#------------------------------------------------------------------------------
#$Date: 2020-06-05 13:47:47 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252785 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/40/7704082.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7704082
loop_
_publ_author_name
'Pyrch, Mikaela M.'
'Bjorklund, Jennifer L.'
'Williams, James M.'
'Parr Iv, Daniel L.'
'Mason, Sara E.'
'Leddy, Johna'
'Forbes, Tori Z.'
_publ_section_title
;
 Impacts of hydrogen bonding interactions with
 Np(v/vi)O₂Cl₄ complexes: vibrational spectroscopy,
 redox behavior, and computational analysis.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6854
_journal_page_last               6866
_journal_paper_doi               10.1039/d0dt00848f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C16 H40 Cl6 N4 Np O6'
_chemical_formula_weight         834.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-12-17 deposited with the CCDC.	2020-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                92.223(4)
_cell_angle_beta                 113.075(3)
_cell_angle_gamma                113.397(4)
_cell_formula_units_Z            1
_cell_length_a                   9.1938(8)
_cell_length_b                   9.3020(10)
_cell_length_c                   10.8819(11)
_cell_measurement_reflns_used    9652
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.57
_cell_volume                     764.66(14)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18181
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.379
_diffrn_reflns_theta_min         2.574
_exptl_absorpt_coefficient_mu    3.956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_description       block
_exptl_crystal_F_000             407
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.745200
_exptl_transmission_factor_min   0.646300
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0166P)²+0.1282P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0377
_refine_ls_wR_factor_ref         0.0380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2752
_reflns_number_total             2786
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt00848f2.cif
_cod_data_source_block           pbarone_final_a
_cod_depositor_comments
'Adding full bibliography for 7704082--7704083.cif.'
_cod_original_cell_volume        764.66(13)
_cod_database_code               7704082
_shelx_shelxl_version_number     2017/1
_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'
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 0.000000 0.500000 0.500000 0.03285(6) Uani 1 2 d S . P . .
Cl1 Cl 0.17685(11) 0.77541(10) 0.69340(9) 0.0617(2) Uani 1 1 d . . . . .
Cl2 Cl 0.22319(11) 0.38952(10) 0.64691(8) 0.0591(2) Uani 1 1 d . . . . .
Cl3 Cl 0.76103(9) 0.98106(9) -0.01745(7) 0.04855(18) Uani 1 1 d . . . . .
O1 O 0.1305(3) 0.5839(2) 0.4155(2) 0.0524(5) Uani 1 1 d . . . . .
O2 O 0.2304(3) 0.5162(3) 0.1062(2) 0.0689(7) Uani 1 1 d . . . . .
O3 O 0.5919(3) 0.8515(3) 0.5113(2) 0.0671(6) Uani 1 1 d . . . . .
N1 N 0.4457(3) 0.7977(3) 0.0539(3) 0.0508(6) Uani 1 1 d . . . . .
H1 H 0.368303 0.833724 0.007996 0.070(11) Uiso 1 1 calc R . . . .
H2 H 0.551087 0.865474 0.061260 0.058(9) Uiso 1 1 calc R . . . .
N2 N 0.8730(3) 0.8763(3) 0.7553(3) 0.0558(7) Uani 1 1 d . . . . .
H3 H 0.970374 0.862965 0.795142 0.096(14) Uiso 1 1 calc R . . . .
H4 H 0.855204 0.915519 0.821109 0.109(16) Uiso 1 1 calc R . . . .
C1 C 0.3914(5) 0.6364(4) -0.0223(4) 0.0668(9) Uani 1 1 d . . . . .
H1A H 0.481316 0.601139 0.022724 0.080 Uiso 1 1 calc R U . . .
H1AB H 0.378681 0.640305 -0.114765 0.080 Uiso 1 1 calc R U . . .
C2 C 0.2192(5) 0.5202(5) -0.0277(4) 0.0735(10) Uani 1 1 d . . . . .
H2A H 0.127745 0.551145 -0.079483 0.088 Uiso 1 1 calc R U . . .
H2AB H 0.186097 0.413380 -0.074927 0.088 Uiso 1 1 calc R U . . .
C3 C 0.2777(5) 0.6705(4) 0.1776(4) 0.0647(9) Uani 1 1 d . . . . .
H3A H 0.281938 0.664672 0.267675 0.078 Uiso 1 1 calc R U . . .
H3AB H 0.188480 0.704791 0.127958 0.078 Uiso 1 1 calc R U . . .
C4 C 0.4553(5) 0.7922(4) 0.1932(3) 0.0583(8) Uani 1 1 d . . . . .
H4A H 0.484434 0.897405 0.240731 0.070 Uiso 1 1 calc R U . . .
H4AB H 0.546370 0.761527 0.246530 0.070 Uiso 1 1 calc R U . . .
C5 C 0.5638(4) 0.7442(4) 0.5972(4) 0.0658(9) Uani 1 1 d . . . . .
H5A H 0.465064 0.641186 0.541662 0.079 Uiso 1 1 calc R U . . .
H5AB H 0.532858 0.786121 0.661241 0.079 Uiso 1 1 calc R U . . .
C6 C 0.7214(5) 0.7201(4) 0.6747(3) 0.0577(8) Uani 1 1 d . . . . .
H6A H 0.699114 0.649704 0.735384 0.069 Uiso 1 1 calc R U . . .
H6AB H 0.747405 0.669686 0.611549 0.069 Uiso 1 1 calc R U . . .
C7 C 0.8983(5) 0.9923(4) 0.6668(4) 0.0717(10) Uani 1 1 d . . . . .
H7A H 0.990393 1.097720 0.723146 0.086 Uiso 1 1 calc R U . . .
H7AB H 0.934812 0.957766 0.603506 0.086 Uiso 1 1 calc R U . . .
C8 C 0.7313(5) 1.0020(4) 0.5893(4) 0.0720(10) Uani 1 1 d . . . . .
H8A H 0.701377 1.046059 0.652981 0.086 Uiso 1 1 calc R U . . .
H8AB H 0.747489 1.074590 0.528901 0.086 Uiso 1 1 calc R U . . .
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'
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 2_566 . ?
O1 Np1 Cl2 90.65(7) 2_566 2_566 ?
O1 Np1 Cl2 89.35(7) . 2_566 ?
O1 Np1 Cl2 89.35(7) 2_566 . ?
O1 Np1 Cl2 90.65(7) . . ?
Cl2 Np1 Cl2 180.00(3) 2_566 . ?
O1 Np1 Cl1 91.05(7) 2_566 2_566 ?
O1 Np1 Cl1 88.95(7) . 2_566 ?
Cl2 Np1 Cl1 91.14(3) 2_566 2_566 ?
Cl2 Np1 Cl1 88.86(3) . 2_566 ?
O1 Np1 Cl1 88.95(7) 2_566 . ?
O1 Np1 Cl1 91.05(7) . . ?
Cl2 Np1 Cl1 88.86(3) 2_566 . ?
Cl2 Np1 Cl1 91.14(3) . . ?
Cl1 Np1 Cl1 180.00(3) 2_566 . ?
C3 O2 C2 110.7(2) . . ?
C8 O3 C5 110.3(3) . . ?
C1 N1 C4 110.5(2) . . ?
C1 N1 H1 109.5 . . ?
C4 N1 H1 109.5 . . ?
C1 N1 H2 109.5 . . ?
C4 N1 H2 109.5 . . ?
H1 N1 H2 108.1 . . ?
C6 N2 C7 110.9(2) . . ?
C6 N2 H3 109.5 . . ?
C7 N2 H3 109.5 . . ?
C6 N2 H4 109.5 . . ?
C7 N2 H4 109.5 . . ?
H3 N2 H4 108.0 . . ?
N1 C1 C2 109.6(3) . . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N1 C1 H1AB 109.8 . . ?
C2 C1 H1AB 109.8 . . ?
H1A C1 H1AB 108.2 . . ?
O2 C2 C1 111.5(3) . . ?
O2 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
O2 C2 H2AB 109.3 . . ?
C1 C2 H2AB 109.3 . . ?
H2A C2 H2AB 108.0 . . ?
O2 C3 C4 111.2(3) . . ?
O2 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
O2 C3 H3AB 109.4 . . ?
C4 C3 H3AB 109.4 . . ?
H3A C3 H3AB 108.0 . . ?
N1 C4 C3 108.3(3) . . ?
N1 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
N1 C4 H4AB 110.0 . . ?
C3 C4 H4AB 110.0 . . ?
H4A C4 H4AB 108.4 . . ?
O3 C5 C6 112.1(3) . . ?
O3 C5 H5A 109.2 . . ?
C6 C5 H5A 109.2 . . ?
O3 C5 H5AB 109.2 . . ?
C6 C5 H5AB 109.2 . . ?
H5A C5 H5AB 107.9 . . ?
N2 C6 C5 109.5(3) . . ?
N2 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N2 C6 H6AB 109.8 . . ?
C5 C6 H6AB 109.8 . . ?
H6A C6 H6AB 108.2 . . ?
C8 C7 N2 109.7(3) . . ?
C8 C7 H7A 109.7 . . ?
N2 C7 H7A 109.7 . . ?
C8 C7 H7AB 109.7 . . ?
N2 C7 H7AB 109.7 . . ?
H7A C7 H7AB 108.2 . . ?
O3 C8 C7 112.0(3) . . ?
O3 C8 H8A 109.2 . . ?
C7 C8 H8A 109.2 . . ?
O3 C8 H8AB 109.2 . . ?
C7 C8 H8AB 109.2 . . ?
H8A C8 H8AB 107.9 . . ?
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 1.7526(18) 2_566 ?
Np1 O1 1.7526(18) . ?
Np1 Cl2 2.6558(8) 2_566 ?
Np1 Cl2 2.6558(8) . ?
Np1 Cl1 2.6884(8) 2_566 ?
Np1 Cl1 2.6884(8) . ?
O2 C3 1.417(4) . ?
O2 C2 1.423(4) . ?
O3 C8 1.398(4) . ?
O3 C5 1.412(4) . ?
N1 C1 1.474(4) . ?
N1 C4 1.489(4) . ?
N1 H1 0.8900 . ?
N1 H2 0.8900 . ?
N2 C6 1.469(4) . ?
N2 C7 1.485(4) . ?
N2 H3 0.8900 . ?
N2 H4 0.8900 . ?
C1 C2 1.498(5) . ?
C1 H1A 0.9700 . ?
C1 H1AB 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2AB 0.9700 . ?
C3 C4 1.508(5) . ?
C3 H3A 0.9700 . ?
C3 H3AB 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4AB 0.9700 . ?
C5 C6 1.475(5) . ?
C5 H5A 0.9700 . ?
C5 H5AB 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6AB 0.9700 . ?
C7 C8 1.475(5) . ?
C7 H7A 0.9700 . ?
C7 H7AB 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8AB 0.9700 . ?
