Molecular and electronic structure of terminal and alkali metal-capped uranium(V) nitride complexes
David M. King; Peter A. Cleaves; Ashley J. Wooles; Benedict M. Gardner; Nicholas F. Chilton; Floriana Tuna; William Lewis; Eric J. L. McInnes; Stephen T. Liddle; Nature Communications 7 (2016) 13773–; doi:10.1038/ncomms13773

data_1548085
_publ_section_title
;
 Molecular and electronic structure of terminal and alkali metal-capped
 uranium(V) nitride complexes
;
_journal_name_full               'Nature Communications'
_journal_page_first              13773
_journal_paper_doi               10.1038/ncomms13773
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C66 H150 Li2 N10 Si6 U2'
_chemical_formula_sum            'C66 H150 Li2 N10 Si6 U2'
_chemical_formula_weight         1742.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 140.685(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.092(2)
_cell_length_b                   15.8045(2)
_cell_length_c                   22.2156(12)
_cell_measurement_reflns_used    17136
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.5620
_cell_measurement_theta_min      3.3600
_cell_volume                     8251(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3271
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
  1 omega  -92.00  -36.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000   60.0000 56
  2 omega  -47.00   32.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -90.0000 79
  3 omega   -6.00   22.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5073  -57.0000   90.0000 28
  4 omega   16.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5073   57.0000   90.0000 93
  5 omega   31.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -94.0000  150.0000 68
  6 omega   41.00  108.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -94.0000   60.0000 67
  7 omega  104.00  138.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526   45.0000 -150.0000 34
  8 omega   30.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -30.0000  -60.0000 58
  9 omega   44.00   93.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -45.0000   30.0000 49
 10 omega   62.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -45.0000  120.0000 26
 11 omega   58.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -30.0000 -120.0000 32
 12 omega   30.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -30.0000 -150.0000 60
 13 omega   95.00  153.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  125.0000    0.0000 58
 14 omega   15.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5073   57.0000  -90.0000 94
 15 omega   15.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5073   57.0000    0.0000 94
 16 omega   15.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5073   57.0000 -180.0000 94
 17 omega   82.00  177.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526   30.0000  -30.0000 95
;
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0577698000
_diffrn_orient_matrix_UB_12      0.0409142000
_diffrn_orient_matrix_UB_13      0.0896787000
_diffrn_orient_matrix_UB_21      0.0291002000
_diffrn_orient_matrix_UB_22      -0.0870167000
_diffrn_orient_matrix_UB_23      0.0322597000
_diffrn_orient_matrix_UB_31      0.0105928000
_diffrn_orient_matrix_UB_32      0.0159360000
_diffrn_orient_matrix_UB_33      -0.0538150000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27178
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.101
_diffrn_reflns_theta_min         3.370
_diffrn_source                   'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.100
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.1226
_exptl_crystal_size_mid          0.0902
_exptl_crystal_size_min          0.0838
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7775
_reflns_number_total             8290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'DIRECT' changed to 'direct'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_atom_sites_solution_secondary' value 'DIFMAP' changed to 'difmap'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        8251.2(14)
_cod_database_code               1548085
_chemical_oxdiff_formula         'C66 H150 N10 Li2 Si6 U2'
_chemical_oxdiff_usercomment
'UDKIOH #12470 IN FOMBLIN FILM ON MIRCOMOUNT FOR DMK/STL'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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:
 C15(H15), C4(H4), C12(H12), C29(H29), C18(H18), C23(H23), C7(H7), C26(H26),
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C32(H32A,H32B), C33(H33A,H33B), C22(H22A,H22B), C21(H21A,
 H21B), C10(H10A,H10B)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C5(H5A,H5B,H5C), C31(H31A,H31B,
 H31C), C28(H28A,H28B,H28C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C30(H30A,
 H30B,H30C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C19(H19A,H19B,H19C),
 C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C9(H9A,H9B,H9C), C14(H14A,H14B,H14C),
  C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              26239
_shelx_hkl_checksum              44175
_olex2_submission_special_instructions 'No special instructions were received'