Ethene Activation and Catalytic Hydrogenation by a Low-Valent Uranium Pentalene Complex.
Tsoureas, Nikolaos; Maron, Laurent; Kilpatrick, Alexander F. R.; Layfield, Richard A.; Cloke, F Geoffrey N; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b11929

data_4133862
_publ_section_title
;
 Ethene Activation and Catalytic Hydrogenation by a Low-Valent Uranium
 Pentalene Complex.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11929
_journal_year                    2019
_chemical_formula_moiety         'C40 H69 O Si2 U'
_chemical_formula_sum            'C40 H69 O Si2 U'
_chemical_formula_weight         860.16
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2943(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.77657(19)
_cell_length_b                   14.5949(3)
_cell_length_c                   23.1173(5)
_cell_measurement_reflns_used    4736
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.5360
_cell_measurement_theta_min      3.5790
_cell_volume                     3972.34(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     58.00 105.00   1.00   30.00    --   37.42  77.00-120.00   47
  2  \w     12.00  39.00   1.00   30.00    --   37.42  77.00-120.00   27
  3  \w     32.00 110.00   1.00   30.00    --   37.42-178.00  60.00   78
  4  \w     11.00 100.00   1.00   30.00    --   37.42  77.00 150.00   89
  5  \w     41.00 107.00   1.00   60.00    --  107.00 -83.00-156.56   66
  6  \w     47.00  74.00   1.00   60.00    --  107.00 -95.00 120.00   27
  7  \w     45.00 134.00   1.00   60.00    --  107.00 -77.00 -90.00   89
  8  \w     81.00 166.00   1.00   60.00    --  107.00  77.00 -30.00   85
  9  \w     95.00 174.00   1.00   60.00    --  107.00  61.00  60.00   79
 10  \w     79.00 173.00   1.00   60.00    --  107.00 111.00 -90.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0330773000
_diffrn_orient_matrix_UB_12      -0.0013831000
_diffrn_orient_matrix_UB_13      -0.0640613000
_diffrn_orient_matrix_UB_21      -0.0248684000
_diffrn_orient_matrix_UB_22      0.1034264000
_diffrn_orient_matrix_UB_23      -0.0044060000
_diffrn_orient_matrix_UB_31      0.1241473000
_diffrn_orient_matrix_UB_32      0.0212106000
_diffrn_orient_matrix_UB_33      0.0177880000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1031
_diffrn_reflns_av_unetI/netI     0.1329
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12563
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.064
_diffrn_reflns_theta_max         67.064
_diffrn_reflns_theta_min         3.582
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.273
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       plate
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.871
_refine_diff_density_min         -3.090
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7007
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0868P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5140
_reflns_number_total             7007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11929_si_002.cif
_cod_data_source_block           1.THF
_cod_original_cell_volume        3972.32(14)
_cod_database_code               4133862
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C40 H69 O1 Si2 U'
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C11) \\sim
Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C5) = Uanis(C8)
Uanis(C13) = Uanis(C14) = Uanis(C10) = Uanis(C12)
Uanis(C1) = Uanis(C7)
Uanis(C18) = Uanis(C19)
Uanis(C31) = Uanis(C29)
3.a Ternary CH refined with riding coordinates:
 C26(H26), C21(H21), C23(H23), C33(H33), C30(H30), C36(H36)
3.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C41(H41A,H41B), C38(H38A,H38B), C39(H39A,H39B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C1(H1), C5(H5)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C18(H18A,H18B,
 H18C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C24(H24A,H24B,H24C), C20(H20A,
 H20B,H20C), C34(H34A,H34B,H34C), C28(H28A,H28B,H28C), C25(H25A,H25B,H25C),
 C37(H37A,H37B,H37C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C), C31(H31A,H31B,H31C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.311
_oxdiff_exptl_absorpt_empirical_full_min 0.336