Small-Molecule Activation Mediated by a Uranium Bipyridyl Metallocene
Zhang, Lei; Zhang, Congcong; Hou, Guohua; Zi, Guofu; Walter, Marc D.; Organometallics  (2017) –; doi:10.1021/acs.organomet.7b00064

data_4087176
_publ_section_title
;
 Small-Molecule Activation Mediated by a Uranium Bipyridyl Metallocene
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.7b00064
_journal_year                    2017
_chemical_formula_moiety         'C70 H92 N4 O4 U2, 2(C6 H6)'
_chemical_formula_sum            'C82 H104 N4 O4 U2'
_chemical_formula_weight         1685.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7962(3)
_cell_length_b                   16.9274(5)
_cell_length_c                   36.1586(12)
_cell_measurement_reflns_used    8746
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.5810
_cell_measurement_theta_min      3.4960
_cell_volume                     7220.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6254
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.893
_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    -31.00  10.00   1.00    3.00    --   12.45 -37.00   0.00   41
  2  \w     49.00  75.00   1.00    3.00    --   12.45  37.00   0.00   26
  3  \w     67.00  92.00   1.00    3.00    --   12.45  19.00-150.00   25
  4  \w     36.00  63.00   1.00    3.00    --   12.45 178.00  30.00   27
  5  \w    -50.00  38.00   1.00    3.00    --   12.45 -57.00 120.00   88
  6  \w     42.00  99.00   1.00    3.00    --   12.45-178.00 120.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0016991000
_diffrn_orient_matrix_UB_12      -0.0206776000
_diffrn_orient_matrix_UB_13      -0.0170448000
_diffrn_orient_matrix_UB_21      0.0265122000
_diffrn_orient_matrix_UB_22      0.0324451000
_diffrn_orient_matrix_UB_23      -0.0089137000
_diffrn_orient_matrix_UB_31      0.0539455000
_diffrn_orient_matrix_UB_32      -0.0166132000
_diffrn_orient_matrix_UB_33      0.0038335000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            47368
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.806
_diffrn_reflns_theta_min         3.381
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.533
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
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    1.551
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.688
_refine_diff_density_min         -1.862
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         9246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0125P)^2^+11.6271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5353
_reflns_number_total             9246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00064_si_002.cif
_cod_data_source_block           compound13b
_cod_database_code               4087176
_chemical_oxdiff_formula         C1H1N1O1U1
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C28(H28), C29(H29), C30(H30)
2.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C36(H36), C37(H37),
 C38(H38), C39(H39), C40(H40), C41(H41)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C33(H33A,H33B,H33C), C35(H35A,H35B,
 H35C)
;
_shelx_res_checksum              3835
_shelx_hkl_checksum              19751
_shelx_shelxl_version_number     2014/7
_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 1.286
_oxdiff_exptl_absorpt_empirical_full_min 0.770