# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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. 
# 
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data_fmmm_betterscale_a
_database_code_depnum_ccdc_archive 'CCDC 1912314'
loop_
_audit_author_name
_audit_author_address
'Tori Z. Forbes'
;University of Iowa
United States of America
;
_audit_update_record             
;
2019-04-25 deposited with the CCDC.	2019-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'Lithium 12-crown-4 neptunyl tetrachloride'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 Cl4 Li2 Np O10'
_chemical_formula_weight         744.84

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_H-M_alt        'F m m m'
_space_group_name_Hall           '-F 2 2'

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

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

_cell_length_a                   13.115(8)
_cell_length_b                   13.371(7)
_cell_length_c                   14.838(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2602(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    956
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      25

_exptl_crystal_description       blade
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_F_000             1372
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    4.447
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3800
_exptl_absorpt_correction_T_max  0.4990
_exptl_absorpt_process_details   SCALE
_exptl_absorpt_special_details   'strong scatterer'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus X-ray'
_diffrn_measurement_device_type  'Bruker Quest'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11439
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.572
_diffrn_reflns_theta_max         26.442
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             766
_reflns_number_gt                766
_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       'APEX3 (Bruker AXS, Madison WI)'
_computing_cell_refinement       'APEX3 (Bruker AXS, Madison WI)'
_computing_data_reduction        'APEX3 (Bruker AXS, Madison WI)'
_computing_structure_solution    'APEX3 (Bruker AXS, Madison WI)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalMaker X'
_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)+(0.0733P)²+109.0648P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         766
_refine_ls_number_parameters     48
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1088
_refine_ls_wR_factor_gt          0.1088
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_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 0.5000 0.5000 0.5000 0.0129(2) Uani 1 8 d S T P . .
O1 O 0.5184(15) 0.5000 0.3814(8) 0.026(6) Uani 0.5 2 d S T P . .
Cl1 Cl 0.6415(2) 0.6382(2) 0.5132(11) 0.032(3) Uani 0.5 1 d . . P . .
Li1 Li 0.5000 0.5000 0.2532(15) 0.021(4) Uani 1 4 d S T P . .
C1A C 0.6968(18) 0.5000 0.1548(16) 0.037(5) Uiso 0.5 2 d S . P A 1
C1B C 0.6406(17) 0.5000 0.1128(15) 0.032(4) Uiso 0.5 2 d S . P A 1
C2 C 0.5000 0.6671(16) 0.1333(14) 0.081(5) Uiso 1 2 d S . P A 1
C3A C 0.614(2) 0.650(2) 0.1637(18) 0.070(6) Uiso 0.5 1 d . . P A 1
C4B C 0.670(2) 0.627(2) 0.1875(18) 0.072(6) Uiso 0.5 1 d . . P A 1
O2A O 0.6317(12) 0.4458(11) 0.2012(10) 0.060(4) Uiso 0.5 1 d . . P A 1
O2B O 0.4445(8) 0.6339(9) 0.2021(7) 0.037(2) Uiso 0.5 1 d . . P A 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 O1 1.776(12) . ?
Np1 O1 1.776(12) 18_556 ?
Np1 O1 1.776(12) 2_665 ?
Np1 O1 1.776(12) 17_666 ?
Np1 Cl1 2.626(3) 17_666 ?
Np1 Cl1 2.626(3) 18_556 ?
Np1 Cl1 2.626(3) 2_665 ?
Np1 Cl1 2.626(3) 20_655 ?
Np1 Cl1 2.626(3) 4_566 ?
Np1 Cl1 2.626(3) 19_565 ?
Np1 Cl1 2.626(3) 3_656 ?
Np1 Cl1 2.626(3) . ?
O1 O1 0.48(4) 2_665 ?
O1 Li1 1.92(2) . ?
Cl1 Cl1 0.39(3) 18_556 ?
Li1 O1 1.92(2) 2_665 ?
Li1 O2A 2.026(17) . ?
Li1 O2A 2.026(17) 20_655 ?
Li1 O2A 2.026(17) 2_665 ?
Li1 O2A 2.026(17) 19_565 ?
Li1 O2B 2.075(14) 19_565 ?
Li1 O2B 2.075(14) 2_665 ?
Li1 O2B 2.075(14) 20_655 ?
Li1 O2B 2.075(14) . ?
Li1 C1B 2.78(3) 2_665 ?
Li1 C1B 2.78(3) . ?
C1A C1B 0.97(3) . ?
C1A O2A 1.31(2) 19_565 ?
C1A O2A 1.31(2) . ?
C1A C4B 1.80(3) 19_565 ?
C1A C4B 1.80(3) . ?
C1B O2A 1.50(2) 19_565 ?
C1B O2A 1.50(2) . ?
C2 O2B 1.33(2) . ?
C2 O2B 1.33(2) 20_655 ?
C2 C3A 1.58(3) . ?
C2 C3A 1.58(3) 20_655 ?
C3A C4B 0.87(3) . ?
C3A O2B 0.98(3) 20_655 ?
C3A O2A 1.42(3) 19_565 ?
C4B O2A 1.11(3) 19_565 ?
C4B O2B 1.52(3) 20_655 ?
O2A C4B 1.11(3) 19_565 ?
O2A C3A 1.42(3) 19_565 ?
O2A O2A 1.45(3) 19_565 ?
O2A O2B 1.461(19) 2_665 ?
O2B C3A 0.98(3) 20_655 ?
O2B O2B 1.46(2) 20_655 ?
O2B O2A 1.461(19) 2_665 ?
O2B C4B 1.52(3) 20_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 Np1 O1 164.4(12) . 18_556 ?
O1 Np1 O1 15.6(12) . 2_665 ?
O1 Np1 O1 180.0 18_556 2_665 ?
O1 Np1 O1 180.0 . 17_666 ?
O1 Np1 O1 15.6(12) 18_556 17_666 ?
O1 Np1 O1 164.4(12) 2_665 17_666 ?
O1 Np1 Cl1 91.3(6) . 17_666 ?
O1 Np1 Cl1 99.8(6) 18_556 17_666 ?
O1 Np1 Cl1 80.2(6) 2_665 17_666 ?
O1 Np1 Cl1 88.7(6) 17_666 17_666 ?
O1 Np1 Cl1 80.2(6) . 18_556 ?
O1 Np1 Cl1 88.7(6) 18_556 18_556 ?
O1 Np1 Cl1 91.3(6) 2_665 18_556 ?
O1 Np1 Cl1 99.8(6) 17_666 18_556 ?
Cl1 Np1 Cl1 171.4(7) 17_666 18_556 ?
O1 Np1 Cl1 99.8(6) . 2_665 ?
O1 Np1 Cl1 91.3(6) 18_556 2_665 ?
O1 Np1 Cl1 88.7(6) 2_665 2_665 ?
O1 Np1 Cl1 80.2(6) 17_666 2_665 ?
Cl1 Np1 Cl1 8.6(7) 17_666 2_665 ?
Cl1 Np1 Cl1 180.0 18_556 2_665 ?
O1 Np1 Cl1 99.8(6) . 20_655 ?
O1 Np1 Cl1 91.3(6) 18_556 20_655 ?
O1 Np1 Cl1 88.7(6) 2_665 20_655 ?
O1 Np1 Cl1 80.2(6) 17_666 20_655 ?
Cl1 Np1 Cl1 90.06(14) 17_666 20_655 ?
Cl1 Np1 Cl1 90.58(15) 18_556 20_655 ?
Cl1 Np1 Cl1 89.42(15) 2_665 20_655 ?
O1 Np1 Cl1 80.2(6) . 4_566 ?
O1 Np1 Cl1 88.7(6) 18_556 4_566 ?
O1 Np1 Cl1 91.3(6) 2_665 4_566 ?
O1 Np1 Cl1 99.8(6) 17_666 4_566 ?
Cl1 Np1 Cl1 89.94(14) 17_666 4_566 ?
Cl1 Np1 Cl1 89.42(15) 18_556 4_566 ?
Cl1 Np1 Cl1 90.58(15) 2_665 4_566 ?
Cl1 Np1 Cl1 180.0 20_655 4_566 ?
O1 Np1 Cl1 88.7(6) . 19_565 ?
O1 Np1 Cl1 80.2(6) 18_556 19_565 ?
O1 Np1 Cl1 99.8(6) 2_665 19_565 ?
O1 Np1 Cl1 91.3(6) 17_666 19_565 ?
Cl1 Np1 Cl1 90.58(15) 17_666 19_565 ?
Cl1 Np1 Cl1 90.06(14) 18_556 19_565 ?
Cl1 Np1 Cl1 89.94(14) 2_665 19_565 ?
Cl1 Np1 Cl1 171.4(7) 20_655 19_565 ?
Cl1 Np1 Cl1 8.6(7) 4_566 19_565 ?
O1 Np1 Cl1 91.3(6) . 3_656 ?
O1 Np1 Cl1 99.8(6) 18_556 3_656 ?
O1 Np1 Cl1 80.2(6) 2_665 3_656 ?
O1 Np1 Cl1 88.7(6) 17_666 3_656 ?
Cl1 Np1 Cl1 89.42(15) 17_666 3_656 ?
Cl1 Np1 Cl1 89.94(14) 18_556 3_656 ?
Cl1 Np1 Cl1 90.06(14) 2_665 3_656 ?
Cl1 Np1 Cl1 8.6(7) 20_655 3_656 ?
Cl1 Np1 Cl1 171.4(7) 4_566 3_656 ?
Cl1 Np1 Cl1 180.0(7) 19_565 3_656 ?
O1 Np1 Cl1 88.7(6) . . ?
O1 Np1 Cl1 80.2(6) 18_556 . ?
O1 Np1 Cl1 99.8(6) 2_665 . ?
O1 Np1 Cl1 91.3(6) 17_666 . ?
Cl1 Np1 Cl1 180.0 17_666 . ?
Cl1 Np1 Cl1 8.6(7) 18_556 . ?
Cl1 Np1 Cl1 171.4(7) 2_665 . ?
Cl1 Np1 Cl1 89.94(14) 20_655 . ?
Cl1 Np1 Cl1 90.06(14) 4_566 . ?
Cl1 Np1 Cl1 89.42(15) 19_565 . ?
Cl1 Np1 Cl1 90.58(15) 3_656 . ?
O1 O1 Np1 82.2(6) 2_665 . ?
O1 O1 Li1 82.8(6) 2_665 . ?
Np1 O1 Li1 165.0(12) . . ?
Cl1 Cl1 Np1 85.7(3) 18_556 . ?
O1 Li1 O1 14.4(11) 2_665 . ?
O1 Li1 O2A 119.0(9) 2_665 . ?
O1 Li1 O2A 105.7(8) . . ?
O1 Li1 O2A 105.7(8) 2_665 20_655 ?
O1 Li1 O2A 119.0(9) . 20_655 ?
O2A Li1 O2A 117.0(12) . 20_655 ?
O1 Li1 O2A 105.7(8) 2_665 2_665 ?
O1 Li1 O2A 119.0(9) . 2_665 ?
O2A Li1 O2A 135.2(14) . 2_665 ?
O2A Li1 O2A 41.9(9) 20_655 2_665 ?
O1 Li1 O2A 119.0(9) 2_665 19_565 ?
O1 Li1 O2A 105.7(8) . 19_565 ?
O2A Li1 O2A 41.9(9) . 19_565 ?
O2A Li1 O2A 135.2(14) 20_655 19_565 ?
O2A Li1 O2A 117.0(12) 2_665 19_565 ?
O1 Li1 O2B 108.5(7) 2_665 19_565 ?
O1 Li1 O2B 114.0(7) . 19_565 ?
O2A Li1 O2B 81.5(7) . 19_565 ?
O2A Li1 O2B 41.7(6) 20_655 19_565 ?
O2A Li1 O2B 82.5(7) 2_665 19_565 ?
O2A Li1 O2B 117.9(9) 19_565 19_565 ?
O1 Li1 O2B 114.0(7) 2_665 2_665 ?
O1 Li1 O2B 108.5(7) . 2_665 ?
O2A Li1 O2B 41.7(6) . 2_665 ?
O2A Li1 O2B 81.5(7) 20_655 2_665 ?
O2A Li1 O2B 117.9(9) 2_665 2_665 ?
O2A Li1 O2B 82.5(7) 19_565 2_665 ?
O2B Li1 O2B 41.1(6) 19_565 2_665 ?
O1 Li1 O2B 114.0(7) 2_665 20_655 ?
O1 Li1 O2B 108.5(7) . 20_655 ?
O2A Li1 O2B 82.5(7) . 20_655 ?
O2A Li1 O2B 117.9(9) 20_655 20_655 ?
O2A Li1 O2B 81.5(7) 2_665 20_655 ?
O2A Li1 O2B 41.7(6) 19_565 20_655 ?
O2B Li1 O2B 137.2(13) 19_565 20_655 ?
O2B Li1 O2B 119.2(10) 2_665 20_655 ?
O1 Li1 O2B 108.5(7) 2_665 . ?
O1 Li1 O2B 114.0(7) . . ?
O2A Li1 O2B 117.9(9) . . ?
O2A Li1 O2B 82.5(7) 20_655 . ?
O2A Li1 O2B 41.7(6) 2_665 . ?
O2A Li1 O2B 81.5(7) 19_565 . ?
O2B Li1 O2B 119.2(10) 19_565 . ?
O2B Li1 O2B 137.2(13) 2_665 . ?
O2B Li1 O2B 41.1(6) 20_655 . ?
O1 Li1 C1B 131.3(8) 2_665 2_665 ?
O1 Li1 C1B 145.7(8) . 2_665 ?
O2A Li1 C1B 106.3(10) . 2_665 ?
O2A Li1 C1B 31.8(6) 20_655 2_665 ?
O2A Li1 C1B 31.8(6) 2_665 2_665 ?
O2A Li1 C1B 106.3(10) 19_565 2_665 ?
O2B Li1 C1B 59.6(5) 19_565 2_665 ?
O2B Li1 C1B 87.7(7) 2_665 2_665 ?
O2B Li1 C1B 87.7(7) 20_655 2_665 ?
O2B Li1 C1B 59.6(5) . 2_665 ?
O1 Li1 C1B 145.7(8) 2_665 . ?
O1 Li1 C1B 131.3(8) . . ?
O2A Li1 C1B 31.8(6) . . ?
O2A Li1 C1B 106.3(10) 20_655 . ?
O2A Li1 C1B 106.3(10) 2_665 . ?
O2A Li1 C1B 31.8(6) 19_565 . ?
O2B Li1 C1B 87.7(7) 19_565 . ?
O2B Li1 C1B 59.6(5) 2_665 . ?
O2B Li1 C1B 59.6(5) 20_655 . ?
O2B Li1 C1B 87.7(7) . . ?
C1B Li1 C1B 83.0(11) 2_665 . ?
C1B C1A O2A 80.9(19) . 19_565 ?
C1B C1A O2A 80.9(19) . . ?
O2A C1A O2A 66.9(18) 19_565 . ?
C1B C1A C4B 91.3(14) . 19_565 ?
O2A C1A C4B 104.5(17) 19_565 19_565 ?
O2A C1A C4B 37.9(10) . 19_565 ?
C1B C1A C4B 91.3(14) . . ?
O2A C1A C4B 37.9(10) 19_565 . ?
O2A C1A C4B 104.5(17) . . ?
C4B C1A C4B 141(2) 19_565 . ?
C1A C1B O2A 59.7(17) . 19_565 ?
C1A C1B O2A 59.7(17) . . ?
O2A C1B O2A 57.6(14) 19_565 . ?
C1A C1B Li1 91(2) . . ?
O2A C1B Li1 45.2(9) 19_565 . ?
O2A C1B Li1 45.2(9) . . ?
O2B C2 O2B 66.3(14) . 20_655 ?
O2B C2 C3A 104.5(17) . . ?
O2B C2 C3A 38.2(10) 20_655 . ?
O2B C2 C3A 38.2(10) . 20_655 ?
O2B C2 C3A 104.5(17) 20_655 20_655 ?
C3A C2 C3A 143(2) . 20_655 ?
C4B C3A O2B 110(3) . 20_655 ?
C4B C3A O2A 52(2) . 19_565 ?
O2B C3A O2A 72.5(19) 20_655 19_565 ?
C4B C3A C2 165(4) . . ?
O2B C3A C2 57.0(17) 20_655 . ?
O2A C3A C2 113(2) 19_565 . ?
C3A C4B O2A 91(3) . 19_565 ?
C3A C4B O2B 37(2) . 20_655 ?
O2A C4B O2B 65.5(16) 19_565 20_655 ?
C3A C4B C1A 113(3) . . ?
O2A C4B C1A 46.7(15) 19_565 . ?
O2B C4B C1A 107.0(18) 20_655 . ?
C4B O2A C1A 95.4(18) 19_565 . ?
C4B O2A C3A 37.8(16) 19_565 19_565 ?
C1A O2A C3A 113.6(17) . 19_565 ?
C4B O2A O2A 151.0(16) 19_565 19_565 ?
C1A O2A O2A 56.5(9) . 19_565 ?
C3A O2A O2A 154.9(12) 19_565 19_565 ?
C4B O2A O2B 70.8(16) 19_565 2_665 ?
C1A O2A O2B 148.4(16) . 2_665 ?
C3A O2A O2B 39.8(12) 19_565 2_665 ?
O2A O2A O2B 136.8(7) 19_565 2_665 ?
C4B O2A C1B 103.1(18) 19_565 . ?
C1A O2A C1B 39.4(13) . . ?
C3A O2A C1B 96.1(14) 19_565 . ?
O2A O2A C1B 61.2(7) 19_565 . ?
O2B O2A C1B 114.4(13) 2_665 . ?
C4B O2A Li1 139.9(18) 19_565 . ?
C1A O2A Li1 123.8(12) . . ?
C3A O2A Li1 109.5(15) 19_565 . ?
O2A O2A Li1 69.1(4) 19_565 . ?
O2B O2A Li1 70.9(8) 2_665 . ?
C1B O2A Li1 103.0(12) . . ?
C3A O2B C2 84.8(19) 20_655 . ?
C3A O2B O2B 141.6(18) 20_655 20_655 ?
C2 O2B O2B 56.8(7) . 20_655 ?
C3A O2B O2A 67.6(18) 20_655 2_665 ?
C2 O2B O2A 127.6(13) . 2_665 ?
O2B O2B O2A 133.2(7) 20_655 2_665 ?
C3A O2B C4B 32.5(18) 20_655 20_655 ?
C2 O2B C4B 116.8(15) . 20_655 ?
O2B O2B C4B 171.0(11) 20_655 20_655 ?
O2A O2B C4B 43.7(12) 2_665 20_655 ?
C3A O2B Li1 132.6(19) 20_655 . ?
C2 O2B Li1 112.1(11) . . ?
O2B O2B Li1 69.5(3) 20_655 . ?
O2A O2B Li1 67.3(8) 2_665 . ?
C4B O2B Li1 110.2(13) 20_655 . ?

_refine_diff_density_max         2.259
_refine_diff_density_min         -1.669
_refine_diff_density_rms         0.223

####################################################################### 
# 
# 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_P21n
_database_code_depnum_ccdc_archive 'CCDC 1912315'
loop_
_audit_author_name
_audit_author_address
'Tori Z. Forbes'
;University of Iowa
United States of America
;
_audit_update_record             
;
2019-04-25 deposited with the CCDC.	2019-05-21 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            'C24 H52 Cl4 Na2 Np O16'
_chemical_formula_weight         1021.43

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'
Na Na 0.0362 0.0249 '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                   14.117(3)
_cell_length_b                   9.517(2)
_cell_length_c                   14.336(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.388(8)
_cell_angle_gamma                90
_cell_volume                     1888.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1127
_cell_measurement_theta_min      2
_cell_measurement_theta_max      25

_exptl_crystal_description       blocky
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_F_000             1014
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    3.122
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   semiempirical
_exptl_absorpt_correction_T_min  0.4871
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Diffrac'
_diffrn_measurement_method       'phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33982
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.260
_diffrn_reflns_theta_max         28.346
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4677
_reflns_number_gt                3972
_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       'APEX3 (Bruker, Madison, WI)'
_computing_cell_refinement       'APEX3 (Bruker, Madison, WI)'
_computing_data_reduction        'APEX3 (Bruker, Madison, WI)'
_computing_structure_solution    'APEX3 (Bruker, Madison, WI)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Crystalmaker X'
_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)+(0.0076P)²+2.2073P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4677
_refine_ls_number_parameters     318
_refine_ls_number_restraints     117
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0204
_refine_ls_wR_factor_ref         0.0468
_refine_ls_wR_factor_gt          0.0439
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.088
_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 0.0000 1.0000 0.5000 0.01095(4) Uani 1 2 d S . P . .
H1 H 0.370(2) 0.147(3) 0.484(2) 0.015(7) Uiso 1 1 d . . . . .
Na1 Na 0.36701(7) 0.61477(10) 0.50442(7) 0.01878(19) Uani 1 1 d . U . . .
Cl1 Cl -0.02173(4) 1.21225(6) 0.61506(4) 0.01973(11) Uani 1 1 d . . . . .
O1 O 0.03374(13) 0.88714(19) 0.59794(12) 0.0193(3) Uani 1 1 d . . . . .
C1 C 0.58459(18) 0.1081(3) 0.34825(18) 0.0185(5) Uani 1 1 d . U . . .
Cl2 Cl 0.18499(4) 1.07040(7) 0.51249(5) 0.02258(12) Uani 1 1 d . . . . .
H2 H 0.373(2) 0.292(3) 0.441(2) 0.022(8) Uiso 1 1 d . . . . .
O2 O 0.49879(11) 0.20001(18) 0.46219(12) 0.0169(3) Uani 1 1 d . U . . .
C2 C 0.48724(18) 0.1295(3) 0.37309(18) 0.0190(5) Uani 1 1 d . U . . .
O3 O 0.46396(12) 0.41821(18) 0.58873(11) 0.0172(3) Uani 1 1 d . U . . .
H3 H 0.574(2) 0.063(3) 0.283(2) 0.023(8) Uiso 1 1 d . . . . .
C3 C 0.40649(17) 0.2270(3) 0.48489(19) 0.0198(5) Uani 1 1 d . U . . .
O4 O 0.65974(12) 0.4905(2) 0.66963(12) 0.0207(3) Uani 1 1 d . U . . .
H4 H 0.695(2) 0.185(3) 0.241(2) 0.016(7) Uiso 1 1 d . . . . .
C4 C 0.42032(19) 0.2820(3) 0.58449(18) 0.0208(5) Uani 1 1 d . U . . .
O5 O 0.80147(12) 0.48978(19) 0.56405(12) 0.0190(3) Uani 1 1 d . U . . .
H5 H 0.762(2) 0.192(3) 0.336(2) 0.017(7) Uiso 1 1 d . . . . .
C5 C 0.49676(19) 0.4634(3) 0.68532(17) 0.0199(5) Uani 1 1 d . U . . .
C6 C 0.59911(19) 0.4199(3) 0.72374(17) 0.0227(5) Uani 1 1 d . U . . .
H6 H 0.895(2) 0.482(3) 0.377(2) 0.021(8) Uiso 1 1 d . . . . .
O6 O 0.75300(12) 0.47249(17) 0.36531(12) 0.0182(3) Uani 1 1 d . U . . .
C7 C 0.75864(19) 0.4824(3) 0.71545(18) 0.0251(5) Uani 1 1 d . U . . .
H7 H 0.862(2) 0.360(3) 0.433(2) 0.022(8) Uiso 1 1 d . . . . .
O7 O 0.62752(12) 0.24200(17) 0.34433(12) 0.0160(3) Uani 1 1 d . U . . .
C8 C 0.81727(19) 0.5576(3) 0.65400(19) 0.0247(5) Uani 1 1 d . U . . .
H8 H 0.929(2) 0.541(3) 0.540(2) 0.028(8) Uiso 1 1 d . . . . .
O8 O 0.73221(14) 0.2046(2) 0.57341(14) 0.0228(4) Uani 1 1 d . . . . .
C9 C 0.86267(18) 0.5443(3) 0.50428(19) 0.0219(5) Uani 1 1 d . U . . .
H9 H 0.797(2) 0.649(3) 0.643(2) 0.022(8) Uiso 1 1 d . . . . .
C10 C 0.84988(17) 0.4552(3) 0.41655(18) 0.0200(5) Uani 1 1 d . U . . .
H10 H 0.887(2) 0.556(3) 0.683(2) 0.025(8) Uiso 1 1 d . . . . .
C11 C 0.73339(18) 0.3892(3) 0.28062(17) 0.0196(5) Uani 1 1 d . U . . .
H11 H 0.769(3) 0.527(4) 0.780(3) 0.035(10) Uiso 1 1 d . . . . .
C12 C 0.70933(18) 0.2390(3) 0.29980(18) 0.0193(5) Uani 1 1 d . U . . .
H13 H 0.616(2) 0.445(3) 0.788(2) 0.015(7) Uiso 1 1 d . . . . .
H14 H 0.610(2) 0.319(3) 0.719(2) 0.019(7) Uiso 1 1 d . . . . .
H15 H 0.456(2) 0.421(3) 0.726(2) 0.024(8) Uiso 1 1 d . . . . .
H16 H 0.496(2) 0.562(4) 0.691(2) 0.028(8) Uiso 1 1 d . . . . .
H17 H 0.357(2) 0.299(3) 0.601(2) 0.025(8) Uiso 1 1 d . . . . .
H18 H 0.844(2) 0.647(4) 0.487(2) 0.025(8) Uiso 1 1 d . . . . .
H19 H 0.679(2) 0.433(3) 0.242(2) 0.017(7) Uiso 1 1 d . . . . .
H20 H 0.456(2) 0.040(4) 0.376(2) 0.029(9) Uiso 1 1 d . . . . .
H21 H 0.462(2) 0.224(4) 0.628(2) 0.028(8) Uiso 1 1 d . . . . .
H22 H 0.788(2) 0.392(4) 0.247(2) 0.030(9) Uiso 1 1 d . . . . .
H23 H 0.449(2) 0.187(4) 0.323(2) 0.029(8) Uiso 1 1 d . . . . .
H24 H 0.626(2) 0.048(4) 0.393(2) 0.025(8) Uiso 1 1 d . . . . .
H25 H 0.744(3) 0.130(5) 0.559(3) 0.040(11) Uiso 1 1 d . . . . .
H26 H 0.780(3) 0.252(5) 0.585(3) 0.061(14) Uiso 1 1 d . . . . .
H12 H 0.781(2) 0.383(4) 0.727(2) 0.035(9) 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
Np1 O1 1.7572(17) 3_576 ?
Np1 O1 1.7572(17) . ?
Np1 Cl1 2.6637(7) . ?
Np1 Cl1 2.6637(7) 3_576 ?
Np1 Cl2 2.6675(8) . ?
Np1 Cl2 2.6676(8) 3_576 ?
Na1 O8 2.355(2) 3_666 ?
Na1 O3 2.486(2) . ?
Na1 O7 2.5496(19) 3_666 ?
Na1 O2 2.563(2) 3_666 ?
Na1 O5 2.586(2) 3_666 ?
Na1 O4 2.646(2) 3_666 ?
Na1 O6 2.880(2) 3_666 ?
Na1 O3 2.9722(19) 3_666 ?
C1 O7 1.417(3) . ?
C1 C2 1.500(3) . ?
C1 H3 1.02(3) . ?
C1 H24 0.96(3) . ?
O2 C2 1.423(3) . ?
O2 C3 1.427(3) . ?
O2 Na1 2.563(2) 3_666 ?
C2 H20 0.97(3) . ?
C2 H23 0.98(3) . ?
O3 C4 1.431(3) . ?
O3 C5 1.436(3) . ?
O3 Na1 2.9722(19) 3_666 ?
C3 C4 1.497(4) . ?
C3 H1 0.92(3) . ?
C3 H2 0.94(3) . ?
O4 C7 1.423(3) . ?
O4 C6 1.431(3) . ?
O4 Na1 2.646(2) 3_666 ?
C4 H17 0.98(3) . ?
C4 H21 0.95(3) . ?
O5 C8 1.420(3) . ?
O5 C9 1.429(3) . ?
O5 Na1 2.586(2) 3_666 ?
C5 C6 1.499(3) . ?
C5 H15 0.99(3) . ?
C5 H16 0.95(4) . ?
C6 H13 0.94(3) . ?
C6 H14 0.98(3) . ?
O6 C10 1.428(3) . ?
O6 C11 1.431(3) . ?
O6 Na1 2.880(2) 3_666 ?
C7 C8 1.503(4) . ?
C7 H11 0.99(4) . ?
C7 H12 1.00(4) . ?
O7 C12 1.426(3) . ?
O7 Na1 2.5495(19) 3_666 ?
C8 H9 0.92(3) . ?
C8 H10 0.98(3) . ?
O8 Na1 2.355(2) 3_666 ?
O8 H25 0.77(4) . ?
O8 H26 0.80(5) . ?
C9 C10 1.498(4) . ?
C9 H8 0.97(3) . ?
C9 H18 1.03(3) . ?
C10 H6 0.96(3) . ?
C10 H7 0.95(3) . ?
C11 C12 1.507(4) . ?
C11 H19 0.95(3) . ?
C11 H22 0.98(3) . ?
C12 H4 0.98(3) . ?
C12 H5 0.93(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Np1 O1 180.00(9) 3_576 . ?
O1 Np1 Cl1 89.15(6) 3_576 . ?
O1 Np1 Cl1 90.85(6) . . ?
O1 Np1 Cl1 90.85(6) 3_576 3_576 ?
O1 Np1 Cl1 89.15(6) . 3_576 ?
Cl1 Np1 Cl1 180.0 . 3_576 ?
O1 Np1 Cl2 90.42(6) 3_576 . ?
O1 Np1 Cl2 89.58(6) . . ?
Cl1 Np1 Cl2 89.93(2) . . ?
Cl1 Np1 Cl2 90.07(2) 3_576 . ?
O1 Np1 Cl2 89.58(6) 3_576 3_576 ?
O1 Np1 Cl2 90.42(6) . 3_576 ?
Cl1 Np1 Cl2 90.07(2) . 3_576 ?
Cl1 Np1 Cl2 89.93(2) 3_576 3_576 ?
Cl2 Np1 Cl2 180.0 . 3_576 ?
O8 Na1 O3 176.95(8) 3_666 . ?
O8 Na1 O7 85.87(7) 3_666 3_666 ?
O3 Na1 O7 93.87(6) . 3_666 ?
O8 Na1 O2 86.27(7) 3_666 3_666 ?
O3 Na1 O2 96.38(7) . 3_666 ?
O7 Na1 O2 64.92(6) 3_666 3_666 ?
O8 Na1 O5 71.62(7) 3_666 3_666 ?
O3 Na1 O5 105.77(7) . 3_666 ?
O7 Na1 O5 113.56(6) 3_666 3_666 ?
O2 Na1 O5 157.83(7) 3_666 3_666 ?
O8 Na1 O4 82.46(7) 3_666 3_666 ?
O3 Na1 O4 97.81(6) . 3_666 ?
O7 Na1 O4 168.32(7) 3_666 3_666 ?
O2 Na1 O4 113.53(7) 3_666 3_666 ?
O5 Na1 O4 63.07(6) 3_666 3_666 ?
O8 Na1 O6 98.44(7) 3_666 3_666 ?
O3 Na1 O6 78.79(6) . 3_666 ?
O7 Na1 O6 61.68(5) 3_666 3_666 ?
O2 Na1 O6 125.80(6) 3_666 3_666 ?
O5 Na1 O6 61.35(6) 3_666 3_666 ?
O4 Na1 O6 120.64(6) 3_666 3_666 ?
O8 Na1 O3 108.62(7) 3_666 3_666 ?
O3 Na1 O3 74.06(6) . 3_666 ?
O7 Na1 O3 123.12(6) 3_666 3_666 ?
O2 Na1 O3 61.78(5) 3_666 3_666 ?
O5 Na1 O3 123.27(6) 3_666 3_666 ?
O4 Na1 O3 60.92(5) 3_666 3_666 ?
O6 Na1 O3 152.63(6) 3_666 3_666 ?
O7 C1 C2 107.84(19) . . ?
O7 C1 H3 109.1(18) . . ?
C2 C1 H3 107.4(17) . . ?
O7 C1 H24 111(2) . . ?
C2 C1 H24 112.5(19) . . ?
H3 C1 H24 109(3) . . ?
C2 O2 C3 109.96(18) . . ?
C2 O2 Na1 116.19(13) . 3_666 ?
C3 O2 Na1 120.54(14) . 3_666 ?
O2 C2 C1 109.21(19) . . ?
O2 C2 H20 110(2) . . ?
C1 C2 H20 110(2) . . ?
O2 C2 H23 110.3(19) . . ?
C1 C2 H23 107.5(18) . . ?
H20 C2 H23 109(3) . . ?
C4 O3 C5 111.48(18) . . ?
C4 O3 Na1 118.02(15) . . ?
C5 O3 Na1 106.57(13) . . ?
C4 O3 Na1 105.21(13) . 3_666 ?
C5 O3 Na1 109.28(13) . 3_666 ?
Na1 O3 Na1 105.94(6) . 3_666 ?
O2 C3 C4 109.1(2) . . ?
O2 C3 H1 112.3(18) . . ?
C4 C3 H1 105.5(18) . . ?
O2 C3 H2 109.0(18) . . ?
C4 C3 H2 111.0(19) . . ?
H1 C3 H2 110(3) . . ?
C7 O4 C6 111.21(19) . . ?
C7 O4 Na1 111.06(14) . 3_666 ?
C6 O4 Na1 110.13(15) . 3_666 ?
O3 C4 C3 109.36(19) . . ?
O3 C4 H17 103.9(19) . . ?
C3 C4 H17 109.9(18) . . ?
O3 C4 H21 107(2) . . ?
C3 C4 H21 112(2) . . ?
H17 C4 H21 114(3) . . ?
C8 O5 C9 112.0(2) . . ?
C8 O5 Na1 119.17(14) . 3_666 ?
C9 O5 Na1 122.12(15) . 3_666 ?
O3 C5 C6 112.05(19) . . ?
O3 C5 H15 109.6(18) . . ?
C6 C5 H15 107.7(18) . . ?
O3 C5 H16 112(2) . . ?
C6 C5 H16 106(2) . . ?
H15 C5 H16 110(3) . . ?
O4 C6 C5 107.9(2) . . ?
O4 C6 H13 110.6(18) . . ?
C5 C6 H13 109.2(18) . . ?
O4 C6 H14 107.7(17) . . ?
C5 C6 H14 113.2(17) . . ?
H13 C6 H14 108(2) . . ?
C10 O6 C11 112.19(19) . . ?
C10 O6 Na1 105.02(13) . 3_666 ?
C11 O6 Na1 110.52(13) . 3_666 ?
O4 C7 C8 107.9(2) . . ?
O4 C7 H11 111(2) . . ?
C8 C7 H11 110(2) . . ?
O4 C7 H12 112(2) . . ?
C8 C7 H12 111(2) . . ?
H11 C7 H12 105(3) . . ?
C1 O7 C12 112.98(18) . . ?
C1 O7 Na1 112.86(13) . 3_666 ?
C12 O7 Na1 120.01(14) . 3_666 ?
O5 C8 C7 108.1(2) . . ?
O5 C8 H9 106.5(19) . . ?
C7 C8 H9 111.6(19) . . ?
O5 C8 H10 109.6(19) . . ?
C7 C8 H10 111.4(19) . . ?
H9 C8 H10 110(3) . . ?
Na1 O8 H25 133(3) 3_666 . ?
Na1 O8 H26 95(3) 3_666 . ?
H25 O8 H26 111(4) . . ?
O5 C9 C10 108.1(2) . . ?
O5 C9 H8 107.9(19) . . ?
C10 C9 H8 111.1(19) . . ?
O5 C9 H18 109.3(17) . . ?
C10 C9 H18 110.5(18) . . ?
H8 C9 H18 110(3) . . ?
O6 C10 C9 108.1(2) . . ?
O6 C10 H6 110.0(19) . . ?
C9 C10 H6 110.9(19) . . ?
O6 C10 H7 110.5(19) . . ?
C9 C10 H7 110.7(19) . . ?
H6 C10 H7 107(2) . . ?
O6 C11 C12 112.6(2) . . ?
O6 C11 H19 104.8(18) . . ?
C12 C11 H19 109.7(19) . . ?
O6 C11 H22 111(2) . . ?
C12 C11 H22 110(2) . . ?
H19 C11 H22 109(3) . . ?
O7 C12 C11 107.13(19) . . ?
O7 C12 H4 110.3(16) . . ?
C11 C12 H4 111.0(17) . . ?
O7 C12 H5 112.9(17) . . ?
C11 C12 H5 112.0(18) . . ?
H4 C12 H5 104(2) . . ?

_refine_diff_density_max         0.832
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.102

####################################################################### 
# 
# 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_p21c
_database_code_depnum_ccdc_archive 'CCDC 1912316'
loop_
_audit_author_name
_audit_author_address
'Tori Z. Forbes'
;University of Iowa
United States of America
;
_audit_update_record             
;
2019-04-25 deposited with the CCDC.	2019-05-21 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            'C24 H49 Cl4 K2 Np O14.50'
_chemical_formula_weight         1026.63

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'
K K 0.2009 0.2494 '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/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   10.0239(17)
_cell_length_b                   9.9861(17)
_cell_length_c                   19.349(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.187(7)
_cell_angle_gamma                90
_cell_volume                     1928.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    611
_cell_measurement_theta_min      2
_cell_measurement_theta_max      25

_exptl_crystal_description       blocky
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    3.244
_shelx_estimated_absorpt_T_min   0.6054
_shelx_estimated_absorpt_T_max   0.7457
_exptl_absorpt_correction_type   semiempirical
_exptl_absorpt_correction_T_min  0.6054
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Diffrac'
_diffrn_measurement_method       'phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37361
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.938
_diffrn_reflns_theta_max         28.351
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4764
_reflns_number_gt                4075
_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       'APEX3 (Bruker, Madison, WI)'
_computing_cell_refinement       'APEX3 (Bruker, Madison, WI)'
_computing_data_reduction        'APEX3 (Bruker, Madison, WI)'
_computing_structure_solution    'APEX3 (Bruker, Madison, WI)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Crystalmaker X'
_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)+(0.0247P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4764
_refine_ls_number_parameters     311
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0409
_refine_ls_wR_factor_gt          0.0392
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.004
_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 0.0000 0.5000 0.5000 0.01494(3) Uani 1 2 d S . P . .
K1 K 0.27223(3) 0.34007(4) 0.65188(2) 0.01684(7) Uani 1 1 d . . . . .
Cl1 Cl 0.17638(4) 0.63357(5) 0.58404(3) 0.02429(10) Uani 1 1 d . . . . .
Cl2 Cl -0.04931(5) 0.35369(6) 0.60981(3) 0.03030(11) Uani 1 1 d . . . . .
OW1 O 0.0594(9) 0.5687(10) 0.9548(5) 0.060(2) Uiso 0.25 1 d D . P . .
O1 O 0.12952(12) 0.38795(15) 0.48321(8) 0.0247(3) Uani 1 1 d . . . . .
O2 O 0.22288(13) 0.06286(14) 0.62178(7) 0.0194(3) Uani 1 1 d . . . . .
O3 O 0.17034(11) 0.16276(13) 0.75266(7) 0.0158(2) Uani 1 1 d . . . . .
O4 O 0.22104(12) 0.42921(14) 0.78803(7) 0.0180(3) Uani 1 1 d . . . . .
O5 O 0.44281(14) 0.53395(14) 0.72969(8) 0.0211(3) Uani 1 1 d . . . . .
O6 O 0.51095(12) 0.43793(15) 0.59936(7) 0.0195(3) Uani 1 1 d . . . . .
O7 O 0.43503(13) 0.17656(14) 0.55709(7) 0.0197(3) Uani 1 1 d . . . . .
C1 C 0.1878(2) -0.02246(18) 0.67628(11) 0.0213(4) Uani 1 1 d . . . . .
C2 C 0.0974(2) 0.0538(2) 0.72018(12) 0.0225(4) Uani 1 1 d . . . . .
C3 C 0.08843(18) 0.23284(19) 0.79714(10) 0.0182(3) Uani 1 1 d . . . . .
C4 C 0.17276(18) 0.3373(2) 0.83630(10) 0.0185(3) Uani 1 1 d . . . . .
C5 C 0.3031(2) 0.5297(2) 0.82238(11) 0.0247(4) Uani 1 1 d . . . . .
C6 C 0.3601(2) 0.6156(2) 0.76864(11) 0.0248(4) Uani 1 1 d . . . . .
C7 C 0.51534(19) 0.6108(2) 0.68361(11) 0.0213(4) Uani 1 1 d . . . . .
C8 C 0.59811(18) 0.5175(2) 0.64437(10) 0.0201(4) Uani 1 1 d . . . . .
C9 C 0.58253(18) 0.3614(2) 0.55285(11) 0.0207(4) Uani 1 1 d . . . . .
C10 C 0.48434(19) 0.2730(2) 0.51143(9) 0.0200(4) Uani 1 1 d . . . . .
C11 C 0.3401(2) 0.0888(2) 0.52175(10) 0.0216(4) Uani 1 1 d . . . . .
C12 C 0.2957(2) -0.0085(2) 0.57362(11) 0.0221(4) Uani 1 1 d . . . . .
H1 H 0.262(2) 0.138(2) 0.5004(13) 0.027(6) Uiso 1 1 d . . . . .
HW1A H 0.013(8) 0.598(9) 0.986(4) 0.050 Uiso 0.25 1 d D U P . .
HW1B H 0.108(9) 0.630(7) 0.942(5) 0.050 Uiso 0.25 1 d D U P . .
H2 H 0.383(3) 0.040(3) 0.4837(15) 0.034(7) Uiso 1 1 d . . . . .
H3 H 0.244(2) -0.080(3) 0.5521(12) 0.021(6) Uiso 1 1 d . . . . .
H4 H 0.375(2) -0.056(2) 0.5998(12) 0.017(5) Uiso 1 1 d . . . . .
H5 H 0.293(2) 0.654(2) 0.7337(13) 0.024(6) Uiso 1 1 d . . . . .
H6 H 0.415(2) 0.680(3) 0.7930(13) 0.031(7) Uiso 1 1 d . . . . .
H7 H 0.253(2) 0.582(3) 0.8545(13) 0.027(6) Uiso 1 1 d . . . . .
H8 H 0.373(3) 0.487(2) 0.8487(14) 0.023(6) Uiso 1 1 d . . . . .
H9 H 0.527(2) 0.226(3) 0.4730(13) 0.029(6) Uiso 1 1 d . . . . .
H10 H 0.410(2) 0.325(2) 0.4915(12) 0.016(5) Uiso 1 1 d . . . . .
H11 H 0.6542(19) 0.310(2) 0.5798(11) 0.015(5) Uiso 1 1 d . . . . .
H12 H 0.627(2) 0.425(3) 0.5257(13) 0.028(6) Uiso 1 1 d . . . . .
H13 H 0.643(2) 0.458(3) 0.6752(15) 0.031(7) Uiso 1 1 d . . . . .
H14 H 0.659(2) 0.567(2) 0.6168(12) 0.016(5) Uiso 1 1 d . . . . .
H15 H 0.571(2) 0.673(2) 0.7098(12) 0.021(6) Uiso 1 1 d . . . . .
H16 H 0.457(2) 0.655(3) 0.6530(14) 0.032(7) Uiso 1 1 d . . . . .
H17 H 0.248(2) 0.296(2) 0.8634(12) 0.018(5) Uiso 1 1 d . . . . .
H18 H 0.125(2) 0.386(2) 0.8694(12) 0.021(6) Uiso 1 1 d . . . . .
H19 H 0.049(2) 0.164(2) 0.8309(11) 0.018(5) Uiso 1 1 d . . . . .
H20 H 0.014(2) 0.277(2) 0.7692(12) 0.022(6) Uiso 1 1 d . . . . .
H21 H 0.020(2) 0.087(2) 0.6916(12) 0.016(5) Uiso 1 1 d . . . . .
H22 H 0.070(3) -0.010(2) 0.7590(15) 0.027(7) Uiso 1 1 d . . . . .
H23 H 0.271(2) -0.049(2) 0.7039(12) 0.017(5) Uiso 1 1 d . . . . .
H24 H 0.143(2) -0.104(2) 0.6594(12) 0.025(6) 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
Np1 O1 1.7662(13) . ?
Np1 O1 1.7662(13) 3_566 ?
Np1 Cl1 2.6513(5) . ?
Np1 Cl1 2.6513(5) 3_566 ?
Np1 Cl2 2.6614(6) . ?
Np1 Cl2 2.6614(6) 3_566 ?
Np1 K1 4.1452(6) . ?
Np1 K1 4.1452(6) 3_566 ?
K1 O6 2.8553(14) . ?
K1 O2 2.8626(15) . ?
K1 O4 2.8706(14) . ?
K1 O3 2.8881(14) . ?
K1 O5 2.9110(15) . ?
K1 O7 3.0387(14) . ?
K1 Cl2 3.2550(8) . ?
K1 Cl1 3.3179(8) . ?
OW1 HW1A 0.837(10) . ?
OW1 HW1B 0.835(10) . ?
O2 C1 1.424(2) . ?
O2 C12 1.426(2) . ?
O3 C2 1.424(2) . ?
O3 C3 1.426(2) . ?
O4 C5 1.423(2) . ?
O4 C4 1.425(2) . ?
O5 C7 1.425(2) . ?
O5 C6 1.426(2) . ?
O6 C8 1.420(2) . ?
O6 C9 1.423(2) . ?
O7 C11 1.423(2) . ?
O7 C10 1.425(2) . ?
C1 C2 1.504(3) . ?
C1 H23 0.98(2) . ?
C1 H24 0.97(2) . ?
C2 H21 0.97(2) . ?
C2 H22 1.04(3) . ?
C3 C4 1.504(3) . ?
C3 H19 1.05(2) . ?
C3 H20 0.99(2) . ?
C4 H17 0.97(2) . ?
C4 H18 0.97(2) . ?
C5 C6 1.500(3) . ?
C5 H7 0.98(2) . ?
C5 H8 0.93(3) . ?
C6 H5 0.99(2) . ?
C6 H6 0.95(3) . ?
C7 C8 1.499(3) . ?
C7 H15 0.95(2) . ?
C7 H16 0.91(3) . ?
C8 H13 0.93(3) . ?
C8 H14 0.98(2) . ?
C9 C10 1.499(3) . ?
C9 H11 0.99(2) . ?
C9 H12 0.96(3) . ?
C10 H9 1.01(3) . ?
C10 H10 0.96(2) . ?
C11 C12 1.493(3) . ?
C11 H1 0.99(2) . ?
C11 H2 1.01(3) . ?
C12 H3 0.95(2) . ?
C12 H4 1.02(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
O1 Np1 O1 180.0 . 3_566 ?
O1 Np1 Cl1 88.34(5) . . ?
O1 Np1 Cl1 91.66(5) 3_566 . ?
O1 Np1 Cl1 91.66(5) . 3_566 ?
O1 Np1 Cl1 88.34(5) 3_566 3_566 ?
Cl1 Np1 Cl1 180.0 . 3_566 ?
O1 Np1 Cl2 89.52(5) . . ?
O1 Np1 Cl2 90.48(5) 3_566 . ?
Cl1 Np1 Cl2 87.03(2) . . ?
Cl1 Np1 Cl2 92.97(2) 3_566 . ?
O1 Np1 Cl2 90.48(5) . 3_566 ?
O1 Np1 Cl2 89.52(5) 3_566 3_566 ?
Cl1 Np1 Cl2 92.97(2) . 3_566 ?
Cl1 Np1 Cl2 87.03(2) 3_566 3_566 ?
Cl2 Np1 Cl2 180.000(13) . 3_566 ?
O1 Np1 K1 55.84(5) . . ?
O1 Np1 K1 124.16(5) 3_566 . ?
Cl1 Np1 K1 53.079(16) . . ?
Cl1 Np1 K1 126.920(15) 3_566 . ?
Cl2 Np1 K1 51.713(14) . . ?
Cl2 Np1 K1 128.287(15) 3_566 . ?
O1 Np1 K1 124.16(5) . 3_566 ?
O1 Np1 K1 55.84(5) 3_566 3_566 ?
Cl1 Np1 K1 126.921(16) . 3_566 ?
Cl1 Np1 K1 53.079(16) 3_566 3_566 ?
Cl2 Np1 K1 128.287(14) . 3_566 ?
Cl2 Np1 K1 51.713(14) 3_566 3_566 ?
K1 Np1 K1 180.0 . 3_566 ?
O6 K1 O2 113.17(4) . . ?
O6 K1 O4 116.46(4) . . ?
O2 K1 O4 116.40(4) . . ?
O6 K1 O3 144.00(4) . . ?
O2 K1 O3 58.62(4) . . ?
O4 K1 O3 57.79(4) . . ?
O6 K1 O5 58.97(4) . . ?
O2 K1 O5 146.20(4) . . ?
O4 K1 O5 57.62(4) . . ?
O3 K1 O5 106.59(4) . . ?
O6 K1 O7 57.05(4) . . ?
O2 K1 O7 56.63(4) . . ?
O4 K1 O7 150.55(4) . . ?
O3 K1 O7 108.67(4) . . ?
O5 K1 O7 110.31(4) . . ?
O6 K1 Cl2 137.68(3) . . ?
O2 K1 Cl2 80.83(3) . . ?
O4 K1 Cl2 87.79(3) . . ?
O3 K1 Cl2 77.99(3) . . ?
O5 K1 Cl2 128.58(3) . . ?
O7 K1 Cl2 116.44(3) . . ?
O6 K1 Cl1 77.23(3) . . ?
O2 K1 Cl1 137.33(3) . . ?
O4 K1 Cl1 91.13(3) . . ?
O3 K1 Cl1 134.53(3) . . ?
O5 K1 Cl1 75.68(3) . . ?
O7 K1 Cl1 112.83(3) . . ?
Cl2 K1 Cl1 67.628(15) . . ?
O6 K1 Np1 97.76(3) . . ?
O2 K1 Np1 97.92(3) . . ?
O4 K1 Np1 111.73(3) . . ?
O3 K1 Np1 117.68(3) . . ?
O5 K1 Np1 115.38(3) . . ?
O7 K1 Np1 97.71(3) . . ?
Cl2 K1 Np1 39.925(11) . . ?
Cl1 K1 Np1 39.706(9) . . ?
Np1 Cl1 K1 87.215(18) . . ?
Np1 Cl2 K1 88.362(16) . . ?
HW1A OW1 HW1B 109(3) . . ?
C1 O2 C12 111.10(15) . . ?
C1 O2 K1 118.53(11) . . ?
C12 O2 K1 121.81(11) . . ?
C2 O3 C3 109.92(13) . . ?
C2 O3 K1 111.65(11) . . ?
C3 O3 K1 111.39(10) . . ?
C5 O4 C4 111.34(15) . . ?
C5 O4 K1 120.23(11) . . ?
C4 O4 K1 120.09(11) . . ?
C7 O5 C6 112.14(15) . . ?
C7 O5 K1 110.10(11) . . ?
C6 O5 K1 108.12(11) . . ?
C8 O6 C9 111.77(14) . . ?
C8 O6 K1 117.54(11) . . ?
C9 O6 K1 121.86(11) . . ?
C11 O7 C10 111.89(14) . . ?
C11 O7 K1 104.39(10) . . ?
C10 O7 K1 104.24(10) . . ?
O2 C1 C2 108.46(15) . . ?
O2 C1 H23 108.2(13) . . ?
C2 C1 H23 110.6(14) . . ?
O2 C1 H24 113.0(14) . . ?
C2 C1 H24 109.2(13) . . ?
H23 C1 H24 107.5(19) . . ?
O3 C2 C1 108.95(15) . . ?
O3 C2 H21 110.3(14) . . ?
C1 C2 H21 110.0(13) . . ?
O3 C2 H22 107.9(14) . . ?
C1 C2 H22 108.2(14) . . ?
H21 C2 H22 111.4(19) . . ?
O3 C3 C4 108.46(14) . . ?
O3 C3 H19 108.8(12) . . ?
C4 C3 H19 111.4(12) . . ?
O3 C3 H20 109.7(14) . . ?
C4 C3 H20 109.3(14) . . ?
H19 C3 H20 109.2(16) . . ?
O4 C4 C3 108.98(15) . . ?
O4 C4 H17 109.6(13) . . ?
C3 C4 H17 110.5(13) . . ?
O4 C4 H18 109.1(14) . . ?
C3 C4 H18 113.2(13) . . ?
H17 C4 H18 105.3(19) . . ?
O4 C5 C6 108.64(16) . . ?
O4 C5 H7 111.1(14) . . ?
C6 C5 H7 112.6(15) . . ?
O4 C5 H8 107.9(14) . . ?
C6 C5 H8 109.0(15) . . ?
H7 C5 H8 107(2) . . ?
O5 C6 C5 108.37(17) . . ?
O5 C6 H5 104.6(14) . . ?
C5 C6 H5 114.9(13) . . ?
O5 C6 H6 108.1(15) . . ?
C5 C6 H6 106.7(16) . . ?
H5 C6 H6 114(2) . . ?
O5 C7 C8 108.62(16) . . ?
O5 C7 H15 109.2(14) . . ?
C8 C7 H15 110.6(13) . . ?
O5 C7 H16 109.4(15) . . ?
C8 C7 H16 109.2(16) . . ?
H15 C7 H16 110(2) . . ?
O6 C8 C7 108.69(15) . . ?
O6 C8 H13 105.8(17) . . ?
C7 C8 H13 109.4(17) . . ?
O6 C8 H14 109.1(13) . . ?
C7 C8 H14 111.1(14) . . ?
H13 C8 H14 113(2) . . ?
O6 C9 C10 108.05(14) . . ?
O6 C9 H11 109.1(12) . . ?
C10 C9 H11 112.6(12) . . ?
O6 C9 H12 106.4(16) . . ?
C10 C9 H12 114.4(15) . . ?
H11 C9 H12 106.0(18) . . ?
O7 C10 C9 108.31(15) . . ?
O7 C10 H9 109.5(15) . . ?
C9 C10 H9 111.7(14) . . ?
O7 C10 H10 108.3(13) . . ?
C9 C10 H10 110.1(13) . . ?
H9 C10 H10 108.8(19) . . ?
O7 C11 C12 107.74(16) . . ?
O7 C11 H1 111.4(14) . . ?
C12 C11 H1 109.5(14) . . ?
O7 C11 H2 109.5(15) . . ?
C12 C11 H2 110.3(15) . . ?
H1 C11 H2 108(2) . . ?
O2 C12 C11 108.36(16) . . ?
O2 C12 H3 111.7(13) . . ?
C11 C12 H3 112.1(14) . . ?
O2 C12 H4 109.3(13) . . ?
C11 C12 H4 112.0(13) . . ?
H3 C12 H4 103.3(19) . . ?

_refine_diff_density_max         0.665
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.076

