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_7041934
_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         'C69 H72 I2 O3 P3 Rh U'
_chemical_formula_sum            'C69 H72 I2 O3 P3 Rh U'
_chemical_formula_weight         1636.91
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-01
_audit_creation_method
;
Olex2 1.2
(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                98.8295(17)
_cell_angle_beta                 97.8140(17)
_cell_angle_gamma                97.5610(17)
_cell_formula_units_Z            2
_cell_length_a                   12.3192(3)
_cell_length_b                   13.5642(3)
_cell_length_c                   26.1759(5)
_cell_measurement_reflns_used    15042
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.3400
_cell_measurement_theta_min      3.1890
_cell_volume                     4229.79(17)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -25.00   23.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -99.0000 -180.0000 48

  2 omega  -47.00   43.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -57.0000 -120.0000 90

  3 omega   -4.00   94.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   38.0000 -180.0000 98

  4 omega  -50.00   47.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -38.0000    0.0000 97

  5 omega    5.00   87.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518 -137.0000   -6.0000 82

  6 omega  -88.00    2.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -57.0000 -120.0000 90

  7 omega  -25.00   23.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -99.0000    0.0000 48

  8 omega   32.00   98.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518 -179.0000 -120.0000 66

  9 omega    1.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   57.0000   60.0000 90

 10 omega  -22.00   95.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   19.0000   30.0000 117

 11 omega  -95.00  -34.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955 -179.0000   90.0000 61

 12 omega  -95.00  -48.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955 -179.0000  -90.0000 47

 13 omega    1.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   57.0000 -120.0000 90

 14 omega    1.00   84.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518 -132.0000  170.0000 83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0277926000
_diffrn_orient_matrix_UB_12      -0.0246688000
_diffrn_orient_matrix_UB_13      -0.0251359000
_diffrn_orient_matrix_UB_21      0.0357536000
_diffrn_orient_matrix_UB_22      0.0317469000
_diffrn_orient_matrix_UB_23      -0.0118156000
_diffrn_orient_matrix_UB_31      0.0375592000
_diffrn_orient_matrix_UB_32      -0.0354066000
_diffrn_orient_matrix_UB_33      -0.0004158000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_unetI/netI     0.0803
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            97387
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.031
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.928
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.1842
_exptl_crystal_size_mid          0.1568
_exptl_crystal_size_min          0.0464
_refine_diff_density_max         1.459
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         19379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14255
_reflns_number_total             19379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04570g2.cif
_cod_data_source_block           3_IUL3RhI
_cod_depositor_comments
'Adding full bibliography for 7041933--7041935.cif.'
_cod_original_cell_volume        4229.79(15)
_cod_database_code               7041934
_chemical_oxdiff_formula         'C60 H70 N8 Ca3'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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:
 C26(H26), C65(H65), C49(H49), C13(H13), C51(H51), C28(H28), C19(H19),
 C66(H66), C61(H61), C69(H69), C23(H23), C60(H60), C45(H45), C3(H3), C43(H43),
 C40(H40), C68(H68), C36(H36), C44(H44), C5(H5), C14(H14), C67(H67), C39(H39),
 C20(H20), C37(H37), C16(H16), C38(H38), C21(H21), C59(H59), C42(H42), C17(H17),
  C46(H46), C63(H63), C62(H62), C15(H15), C22(H22)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C9(H9A,H9B,H9C),
 C34(H34A,H34B,H34C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C57(H57A,H57B,
 H57C), C56(H56A,H56B,H56C), C11(H11A,H11B,H11C), C33(H33A,H33B,H33C), C10(H10A,
 H10B,H10C)
;
_shelx_res_checksum              83496
_shelx_fab_checksum              60537
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'