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0157
_refine_ls_wR_factor_ref         0.0157
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_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
Np01 Np 0.500000 0.68630(2) 0.250000 0.00480(6) Uani 1 2 d S T P . .
Rb02 Rb 0.500000 0.86058(2) 0.750000 0.01000(7) Uani 1 2 d S T P . .
Cl03 Cl 0.19064(6) 0.60992(4) -0.05716(7) 0.00980(11) Uani 1 1 d . . . . .
O004 O 0.39751(19) 0.68505(13) 0.4229(2) 0.0090(3) Uani 1 1 d . . . . .
O005 O 0.500000 0.4711(2) 0.250000 0.0105(5) Uani 1 2 d S T P . .
H005 H 0.531(4) 0.435(3) 0.338(4) 0.021(8) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Np01 Rb02 4.28286(19) 7_666 ?
Np01 Rb02 4.2195(3) 1_554 ?
Np01 Rb02 4.28286(19) 7_566 ?
Np01 Rb02 4.2195(3) . ?
Np01 Cl03 2.8231(5) 2_655 ?
Np01 Cl03 2.8587(5) 7_565 ?
Np01 Cl03 2.8587(5) 8_566 ?
Np01 Cl03 2.8232(5) . ?
Np01 O004 1.8265(15) 2_655 ?
Np01 O004 1.8265(15) . ?
Np01 O005 2.452(2) . ?
Rb02 Cl03 3.3177(5) 7_566 ?
Rb02 Cl03 3.3177(5) 8_566 ?
Rb02 Cl03 3.2943(6) 4 ?
Rb02 Cl03 3.2943(6) 3_556 ?
Rb02 O004 3.1264(15) 7_566 ?
Rb02 O004 2.9920(15) . ?
Rb02 O004 3.1264(15) 8_566 ?
Rb02 O004 2.9919(15) 2_656 ?
O005 H005 0.73(3) . ?
O005 H005 0.73(3) 2_655 ?

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
Rb02 Np01 Rb02 123.845(9) . 1_554 ?
Rb02 Np01 Rb02 165.668(8) 7_566 7_666 ?
Rb02 Np01 Rb02 114.686(2) . 7_666 ?
Rb02 Np01 Rb02 114.686(2) 1_554 7_566 ?
Rb02 Np01 Rb02 72.530(3) . 7_566 ?
Rb02 Np01 Rb02 72.530(3) 1_554 7_666 ?
Cl03 Np01 Rb02 121.534(11) 2_655 1_554 ?
Cl03 Np01 Rb02 117.346(11) 8_566 7_566 ?
Cl03 Np01 Rb02 81.709(11) 7_565 . ?
Cl03 Np01 Rb02 123.780(11) . 7_666 ?
Cl03 Np01 Rb02 123.779(11) 2_655 7_566 ?
Cl03 Np01 Rb02 117.346(11) 7_565 7_666 ?
Cl03 Np01 Rb02 121.533(11) . . ?
Cl03 Np01 Rb02 51.648(11) 7_565 1_554 ?
Cl03 Np01 Rb02 51.648(11) 8_566 . ?
Cl03 Np01 Rb02 50.734(11) 2_655 7_666 ?
Cl03 Np01 Rb02 75.127(11) 7_565 7_566 ?
Cl03 Np01 Rb02 76.541(12) . 1_554 ?
Cl03 Np01 Rb02 50.733(11) . 7_566 ?
Cl03 Np01 Rb02 76.541(11) 2_655 . ?
Cl03 Np01 Rb02 75.127(11) 8_566 7_666 ?
Cl03 Np01 Rb02 81.709(12) 8_566 1_554 ?
Cl03 Np01 Cl03 72.288(17) . 7_565 ?
Cl03 Np01 Cl03 71.35(2) 8_566 7_565 ?
Cl03 Np01 Cl03 143.629(12) 2_655 7_565 ?
Cl03 Np01 Cl03 143.628(12) . 8_566 ?
Cl03 Np01 Cl03 72.289(17) 2_655 8_566 ?
Cl03 Np01 Cl03 144.08(2) 2_655 . ?
O004 Np01 Rb02 37.74(5) 2_655 1_554 ?
O004 Np01 Rb02 142.95(5) . 1_554 ?
O004 Np01 Rb02 139.37(5) 2_655 7_566 ?
O004 Np01 Rb02 139.37(5) . 7_666 ?
O004 Np01 Rb02 142.95(5) 2_655 . ?
O004 Np01 Rb02 37.74(5) . . ?
O004 Np01 Rb02 40.46(5) . 7_566 ?
O004 Np01 Rb02 40.46(5) 2_655 7_666 ?
O004 Np01 Cl03 91.40(5) 2_655 8_566 ?
O004 Np01 Cl03 90.79(5) . . ?
O004 Np01 Cl03 89.32(5) 2_655 7_565 ?
O004 Np01 Cl03 88.94(5) . 2_655 ?
O004 Np01 Cl03 89.32(5) . 8_566 ?
O004 Np01 Cl03 90.79(5) 2_655 2_655 ?
O004 Np01 Cl03 91.41(5) . 7_565 ?
O004 Np01 Cl03 88.94(5) 2_655 . ?
O004 Np01 O004 179.10(9) . 2_655 ?
O004 Np01 O005 89.55(5) 2_655 . ?
O004 Np01 O005 89.55(5) . . ?
O005 Np01 Rb02 82.834(4) . 7_666 ?
O005 Np01 Rb02 118.077(4) . 1_554 ?
O005 Np01 Rb02 82.834(4) . 7_566 ?
O005 Np01 Rb02 118.077(4) . . ?
O005 Np01 Cl03 72.041(11) . . ?
O005 Np01 Cl03 144.326(10) . 7_565 ?
O005 Np01 Cl03 72.040(11) . 2_655 ?
O005 Np01 Cl03 144.326(10) . 8_566 ?
Np01 Rb02 Np01 165.667(8) 7_566 7_666 ?
Np01 Rb02 Np01 107.470(3) 1_556 7_666 ?
Np01 Rb02 Np01 123.846(8) 1_556 . ?
Np01 Rb02 Np01 107.470(3) . 7_566 ?
Np01 Rb02 Np01 65.314(2) 1_556 7_566 ?
Np01 Rb02 Np01 65.314(2) . 7_666 ?
Cl03 Rb02 Np01 101.495(10) 4 . ?
Cl03 Rb02 Np01 114.726(10) 3_556 7_566 ?
Cl03 Rb02 Np01 41.208(9) 7_566 7_566 ?
Cl03 Rb02 Np01 42.508(9) 7_566 1_556 ?
Cl03 Rb02 Np01 127.778(10) 4 1_556 ?
Cl03 Rb02 Np01 141.042(9) 7_566 7_666 ?
Cl03 Rb02 Np01 78.283(9) 4 7_566 ?
Cl03 Rb02 Np01 146.364(10) 7_566 . ?
Cl03 Rb02 Np01 114.726(10) 4 7_666 ?
Cl03 Rb02 Np01 78.283(9) 3_556 7_666 ?
Cl03 Rb02 Np01 127.778(10) 3_556 . ?
Cl03 Rb02 Np01 141.042(9) 8_566 7_566 ?
Cl03 Rb02 Np01 146.364(10) 8_566 1_556 ?
Cl03 Rb02 Np01 101.495(10) 3_556 1_556 ?
Cl03 Rb02 Np01 41.208(9) 8_566 7_666 ?
Cl03 Rb02 Np01 42.508(9) 8_566 . ?
Cl03 Rb02 Cl03 168.37(2) 7_566 8_566 ?
Cl03 Rb02 Cl03 85.477(13) 4 7_566 ?
Cl03 Rb02 Cl03 84.494(14) 3_556 7_566 ?
Cl03 Rb02 Cl03 60.803(18) 3_556 4 ?
Cl03 Rb02 Cl03 85.477(13) 3_556 8_566 ?
Cl03 Rb02 Cl03 84.494(14) 4 8_566 ?
O004 Rb02 Np01 152.11(3) 7_566 7_666 ?
O004 Rb02 Np01 83.92(3) 7_566 1_556 ?
O004 Rb02 Np01 107.35(3) 2_656 . ?
O004 Rb02 Np01 87.09(3) 7_566 . ?
O004 Rb02 Np01 83.92(3) 8_566 . ?
O004 Rb02 Np01 87.64(3) 2_656 7_666 ?
O004 Rb02 Np01 21.94(3) 2_656 1_556 ?
O004 Rb02 Np01 87.64(3) . 7_566 ?
O004 Rb02 Np01 87.09(3) 8_566 1_556 ?
O004 Rb02 Np01 22.28(3) 8_566 7_666 ?
O004 Rb02 Np01 152.11(3) 8_566 7_566 ?
O004 Rb02 Np01 82.78(3) . 7_666 ?
O004 Rb02 Np01 21.94(3) . . ?
O004 Rb02 Np01 22.28(3) 7_566 7_566 ?
O004 Rb02 Np01 82.78(3) 2_656 7_566 ?
O004 Rb02 Np01 107.35(3) . 1_556 ?
O004 Rb02 Cl03 124.57(3) 2_656 8_566 ?
O004 Rb02 Cl03 149.14(3) 2_656 4 ?
O004 Rb02 Cl03 73.06(3) 7_566 4 ?
O004 Rb02 Cl03 149.14(3) . 3_556 ?
O004 Rb02 Cl03 107.15(3) 2_656 3_556 ?
O004 Rb02 Cl03 118.92(3) 8_566 7_566 ?
O004 Rb02 Cl03 107.15(3) . 4 ?
O004 Rb02 Cl03 64.41(3) . 8_566 ?
O004 Rb02 Cl03 63.26(3) 7_566 7_566 ?
O004 Rb02 Cl03 124.57(3) . 7_566 ?
O004 Rb02 Cl03 125.33(3) 7_566 3_556 ?
O004 Rb02 Cl03 73.06(3) 8_566 3_556 ?
O004 Rb02 Cl03 125.33(3) 8_566 4 ?
O004 Rb02 Cl03 63.26(3) 8_566 8_566 ?
O004 Rb02 Cl03 64.41(3) 2_656 7_566 ?
O004 Rb02 Cl03 118.92(3) 7_566 8_566 ?
O004 Rb02 O004 97.40(4) . 8_566 ?
O004 Rb02 O004 69.44(5) . 7_566 ?
O004 Rb02 O004 160.85(5) 7_566 8_566 ?
O004 Rb02 O004 69.44(5) 2_656 8_566 ?
O004 Rb02 O004 97.40(4) 2_656 7_566 ?
O004 Rb02 O004 96.09(6) 2_656 . ?
Np01 Cl03 Np01 107.713(17) . 7_565 ?
Np01 Cl03 Rb02 85.845(14) 7_565 7_566 ?
Np01 Cl03 Rb02 113.924(16) 7_565 3_444 ?
Np01 Cl03 Rb02 88.058(14) . 7_566 ?
Np01 Cl03 Rb02 138.356(18) . 3_444 ?
Rb02 Cl03 Rb02 95.506(14) 3_444 7_566 ?
Np01 O004 Rb02 120.31(6) . . ?
Np01 O004 Rb02 117.27(6) . 7_566 ?
Rb02 O004 Rb02 110.56(5) . 7_566 ?
Np01 O005 H005 125(2) . . ?
Np01 O005 H005 125(2) . 2_655 ?
H005 O005 H005 111(5) . 2_655 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rb02 Np01 O004 Rb02 -157.87(2) 7_666 . . 7_566 ?
Rb02 Np01 O004 Rb02 -139.38(11) 7_566 . . . ?
Rb02 Np01 O004 Rb02 -78.40(10) 1_554 . . . ?
Rb02 Np01 O004 Rb02 139.38(11) . . . 7_566 ?
Rb02 Np01 O004 Rb02 60.98(10) 1_554 . . 7_566 ?
Rb02 Np01 O004 Rb02 62.75(10) 7_666 . . . ?
Cl03 Np01 O004 Rb02 -74.49(6) 7_565 . . . ?
Cl03 Np01 O004 Rb02 -7.42(6) . . . 7_566 ?
Cl03 Np01 O004 Rb02 -146.80(6) . . . . ?
Cl03 Np01 O004 Rb02 -3.17(6) 8_566 . . . ?
Cl03 Np01 O004 Rb02 136.21(5) 8_566 . . 7_566 ?
Cl03 Np01 O004 Rb02 -151.50(6) 2_655 . . 7_566 ?
Cl03 Np01 O004 Rb02 69.13(6) 2_655 . . . ?
Cl03 Np01 O004 Rb02 64.88(5) 7_565 . . 7_566 ?
O005 Np01 O004 Rb02 -79.45(5) . . . 7_566 ?
O005 Np01 O004 Rb02 141.17(6) . . . . ?

_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_19
_database_code_depnum_ccdc_archive 'CCDC 2287578'
loop_
_audit_author_name
_audit_author_address
'Harindu Rajapaksha'
;The University of Iowa
United States of America
;
_audit_update_record             
;
2023-08-08 deposited with the CCDC.	2024-01-17 downloaded from the CCDC.
;
_audit_creation_date             2023-04-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl3 Np O2, 2(C H6 N3)'
_chemical_formula_sum            'C2 H12 Cl3 N6 Np O2'
_chemical_formula_weight         495.53
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'
Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.6197(3)
_cell_length_b                   9.7216(4)
_cell_length_c                   14.5517(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1219.39(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9530
_cell_measurement_temperature    136.01
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.52
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.168
_exptl_absorpt_correction_T_max  0.3343
_exptl_absorpt_correction_T_min  0.2518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    2.699
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             904
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   0.3343
_exptl_transmission_factor_min   0.2518
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0102
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47334
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.340
_diffrn_reflns_theta_min         2.520
_diffrn_ambient_temperature      136.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.708
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2224
_reflns_number_total             2236
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.012(10)
_refine_ls_extinction_coef       0.00187(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2236
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0071
_refine_ls_R_factor_gt           0.0070
_refine_ls_restrained_S_all      1.161
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0049P)²+0.5427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0174
_refine_ls_wR_factor_ref         0.0174
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.988(10)
 0.012(10)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
3.a X=CH2 refined with riding coordinates:
 N007(H00a,H00b), N008(H00g,H00h), N009(H00c,H00d), N00B(H00i,H00j), N00C(H00e,
 H00f), N00D(H00k,H00l)
;
_atom_sites_solution_hydrogens   geom
_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
Np01 Np 0.27166(2) 0.32181(2) 0.48391(2) 0.00914(4) Uani 1 1 d . . . . .
Cl02 Cl 0.58518(7) 0.41735(7) 0.48221(6) 0.01511(14) Uani 1 1 d . . . . .
Cl03 Cl -0.03811(8) 0.37921(8) 0.42773(5) 0.01553(16) Uani 1 1 d . . . . .
Cl04 Cl 0.27114(9) 0.58938(7) 0.40636(5) 0.01698(15) Uani 1 1 d . . . . .
O005 O 0.3123(2) 0.2483(2) 0.37123(14) 0.0146(5) Uani 1 1 d . . . . .
O006 O 0.2300(3) 0.3944(2) 0.59598(13) 0.0155(4) Uani 1 1 d . . . . .
N007 N 0.4424(4) 0.7437(3) 0.5837(2) 0.0261(7) Uani 1 1 d . . . . .
H00A H 0.502287 0.811166 0.564640 0.031 Uiso 1 1 calc R U . . .
H00B H 0.414038 0.678420 0.545303 0.031 Uiso 1 1 calc R U . . .
N008 N 0.8506(4) 0.6881(3) 0.7595(2) 0.0297(7) Uani 1 1 d . . . . .
H00G H 0.870797 0.689696 0.818727 0.036 Uiso 1 1 calc R U . . .
H00H H 0.810827 0.761071 0.732496 0.036 Uiso 1 1 calc R U . . .
N009 N 0.4383(4) 0.8386(3) 0.7271(2) 0.0279(7) Uani 1 1 d . . . . .
H00C H 0.498194 0.905917 0.707699 0.033 Uiso 1 1 calc R U . . .
H00D H 0.407103 0.836875 0.784720 0.033 Uiso 1 1 calc R U . . .
C00A C 0.8796(4) 0.5774(3) 0.7115(2) 0.0204(7) Uani 1 1 d . . . . .
N00B N 0.9390(4) 0.4683(3) 0.7517(2) 0.0323(8) Uani 1 1 d . . . . .
H00I H 0.959275 0.469793 0.810950 0.039 Uiso 1 1 calc R U . . .
H00J H 0.958521 0.393833 0.719321 0.039 Uiso 1 1 calc R U . . .
N00C N 0.3056(4) 0.6382(3) 0.6993(2) 0.0325(8) Uani 1 1 d . . . . .
H00E H 0.277519 0.572384 0.661194 0.039 Uiso 1 1 calc R U . . .
H00F H 0.274343 0.636287 0.756824 0.039 Uiso 1 1 calc R U . . .
N00D N 0.8558(5) 0.5764(3) 0.6216(2) 0.0442(10) Uani 1 1 d . . . . .
H00K H 0.820323 0.650400 0.593855 0.053 Uiso 1 1 calc R U . . .
H00L H 0.875525 0.501591 0.589528 0.053 Uiso 1 1 calc R U . . .
C00E C 0.3951(4) 0.7402(4) 0.6699(2) 0.0205(7) 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
Np01 Cl02 2.8693(7) 4_456 ?
Np01 Cl02 2.8577(6) . ?
Np01 Cl03 2.8477(7) . ?
Np01 Cl03 2.8568(7) 4_556 ?
Np01 Cl04 2.8354(7) . ?
Np01 O005 1.823(2) . ?
Np01 O006 1.813(2) . ?
N007 H00A 0.8800 . ?
N007 H00B 0.8800 . ?
N007 C00E 1.319(5) . ?
N008 H00G 0.8800 . ?
N008 H00H 0.8800 . ?
N008 C00A 1.307(5) . ?
N009 H00C 0.8800 . ?
N009 H00D 0.8800 . ?
N009 C00E 1.322(5) . ?
C00A N00B 1.315(5) . ?
C00A N00D 1.325(5) . ?
N00B H00I 0.8800 . ?
N00B H00J 0.8800 . ?
N00C H00E 0.8800 . ?
N00C H00F 0.8800 . ?
N00C C00E 1.328(4) . ?
N00D H00K 0.8800 . ?
N00D H00L 0.8800 . ?

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
Cl02 Np01 Cl02 142.620(16) . 4_456 ?
Cl03 Np01 Cl02 71.55(2) 4_556 . ?
Cl03 Np01 Cl02 71.51(2) . 4_456 ?
Cl03 Np01 Cl02 71.93(2) 4_556 4_456 ?
Cl03 Np01 Cl02 145.14(2) . . ?
Cl03 Np01 Cl03 143.269(17) . 4_556 ?
Cl04 Np01 Cl02 72.53(2) . . ?
Cl04 Np01 Cl02 144.18(2) . 4_456 ?
Cl04 Np01 Cl03 72.81(2) . . ?
Cl04 Np01 Cl03 143.86(2) . 4_556 ?
O005 Np01 Cl02 86.80(7) . 4_456 ?
O005 Np01 Cl02 86.46(7) . . ?
O005 Np01 Cl03 89.92(7) . . ?
O005 Np01 Cl03 91.51(7) . 4_556 ?
O005 Np01 Cl04 90.13(7) . . ?
O006 Np01 Cl02 93.93(8) . . ?
O006 Np01 Cl02 92.86(7) . 4_456 ?
O006 Np01 Cl03 89.79(8) . . ?
O006 Np01 Cl03 88.57(7) . 4_556 ?
O006 Np01 Cl04 90.04(6) . . ?
O006 Np01 O005 179.61(11) . . ?
Np01 Cl02 Np01 105.36(2) . 4_556 ?
Np01 Cl03 Np01 105.96(2) . 4_456 ?
H00A N007 H00B 120.0 . . ?
C00E N007 H00A 120.0 . . ?
C00E N007 H00B 120.0 . . ?
H00G N008 H00H 120.0 . . ?
C00A N008 H00G 120.0 . . ?
C00A N008 H00H 120.0 . . ?
H00C N009 H00D 120.0 . . ?
C00E N009 H00C 120.0 . . ?
C00E N009 H00D 120.0 . . ?
N008 C00A N00B 120.1(3) . . ?
N008 C00A N00D 120.3(3) . . ?
N00B C00A N00D 119.6(3) . . ?
C00A N00B H00I 120.0 . . ?
C00A N00B H00J 120.0 . . ?
H00I N00B H00J 120.0 . . ?
H00E N00C H00F 120.0 . . ?
C00E N00C H00E 120.0 . . ?
C00E N00C H00F 120.0 . . ?
C00A N00D H00K 120.0 . . ?
C00A N00D H00L 120.0 . . ?
H00K N00D H00L 120.0 . . ?
N007 C00E N009 119.6(3) . . ?
N007 C00E N00C 120.3(3) . . ?
N009 C00E N00C 120.1(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.988(10)
2 0.012(10)

