#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:46:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179513 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/10/4341019.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_4341019
loop_
_publ_author_name
'Ward, Matthew D.'
'Chan, Ian Y.'
'Lebègue, Sébastien'
'Ibers, James A.'
_publ_section_title
;
 The synthesis and characterization of four new uranium(IV)
 chlorophosphates: UCl₄(POCl₃),
 [U₂Cl₉][PCl₄], UCl₃(PO₂Cl₂),
 and U₂Cl₈(POCl₃).
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9969
_journal_page_last               9975
_journal_paper_doi               10.1021/ic501781h
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'Cl7 O P U'
_chemical_formula_sum            'Cl7 O P U'
_chemical_formula_weight         533.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-07-22 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 120.5202(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9155(2)
_cell_length_b                   8.4329(2)
_cell_length_c                   17.1934(4)
_cell_measurement_reflns_used    8520
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.01
_cell_measurement_theta_min      2.65
_cell_volume                     1113.56(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Crystalmaker (Palmer, 2009)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29562
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.438
_diffrn_reflns_theta_min         2.779
_exptl_absorpt_coefficient_mu    16.340
_exptl_absorpt_correction_T_max  0.7667
_exptl_absorpt_correction_T_min  0.2076
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed, SADABS (Sheldrick, 2008b)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    3.180
_exptl_crystal_description       Plate
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.021
_refine_diff_density_max         2.081
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.327
_refine_ls_extinction_coef       0.00325(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         5417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0232P)²] where P=(1.0000Fo²+0.0000Fc²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4460
_reflns_number_total             5417
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic501781h_si_001.cif
_cod_data_source_block           UCl4(POCl3)
_cod_depositor_comments
'Adding full bibliography for 4341019--4341022.cif.'
_cod_database_code               4341019
#BEGIN Tags that were not found in dictionaries:
_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   0.057
_shelx_estimated_absorpt_t_max   0.725
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
U1 U 0.58944(2) 0.21543(2) 0.27612(2) 0.00912(4) Uani 1 1 d
Cl1 Cl 0.08442(12) 0.30250(13) 0.27755(7) 0.02182(18) Uani 1 1 d
Cl2 Cl 0.18963(13) 0.41250(13) 0.47249(7) 0.0250(2) Uani 1 1 d
Cl3 Cl 0.21973(12) 0.05196(13) 0.43419(7) 0.0242(2) Uani 1 1 d
Cl4 Cl 0.29513(10) 0.02587(10) 0.20304(6) 0.01412(15) Uani 1 1 d
Cl5 Cl 0.30278(10) 0.40581(10) 0.17132(6) 0.01303(14) Uani 1 1 d
Cl6 Cl 0.56947(12) 0.25579(11) 0.41676(6) 0.01555(15) Uani 1 1 d
Cl7 Cl 0.62813(12) 0.18122(11) 0.14140(6) 0.01693(16) Uani 1 1 d
P1 P 0.07544(11) 0.24222(11) 0.38490(6) 0.01209(16) Uani 1 1 d
O1 O 0.1039(3) 0.7130(3) 0.13503(18) 0.0132(4) Uani 1 1 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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 Cl7 86.54(7) 2_645 .
O1 U1 Cl6 90.19(7) 2_645 .
Cl7 U1 Cl6 176.52(3) . .
O1 U1 Cl4 72.06(6) 2_645 2_655
Cl7 U1 Cl4 90.67(3) . 2_655
Cl6 U1 Cl4 87.20(3) . 2_655
O1 U1 Cl4 143.92(6) 2_645 .
Cl7 U1 Cl4 93.28(3) . .
Cl6 U1 Cl4 90.05(3) . .
Cl4 U1 Cl4 143.97(2) 2_655 .
O1 U1 Cl5 71.63(6) 2_645 2_645
Cl7 U1 Cl5 90.30(3) . 2_645
Cl6 U1 Cl5 89.78(3) . 2_645
Cl4 U1 Cl5 143.54(2) 2_655 2_645
Cl4 U1 Cl5 72.29(2) . 2_645
O1 U1 Cl5 143.97(6) 2_645 .
Cl7 U1 Cl5 88.87(3) . .
Cl6 U1 Cl5 93.10(3) . .
Cl4 U1 Cl5 72.29(2) 2_655 .
Cl4 U1 Cl5 72.00(2) . .
Cl5 U1 Cl5 144.17(2) 2_645 .
U1 Cl4 U1 106.42(3) 2_645 .
U1 Cl5 U1 106.34(3) 2_655 .
O1 P1 Cl2 112.40(12) 2_545 .
O1 P1 Cl1 112.52(12) 2_545 .
Cl2 P1 Cl1 106.37(6) . .
O1 P1 Cl3 111.09(12) 2_545 .
Cl2 P1 Cl3 107.34(6) . .
Cl1 P1 Cl3 106.77(6) . .
P1 O1 U1 155.72(17) 2 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 2.360(2) 2_645
U1 Cl7 2.5256(9) .
U1 Cl6 2.5361(9) .
U1 Cl4 2.7689(8) 2_655
U1 Cl4 2.7695(8) .
U1 Cl5 2.7705(8) 2_645
U1 Cl5 2.7711(8) .
Cl1 P1 1.9548(13) .
Cl2 P1 1.9517(14) .
Cl3 P1 1.9596(13) .
Cl4 U1 2.7689(8) 2_645
Cl5 U1 2.7704(8) 2_655
P1 O1 1.475(3) 2_545
O1 P1 1.475(3) 2
O1 U1 2.360(2) 2_655
