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_4087177
_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         'C30 H38 N2 U, I'
_chemical_formula_sum            'C30 H38 I N2 U'
_chemical_formula_weight         791.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3949(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.55171(9)
_cell_length_b                   14.42242(14)
_cell_length_c                   18.30773(16)
_cell_measurement_reflns_used    7790
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.1690
_cell_measurement_theta_min      3.9010
_cell_volume                     2786.03(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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    -66.00 -26.00   1.00    1.00    --  -41.49  37.00  60.00   40
  2  \w    -66.00  27.00   1.00    1.00    --  -41.49  37.00 -30.00   93
  3  \w    -95.00 -70.00   1.00    1.00    --  -41.49 125.00 -30.00   25
  4  \w     71.00 121.00   1.00    1.00    --  107.19 -45.00  30.00   50
  5  \w     81.00 143.00   1.00    1.00    --  107.19  45.00   0.00   62
  6  \w     98.00 169.00   1.00    1.00    --  107.19 125.00-180.00   71
  7  \w    144.00 176.00   1.00    1.00    --  107.19  45.00-180.00   32
  8  \w     46.00 101.00   1.00    1.00    --  107.19 -94.00-180.00   55
  9  \w    -65.00   7.00   1.00    1.00    --  -41.74  37.00 -90.00   72
 10  \w     60.00  97.00   1.00    1.00    --   41.74  37.00-150.00   37
 11  \w     87.00 176.00   1.00    1.00    --  107.19  45.00  90.00   89
 12  \w     80.00 108.00   1.00    1.00    --  107.19 -94.00-150.00   28
 13  \w     32.00  58.00   1.00    1.00    --  107.19 -94.00-150.00   26
 14  \w     89.00 136.00   1.00    1.00    --  107.19  45.00-180.00   47
 15  \w     75.00 101.00   1.00    1.00    --  107.19 -45.00   0.00   26
;
_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      0.1270761000
_diffrn_orient_matrix_UB_12      -0.0192101000
_diffrn_orient_matrix_UB_13      -0.0381341000
_diffrn_orient_matrix_UB_21      -0.0680910000
_diffrn_orient_matrix_UB_22      0.0000696000
_diffrn_orient_matrix_UB_23      -0.0746942000
_diffrn_orient_matrix_UB_31      0.0232917000
_diffrn_orient_matrix_UB_32      0.1050544000
_diffrn_orient_matrix_UB_33      -0.0068746000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12222
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.277
_diffrn_reflns_theta_min         3.902
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.236
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56816
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_description       block
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.097
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.157
_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     317
_refine_ls_number_reflns         5434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0301P)^2^+1.7451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5029
_reflns_number_total             5434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00064_si_002.cif
_cod_data_source_block           compound14
_cod_database_code               4087177
_chemical_oxdiff_formula         C1H1N1I1U1
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30)
2.b 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)
;
_shelx_res_checksum              19958
_shelx_hkl_checksum              25634
_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 1.481
_oxdiff_exptl_absorpt_empirical_full_min 0.760