# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_apx2586
_database_code_depnum_ccdc_archive 'CCDC 1830523'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H24 Cl3.50 O3 Pu'
_chemical_formula_weight         579.41

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'
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'
Pu Pu -9.4100 4.3056 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 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, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   12.264(3)
_cell_length_b                   11.172(3)
_cell_length_c                   13.938(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.374(3)
_cell_angle_gamma                90
_cell_volume                     1850.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    9926
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      28.31

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_F_000             1094
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.270
_exptl_absorpt_coefficient_mu    4.070
_shelx_estimated_absorpt_T_min   0.338
_shelx_estimated_absorpt_T_max   0.406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.192
_exptl_absorpt_correction_T_max  0.253
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20230
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.714
_diffrn_reflns_theta_max         28.615
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             4435
_reflns_number_gt                4006
_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       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_publication_material  'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_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)+(0.0073P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4435
_refine_ls_number_parameters     179
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0662
_refine_ls_wR_factor_gt          0.0654
_refine_ls_goodness_of_fit_ref   1.742
_refine_ls_restrained_S_all      1.742
_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
Pu1 Pu 1.0000 0.68096(2) 0.2500 0.02327(7) Uani 1 2 d S T P . .
Pu2 Pu 0.5000 0.20570(2) 0.2500 0.02423(7) Uani 1 2 d S T P . .
Cl1 Cl 0.5000 0.43260(14) 0.2500 0.0401(4) Uani 1 2 d S T P . .
Cl2 Cl 0.50161(13) 0.19223(10) 0.06673(9) 0.0417(3) Uani 1 1 d . . . . .
Cl3 Cl 0.28357(11) 0.19141(11) 0.19900(10) 0.0450(3) Uani 1 1 d . . . . .
Cl4 Cl 1.11368(12) 0.68818(11) 0.10958(9) 0.0424(3) Uani 1 1 d . . . . .
O1 O 1.0000 0.4607(3) 0.2500 0.0320(10) Uani 1 2 d S T P . .
O2 O 0.8222(3) 0.6120(3) 0.1373(2) 0.0387(8) Uani 1 1 d . . . . .
O3 O 0.9012(3) 0.8587(3) 0.1631(3) 0.0438(8) Uani 1 1 d . . . . .
O4 O 0.5000 -0.0104(3) 0.2500 0.0303(10) Uani 1 2 d S T P . .
C1 C 1.0090(5) 0.3849(5) 0.1678(4) 0.0521(15) Uani 1 1 d . . . . .
H1A H 1.0847 0.3872 0.1584 0.063 Uiso 1 1 calc R U . . .
H1B H 0.9566 0.4105 0.1070 0.063 Uiso 1 1 calc R U . . .
C2 C 0.9813(7) 0.2651(6) 0.1954(6) 0.100(3) Uani 1 1 d . . . . .
H2A H 1.0211 0.2048 0.1673 0.120 Uiso 1 1 calc R U . . .
H2B H 0.9011 0.2503 0.1733 0.120 Uiso 1 1 calc R U . . .
C3 C 0.7347(4) 0.5385(5) 0.1628(4) 0.0439(12) Uani 1 1 d . . . . .
H3A H 0.7017 0.5799 0.2099 0.053 Uiso 1 1 calc R U . . .
H3B H 0.7659 0.4631 0.1916 0.053 Uiso 1 1 calc R U . . .
C4 C 0.6498(5) 0.5178(6) 0.0697(4) 0.0708(19) Uani 1 1 d . . . . .
H4A H 0.5897 0.5763 0.0611 0.085 Uiso 1 1 calc R U . . .
H4B H 0.6178 0.4383 0.0685 0.085 Uiso 1 1 calc R U . . .
C5 C 0.7110(5) 0.5306(5) -0.0088(4) 0.0536(15) Uani 1 1 d . . . . .
H5A H 0.6606 0.5556 -0.0707 0.064 Uiso 1 1 calc R U . . .
H5B H 0.7466 0.4558 -0.0192 0.064 Uiso 1 1 calc R U . . .
C6 C 0.7964(5) 0.6243(6) 0.0303(4) 0.0605(17) Uani 1 1 d . . . . .
H6A H 0.8634 0.6120 0.0064 0.073 Uiso 1 1 calc R U . . .
H6B H 0.7665 0.7033 0.0102 0.073 Uiso 1 1 calc R U . . .
C7 C 0.7933(6) 0.9012(7) 0.1732(5) 0.086(2) Uani 1 1 d . . . . .
H7A H 0.7407 0.8351 0.1670 0.103 Uiso 1 1 calc R U . . .
H7B H 0.8012 0.9382 0.2375 0.103 Uiso 1 1 calc R U . . .
C8 C 0.7528(6) 0.9874(6) 0.0956(5) 0.0703(18) Uani 1 1 d . . . . .
H8A H 0.7415 1.0642 0.1240 0.084 Uiso 1 1 calc R U . . .
H8B H 0.6815 0.9612 0.0535 0.084 Uiso 1 1 calc R U . . .
C9 C 0.8355(6) 0.9987(5) 0.0378(4) 0.0623(17) Uani 1 1 d . . . . .
H9A H 0.8083 0.9617 -0.0267 0.075 Uiso 1 1 calc R U . . .
H9B H 0.8515 1.0823 0.0285 0.075 Uiso 1 1 calc R U . . .
C10 C 0.9359(5) 0.9377(5) 0.0942(6) 0.078(2) Uani 1 1 d . . . . .
H10A H 0.9703 0.8922 0.0502 0.093 Uiso 1 1 calc R U . . .
H10B H 0.9903 0.9954 0.1296 0.093 Uiso 1 1 calc R U . . .
C11 C 0.4361(4) -0.0854(4) 0.1695(3) 0.0416(12) Uani 1 1 d . . . . .
H11A H 0.4501 -0.0617 0.1067 0.050 Uiso 1 1 calc R U . . .
H11B H 0.3560 -0.0793 0.1647 0.050 Uiso 1 1 calc R U . . .
C12 C 0.4769(6) -0.2100(4) 0.1961(4) 0.0555(17) Uani 1 1 d . . . . .
H12A H 0.4154 -0.2667 0.1774 0.067 Uiso 1 1 calc R U . . .
H12B H 0.5347 -0.2314 0.1626 0.067 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
Pu1 O1 2.461(4) . ?
Pu1 O2 2.473(3) . ?
Pu1 O2 2.473(3) 2_755 ?
Pu1 O3 2.480(3) 2_755 ?
Pu1 O3 2.480(3) . ?
Pu1 Cl4 2.6712(13) . ?
Pu1 Cl4 2.6712(13) 2_755 ?
Pu2 O4 2.415(4) . ?
Pu2 Cl1 2.5350(17) . ?
Pu2 Cl2 2.5639(14) . ?
Pu2 Cl2 2.5639(14) 2_655 ?
Pu2 Cl3 2.5767(15) . ?
Pu2 Cl3 2.5767(15) 2_655 ?
O1 C1 1.451(5) . ?
O1 C1 1.451(5) 2_755 ?
O2 C6 1.452(5) . ?
O2 C3 1.463(5) . ?
O3 C10 1.444(6) . ?
O3 C7 1.445(6) . ?
O4 C11 1.462(5) 2_655 ?
O4 C11 1.462(5) . ?
C1 C2 1.456(9) . ?
C2 C2 1.476(16) 2_755 ?
C3 C4 1.467(7) . ?
C4 C5 1.478(8) . ?
C5 C6 1.486(7) . ?
C7 C8 1.441(8) . ?
C8 C9 1.448(9) . ?
C9 C10 1.456(8) . ?
C11 C12 1.495(7) . ?
C12 C12 1.469(10) 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
O1 Pu1 O2 71.85(8) . . ?
O1 Pu1 O2 71.85(8) . 2_755 ?
O2 Pu1 O2 143.71(15) . 2_755 ?
O1 Pu1 O3 143.20(8) . 2_755 ?
O2 Pu1 O3 143.77(11) . 2_755 ?
O2 Pu1 O3 72.07(11) 2_755 2_755 ?
O1 Pu1 O3 143.20(8) . . ?
O2 Pu1 O3 72.07(11) . . ?
O2 Pu1 O3 143.77(11) 2_755 . ?
O3 Pu1 O3 73.61(16) 2_755 . ?
O1 Pu1 Cl4 91.73(3) . . ?
O2 Pu1 Cl4 94.72(8) . . ?
O2 Pu1 Cl4 86.36(8) 2_755 . ?
O3 Pu1 Cl4 93.04(8) 2_755 . ?
O3 Pu1 Cl4 84.18(8) . . ?
O1 Pu1 Cl4 91.73(3) . 2_755 ?
O2 Pu1 Cl4 86.36(8) . 2_755 ?
O2 Pu1 Cl4 94.72(8) 2_755 2_755 ?
O3 Pu1 Cl4 84.18(8) 2_755 2_755 ?
O3 Pu1 Cl4 93.04(8) . 2_755 ?
Cl4 Pu1 Cl4 176.54(5) . 2_755 ?
O4 Pu2 Cl1 180.0 . . ?
O4 Pu2 Cl2 86.63(3) . . ?
Cl1 Pu2 Cl2 93.37(3) . . ?
O4 Pu2 Cl2 86.63(3) . 2_655 ?
Cl1 Pu2 Cl2 93.37(3) . 2_655 ?
Cl2 Pu2 Cl2 173.27(5) . 2_655 ?
O4 Pu2 Cl3 86.45(3) . . ?
Cl1 Pu2 Cl3 93.55(3) . . ?
Cl2 Pu2 Cl3 89.07(5) . . ?
Cl2 Pu2 Cl3 90.52(5) 2_655 . ?
O4 Pu2 Cl3 86.45(3) . 2_655 ?
Cl1 Pu2 Cl3 93.55(3) . 2_655 ?
Cl2 Pu2 Cl3 90.52(5) . 2_655 ?
Cl2 Pu2 Cl3 89.07(5) 2_655 2_655 ?
Cl3 Pu2 Cl3 172.89(6) . 2_655 ?
C1 O1 C1 108.6(5) . 2_755 ?
C1 O1 Pu1 125.7(3) . . ?
C1 O1 Pu1 125.7(3) 2_755 . ?
C6 O2 C3 108.5(3) . . ?
C6 O2 Pu1 123.7(3) . . ?
C3 O2 Pu1 127.2(2) . . ?
C10 O3 C7 107.0(4) . . ?
C10 O3 Pu1 128.7(3) . . ?
C7 O3 Pu1 124.3(3) . . ?
C11 O4 C11 110.1(5) 2_655 . ?
C11 O4 Pu2 124.9(2) 2_655 . ?
C11 O4 Pu2 124.9(2) . . ?
O1 C1 C2 105.0(5) . . ?
C1 C2 C2 103.9(4) . 2_755 ?
O2 C3 C4 106.0(4) . . ?
C3 C4 C5 105.1(5) . . ?
C4 C5 C6 103.8(4) . . ?
O2 C6 C5 105.3(4) . . ?
C8 C7 O3 107.4(5) . . ?
C7 C8 C9 108.5(5) . . ?
C10 C9 C8 105.9(5) . . ?
O3 C10 C9 107.2(5) . . ?
O4 C11 C12 105.1(4) . . ?
C12 C12 C11 105.9(3) 2_655 . ?

_refine_diff_density_max         1.571
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.156

_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# 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_apx2588a_sq
_database_code_depnum_ccdc_archive 'CCDC 1830525'
_audit_update_record             
;
2018-03-17 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_CHEMW03_apx2588a_sq         
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Molecular formula is correct. PLATON SQUEEZE used to 
treat disordered diethyl ether solvent molecules that are not 
included in the refinement model.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H40 Cl3 N4 Np O2'
_chemical_formula_weight         807.99

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           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                   12.5752(8)
_cell_length_b                   15.7756(10)
_cell_length_c                   15.1347(14)
_cell_angle_alpha                90
_cell_angle_beta                 108.7108(7)
_cell_angle_gamma                90
_cell_volume                     2843.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    8129
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.08

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    3.970
_shelx_estimated_absorpt_T_min   0.300
_shelx_estimated_absorpt_T_max   0.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.304
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16224
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.142
_diffrn_reflns_theta_max         28.590
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3452
_reflns_number_gt                3024
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_publication_material  'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_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)+(0.0249P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3452
_refine_ls_number_parameters     128
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0462
_refine_ls_wR_factor_gt          0.0446
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_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 1.0000 0.39642(2) 0.2500 0.01640(5) Uani 1 2 d S T P . .
Cl1 Cl 1.08196(6) 0.40173(5) 0.10492(5) 0.03252(16) Uani 1 1 d . . . . .
Cl2 Cl 1.0000 0.22335(6) 0.2500 0.02409(19) Uani 1 2 d S T P . .
N1 N 0.8023(2) 0.35988(15) 0.13153(17) 0.0307(6) Uani 1 1 d . . . . .
N2 N 0.88031(18) 0.53460(14) 0.18930(15) 0.0252(5) Uani 1 1 d . . . . .
C1 C 0.7742(3) 0.37611(19) 0.0399(2) 0.0379(8) Uani 1 1 d . . . . .
H1 H 0.8231 0.4079 0.0184 0.046 Uiso 1 1 calc R U . . .
C2 C 0.6749(3) 0.3473(2) -0.0240(2) 0.0488(10) Uani 1 1 d . . . . .
H2 H 0.6574 0.3601 -0.0870 0.059 Uiso 1 1 calc R U . . .
C3 C 0.6030(3) 0.2996(2) 0.0073(3) 0.0548(11) Uani 1 1 d . . . . .
H3 H 0.5367 0.2786 -0.0344 0.066 Uiso 1 1 calc R U . . .
C4 C 0.6305(3) 0.2833(2) 0.1008(3) 0.0510(10) Uani 1 1 d . . . . .
H4 H 0.5829 0.2515 0.1237 0.061 Uiso 1 1 calc R U . . .
C5 C 0.7300(2) 0.3149(2) 0.1605(2) 0.0390(7) Uani 1 1 d . . . . .
H5 H 0.7475 0.3044 0.2240 0.047 Uiso 1 1 calc R U . . .
C6 C 0.7956(3) 0.5559(2) 0.2196(2) 0.0360(7) Uani 1 1 d . . . . .
H6 H 0.7785 0.5204 0.2622 0.043 Uiso 1 1 calc R U . . .
C7 C 0.7316(3) 0.6285(2) 0.1908(3) 0.0456(9) Uani 1 1 d . . . . .
H7 H 0.6730 0.6409 0.2136 0.055 Uiso 1 1 calc R U . . .
C8 C 0.7556(3) 0.6811(2) 0.1286(2) 0.0453(9) Uani 1 1 d . . . . .
H8 H 0.7144 0.7305 0.1090 0.054 Uiso 1 1 calc R U . . .
C9 C 0.8422(3) 0.6599(2) 0.0952(2) 0.0411(8) Uani 1 1 d . . . . .
H9 H 0.8600 0.6945 0.0522 0.049 Uiso 1 1 calc R U . . .
C10 C 0.9019(3) 0.58628(18) 0.1269(2) 0.0313(7) Uani 1 1 d . . . . .
H10 H 0.9598 0.5720 0.1039 0.038 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 2.620(2) 2_755 ?
Np1 N1 2.620(2) . ?
Np1 N2 2.641(2) . ?
Np1 N2 2.641(2) 2_755 ?
Np1 Cl1 2.7097(7) . ?
Np1 Cl1 2.7097(7) 2_755 ?
Np1 Cl2 2.7303(9) . ?
N1 C5 1.333(4) . ?
N1 C1 1.341(4) . ?
N2 C6 1.331(4) . ?
N2 C10 1.339(4) . ?
C1 C2 1.388(4) . ?
C2 C3 1.372(6) . ?
C3 C4 1.369(6) . ?
C4 C5 1.381(4) . ?
C6 C7 1.387(4) . ?
C7 C8 1.359(5) . ?
C8 C9 1.381(5) . ?
C9 C10 1.383(4) . ?

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 154.58(11) 2_755 . ?
N1 Np1 N2 136.83(7) 2_755 . ?
N1 Np1 N2 68.52(7) . . ?
N1 Np1 N2 68.53(7) 2_755 2_755 ?
N1 Np1 N2 136.83(7) . 2_755 ?
N2 Np1 N2 68.73(9) . 2_755 ?
N1 Np1 Cl1 92.14(6) 2_755 . ?
N1 Np1 Cl1 88.64(6) . . ?
N2 Np1 Cl1 90.86(5) . . ?
N2 Np1 Cl1 86.21(5) 2_755 . ?
N1 Np1 Cl1 88.64(6) 2_755 2_755 ?
N1 Np1 Cl1 92.14(6) . 2_755 ?
N2 Np1 Cl1 86.21(5) . 2_755 ?
N2 Np1 Cl1 90.87(5) 2_755 2_755 ?
Cl1 Np1 Cl1 176.46(3) . 2_755 ?
N1 Np1 Cl2 77.29(5) 2_755 . ?
N1 Np1 Cl2 77.29(5) . . ?
N2 Np1 Cl2 145.63(5) . . ?
N2 Np1 Cl2 145.64(5) 2_755 . ?
Cl1 Np1 Cl2 91.770(17) . . ?
Cl1 Np1 Cl2 91.769(17) 2_755 . ?
C5 N1 C1 117.4(3) . . ?
C5 N1 Np1 119.29(19) . . ?
C1 N1 Np1 122.9(2) . . ?
C6 N2 C10 117.0(3) . . ?
C6 N2 Np1 121.23(19) . . ?
C10 N2 Np1 121.73(18) . . ?
N1 C1 C2 122.6(4) . . ?
C3 C2 C1 119.0(3) . . ?
C4 C3 C2 118.9(3) . . ?
C3 C4 C5 118.9(4) . . ?
N1 C5 C4 123.2(3) . . ?
N2 C6 C7 123.2(3) . . ?
C8 C7 C6 119.1(3) . . ?
C7 C8 C9 118.8(3) . . ?
C8 C9 C10 118.7(3) . . ?
N2 C10 C9 123.0(3) . . ?

_refine_diff_density_max         1.381
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.112


_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# 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_apx2580a
_database_code_depnum_ccdc_archive 'CCDC 1830524'
_audit_update_record             
;
2018-03-17 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT410_apx2580a            
;
PROBLEM: Short Intra H...H Contact  H9A      ..H10D             1.82 Ang.  
RESPONSE: disordered group
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H24 Cl4 Np O3'
_chemical_formula_weight         595.11

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'
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           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                   7.8064(13)
_cell_length_b                   14.381(3)
_cell_length_c                   8.4636(15)
_cell_angle_alpha                90
_cell_angle_beta                 100.8372(19)
_cell_angle_gamma                90
_cell_volume                     933.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    6250
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      28.11

_exptl_crystal_description       plate
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.118
_exptl_crystal_F_000             562
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    6.143
_shelx_estimated_absorpt_T_min   0.193
_shelx_estimated_absorpt_T_max   0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.086
_exptl_absorpt_correction_T_max  0.612
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10636
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.450
_diffrn_reflns_theta_max         28.537
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4354
_reflns_number_gt                3963
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_max     0.951
_reflns_Friedel_fraction_full    0.999

_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       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_publication_material  'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_refine_special_details          
;
 Refined as a 2-component inversion 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)+(0.0234P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.38(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4354
_refine_ls_number_parameters     200
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0546
_refine_ls_wR_factor_gt          0.0535
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      0.980
_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 0.11799(3) 0.25008(3) 0.33301(3) 0.01746(8) Uani 1 1 d . . . . .
Cl1 Cl 0.1420(3) 0.07803(16) 0.2426(3) 0.0371(6) Uani 1 1 d . . . . .
Cl2 Cl 0.4308(3) 0.21540(16) 0.4883(3) 0.0357(6) Uani 1 1 d . . . . .
Cl3 Cl -0.0665(3) 0.19589(16) 0.5369(3) 0.0298(5) Uani 1 1 d . . . . .
Cl4 Cl 0.2564(3) 0.32477(18) 0.1106(3) 0.0334(5) Uani 1 1 d . . . . .
O1 O -0.1311(7) 0.2278(4) 0.1104(7) 0.0240(17) Uani 1 1 d . . . . .
O2 O -0.0766(7) 0.3887(4) 0.2818(7) 0.0240(13) Uani 1 1 d . . . . .
O3 O 0.1905(7) 0.3739(4) 0.5337(7) 0.0242(13) Uani 1 1 d . . . . .
C1 C -0.1217(12) 0.1976(7) -0.0515(11) 0.034(2) Uani 1 1 d . . . . .
H1A H -0.0165 0.1618 -0.0517 0.041 Uiso 1 1 calc R U . . .
H1B H -0.1221 0.2507 -0.1224 0.041 Uiso 1 1 calc R U . . .
C2 C -0.2809(15) 0.1387(8) -0.1045(13) 0.050(3) Uani 1 1 d . . . . .
H2A H -0.3192 0.1407 -0.2203 0.061 Uiso 1 1 calc R U . . .
H2B H -0.2602 0.0746 -0.0705 0.061 Uiso 1 1 calc R U . . .
C3 C -0.4095(13) 0.1846(9) -0.0193(16) 0.058(4) Uani 1 1 d . . . . .
H3A H -0.4923 0.1392 0.0059 0.070 Uiso 1 1 calc R U . . .
H3B H -0.4734 0.2323 -0.0872 0.070 Uiso 1 1 calc R U . . .
C4 C -0.3117(10) 0.2264(7) 0.1301(11) 0.038(3) Uani 1 1 d . . . . .
H4A H -0.3528 0.2890 0.1442 0.045 Uiso 1 1 calc R U . . .
H4B H -0.3248 0.1894 0.2229 0.045 Uiso 1 1 calc R U . . .
C5 C -0.1127(12) 0.4442(7) 0.1355(11) 0.034(2) Uani 1 1 d . . . . .
H5A H -0.1709 0.4069 0.0456 0.040 Uiso 1 1 calc R U . . .
H5B H -0.0054 0.4686 0.1098 0.040 Uiso 1 1 calc R U . . .
C6 C -0.2289(15) 0.5219(8) 0.1700(14) 0.049(3) Uani 1 1 d . . . . .
H6A H -0.1607 0.5767 0.2076 0.059 Uiso 1 1 calc R U . . .
H6B H -0.3129 0.5381 0.0742 0.059 Uiso 1 1 calc R U . . .
C7 C -0.3181(16) 0.4855(9) 0.2964(15) 0.040(3) Uani 1 1 d . . . . .
H7A H -0.4191 0.4485 0.2507 0.048 Uiso 1 1 calc R U . . .
H7B H -0.3542 0.5355 0.3598 0.048 Uiso 1 1 calc R U . . .
C8 C -0.1801(13) 0.4275(7) 0.3944(12) 0.040(2) Uani 1 1 d . . . . .
H8A H -0.1072 0.4650 0.4757 0.048 Uiso 1 1 calc R U . . .
H8B H -0.2319 0.3779 0.4475 0.048 Uiso 1 1 calc R U . . .
C9 C 0.2865(14) 0.4548(7) 0.4918(12) 0.039(3) Uani 1 1 d . . . . .
H9A H 0.2114 0.5088 0.4702 0.047 Uiso 1 1 calc R U . A 1
H9B H 0.3393 0.4423 0.3990 0.047 Uiso 1 1 calc R U . A 1
C10' C 0.424(3) 0.4681(17) 0.643(3) 0.034(6) Uani 0.5 1 d D U P B 1
H10A H 0.5195 0.4245 0.6480 0.041 Uiso 0.5 1 calc R U P B 1
H10B H 0.4690 0.5312 0.6516 0.041 Uiso 0.5 1 calc R U P B 1
C11' C 0.316(3) 0.448(2) 0.765(3) 0.033(6) Uani 0.5 1 d D U P B 1
H11A H 0.3889 0.4385 0.8701 0.040 Uiso 0.5 1 calc R U P B 1
H11B H 0.2357 0.4986 0.7724 0.040 Uiso 0.5 1 calc R U P B 1
C10 C 0.358(4) 0.5011(16) 0.650(3) 0.040(8) Uani 0.5 1 d D . P B 2
H10C H 0.4639 0.5350 0.6450 0.048 Uiso 0.5 1 calc R U P B 2
H10D H 0.2730 0.5438 0.6801 0.048 Uiso 0.5 1 calc R U P B 2
C11 C 0.393(3) 0.4235(16) 0.766(3) 0.033(6) Uani 0.5 1 d D . P B 2
H11C H 0.4022 0.4447 0.8766 0.039 Uiso 0.5 1 calc R U P B 2
H11D H 0.4975 0.3896 0.7558 0.039 Uiso 0.5 1 calc R U P B 2
C12 C 0.2220(14) 0.3636(7) 0.7090(11) 0.034(2) Uani 1 1 d . . . . .
H12A H 0.1131 0.3594 0.7481 0.040 Uiso 1 1 calc R U . B 1
H12B H 0.2917 0.3088 0.7430 0.040 Uiso 1 1 calc R U . B 1


_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 O3 2.452(6) . ?
Np1 O1 2.461(5) . ?
Np1 O2 2.495(6) . ?
Np1 Cl3 2.568(2) . ?
Np1 Cl4 2.575(2) . ?
Np1 Cl2 2.595(2) . ?
Np1 Cl1 2.607(2) . ?
O1 C4 1.450(9) . ?
O1 C1 1.453(10) . ?
O2 C5 1.455(10) . ?
O2 C8 1.470(10) . ?
O3 C9 1.462(10) . ?
O3 C12 1.465(10) . ?
C1 C2 1.501(14) . ?
C2 C3 1.496(14) . ?
C3 C4 1.477(13) . ?
C5 C6 1.503(13) . ?
C6 C7 1.478(16) . ?
C7 C8 1.486(14) . ?
C9 C10 1.51(3) . ?
C9 C10' 1.52(3) . ?
C10' C11' 1.48(2) . ?
C11' C12 1.45(3) . ?
C10 C11 1.48(2) . ?
C11 C12 1.59(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Np1 O1 132.14(18) . . ?
O3 Np1 O2 66.03(19) . . ?
O1 Np1 O2 66.63(18) . . ?
O3 Np1 Cl3 80.82(14) . . ?
O1 Np1 Cl3 90.73(14) . . ?
O2 Np1 Cl3 87.66(14) . . ?
O3 Np1 Cl4 97.44(14) . . ?
O1 Np1 Cl4 82.79(14) . . ?
O2 Np1 Cl4 82.25(14) . . ?
Cl3 Np1 Cl4 169.55(7) . . ?
O3 Np1 Cl2 73.51(15) . . ?
O1 Np1 Cl2 153.61(13) . . ?
O2 Np1 Cl2 136.55(15) . . ?
Cl3 Np1 Cl2 101.21(8) . . ?
Cl4 Np1 Cl2 88.07(8) . . ?
O3 Np1 Cl1 150.74(15) . . ?
O1 Np1 Cl1 75.04(13) . . ?
O2 Np1 Cl1 141.49(15) . . ?
Cl3 Np1 Cl1 89.40(8) . . ?
Cl4 Np1 Cl1 96.78(8) . . ?
Cl2 Np1 Cl1 81.58(8) . . ?
C4 O1 C1 109.1(6) . . ?
C4 O1 Np1 124.0(5) . . ?
C1 O1 Np1 126.0(5) . . ?
C5 O2 C8 107.6(6) . . ?
C5 O2 Np1 126.9(5) . . ?
C8 O2 Np1 125.5(5) . . ?
C9 O3 C12 109.3(7) . . ?
C9 O3 Np1 118.1(5) . . ?
C12 O3 Np1 126.9(5) . . ?
O1 C1 C2 105.3(7) . . ?
C3 C2 C1 101.5(8) . . ?
C2 C3 C4 107.8(8) . . ?
O1 C4 C3 105.3(7) . . ?
O2 C5 C6 105.6(8) . . ?
C7 C6 C5 105.1(9) . . ?
C6 C7 C8 102.3(9) . . ?
O2 C8 C7 106.3(8) . . ?
O3 C9 C10 104.8(11) . . ?
O3 C9 C10' 102.2(11) . . ?
C11' C10' C9 99.2(17) . . ?
C12 C11' C10' 104.6(18) . . ?
C11 C10 C9 104.5(18) . . ?
C10 C11 C12 99.5(16) . . ?
C11' C12 O3 103.0(11) . . ?
O3 C12 C11 103.1(10) . . ?

_refine_diff_density_max         1.220
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.141

_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

