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#$Date: 2024-07-05 16:25:23 +0300 (Fri, 05 Jul 2024) $
#$Revision: 292803 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/30/7133001.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.
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data_7133001
loop_
_publ_author_name
'Lopez, Lauren M.'
'Uible, Madeleine C.'
'Zeller, Matthias'
'Bart, Suzanne C.'
_publ_section_title
;
 Lewis base adducts of NpCl₄.
;
_journal_issue                   46
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5956
_journal_page_last               5959
_journal_paper_doi               10.1039/d4cc01560f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C8 H12 Cl4 N4 Np'
_chemical_formula_sum            'C8 H12 Cl4 N4 Np'
_chemical_formula_weight         543.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   none
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-02-26 deposited with the CCDC.	2024-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.6870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6308(5)
_cell_length_b                   8.4327(3)
_cell_length_c                   13.7095(5)
_cell_measurement_reflns_used    9757
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.1300
_cell_measurement_theta_min      2.7857
_cell_volume                     1690.71(10)
_computing_cell_refinement       ' SAINT V8.40B (Bruker, 2020)'
_computing_data_collection       ' Apex4 v2022.10-1 (Bruker, 2022) '
_computing_data_reduction        ' SAINT V8.40B (Bruker, 2020)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015b)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type
'PhotonII charge-integrating pixel array (CPAD)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS D8 Quest'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10988
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.153
_diffrn_reflns_theta_min         2.786
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    6.764
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.3794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.133
_exptl_crystal_description       plate
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.566
_exptl_crystal_size_mid          0.446
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.00323(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         3213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.0161
_refine_ls_R_factor_gt           0.0157
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+1.9835P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0375
_refine_ls_wR_factor_ref         0.0376
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3174
_reflns_number_total             3213
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc01560f2.cif
_cod_data_source_block           MCU_Np_1025_0m_a
_cod_depositor_comments
'Adding full bibliography for 7133000--7133003.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7133001
_shelx_shelxl_version_number     2019/3
_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.
;
_shelx_estimated_absorpt_t_min   0.114
_shelx_estimated_absorpt_t_max   0.430
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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Np1 Np 0.500000 0.32138(2) 0.250000 0.01820(4) Uani 1 2 d S T P . .
Cl1 Cl 0.65172(3) 0.41011(6) 0.33983(4) 0.03088(9) Uani 1 1 d . . . . .
Cl2 Cl 0.57753(3) 0.23198(6) 0.09030(3) 0.02938(9) Uani 1 1 d . . . . .
N1 N 0.45230(13) 0.5731(2) 0.33858(12) 0.0307(3) Uani 1 1 d . . . . .
N2 N 0.41321(12) 0.06796(19) 0.19915(12) 0.0293(3) Uani 1 1 d . . . . .
C1 C 0.42313(14) 0.6780(2) 0.37946(14) 0.0256(3) Uani 1 1 d . . . . .
C2 C 0.38414(17) 0.8113(2) 0.43038(15) 0.0326(4) Uani 1 1 d . . . . .
H2A H 0.421311 0.906043 0.419823 0.049 Uiso 1 1 calc R U . . .
H2B H 0.383104 0.787869 0.500363 0.049 Uiso 1 1 calc R U . . .
H2C H 0.321617 0.829976 0.405408 0.049 Uiso 1 1 calc R U . . .
C3 C 0.36894(13) -0.0351(2) 0.17244(13) 0.0262(3) Uani 1 1 d . . . . .
C4 C 0.31199(17) -0.1654(3) 0.13830(19) 0.0403(5) Uani 1 1 d . . . . .
H4A H 0.289163 -0.143210 0.071773 0.060 Uiso 1 1 calc R U . . .
H4B H 0.260216 -0.177719 0.181417 0.060 Uiso 1 1 calc R U . . .
H4C H 0.348045 -0.263314 0.138610 0.060 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Np1 N1 67.51(8) 2_655 . ?
N1 Np1 N2 132.86(6) 2_655 2_655 ?
N1 Np1 N2 134.56(5) . 2_655 ?
N1 Np1 N2 134.56(5) 2_655 . ?
N1 Np1 N2 132.86(6) . . ?
N2 Np1 N2 67.60(8) 2_655 . ?
N1 Np1 Cl2 73.09(4) 2_655 . ?
N1 Np1 Cl2 140.52(4) . . ?
N2 Np1 Cl2 76.33(4) 2_655 . ?
N2 Np1 Cl2 75.85(4) . . ?
N1 Np1 Cl2 140.52(4) 2_655 2_655 ?
N1 Np1 Cl2 73.09(4) . 2_655 ?
N2 Np1 Cl2 75.85(4) 2_655 2_655 ?
N2 Np1 Cl2 76.33(4) . 2_655 ?
Cl2 Np1 Cl2 146.38(2) . 2_655 ?
N1 Np1 Cl1 77.19(4) 2_655 2_655 ?
N1 Np1 Cl1 75.29(4) . 2_655 ?
N2 Np1 Cl1 140.42(4) 2_655 2_655 ?
N2 Np1 Cl1 72.82(4) . 2_655 ?
Cl2 Np1 Cl1 94.100(16) . 2_655 ?
Cl2 Np1 Cl1 95.392(16) 2_655 2_655 ?
N1 Np1 Cl1 75.29(4) 2_655 . ?
N1 Np1 Cl1 77.19(4) . . ?
N2 Np1 Cl1 72.82(4) 2_655 . ?
N2 Np1 Cl1 140.42(4) . . ?
Cl2 Np1 Cl1 95.392(16) . . ?
Cl2 Np1 Cl1 94.098(16) 2_655 . ?
Cl1 Np1 Cl1 146.76(2) 2_655 . ?
C1 N1 Np1 173.30(17) . . ?
C3 N2 Np1 173.58(16) . . ?
N1 C1 C2 178.8(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 C4 179.5(2) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Np1 N1 2.5526(17) 2_655 ?
Np1 N1 2.5526(17) . ?
Np1 N2 2.5716(16) 2_655 ?
Np1 N2 2.5716(16) . ?
Np1 Cl2 2.6067(4) . ?
Np1 Cl2 2.6067(4) 2_655 ?
Np1 Cl1 2.6159(4) 2_655 ?
Np1 Cl1 2.6159(4) . ?
N1 C1 1.137(2) . ?
N2 C3 1.138(2) . ?
C1 C2 1.449(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.448(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
