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_7041933
_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         'C31 H36 O P Rh'
_chemical_formula_sum            'C31 H36 O P Rh'
_chemical_formula_weight         558.48
_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             2016-01-29
_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                102.7983(18)
_cell_angle_beta                 102.8779(19)
_cell_angle_gamma                93.4883(18)
_cell_formula_units_Z            2
_cell_length_a                   9.7178(2)
_cell_length_b                   11.5025(2)
_cell_length_c                   12.6599(3)
_cell_measurement_reflns_used    17770
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.6560
_cell_measurement_theta_min      3.6470
_cell_volume                     1336.17(5)
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -45.00   53.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955   37.0000   60.0000 98

  2 omega  -92.00    7.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -37.0000 -120.0000 99

  3 omega  -25.00   23.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -99.0000    0.0000 48

  4 omega  -88.00    2.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -57.0000   90.0000 90

  5 omega   32.00   98.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518 -179.0000  -60.0000 66

  6 omega  -92.00    7.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -37.0000  -30.0000 99

  7 omega  -88.00    2.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -57.0000  150.0000 90

  8 omega  -25.00   23.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -99.0000  150.0000 48

  9 omega  -88.00    2.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -57.0000    0.0000 90

 10 omega  -95.00  -34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955 -179.0000   30.0000 61

 11 omega  -25.00   64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -99.0000  -90.0000 89

 12 omega  -25.00   64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -99.0000   90.0000 89

 13 omega   34.00   98.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  179.0000   30.0000 64

 14 omega  -25.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -99.0000  -30.0000 81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0415703000
_diffrn_orient_matrix_UB_12      0.0249295000
_diffrn_orient_matrix_UB_13      -0.0411359000
_diffrn_orient_matrix_UB_21      -0.0626609000
_diffrn_orient_matrix_UB_22      -0.0296788000
_diffrn_orient_matrix_UB_23      0.0064358000
_diffrn_orient_matrix_UB_31      -0.0052854000
_diffrn_orient_matrix_UB_32      0.0505072000
_diffrn_orient_matrix_UB_33      0.0421225000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30827
_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         27.485
_diffrn_reflns_theta_min         3.061
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.912
_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    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethylether'
_exptl_crystal_size_max          0.2734
_exptl_crystal_size_mid          0.2443
_exptl_crystal_size_min          0.1046
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6119
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0341P)^2^+0.5075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5687
_reflns_number_total             6119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04570g2.cif
_cod_data_source_block           4_codRhL
_cod_depositor_comments
'Adding full bibliography for 7041933--7041935.cif.'
_cod_original_cell_volume        1336.16(5)
_cod_database_code               7041933
_chemical_oxdiff_formula         'C50 H50 Rh1 O1 P1'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C30-C29 \\sim C30A-C29A
 with sigma of 0.02
 C31-C30 \\sim C29A-C28
 with sigma of 0.02
 C31-C30A \\sim C29-C28
 with sigma of 0.02
 C26-C25 \\sim C26A-C25A
 with sigma of 0.02
 C25-C24 \\sim C27-C26A
 with sigma of 0.02
 C25A-C24 \\sim C27-C26
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C25, C25A, C26, C26A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, C30A, C29, C29A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=1-FVAR(1)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=FVAR(1)
 Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=1-FVAR(2)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C24(H24), C27(H27), C28(H28), C31(H31)
5.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C29(H29A,H29B), C30(H30A,H30B), C29A(H29C,
 H29D), C30A(H30C,H30D), C26A(H26C,H26D), C25A(H25C,H25D)
5.c 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)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              64446
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'