#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:47:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179394 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/91/4329195.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_4329195
loop_
_publ_author_name
'Stefan G. Minasian'
'Kevin S. Boland'
'Russell K. Feller'
'Andrew J. Gaunt'
'Stosh A. Kozimor'
'Iain May'
'Sean D. Reilly'
'Brian L. Scott'
'David K. Shuh'
_publ_contact_author_address     'Los Alamos National Laboratory'
_publ_contact_author_email       stosh@lanl.gov
_publ_contact_author_name        'Stosh A. Kozimor'
_publ_contact_author_phone       505-665-4521
_publ_section_title
;
 Synthesis and Structure of (Ph4P)2MCl6 (M = Ti, Zr, Hf, Th, U, Np, Pu)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5728
_journal_page_last               5736
_journal_paper_doi               10.1021/ic300179d
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C56 H52 Cl6 N4 P2 Th'
_chemical_formula_weight         1287.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.0870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6163(8)
_cell_length_b                   19.4637(16)
_cell_length_c                   15.1524(12)
_cell_measurement_temperature    140(1)
_cell_volume                     2807.9(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. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26950
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.037
_exptl_absorpt_correction_T_max  0.6758
_exptl_absorpt_correction_T_min  0.6109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       block
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0031P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0443
_reflns_number_gt                3970
_reflns_number_total             5136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300179d_si_002_6.cif
_cod_data_source_block           apx699
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329195
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Th1 Th 0.0000 0.5000 0.5000 0.01231(5) Uani 1 2 d S
Cl1 Cl 0.13062(9) 0.51098(5) 0.35486(5) 0.0211(2) Uani 1 1 d .
Cl2 Cl 0.23713(9) 0.45883(5) 0.59896(6) 0.0193(2) Uani 1 1 d .
Cl3 Cl 0.06447(9) 0.63060(4) 0.54519(6) 0.0204(2) Uani 1 1 d .
N1 N 0.6450(4) 0.20700(19) 0.3303(3) 0.0582(13) Uani 1 1 d .
N2 N 0.2746(4) -0.02385(16) 0.5976(2) 0.0379(10) Uani 1 1 d .
P1 P 0.34014(10) 0.19480(5) 0.56621(6) 0.0146(2) Uani 1 1 d .
C1 C 0.4817(3) 0.14470(17) 0.6225(2) 0.0146(8) Uani 1 1 d .
C2 C 0.5496(4) 0.09700(17) 0.5758(2) 0.0197(9) Uani 1 1 d .
H2 H 0.5162 0.0879 0.5164 0.024 Uiso 1 1 calc R
C3 C 0.6671(4) 0.06296(18) 0.6175(2) 0.0217(9) Uani 1 1 d .
H3 H 0.7121 0.0307 0.5862 0.026 Uiso 1 1 calc R
C4 C 0.7176(4) 0.07696(19) 0.7058(3) 0.0241(10) Uani 1 1 d .
H4 H 0.7977 0.0547 0.7334 0.029 Uiso 1 1 calc R
C5 C 0.6497(4) 0.12373(18) 0.7528(2) 0.0228(9) Uani 1 1 d .
H5 H 0.6833 0.1325 0.8123 0.027 Uiso 1 1 calc R
C6 C 0.5317(4) 0.15771(18) 0.7119(2) 0.0191(9) Uani 1 1 d .
H6 H 0.4858 0.1892 0.7439 0.023 Uiso 1 1 calc R
C7 C 0.2094(3) 0.20880(18) 0.6379(2) 0.0147(8) Uani 1 1 d .
C8 C 0.1795(4) 0.15677(18) 0.6962(2) 0.0190(9) Uani 1 1 d .
H8 H 0.2330 0.1168 0.7019 0.023 Uiso 1 1 calc R
C9 C 0.0696(4) 0.16526(19) 0.7452(2) 0.0246(10) Uani 1 1 d .
H9 H 0.0491 0.1310 0.7841 0.030 Uiso 1 1 calc R
C10 C -0.0095(4) 0.22458(19) 0.7361(2) 0.0250(10) Uani 1 1 d .
H10 H -0.0833 0.2301 0.7690 0.030 Uiso 1 1 calc R
C11 C 0.0197(4) 0.27597(19) 0.6786(2) 0.0216(9) Uani 1 1 d .
H11 H -0.0344 0.3157 0.6729 0.026 Uiso 1 1 calc R
C12 C 0.1301(3) 0.26827(18) 0.6290(2) 0.0175(9) Uani 1 1 d .
H12 H 0.1504 0.3028 0.5903 0.021 Uiso 1 1 calc R
C13 C 0.4095(4) 0.27445(17) 0.5322(2) 0.0152(8) Uani 1 1 d .
C14 C 0.3370(4) 0.31179(18) 0.4624(2) 0.0210(9) Uani 1 1 d .
H14 H 0.2506 0.2962 0.4344 0.025 Uiso 1 1 calc R
C15 C 0.3933(4) 0.3724(2) 0.4345(3) 0.0246(10) Uani 1 1 d .
H15 H 0.3445 0.3975 0.3879 0.030 Uiso 1 1 calc R
C16 C 0.5222(4) 0.39518(19) 0.4763(3) 0.0269(10) Uani 1 1 d .
H16 H 0.5609 0.4353 0.4568 0.032 Uiso 1 1 calc R
C17 C 0.5932(4) 0.3591(2) 0.5461(3) 0.0262(11) Uani 1 1 d .
H17 H 0.6794 0.3750 0.5741 0.031 Uiso 1 1 calc R
C18 C 0.5372(4) 0.29910(18) 0.5750(2) 0.0203(9) Uani 1 1 d .
H18 H 0.5849 0.2752 0.6231 0.024 Uiso 1 1 calc R
C19 C 0.2596(4) 0.15128(17) 0.4678(2) 0.0133(8) Uani 1 1 d .
C20 C 0.1395(4) 0.11166(18) 0.4705(2) 0.0207(9) Uani 1 1 d .
H20 H 0.1022 0.1067 0.5235 0.025 Uiso 1 1 calc R
C21 C 0.0758(4) 0.07957(19) 0.3934(3) 0.0281(10) Uani 1 1 d .
H21 H -0.0044 0.0531 0.3945 0.034 Uiso 1 1 calc R
C22 C 0.1327(4) 0.08730(19) 0.3143(3) 0.0318(11) Uani 1 1 d .
H22 H 0.0887 0.0670 0.2622 0.038 Uiso 1 1 calc R
C23 C 0.2533(4) 0.12464(19) 0.3129(2) 0.0269(10) Uani 1 1 d .
H23 H 0.2922 0.1283 0.2602 0.032 Uiso 1 1 calc R
C24 C 0.3172(4) 0.15676(18) 0.3888(2) 0.0202(9) Uani 1 1 d .
H24 H 0.3989 0.1821 0.3874 0.024 Uiso 1 1 calc R
C25 C 0.7191(5) 0.2035(2) 0.3942(3) 0.0349(12) Uani 1 1 d .
C26 C 0.8140(4) 0.1981(2) 0.4779(3) 0.0367(11) Uani 1 1 d .
H26A H 0.8222 0.1508 0.4959 0.055 Uiso 1 1 calc R
H26B H 0.7773 0.2244 0.5231 0.055 Uiso 1 1 calc R
H26C H 0.9048 0.2155 0.4700 0.055 Uiso 1 1 calc R
C27 C 0.3442(4) -0.03154(19) 0.6637(3) 0.0268(10) Uani 1 1 d .
C28 C 0.4329(4) -0.0424(2) 0.7493(2) 0.0332(11) Uani 1 1 d .
H28A H 0.4403 -0.0907 0.7618 0.050 Uiso 1 1 calc R
H28B H 0.3918 -0.0197 0.7957 0.050 Uiso 1 1 calc R
H28C H 0.5247 -0.0238 0.7467 0.050 Uiso 1 1 calc R
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'
P P 0.1023 0.0942 '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'
Th Th -7.2400 8.8979 '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'
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
Cl2 Th1 Cl2 180.00(4) 3_566 .
Cl2 Th1 Cl3 89.57(3) 3_566 3_566
Cl2 Th1 Cl3 90.43(3) . 3_566
Cl2 Th1 Cl3 90.43(3) 3_566 .
Cl2 Th1 Cl3 89.58(3) . .
Cl3 Th1 Cl3 180.0 3_566 .
Cl2 Th1 Cl1 91.31(3) 3_566 3_566
Cl2 Th1 Cl1 88.69(3) . 3_566
Cl3 Th1 Cl1 90.90(3) 3_566 3_566
Cl3 Th1 Cl1 89.10(3) . 3_566
Cl2 Th1 Cl1 88.69(3) 3_566 .
Cl2 Th1 Cl1 91.31(3) . .
Cl3 Th1 Cl1 89.10(3) 3_566 .
Cl3 Th1 Cl1 90.90(3) . .
Cl1 Th1 Cl1 180.0 3_566 .
C1 P1 C13 108.64(16) . .
C1 P1 C19 110.45(16) . .
C13 P1 C19 107.71(16) . .
C1 P1 C7 110.16(16) . .
C13 P1 C7 111.33(16) . .
C19 P1 C7 108.51(16) . .
C2 C1 C6 119.6(3) . .
C2 C1 P1 120.2(3) . .
C6 C1 P1 119.9(3) . .
C3 C2 C1 120.1(3) . .
C2 C3 C4 120.0(4) . .
C5 C4 C3 120.1(4) . .
C4 C5 C6 120.3(4) . .
C5 C6 C1 119.8(3) . .
C12 C7 C8 120.5(3) . .
C12 C7 P1 119.5(3) . .
C8 C7 P1 119.7(3) . .
C9 C8 C7 119.5(3) . .
C10 C9 C8 119.9(4) . .
C9 C10 C11 120.8(4) . .
C10 C11 C12 120.0(3) . .
C7 C12 C11 119.3(3) . .
C14 C13 C18 119.4(3) . .
C14 C13 P1 120.4(3) . .
C18 C13 P1 120.3(3) . .
C13 C14 C15 120.2(4) . .
C16 C15 C14 119.7(4) . .
C17 C16 C15 120.4(4) . .
C16 C17 C18 120.2(4) . .
C17 C18 C13 120.1(4) . .
C24 C19 C20 119.9(3) . .
C24 C19 P1 120.1(3) . .
C20 C19 P1 120.0(3) . .
C21 C20 C19 119.6(4) . .
C20 C21 C22 119.6(4) . .
C23 C22 C21 120.4(4) . .
C22 C23 C24 120.4(4) . .
C23 C24 C19 119.9(4) . .
N1 C25 C26 178.9(5) . .
N2 C27 C28 179.2(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Th1 Cl2 2.6699(9) 3_566
Th1 Cl2 2.6699(9) .
Th1 Cl3 2.6824(9) 3_566
Th1 Cl3 2.6825(9) .
Th1 Cl1 2.6901(8) 3_566
Th1 Cl1 2.6901(8) .
N1 C25 1.121(5) .
N2 C27 1.134(5) .
P1 C1 1.790(3) .
P1 C13 1.792(3) .
P1 C19 1.793(3) .
P1 C7 1.794(3) .
C1 C2 1.385(4) .
C1 C6 1.396(4) .
C2 C3 1.383(4) .
C3 C4 1.385(5) .
C4 C5 1.376(5) .
C5 C6 1.382(4) .
C7 C12 1.382(4) .
C7 C8 1.400(4) .
C8 C9 1.384(5) .
C9 C10 1.378(5) .
C10 C11 1.381(5) .
C11 C12 1.392(4) .
C13 C14 1.387(4) .
C13 C18 1.391(4) .
C14 C15 1.388(5) .
C15 C16 1.384(5) .
C16 C17 1.369(5) .
C17 C18 1.383(5) .
C19 C24 1.392(4) .
C19 C20 1.394(4) .
C20 C21 1.389(5) .
C21 C22 1.393(5) .
C22 C23 1.371(5) .
C23 C24 1.376(5) .
C25 C26 1.459(5) .
C27 C28 1.465(5) .
