#------------------------------------------------------------------------------
#$Date: 2019-11-17 06:14:16 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228356 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/16/7121610.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_7121610
loop_
_publ_author_name
'Pattenaude, Scott A.'
'Anderson, Nickolas H.'
'Bart, Suzanne C.'
'Gaunt, Andrew J.'
'Scott, Brian L.'
_publ_section_title
;
 Non-aqueous neptunium and plutonium redox behaviour in THF - access to a
 rare Np(iii) synthetic precursor.
;
_journal_issue                   48
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6113
_journal_page_last               6116
_journal_paper_doi               10.1039/c8cc02611d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C28 H40 Cl3 N4 Np O2'
_chemical_formula_weight         807.99
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-03-17 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.7108(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5752(8)
_cell_length_b                   15.7756(10)
_cell_length_c                   15.1347(14)
_cell_measurement_reflns_used    8129
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.25
_cell_volume                     2843.8(4)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_publication_material  'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16224
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.590
_diffrn_reflns_theta_min         2.142
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.970
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_correction_T_min  0.304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_description       needle
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.381
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         3452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0222
_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)+(0.0249P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0446
_refine_ls_wR_factor_ref         0.0462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3024
_reflns_number_total             3452
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc02611d2.cif
_cod_data_source_block           apx2588a_sq
_cod_depositor_comments
'Adding full bibliography for 7121609--7121611.cif.'
_cod_database_code               7121610
_shelx_shelxl_version_number     2014/7
_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   0.300
_shelx_estimated_absorpt_t_max   0.647
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
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 .
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'
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
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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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) .
