Preparation of a uranium metallacyclocumulene and its reactivity towards unsaturated organic molecules.
Zhang, Lei; Hou, Guohua; Zi, Guofu; Ding, Wanjian; Walter, Marc D.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3716–3728; doi:10.1039/c7dt00396j

data_7042325
_publ_section_title
;
 Preparation of a uranium metallacyclocumulene and its reactivity towards
 unsaturated organic molecules.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3716
_journal_page_last               3728
_journal_paper_doi               10.1039/c7dt00396j
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C58 H68 N2 U, C6 H14'
_chemical_formula_sum            'C64 H82 N2 U'
_chemical_formula_weight         1117.34
_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_block_doi                 10.5517/ccdc.csd.cc1nbcn0
_audit_creation_date             2017-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-01-24 deposited with the CCDC.
2017-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                76.408(3)
_cell_angle_beta                 88.112(3)
_cell_angle_gamma                86.399(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9194(4)
_cell_length_b                   14.2942(5)
_cell_length_c                   18.0576(5)
_cell_measurement_reflns_used    11002
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.0830
_cell_measurement_theta_min      3.9300
_cell_volume                     2733.68(16)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.821
_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    -16.00  11.00   1.00    8.00    --   12.76 -37.00  30.00   27
  2  \w    -19.00  23.00   1.00    8.00    --  -11.04 -99.00-120.00   42
  3  \w    -47.00  39.00   1.00    8.00    --   12.76 -77.00-120.00   86
  4  \w    -12.00  78.00   1.00    8.00    --   12.76  37.00-180.00   90
  5  \w    -15.00  87.00   1.00    8.00    --   12.76  77.00   0.00  102
;
_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      -0.0574535000
_diffrn_orient_matrix_UB_12      0.0203883000
_diffrn_orient_matrix_UB_13      0.0097174000
_diffrn_orient_matrix_UB_21      -0.0114694000
_diffrn_orient_matrix_UB_22      0.0196594000
_diffrn_orient_matrix_UB_23      -0.0391779000
_diffrn_orient_matrix_UB_31      -0.0283785000
_diffrn_orient_matrix_UB_32      -0.0425735000
_diffrn_orient_matrix_UB_33      -0.0021001000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25416
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.971
_diffrn_reflns_theta_min         3.291
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.009
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66889
_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    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.589
_refine_diff_density_min         -1.681
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         13062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0365P)^2^+6.4817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11453
_reflns_number_total             13062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00396j2.cif
_cod_data_source_block           compound6
_cod_depositor_comments
'Adding full bibliography for 7042322--7042330.cif.'
_cod_original_cell_volume        2733.65(17)
_cod_database_code               7042325
_chemical_oxdiff_formula         C1H1N1U1
_reflns_odcompleteness_completeness 99.78
_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. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(C15)
Uanis(C19) = Uanis(C22)
Uanis(C23) = Uanis(C26)
3.a Ternary CH refined with riding coordinates:
 C34(H34)
3.b Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C28(H28), C29(H29),
 C31(H31), C32(H32), C35(H35), C37(H37), C38(H38), C40(H40), C41(H41), C48(H48),
  C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56),
 C57(H57), C58(H58)
3.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C59(H59A,H59B,H59C),
 C64(H64A,H64B,H64C)
;
_shelx_res_checksum              13060
_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 1.328
_oxdiff_exptl_absorpt_empirical_full_min 0.768