#------------------------------------------------------------------------------
#$Date: 2019-11-17 06:14:16 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228356 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/16/7121609.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_7121609
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            'C12 H24 Cl3.5 O3 Pu'
_chemical_formula_weight         579.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-03-27 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.374(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.264(3)
_cell_length_b                   11.172(3)
_cell_length_c                   13.938(4)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.50
_cell_volume                     1849.9(9)
_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 0.989
_diffrn_measured_fraction_theta_max 0.935
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20230
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.615
_diffrn_reflns_theta_min         1.714
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.070
_exptl_absorpt_correction_T_max  0.253
_exptl_absorpt_correction_T_min  0.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_description       block
_exptl_crystal_F_000             1094
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.270
_refine_diff_density_max         1.571
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.742
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.742
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0315
_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)+(0.0073P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4006
_reflns_number_total             4435
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc02611d2.cif
_cod_data_source_block           apx2586
_cod_depositor_comments
'Adding full bibliography for 7121609--7121611.cif.'
_cod_original_cell_volume        1850.0(8)
_cod_original_formula_sum        'C12 H24 Cl3.50 O3 Pu'
_cod_database_code               7121609
_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   0.338
_shelx_estimated_absorpt_t_max   0.406
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
Pu1 Pu 1.0000 0.68096(2) 0.2500 0.02327(7) Uani 1 2 d S T P
Pu2 Pu 0.5000 0.20570(2) 0.2500 0.02423(7) Uani 1 2 d S T P
Cl1 Cl 0.5000 0.43260(14) 0.2500 0.0401(4) Uani 1 2 d S T P
Cl2 Cl 0.50161(13) 0.19223(10) 0.06673(9) 0.0417(3) Uani 1 1 d . . .
Cl3 Cl 0.28357(11) 0.19141(11) 0.19900(10) 0.0450(3) Uani 1 1 d . . .
Cl4 Cl 1.11368(12) 0.68818(11) 0.10958(9) 0.0424(3) Uani 1 1 d . . .
O1 O 1.0000 0.4607(3) 0.2500 0.0320(10) Uani 1 2 d S T P
O2 O 0.8222(3) 0.6120(3) 0.1373(2) 0.0387(8) Uani 1 1 d . . .
O3 O 0.9012(3) 0.8587(3) 0.1631(3) 0.0438(8) Uani 1 1 d . . .
O4 O 0.5000 -0.0104(3) 0.2500 0.0303(10) Uani 1 2 d S T P
C1 C 1.0090(5) 0.3849(5) 0.1678(4) 0.0521(15) Uani 1 1 d . . .
H1A H 1.0847 0.3872 0.1584 0.063 Uiso 1 1 calc R U .
H1B H 0.9566 0.4105 0.1070 0.063 Uiso 1 1 calc R U .
C2 C 0.9813(7) 0.2651(6) 0.1954(6) 0.100(3) Uani 1 1 d . . .
H2A H 1.0211 0.2048 0.1673 0.120 Uiso 1 1 calc R U .
H2B H 0.9011 0.2503 0.1733 0.120 Uiso 1 1 calc R U .
C3 C 0.7347(4) 0.5385(5) 0.1628(4) 0.0439(12) Uani 1 1 d . . .
H3A H 0.7017 0.5799 0.2099 0.053 Uiso 1 1 calc R U .
H3B H 0.7659 0.4631 0.1916 0.053 Uiso 1 1 calc R U .
C4 C 0.6498(5) 0.5178(6) 0.0697(4) 0.0708(19) Uani 1 1 d . . .
H4A H 0.5897 0.5763 0.0611 0.085 Uiso 1 1 calc R U .
H4B H 0.6178 0.4383 0.0685 0.085 Uiso 1 1 calc R U .
C5 C 0.7110(5) 0.5306(5) -0.0088(4) 0.0536(15) Uani 1 1 d . . .
H5A H 0.6606 0.5556 -0.0707 0.064 Uiso 1 1 calc R U .
H5B H 0.7466 0.4558 -0.0192 0.064 Uiso 1 1 calc R U .
C6 C 0.7964(5) 0.6243(6) 0.0303(4) 0.0605(17) Uani 1 1 d . . .
H6A H 0.8634 0.6120 0.0064 0.073 Uiso 1 1 calc R U .
H6B H 0.7665 0.7033 0.0102 0.073 Uiso 1 1 calc R U .
C7 C 0.7933(6) 0.9012(7) 0.1732(5) 0.086(2) Uani 1 1 d . . .
H7A H 0.7407 0.8351 0.1670 0.103 Uiso 1 1 calc R U .
H7B H 0.8012 0.9382 0.2375 0.103 Uiso 1 1 calc R U .
C8 C 0.7528(6) 0.9874(6) 0.0956(5) 0.0703(18) Uani 1 1 d . . .
H8A H 0.7415 1.0642 0.1240 0.084 Uiso 1 1 calc R U .
H8B H 0.6815 0.9612 0.0535 0.084 Uiso 1 1 calc R U .
C9 C 0.8355(6) 0.9987(5) 0.0378(4) 0.0623(17) Uani 1 1 d . . .
H9A H 0.8083 0.9617 -0.0267 0.075 Uiso 1 1 calc R U .
H9B H 0.8515 1.0823 0.0285 0.075 Uiso 1 1 calc R U .
C10 C 0.9359(5) 0.9377(5) 0.0942(6) 0.078(2) Uani 1 1 d . . .
H10A H 0.9703 0.8922 0.0502 0.093 Uiso 1 1 calc R U .
H10B H 0.9903 0.9954 0.1296 0.093 Uiso 1 1 calc R U .
C11 C 0.4361(4) -0.0854(4) 0.1695(3) 0.0416(12) Uani 1 1 d . . .
H11A H 0.4501 -0.0617 0.1067 0.050 Uiso 1 1 calc R U .
H11B H 0.3560 -0.0793 0.1647 0.050 Uiso 1 1 calc R U .
C12 C 0.4769(6) -0.2100(4) 0.1961(4) 0.0555(17) Uani 1 1 d . . .
H12A H 0.4154 -0.2667 0.1774 0.067 Uiso 1 1 calc R U .
H12B H 0.5347 -0.2314 0.1626 0.067 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'
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'
Pu Pu -9.4100 4.3056 '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
O1 Pu1 O2 71.85(8) . .
O1 Pu1 O2 71.85(8) . 2_755
O2 Pu1 O2 143.71(15) . 2_755
O1 Pu1 O3 143.20(8) . 2_755
O2 Pu1 O3 143.77(11) . 2_755
O2 Pu1 O3 72.07(11) 2_755 2_755
O1 Pu1 O3 143.20(8) . .
O2 Pu1 O3 72.07(11) . .
O2 Pu1 O3 143.77(11) 2_755 .
O3 Pu1 O3 73.61(16) 2_755 .
O1 Pu1 Cl4 91.73(3) . .
O2 Pu1 Cl4 94.72(8) . .
O2 Pu1 Cl4 86.36(8) 2_755 .
O3 Pu1 Cl4 93.04(8) 2_755 .
O3 Pu1 Cl4 84.18(8) . .
O1 Pu1 Cl4 91.73(3) . 2_755
O2 Pu1 Cl4 86.36(8) . 2_755
O2 Pu1 Cl4 94.72(8) 2_755 2_755
O3 Pu1 Cl4 84.18(8) 2_755 2_755
O3 Pu1 Cl4 93.04(8) . 2_755
Cl4 Pu1 Cl4 176.54(5) . 2_755
O4 Pu2 Cl1 180.0 . .
O4 Pu2 Cl2 86.63(3) . .
Cl1 Pu2 Cl2 93.37(3) . .
O4 Pu2 Cl2 86.63(3) . 2_655
Cl1 Pu2 Cl2 93.37(3) . 2_655
Cl2 Pu2 Cl2 173.27(5) . 2_655
O4 Pu2 Cl3 86.45(3) . .
Cl1 Pu2 Cl3 93.55(3) . .
Cl2 Pu2 Cl3 89.07(5) . .
Cl2 Pu2 Cl3 90.52(5) 2_655 .
O4 Pu2 Cl3 86.45(3) . 2_655
Cl1 Pu2 Cl3 93.55(3) . 2_655
Cl2 Pu2 Cl3 90.52(5) . 2_655
Cl2 Pu2 Cl3 89.07(5) 2_655 2_655
Cl3 Pu2 Cl3 172.89(6) . 2_655
C1 O1 C1 108.6(5) . 2_755
C1 O1 Pu1 125.7(3) . .
C1 O1 Pu1 125.7(3) 2_755 .
C6 O2 C3 108.5(3) . .
C6 O2 Pu1 123.7(3) . .
C3 O2 Pu1 127.2(2) . .
C10 O3 C7 107.0(4) . .
C10 O3 Pu1 128.7(3) . .
C7 O3 Pu1 124.3(3) . .
C11 O4 C11 110.1(5) 2_655 .
C11 O4 Pu2 124.9(2) 2_655 .
C11 O4 Pu2 124.9(2) . .
O1 C1 C2 105.0(5) . .
C1 C2 C2 103.9(4) . 2_755
O2 C3 C4 106.0(4) . .
C3 C4 C5 105.1(5) . .
C4 C5 C6 103.8(4) . .
O2 C6 C5 105.3(4) . .
C8 C7 O3 107.4(5) . .
C7 C8 C9 108.5(5) . .
C10 C9 C8 105.9(5) . .
O3 C10 C9 107.2(5) . .
O4 C11 C12 105.1(4) . .
C12 C12 C11 105.9(3) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pu1 O1 2.461(4) .
Pu1 O2 2.473(3) .
Pu1 O2 2.473(3) 2_755
Pu1 O3 2.480(3) 2_755
Pu1 O3 2.480(3) .
Pu1 Cl4 2.6712(13) .
Pu1 Cl4 2.6712(13) 2_755
Pu2 O4 2.415(4) .
Pu2 Cl1 2.5350(17) .
Pu2 Cl2 2.5639(14) .
Pu2 Cl2 2.5639(14) 2_655
Pu2 Cl3 2.5767(15) .
Pu2 Cl3 2.5767(15) 2_655
O1 C1 1.451(5) .
O1 C1 1.451(5) 2_755
O2 C6 1.452(5) .
O2 C3 1.463(5) .
O3 C10 1.444(6) .
O3 C7 1.445(6) .
O4 C11 1.462(5) 2_655
O4 C11 1.462(5) .
C1 C2 1.456(9) .
C2 C2 1.476(16) 2_755
C3 C4 1.467(7) .
C4 C5 1.478(8) .
C5 C6 1.486(7) .
C7 C8 1.441(8) .
C8 C9 1.448(9) .
C9 C10 1.456(8) .
C11 C12 1.495(7) .
C12 C12 1.469(10) 2_655
