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_4087175
_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         'C39 H63 N3 U'
_chemical_formula_sum            'C39 H63 N3 U'
_chemical_formula_weight         811.95
_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             2016-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.029(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0513(3)
_cell_length_b                   20.1950(6)
_cell_length_c                   17.8977(5)
_cell_measurement_reflns_used    9404
_cell_measurement_temperature    100.2(9)
_cell_measurement_theta_max      28.4790
_cell_measurement_theta_min      3.6510
_cell_volume                     3632.98(18)
_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      100.2(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.862
_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    -17.00   9.00   1.00   15.00    --  -11.20 -99.00   0.00   26
  2  \w    -50.00 -12.00   1.00   15.00    --   12.45 -37.00-180.00   38
  3  \w    -61.00  24.00   1.00   15.00    --   12.45 -57.00-120.00   85
  4  \w    -62.00  13.00   1.00   15.00    --   12.45 -37.00 -30.00   75
  5  \w     28.00  54.00   1.00   15.00    --   12.45  57.00  60.00   26
  6  \w    -14.00  28.00   1.00   15.00    --  -11.20 -99.00  90.00   42
  7  \w    -24.00   2.00   1.00   15.00    --   12.45 -57.00  90.00   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      0.0426260000
_diffrn_orient_matrix_UB_12      -0.0090901000
_diffrn_orient_matrix_UB_13      -0.0298723000
_diffrn_orient_matrix_UB_21      0.0331990000
_diffrn_orient_matrix_UB_22      0.0308795000
_diffrn_orient_matrix_UB_23      0.0029908000
_diffrn_orient_matrix_UB_31      0.0453839000
_diffrn_orient_matrix_UB_32      -0.0140478000
_diffrn_orient_matrix_UB_33      0.0258776000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29733
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.794
_diffrn_reflns_theta_min         3.233
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67954
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.145
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         8959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+1.3540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6864
_reflns_number_total             8959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00064_si_002.cif
_cod_data_source_block           compound8
_cod_database_code               4087175
_chemical_oxdiff_formula         c1h1n1U1
_reflns_odcompleteness_completeness 99.71
_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:
 C21(H21), C28(H28), C34(H34)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
 C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B)
2.c 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              76385
_shelx_hkl_checksum              21100
_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 1.785
_oxdiff_exptl_absorpt_empirical_full_min 0.735