#------------------------------------------------------------------------------
#$Date: 2023-11-10 21:21:08 +0200 (Fri, 10 Nov 2023) $
#$Revision: 287519 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/75/4307534.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_4307534
loop_
_publ_author_name
'L. Jonas L Häller'
'Nikolas Kaltsoyannis'
'Mark J. Sarsfield'
'Iain May'
'Stéphanie M. Cornet'
'Michael P. Redmond'
'Madeleine Helliwell'
_publ_section_title
;
A Structural and Theoretical Investigation of Equatorial cis and trans
Uranyl Phosphinimine and Uranyl Phosphine Oxide Complexes
UO2Cl2(Cy3PNH)2 and UO2Cl2(Cy3PO)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4868
_journal_page_last               4875
_journal_paper_doi               10.1021/ic062031m
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C38 H72 Cl6 N2 O2 P2 U'
_chemical_formula_weight         1101.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 113.6010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.453(3)
_cell_length_b                   8.8971(9)
_cell_length_c                   20.764(2)
_cell_measurement_reflns_used    5092
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2315
_cell_measurement_theta_min      2.428
_cell_volume                     4647.4(8)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'XSHELL, Bruker'
_computing_publication_material  'XP, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'SMART platform CCD, Bruker'
_diffrn_measurement_method       'omega 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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19157
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    3.940
_exptl_absorpt_correction_T_max  0.8910
_exptl_absorpt_correction_T_min  0.3844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_crystal_colour            'reactangular block'
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'pale yellow'
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.941
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0406P)²+8.2381P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0685
_reflns_number_gt                5157
_reflns_number_total             5486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062031msi20061023_031052.cif
_cod_data_source_block           s1245patt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4647.3(8)
_cod_database_code               4307534
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
C7 C 0.35916(12) 0.4923(3) 0.70450(17) 0.0241(6) Uani 1 1 d . . .
H7 H 0.3816 0.4011 0.7091 0.029 Uiso 1 1 calc R . .
C12 C 0.30184(12) 0.4463(4) 0.65717(18) 0.0269(7) Uani 1 1 d . . .
H12A H 0.2777 0.5326 0.6517 0.032 Uiso 1 1 calc R . .
H12B H 0.2999 0.4189 0.6100 0.032 Uiso 1 1 calc R . .
C8 C 0.36312(13) 0.5280(4) 0.77872(17) 0.0265(6) Uani 1 1 d . . .
H8A H 0.4005 0.5512 0.8095 0.032 Uiso 1 1 calc R . .
H8B H 0.3414 0.6180 0.7770 0.032 Uiso 1 1 calc R . .
C9 C 0.34385(14) 0.3960(4) 0.80984(19) 0.0304(7) Uani 1 1 d . . .
H9A H 0.3682 0.3096 0.8170 0.036 Uiso 1 1 calc R . .
H9B H 0.3446 0.4253 0.8562 0.036 Uiso 1 1 calc R . .
C10 C 0.28752(14) 0.3490(4) 0.7616(2) 0.0333(8) Uani 1 1 d . . .
H10A H 0.2772 0.2594 0.7815 0.040 Uiso 1 1 calc R . .
H10B H 0.2625 0.4312 0.7591 0.040 Uiso 1 1 calc R . .
C11 C 0.28359(14) 0.3133(4) 0.6883(2) 0.0323(7) Uani 1 1 d . . .
H11A H 0.2463 0.2882 0.6577 0.039 Uiso 1 1 calc R . .
H11B H 0.3059 0.2246 0.6903 0.039 Uiso 1 1 calc R . .
C1 C 0.33351(11) 0.7596(3) 0.60968(15) 0.0222(6) Uani 1 1 d . . .
H1 H 0.3053 0.6922 0.5770 0.027 Uiso 1 1 calc R . .
C6 C 0.30853(12) 0.8517(4) 0.65089(16) 0.0232(6) Uani 1 1 d . . .
H6A H 0.3358 0.9178 0.6848 0.028 Uiso 1 1 calc R . .
H6B H 0.2952 0.7832 0.6778 0.028 Uiso 1 1 calc R . .
C5 C 0.26254(13) 0.9478(4) 0.60100(18) 0.0273(7) Uani 1 1 d . . .
H5A H 0.2340 0.8814 0.5694 0.033 Uiso 1 1 calc R . .
H5B H 0.2476 1.0087 0.6287 0.033 Uiso 1 1 calc R . .
C2 C 0.35210(13) 0.8632(4) 0.56460(17) 0.0260(6) Uani 1 1 d . . .
H2A H 0.3814 0.9279 0.5957 0.031 Uiso 1 1 calc R . .
H2B H 0.3658 0.8014 0.5359 0.031 Uiso 1 1 calc R . .
C3 C 0.30650(13) 0.9620(4) 0.51619(17) 0.0288(7) Uani 1 1 d . . .
H3A H 0.3202 1.0321 0.4903 0.035 Uiso 1 1 calc R . .
H3B H 0.2791 0.8978 0.4813 0.035 Uiso 1 1 calc R . .
C4 C 0.28136(14) 1.0514(4) 0.55722(18) 0.0293(7) Uani 1 1 d . . .
H4A H 0.2508 1.1094 0.5242 0.035 Uiso 1 1 calc R . .
H4B H 0.3076 1.1237 0.5885 0.035 Uiso 1 1 calc R . .
C13 C 0.41786(12) 0.5560(4) 0.61289(17) 0.0239(6) Uani 1 1 d . . .
H13 H 0.4290 0.6412 0.5904 0.029 Uiso 1 1 calc R . .
C14 C 0.37789(14) 0.4611(4) 0.55231(18) 0.0331(8) Uani 1 1 d . . .
H14A H 0.3659 0.3743 0.5720 0.040 Uiso 1 1 calc R . .
H14B H 0.3464 0.5230 0.5250 0.040 Uiso 1 1 calc R . .
C18 C 0.46810(12) 0.4658(4) 0.65427(17) 0.0242(6) Uani 1 1 d . . .
H18A H 0.4591 0.3801 0.6779 0.029 Uiso 1 1 calc R . .
H18B H 0.4940 0.5304 0.6909 0.029 Uiso 1 1 calc R . .
C15 C 0.40386(16) 0.4048(5) 0.5039(2) 0.0437(10) Uani 1 1 d . . .
H15A H 0.3784 0.3408 0.4666 0.052 Uiso 1 1 calc R . .
H15B H 0.4130 0.4917 0.4810 0.052 Uiso 1 1 calc R . .
C17 C 0.49288(14) 0.4074(4) 0.60494(19) 0.0323(8) Uani 1 1 d . . .
H17A H 0.5055 0.4936 0.5856 0.039 Uiso 1 1 calc R . .
H17B H 0.5241 0.3442 0.6320 0.039 Uiso 1 1 calc R . .
C16 C 0.45364(16) 0.3156(5) 0.5446(2) 0.0443(10) Uani 1 1 d . . .
H16A H 0.4706 0.2850 0.5126 0.053 Uiso 1 1 calc R . .
H16B H 0.4440 0.2233 0.5635 0.053 Uiso 1 1 calc R . .
C1S C 0.42735(16) 0.9898(5) 0.3965(2) 0.0403(9) Uani 1 1 d . . .
H1S1 H 0.4338 0.9191 0.3640 0.048 Uiso 1 1 calc R . .
H1S2 H 0.4549 1.0693 0.4091 0.048 Uiso 1 1 calc R . .
Cl1 Cl 0.42628(3) 1.12538(8) 0.72977(4) 0.02488(16) Uani 1 1 d . . .
Cl2 Cl 0.43250(5) 0.89383(13) 0.47233(6) 0.0517(3) Uani 1 1 d . . .
Cl3 Cl 0.36378(7) 1.07219(15) 0.35375(7) 0.0722(4) Uani 1 1 d . . .
H1N H 0.4267(14) 0.743(4) 0.764(2) 0.027(10) Uiso 1 1 d . . .
N1 N 0.43196(10) 0.7348(3) 0.73083(14) 0.0206(5) Uani 1 1 d . . .
O1 O 0.48808(9) 0.9014(2) 0.65923(11) 0.0221(4) Uani 1 1 d . . .
P1 P 0.38716(3) 0.64026(9) 0.66787(4) 0.01970(15) Uani 1 1 d . . .
U1 U 0.5000 0.911441(16) 0.7500 0.01594(6) Uani 1 2 d S . .
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'
N N 0.0061 0.0033 '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
_geom_angle_publ_flag
C8 C7 C12 109.9(3) . . ?
C8 C7 P1 113.3(2) . . ?
C12 C7 P1 114.6(2) . . ?
C11 C12 C7 111.1(3) . . ?
C9 C8 C7 111.5(3) . . ?
C10 C9 C8 111.3(3) . . ?
C11 C10 C9 111.2(3) . . ?
C10 C11 C12 111.1(3) . . ?
C6 C1 C2 110.5(3) . . ?
C6 C1 P1 111.4(2) . . ?
C2 C1 P1 112.0(2) . . ?
C1 C6 C5 110.7(3) . . ?
C4 C5 C6 110.9(3) . . ?
C3 C2 C1 111.1(3) . . ?
C4 C3 C2 111.6(3) . . ?
C3 C4 C5 110.9(3) . . ?
C18 C13 C14 110.9(3) . . ?
C18 C13 P1 113.7(2) . . ?
C14 C13 P1 112.2(2) . . ?
C15 C14 C13 110.3(3) . . ?
C13 C18 C17 110.2(3) . . ?
C16 C15 C14 111.1(3) . . ?
C16 C17 C18 112.1(3) . . ?
C15 C16 C17 111.2(3) . . ?
Cl2 C1S Cl3 111.2(2) . . ?
P1 N1 U1 140.93(15) . . ?
N1 P1 C1 112.45(14) . . ?
N1 P1 C13 108.95(14) . . ?
C1 P1 C13 106.05(14) . . ?
N1 P1 C7 110.19(14) . . ?
C1 P1 C7 109.29(14) . . ?
C13 P1 C7 109.81(15) . . ?
O1 U1 O1 174.24(13) 2_656 . ?
O1 U1 N1 86.70(10) 2_656 . ?
O1 U1 N1 89.45(10) . . ?
O1 U1 N1 89.45(9) 2_656 2_656 ?
O1 U1 N1 86.70(9) . 2_656 ?
N1 U1 N1 96.04(13) . 2_656 ?
O1 U1 Cl1 93.58(7) 2_656 2_656 ?
O1 U1 Cl1 90.50(7) . 2_656 ?
N1 U1 Cl1 176.84(6) . 2_656 ?
N1 U1 Cl1 87.10(7) 2_656 2_656 ?
O1 U1 Cl1 90.50(7) 2_656 . ?
O1 U1 Cl1 93.58(7) . . ?
N1 U1 Cl1 87.10(7) . . ?
N1 U1 Cl1 176.84(6) 2_656 . ?
Cl1 U1 Cl1 89.75(3) 2_656 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C7 C8 1.534(4) . ?
C7 C12 1.540(4) . ?
C7 P1 1.836(3) . ?
C12 C11 1.527(5) . ?
C8 C9 1.533(4) . ?
C9 C10 1.526(5) . ?
C10 C11 1.516(5) . ?
C1 C6 1.531(4) . ?
C1 C2 1.539(4) . ?
C1 P1 1.825(3) . ?
C6 C5 1.533(4) . ?
C5 C4 1.523(5) . ?
C2 C3 1.531(4) . ?
C3 C4 1.519(5) . ?
C13 C18 1.528(4) . ?
C13 C14 1.547(4) . ?
C13 P1 1.829(3) . ?
C14 C15 1.531(5) . ?
C18 C17 1.530(5) . ?
C15 C16 1.512(6) . ?
C17 C16 1.522(5) . ?
C1S Cl2 1.747(4) . ?
C1S Cl3 1.769(4) . ?
Cl1 U1 2.6861(7) . ?
N1 P1 1.625(3) . ?
N1 U1 2.350(2) . ?
O1 U1 1.781(2) . ?
U1 O1 1.781(2) 2_656 ?
U1 N1 2.350(2) 2_656 ?
U1 Cl1 2.6861(7) 2_656 ?
_cod_duplicate_entry 4307532
