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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/7/13/30/7133000.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_7133000
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_sum            'C20 H20 Cl4 N4 Np'
_chemical_formula_weight         695.20
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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                 127.5220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2449(8)
_cell_length_b                   9.5303(4)
_cell_length_c                   15.6081(11)
_cell_measurement_reflns_used    61182
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.1838
_cell_measurement_theta_min      2.5196
_cell_volume                     2270.4(2)
_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 2014/4 (Sheldrick, 2014)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35651
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.192
_diffrn_reflns_theta_min         2.669
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    5.062
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D. (2015). J. Appl. Cryst. 48, 3-10.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_description       block
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.243
_refine_diff_density_max         1.537
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.00027(6)
_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   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         4351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0170
_refine_ls_R_factor_gt           0.0162
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0165P)²+3.0428P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0399
_refine_ls_wR_factor_ref         0.0403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4231
_reflns_number_total             4351
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc01560f2.cif
_cod_data_source_block           MCU_LML_Np_1027_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__computing_data_collection' was replaced with
'_computing_data_collection'.

Automatic conversion script
Id: cif_correct_tags 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133000--7133003.cif.
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7133000
_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   0.314
_shelx_estimated_absorpt_t_max   0.373
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 0.64151(2) 0.250000 0.01418(3) Uani 1 2 d S T P . .
Cl1 Cl 0.64173(2) 0.72708(4) 0.27650(3) 0.02232(7) Uani 1 1 d . . . . .
Cl2 Cl 0.41527(3) 0.55581(4) 0.05018(3) 0.02462(8) Uani 1 1 d . . . . .
N1 N 0.55375(9) 0.87143(14) 0.37510(11) 0.0187(2) Uani 1 1 d . . . . .
N2 N 0.41344(9) 0.41349(15) 0.24030(11) 0.0189(2) Uani 1 1 d . . . . .
C1 C 0.49975(10) 0.97673(17) 0.35676(13) 0.0205(3) Uani 1 1 d . . . . .
H1 H 0.441263 0.974928 0.292050 0.025 Uiso 1 1 calc R U . . .
C2 C 0.52508(11) 1.08782(18) 0.42746(15) 0.0235(3) Uani 1 1 d . . . . .
H2 H 0.484700 1.160228 0.410928 0.028 Uiso 1 1 calc R U . . .
C3 C 0.61013(12) 1.09205(19) 0.52271(14) 0.0248(3) Uani 1 1 d . . . . .
H3 H 0.628682 1.165604 0.573503 0.030 Uiso 1 1 calc R U . . .
C4 C 0.66730(11) 0.98587(19) 0.54168(13) 0.0240(3) Uani 1 1 d . . . . .
H4 H 0.726391 0.986499 0.605177 0.029 Uiso 1 1 calc R U . . .
C5 C 0.63687(11) 0.87889(17) 0.46656(14) 0.0214(3) Uani 1 1 d . . . . .
H5 H 0.676654 0.806992 0.480191 0.026 Uiso 1 1 calc R U . . .
C6 C 0.38717(10) 0.40907(18) 0.30306(13) 0.0196(3) Uani 1 1 d . . . . .
H6 H 0.408571 0.478743 0.357301 0.024 Uiso 1 1 calc R U . . .
C7 C 0.33052(11) 0.30804(19) 0.29244(14) 0.0224(3) Uani 1 1 d . . . . .
H7 H 0.313017 0.309971 0.337685 0.027 Uiso 1 1 calc R U . . .
C8 C 0.29978(11) 0.20417(19) 0.21492(15) 0.0245(3) Uani 1 1 d . . . . .
H8 H 0.260400 0.134265 0.205338 0.029 Uiso 1 1 calc R U . . .
C9 C 0.32800(12) 0.20509(18) 0.15191(15) 0.0250(3) Uani 1 1 d . . . . .
H9 H 0.309181 0.134290 0.099092 0.030 Uiso 1 1 calc R U . . .
C10 C 0.38411(11) 0.31059(18) 0.16668(14) 0.0218(3) Uani 1 1 d . . . . .
H10 H 0.402744 0.310116 0.122595 0.026 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
Cl2 Np1 Cl2 143.656(19) . 2_655 ?
Cl2 Np1 Cl1 94.338(13) . 2_655 ?
Cl2 Np1 Cl1 96.775(14) 2_655 2_655 ?
Cl2 Np1 Cl1 96.776(14) . . ?
Cl2 Np1 Cl1 94.340(13) 2_655 . ?
Cl1 Np1 Cl1 143.829(18) 2_655 . ?
Cl2 Np1 N2 74.32(3) . 2_655 ?
Cl2 Np1 N2 76.44(3) 2_655 2_655 ?
Cl1 Np1 N2 143.99(3) 2_655 2_655 ?
Cl1 Np1 N2 72.15(3) . 2_655 ?
Cl2 Np1 N2 76.44(3) . . ?
Cl2 Np1 N2 74.32(3) 2_655 . ?
Cl1 Np1 N2 72.15(3) 2_655 . ?
Cl1 Np1 N2 143.99(3) . . ?
N2 Np1 N2 71.97(6) 2_655 . ?
Cl2 Np1 N1 143.56(3) . . ?
Cl2 Np1 N1 72.79(3) 2_655 . ?
Cl1 Np1 N1 76.39(3) 2_655 . ?
Cl1 Np1 N1 74.29(3) . . ?
N2 Np1 N1 131.89(4) 2_655 . ?
N2 Np1 N1 130.67(4) . . ?
Cl2 Np1 N1 72.79(3) . 2_655 ?
Cl2 Np1 N1 143.56(3) 2_655 2_655 ?
Cl1 Np1 N1 74.29(3) 2_655 2_655 ?
Cl1 Np1 N1 76.39(3) . 2_655 ?
N2 Np1 N1 130.67(4) 2_655 2_655 ?
N2 Np1 N1 131.89(4) . 2_655 ?
N1 Np1 N1 70.77(6) . 2_655 ?
C1 N1 C5 116.79(14) . . ?
C1 N1 Np1 123.26(10) . . ?
C5 N1 Np1 119.69(10) . . ?
C10 N2 C6 116.71(14) . . ?
C10 N2 Np1 124.13(11) . . ?
C6 N2 Np1 118.56(10) . . ?
N1 C1 C2 123.32(15) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 119.24(16) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C4 C3 C2 118.15(16) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C5 C4 C3 118.97(15) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
N1 C5 C4 123.48(15) . . ?
N1 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
N2 C6 C7 123.35(15) . . ?
N2 C6 H6 118.3 . . ?
C7 C6 H6 118.3 . . ?
C8 C7 C6 119.13(16) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C7 118.19(16) . . ?
C9 C8 H8 120.9 . . ?
C7 C8 H8 120.9 . . ?
C8 C9 C10 119.29(16) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N2 C10 C9 123.29(16) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
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 Cl2 2.6188(4) . ?
Np1 Cl2 2.6188(4) 2_655 ?
Np1 Cl1 2.6269(4) 2_655 ?
Np1 Cl1 2.6270(4) . ?
Np1 N2 2.6857(14) 2_655 ?
Np1 N2 2.6857(14) . ?
Np1 N1 2.6877(14) . ?
Np1 N1 2.6877(14) 2_655 ?
N1 C1 1.344(2) . ?
N1 C5 1.349(2) . ?
N2 C10 1.346(2) . ?
N2 C6 1.349(2) . ?
C1 C2 1.386(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.388(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(2) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.387(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.386(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.388(2) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 -1.4(3) . . . . ?
Np1 N1 C1 C2 172.67(13) . . . . ?
N1 C1 C2 C3 -0.3(3) . . . . ?
C1 C2 C3 C4 1.8(3) . . . . ?
C2 C3 C4 C5 -1.5(3) . . . . ?
C1 N1 C5 C4 1.8(3) . . . . ?
Np1 N1 C5 C4 -172.57(14) . . . . ?
C3 C4 C5 N1 -0.3(3) . . . . ?
C10 N2 C6 C7 -2.1(2) . . . . ?
Np1 N2 C6 C7 169.42(13) . . . . ?
N2 C6 C7 C8 1.1(3) . . . . ?
C6 C7 C8 C9 0.7(3) . . . . ?
C7 C8 C9 C10 -1.3(3) . . . . ?
C6 N2 C10 C9 1.4(2) . . . . ?
Np1 N2 C10 C9 -169.58(13) . . . . ?
C8 C9 C10 N2 0.3(3) . . . . ?
