#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:47:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179394 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/91/4329197.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_4329197
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            'C48 H40 Cl6 Np P'
_chemical_formula_weight         1097.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.067(7)
_cell_angle_beta                 99.243(7)
_cell_angle_gamma                116.144(6)
_cell_formula_units_Z            1
_cell_length_a                   10.178(6)
_cell_length_b                   10.316(6)
_cell_length_c                   12.108(7)
_cell_measurement_temperature    141(2)
_cell_volume                     1115.3(11)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.10 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART 1k CCD'
_diffrn_measurement_method       'φ 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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10535
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.758
_exptl_absorpt_correction_T_max  0.5342
_exptl_absorpt_correction_T_min  0.4723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       block
_exptl_crystal_F_000             538
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_refine_diff_density_max         2.972
_refine_diff_density_min         -2.194
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0732P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                3825
_reflns_number_total             3924
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300179d_si_002_8.cif
_cod_data_source_block           xpl057
_cod_database_code               4329197
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Np1 Np 0.5000 1.0000 0.5000 0.01247(10) Uani 1 2 d S
P1 P 0.31662(11) 0.38603(11) 0.18046(8) 0.0130(2) Uani 1 1 d .
Cl3 Cl 0.51569(12) 1.08676(11) 0.30095(8) 0.0218(2) Uani 1 1 d .
Cl1 Cl 0.22223(11) 0.80252(11) 0.42080(9) 0.0222(2) Uani 1 1 d .
Cl2 Cl 0.59156(11) 0.81598(10) 0.43787(8) 0.0191(2) Uani 1 1 d .
C1 C 0.2656(4) 0.5136(4) 0.1123(3) 0.0154(8) Uani 1 1 d .
C2 C 0.2735(5) 0.6318(5) 0.1795(3) 0.0191(8) Uani 1 1 d .
H2 H 0.3109 0.6478 0.2569 0.023 Uiso 1 1 calc R
C3 C 0.2250(5) 0.7254(5) 0.1297(4) 0.0234(9) Uani 1 1 d .
H3 H 0.2280 0.8035 0.1741 0.028 Uiso 1 1 calc R
C4 C 0.1717(5) 0.7023(5) 0.0132(4) 0.0241(9) Uani 1 1 d .
H4 H 0.1384 0.7646 -0.0198 0.029 Uiso 1 1 calc R
C5 C 0.1682(5) 0.5873(5) -0.0533(4) 0.0211(9) Uani 1 1 d .
H5 H 0.1345 0.5734 -0.1312 0.025 Uiso 1 1 calc R
C6 C 0.2148(4) 0.4929(4) -0.0039(3) 0.0175(8) Uani 1 1 d .
H6 H 0.2121 0.4152 -0.0486 0.021 Uiso 1 1 calc R
C7 C 0.5016(4) 0.4815(4) 0.2652(3) 0.0149(8) Uani 1 1 d .
C8 C 0.6118(5) 0.5929(5) 0.2236(3) 0.0184(8) Uani 1 1 d .
H8 H 0.5867 0.6255 0.1572 0.022 Uiso 1 1 calc R
C9 C 0.7588(5) 0.6548(5) 0.2815(4) 0.0221(9) Uani 1 1 d .
H9 H 0.8327 0.7293 0.2542 0.026 Uiso 1 1 calc R
C10 C 0.7963(5) 0.6053(5) 0.3812(4) 0.0234(9) Uani 1 1 d .
H10 H 0.8955 0.6455 0.4193 0.028 Uiso 1 1 calc R
C11 C 0.6866(5) 0.4971(5) 0.4230(4) 0.0229(9) Uani 1 1 d .
H11 H 0.7121 0.4657 0.4900 0.027 Uiso 1 1 calc R
C12 C 0.5385(5) 0.4345(4) 0.3665(3) 0.0182(8) Uani 1 1 d .
H12 H 0.4647 0.3622 0.3956 0.022 Uiso 1 1 calc R
C13 C 0.1786(4) 0.2842(4) 0.2598(3) 0.0152(8) Uani 1 1 d .
C14 C 0.0696(5) 0.3238(5) 0.2799(3) 0.0192(8) Uani 1 1 d .
H14 H 0.0704 0.4083 0.2561 0.023 Uiso 1 1 calc R
C15 C -0.0405(5) 0.2373(5) 0.3353(4) 0.0224(9) Uani 1 1 d .
H15 H -0.1143 0.2631 0.3477 0.027 Uiso 1 1 calc R
C16 C -0.0405(5) 0.1124(5) 0.3721(3) 0.0230(9) Uani 1 1 d .
H16 H -0.1147 0.0540 0.4088 0.028 Uiso 1 1 calc R
C17 C 0.0698(5) 0.0746(5) 0.3544(3) 0.0201(9) Uani 1 1 d .
H17 H 0.0704 -0.0082 0.3807 0.024 Uiso 1 1 calc R
C18 C 0.1793(4) 0.1585(4) 0.2980(3) 0.0168(8) Uani 1 1 d .
H18 H 0.2524 0.1318 0.2855 0.020 Uiso 1 1 calc R
C19 C 0.3145(5) 0.2553(4) 0.0750(3) 0.0151(8) Uani 1 1 d .
C20 C 0.4446(4) 0.2456(4) 0.0659(3) 0.0158(8) Uani 1 1 d .
H20 H 0.5341 0.3056 0.1158 0.019 Uiso 1 1 calc R
C21 C 0.4396(5) 0.1453(5) -0.0187(4) 0.0212(9) Uani 1 1 d .
H21 H 0.5262 0.1378 -0.0243 0.025 Uiso 1 1 calc R
C22 C 0.3078(5) 0.0570(5) -0.0941(4) 0.0229(9) Uani 1 1 d .
H22 H 0.3063 -0.0067 -0.1521 0.028 Uiso 1 1 calc R
C23 C 0.1771(5) 0.0639(5) -0.0826(4) 0.0217(9) Uani 1 1 d .
H23 H 0.0876 0.0023 -0.1320 0.026 Uiso 1 1 calc R
C24 C 0.1789(5) 0.1613(4) 0.0013(3) 0.0190(8) Uani 1 1 d .
H24 H 0.0909 0.1646 0.0089 0.023 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'
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'
P P 0.1023 0.0942 '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 Np1 Cl2 180.000(2) . 2_676
Cl2 Np1 Cl3 91.69(4) . 2_676
Cl2 Np1 Cl3 88.31(4) 2_676 2_676
Cl2 Np1 Cl3 88.31(4) . .
Cl2 Np1 Cl3 91.69(4) 2_676 .
Cl3 Np1 Cl3 180.000(1) 2_676 .
Cl2 Np1 Cl1 90.41(6) . 2_676
Cl2 Np1 Cl1 89.59(6) 2_676 2_676
Cl3 Np1 Cl1 89.93(4) 2_676 2_676
Cl3 Np1 Cl1 90.07(4) . 2_676
Cl2 Np1 Cl1 89.59(6) . .
Cl2 Np1 Cl1 90.41(6) 2_676 .
Cl3 Np1 Cl1 90.07(4) 2_676 .
Cl3 Np1 Cl1 89.93(4) . .
Cl1 Np1 Cl1 179.999(2) 2_676 .
C7 P1 C19 108.49(19) . .
C7 P1 C13 113.09(18) . .
C19 P1 C13 106.35(19) . .
C7 P1 C1 109.68(19) . .
C19 P1 C1 109.48(19) . .
C13 P1 C1 109.66(19) . .
C6 C1 C2 120.2(4) . .
C6 C1 P1 121.3(3) . .
C2 C1 P1 118.4(3) . .
C3 C2 C1 119.4(4) . .
C2 C3 C4 120.0(4) . .
C5 C4 C3 120.4(4) . .
C6 C5 C4 119.8(4) . .
C5 C6 C1 120.2(4) . .
C8 C7 C12 120.3(4) . .
C8 C7 P1 119.2(3) . .
C12 C7 P1 120.2(3) . .
C9 C8 C7 119.7(4) . .
C8 C9 C10 120.0(4) . .
C11 C10 C9 120.0(4) . .
C10 C11 C12 120.8(4) . .
C11 C12 C7 119.2(4) . .
C14 C13 C18 119.9(4) . .
C14 C13 P1 121.8(3) . .
C18 C13 P1 118.2(3) . .
C15 C14 C13 120.1(4) . .
C16 C15 C14 120.0(4) . .
C17 C16 C15 120.0(4) . .
C18 C17 C16 120.8(4) . .
C17 C18 C13 119.2(4) . .
C20 C19 C24 119.8(4) . .
C20 C19 P1 121.0(3) . .
C24 C19 P1 119.2(3) . .
C19 C20 C21 119.5(4) . .
C22 C21 C20 120.7(4) . .
C21 C22 C23 119.6(4) . .
C24 C23 C22 120.7(4) . .
C23 C24 C19 119.6(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Np1 Cl2 2.5826(14) .
Np1 Cl2 2.5826(14) 2_676
Np1 Cl3 2.6198(16) 2_676
Np1 Cl3 2.6198(16) .
Np1 Cl1 2.6281(16) 2_676
Np1 Cl1 2.6281(16) .
P1 C7 1.790(4) .
P1 C19 1.797(4) .
P1 C13 1.800(4) .
P1 C1 1.806(4) .
C1 C6 1.388(6) .
C1 C2 1.394(6) .
C2 C3 1.388(6) .
C3 C4 1.395(7) .
C4 C5 1.381(7) .
C5 C6 1.382(6) .
C7 C8 1.393(6) .
C7 C12 1.398(6) .
C8 C9 1.382(6) .
C9 C10 1.397(6) .
C10 C11 1.375(7) .
C11 C12 1.385(6) .
C13 C14 1.391(6) .
C13 C18 1.402(6) .
C14 C15 1.388(6) .
C15 C16 1.386(7) .
C16 C17 1.383(7) .
C17 C18 1.384(6) .
C19 C20 1.392(6) .
C19 C24 1.405(6) .
C20 C21 1.396(6) .
C21 C22 1.380(6) .
C22 C23 1.391(7) .
C23 C24 1.383(6) .
