#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:50:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179515 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/12/4341268.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_4341268
loop_
_publ_author_name
'Schnaars, David D.'
'Wilson, Richard E.'
_publ_section_title
;
 Lattice Solvent and Crystal Phase Effects on the Vibrational Spectra of
 UO2Cl4(2-).
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11036
_journal_page_last               11045
_journal_paper_doi               10.1021/ic501553m
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C48 H40 Cl4 O2 P2 U'
_chemical_formula_weight         1090.57
_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                99.6630(10)
_cell_angle_beta                 93.3890(10)
_cell_angle_gamma                114.3080(10)
_cell_formula_units_Z            1
_cell_length_a                   10.0272(6)
_cell_length_b                   10.0808(6)
_cell_length_c                   12.0598(7)
_cell_measurement_reflns_used    5971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.25
_cell_volume                     1083.99(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       '0.5 deg w/ exposures'
_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  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15401
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    4.103
_exptl_absorpt_correction_T_max  0.6797
_exptl_absorpt_correction_T_min  0.5707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow-Green
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.637
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         5971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0257
_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)+(0.0239P)²+0.4749P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0549
_reflns_number_gt                5794
_reflns_number_total             5971
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501553m_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4341268--4341273.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4341268
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
U1 U 0.5000 0.0000 0.0000 0.01631(4) Uani 1 2 d S
Cl1 Cl 0.43392(7) -0.01107(7) 0.21038(5) 0.02236(13) Uani 1 1 d .
Cl2 Cl 0.70619(7) 0.28097(7) 0.07543(5) 0.02245(13) Uani 1 1 d .
P1 P 0.11747(7) 0.18673(7) 0.31440(5) 0.01305(12) Uani 1 1 d .
O1 O 0.6342(2) -0.0679(2) 0.02594(16) 0.0239(4) Uani 1 1 d .
C4 C 0.3941(3) 0.5436(3) 0.1280(2) 0.0201(5) Uani 1 1 d .
H4 H 0.4548 0.6199 0.0925 0.024 Uiso 1 1 calc R
C3 C 0.2661(3) 0.5455(3) 0.1644(2) 0.0194(5) Uani 1 1 d .
H3 H 0.2388 0.6224 0.1528 0.023 Uiso 1 1 calc R
C2 C 0.1783(3) 0.4359(3) 0.2176(2) 0.0173(5) Uani 1 1 d .
H2 H 0.0900 0.4366 0.2415 0.021 Uiso 1 1 calc R
C1 C 0.2197(3) 0.3239(3) 0.23612(19) 0.0147(4) Uani 1 1 d .
C13 C 0.2493(3) 0.1844(3) 0.42025(19) 0.0138(4) Uani 1 1 d .
C14 C 0.2547(3) 0.0521(3) 0.4337(2) 0.0159(5) Uani 1 1 d .
H14 H 0.1919 -0.0392 0.3834 0.019 Uiso 1 1 calc R
C15 C 0.3525(3) 0.0548(3) 0.5212(2) 0.0182(5) Uani 1 1 d .
H15 H 0.3567 -0.0352 0.5303 0.022 Uiso 1 1 calc R
C16 C 0.4437(3) 0.1867(3) 0.5952(2) 0.0189(5) Uani 1 1 d .
H16 H 0.5086 0.1868 0.6559 0.023 Uiso 1 1 calc R
C10 C -0.2025(3) 0.3366(3) 0.4916(2) 0.0238(6) Uani 1 1 d .
H10 H -0.2668 0.3720 0.5277 0.029 Uiso 1 1 calc R
C9 C -0.0870(3) 0.3310(3) 0.5566(2) 0.0205(5) Uani 1 1 d .
H9 H -0.0740 0.3596 0.6370 0.025 Uiso 1 1 calc R
C8 C 0.0096(3) 0.2836(3) 0.5038(2) 0.0170(5) Uani 1 1 d .
H8 H 0.0896 0.2808 0.5481 0.020 Uiso 1 1 calc R
C7 C -0.0109(3) 0.2400(3) 0.3857(2) 0.0152(5) Uani 1 1 d .
C12 C -0.1302(3) 0.2415(3) 0.3206(2) 0.0191(5) Uani 1 1 d .
H12 H -0.1464 0.2090 0.2403 0.023 Uiso 1 1 calc R
C11 C -0.2250(3) 0.2911(3) 0.3746(2) 0.0233(5) Uani 1 1 d .
H11 H -0.3055 0.2937 0.3310 0.028 Uiso 1 1 calc R
C5 C 0.4335(3) 0.4304(3) 0.1433(2) 0.0186(5) Uani 1 1 d .
H5 H 0.5194 0.4277 0.1157 0.022 Uiso 1 1 calc R
C6 C 0.3485(3) 0.3211(3) 0.1986(2) 0.0163(5) Uani 1 1 d .
H6 H 0.3771 0.2453 0.2109 0.020 Uiso 1 1 calc R
C17 C 0.4406(3) 0.3198(3) 0.5808(2) 0.0184(5) Uani 1 1 d .
H17 H 0.5044 0.4109 0.6310 0.022 Uiso 1 1 calc R
C18 C 0.3443(3) 0.3188(3) 0.4933(2) 0.0168(5) Uani 1 1 d .
H18 H 0.3428 0.4095 0.4828 0.020 Uiso 1 1 calc R
C19 C 0.0202(3) 0.0041(3) 0.2266(2) 0.0159(5) Uani 1 1 d .
C20 C -0.1022(3) -0.0992(3) 0.2632(2) 0.0223(5) Uani 1 1 d .
H20 H -0.1410 -0.0685 0.3275 0.027 Uiso 1 1 calc R
C21 C -0.1664(3) -0.2456(3) 0.2057(2) 0.0278(6) Uani 1 1 d .
H21 H -0.2493 -0.3163 0.2306 0.033 Uiso 1 1 calc R
C22 C -0.1101(3) -0.2899(3) 0.1112(2) 0.0253(6) Uani 1 1 d .
H22 H -0.1537 -0.3914 0.0725 0.030 Uiso 1 1 calc R
C23 C 0.0090(3) -0.1872(3) 0.0733(2) 0.0244(6) Uani 1 1 d .
H23 H 0.0459 -0.2181 0.0080 0.029 Uiso 1 1 calc R
C24 C 0.0746(3) -0.0395(3) 0.1303(2) 0.0196(5) Uani 1 1 d .
H24 H 0.1559 0.0314 0.1040 0.024 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'
O O 0.0106 0.0060 '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'
U U -9.6767 9.6646 '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 U1 O1 180.0 . 2_655
O1 U1 Cl1 90.47(6) . .
O1 U1 Cl1 89.53(6) 2_655 .
O1 U1 Cl1 89.53(6) . 2_655
O1 U1 Cl1 90.47(6) 2_655 2_655
Cl1 U1 Cl1 180.0 . 2_655
O1 U1 Cl2 90.15(6) . .
O1 U1 Cl2 89.85(6) 2_655 .
Cl1 U1 Cl2 89.79(2) . .
Cl1 U1 Cl2 90.21(2) 2_655 .
O1 U1 Cl2 89.85(6) . 2_655
O1 U1 Cl2 90.15(6) 2_655 2_655
Cl1 U1 Cl2 90.21(2) . 2_655
Cl1 U1 Cl2 89.79(2) 2_655 2_655
Cl2 U1 Cl2 180.0 . 2_655
C19 P1 C13 109.25(11) . .
C19 P1 C7 109.48(11) . .
C13 P1 C7 108.11(11) . .
C19 P1 C1 112.83(11) . .
C13 P1 C1 106.74(11) . .
C7 P1 C1 110.28(11) . .
C3 C4 C5 120.2(2) . .
C3 C4 H4 119.9 . .
C5 C4 H4 119.9 . .
C2 C3 C4 120.2(2) . .
C2 C3 H3 119.9 . .
C4 C3 H3 119.9 . .
C3 C2 C1 119.9(2) . .
C3 C2 H2 120.1 . .
C1 C2 H2 120.1 . .
C2 C1 C6 120.0(2) . .
C2 C1 P1 121.84(18) . .
C6 C1 P1 118.04(18) . .
C14 C13 C18 119.9(2) . .
C14 C13 P1 121.56(18) . .
C18 C13 P1 118.52(18) . .
C15 C14 C13 119.5(2) . .
C15 C14 H14 120.3 . .
C13 C14 H14 120.3 . .
C16 C15 C14 120.8(2) . .
C16 C15 H15 119.6 . .
C14 C15 H15 119.6 . .
C15 C16 C17 119.9(2) . .
C15 C16 H16 120.0 . .
C17 C16 H16 120.0 . .
C11 C10 C9 120.5(2) . .
C11 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
C10 C9 C8 119.9(2) . .
C10 C9 H9 120.1 . .
C8 C9 H9 120.1 . .
C9 C8 C7 119.9(2) . .
C9 C8 H8 120.1 . .
C7 C8 H8 120.1 . .
C8 C7 C12 120.1(2) . .
C8 C7 P1 120.98(19) . .
C12 C7 P1 118.90(18) . .
C11 C12 C7 119.3(2) . .
C11 C12 H12 120.4 . .
C7 C12 H12 120.4 . .
C10 C11 C12 120.3(2) . .
C10 C11 H11 119.8 . .
C12 C11 H11 119.8 . .
C4 C5 C6 120.5(2) . .
C4 C5 H5 119.8 . .
C6 C5 H5 119.8 . .
C5 C6 C1 119.2(2) . .
C5 C6 H6 120.4 . .
C1 C6 H6 120.4 . .
C18 C17 C16 119.8(2) . .
C18 C17 H17 120.1 . .
C16 C17 H17 120.1 . .
C17 C18 C13 120.1(2) . .
C17 C18 H18 120.0 . .
C13 C18 H18 120.0 . .
C24 C19 C20 120.3(2) . .
C24 C19 P1 120.71(19) . .
C20 C19 P1 118.60(18) . .
C21 C20 C19 119.7(2) . .
C21 C20 H20 120.2 . .
C19 C20 H20 120.2 . .
C20 C21 C22 120.1(3) . .
C20 C21 H21 120.0 . .
C22 C21 H21 120.0 . .
C23 C22 C21 120.3(2) . .
C23 C22 H22 119.8 . .
C21 C22 H22 119.8 . .
C22 C23 C24 120.3(2) . .
C22 C23 H23 119.9 . .
C24 C23 H23 119.9 . .
C23 C24 C19 119.3(2) . .
C23 C24 H24 120.3 . .
C19 C24 H24 120.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.7764(18) .
U1 O1 1.7764(18) 2_655
U1 Cl1 2.6686(6) .
U1 Cl1 2.6686(6) 2_655
U1 Cl2 2.6863(6) .
U1 Cl2 2.6863(6) 2_655
P1 C19 1.791(2) .
P1 C13 1.792(2) .
P1 C7 1.797(2) .
P1 C1 1.800(2) .
C4 C3 1.387(4) .
C4 C5 1.388(4) .
C4 H4 0.9500 .
C3 C2 1.382(3) .
C3 H3 0.9500 .
C2 C1 1.398(3) .
C2 H2 0.9500 .
C1 C6 1.403(3) .
C13 C14 1.393(3) .
C13 C18 1.399(3) .
C14 C15 1.386(3) .
C14 H14 0.9500 .
C15 C16 1.381(4) .
C15 H15 0.9500 .
C16 C17 1.393(3) .
C16 H16 0.9500 .
C10 C11 1.382(4) .
C10 C9 1.385(4) .
C10 H10 0.9500 .
C9 C8 1.387(3) .
C9 H9 0.9500 .
C8 C7 1.394(3) .
C8 H8 0.9500 .
C7 C12 1.399(3) .
C12 C11 1.390(3) .
C12 H12 0.9500 .
C11 H11 0.9500 .
C5 C6 1.388(3) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C17 C18 1.384(3) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C19 C24 1.392(3) .
C19 C20 1.397(3) .
C20 C21 1.377(4) .
C20 H20 0.9500 .
C21 C22 1.388(4) .
C21 H21 0.9500 .
C22 C23 1.383(4) .
C22 H22 0.9500 .
C23 C24 1.386(4) .
C23 H23 0.9500 .
C24 H24 0.9500 .
