Uranium rhodium bonding in heterometallic complexes.
Hlina, J. A.; Wells, J. A. L.; Pankhurst, J. R.; Love, Jason B.; Arnold, P. L.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5540–5545; doi:10.1039/c6dt04570g

data_7041935
_publ_section_title
;
 Uranium rhodium bonding in heterometallic complexes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5540
_journal_page_last               5545
_journal_paper_doi               10.1039/c6dt04570g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C92 H96 I6 O4 P4 Rh2 U2'
_chemical_formula_sum            'C92 H96 I6 O4 P4 Rh2 U2'
_chemical_formula_weight         2832.84
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-11-29 deposited with the CCDC.
2017-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.6036(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.06093(18)
_cell_length_b                   15.91912(19)
_cell_length_c                   19.8049(2)
_cell_measurement_reflns_used    33888
_cell_measurement_temperature    170
_cell_measurement_theta_max      29.8370
_cell_measurement_theta_min      3.2210
_cell_volume                     5331.62(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -89.00  -10.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  145.0000   -8.4101 79

  2 omega  -25.00   23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -99.0000 -150.0000 48

  3 omega   34.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  179.0000 -120.0000 64

  4 omega    1.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   57.0000    0.0000 90

  5 omega  -51.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -19.0000 -180.0000 117

  6 omega  -95.00  -34.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955 -179.0000 -120.0000 61

  7 omega  -25.00   23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -99.0000   60.0000 48

  8 omega    1.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   57.0000   90.0000 90

  9 omega  -25.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -99.0000  -90.0000 89

 10 omega    1.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   57.0000  -90.0000 90

 11 omega  -50.00  -25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -38.0000   30.0000 25

 12 omega   -4.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   38.0000 -150.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0103798000
_diffrn_orient_matrix_UB_12      -0.0391352000
_diffrn_orient_matrix_UB_13      -0.0158219000
_diffrn_orient_matrix_UB_21      -0.0034459000
_diffrn_orient_matrix_UB_22      0.0195783000
_diffrn_orient_matrix_UB_23      -0.0324285000
_diffrn_orient_matrix_UB_31      0.0404994000
_diffrn_orient_matrix_UB_32      -0.0083514000
_diffrn_orient_matrix_UB_33      -0.0018712000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            97286
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.828
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.5370
_exptl_crystal_size_mid          0.1936
_exptl_crystal_size_min          0.1419
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         12211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0227
_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/[\s^2^(Fo^2^)+(0.0214P)^2^+8.1946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10824
_reflns_number_total             12211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04570g2.cif
_cod_data_source_block           2_I2UL2RhI-dimer
_cod_depositor_comments
'Adding full bibliography for 7041933--7041935.cif.'
_cod_database_code               7041935
_chemical_oxdiff_formula         'C100 H100 O4 P4 U2 Rh2 I4'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_platon_squeeze_void_probe_radius 1.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C28(H28), C36(H36), C37(H37),
  C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C)
;
_shelx_fab_checksum              42200
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'