Triamidoamine uranium(IV)-arsenic complexes containing one-, two- and threefold U-As bonding interactions
Benedict M. Gardner; Gabor Balazs; Manfred Scheer; Floriana Tuna; Eric J. L. McInnes; Jonathan McMaster; William Lewis; Alexander J. Blake; Stephen T. Liddle; Nature Chemistry 7 (2015) 582–590; doi:10.1038/nchem.2279

data_1551962
_publ_section_title
;
 Triamidoamine uranium(IV)-arsenic complexes containing one-, two- and
 threefold U-As bonding interactions
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              582
_journal_page_last               590
_journal_paper_doi               10.1038/nchem.2279
_journal_volume                  7
_journal_year                    2015
_chemical_formula_moiety         'C33 H77 As N4 Si3 U'
_chemical_formula_sum            'C33 H77 As N4 Si3 U'
_chemical_formula_weight         927.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2n 2a'
_space_group_name_H-M_alt        'P m c n'
_atom_sites_solution_hydrogens   'geom, Me and AsH2 from difmap'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8958(2)
_cell_length_b                   12.54925(11)
_cell_length_c                   16.04531(16)
_cell_measurement_reflns_used    84509
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      76.6850
_cell_measurement_theta_min      4.0760
_cell_volume                     4207.51(7)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'w scans'
_diffrn_orient_matrix_UB_11      0.0058133000
_diffrn_orient_matrix_UB_12      0.1168622000
_diffrn_orient_matrix_UB_13      -0.0284683000
_diffrn_orient_matrix_UB_21      -0.0555184000
_diffrn_orient_matrix_UB_22      0.0309434000
_diffrn_orient_matrix_UB_23      0.0583616000
_diffrn_orient_matrix_UB_31      0.0481468000
_diffrn_orient_matrix_UB_32      0.0214674000
_diffrn_orient_matrix_UB_33      0.0707208000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuKa
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            142576
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.026
_diffrn_reflns_theta_min         4.109
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    12.731
_exptl_absorpt_correction_T_max  0.187
_exptl_absorpt_correction_T_min  0.009
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Numerical absorption correction based on gaussian integration over a multifaceted crystal model 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    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.433
_exptl_crystal_size_mid          0.3712
_exptl_crystal_size_min          0.1921
_refine_diff_density_max         7.573
_refine_diff_density_min         -10.771
_refine_diff_density_rms         0.440
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         4558
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.1376
_refine_ls_shift/su_max          1.333
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+(0.0615P)^2^+474.9184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3172
_refine_ls_wR_factor_ref         0.3173
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4552
_reflns_number_total             4558
_reflns_threshold_expression     'I > 2s(I)'
_cod_data_source_file            nchem.2279-s2.cif
_cod_data_source_block           1
_cod_original_cell_volume        4207.50(7)
_cod_database_code               1551962
_chemical_oxdiff_formula         C33H77AsN4Si3U
_chemical_oxdiff_usercomment
'UBMGNZ #13549 SN-141 for BMG/STL in fomblin oil on micromount'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All As(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2A_$2-H2A
 -1.75 with sigma of 0.02
 H2B_$2-H2B
 -1.75 with sigma of 0.02
 C3-C2
 -2.55 with sigma of 0.02
 C10-C17_$2
 -2.2 with sigma of 0.02
 C17-C10_$2
 -2.2 with sigma of 0.02
 H14B_$2-H14B
 -1.8 with sigma of 0.02
 C13-C14
 -2.55 with sigma of 0.02
 H2C-H5B
 -1.75 with sigma of 0.02
 H5B-H2C
 -1.75 with sigma of 0.02
 H1_$2-H1
 2.2 with sigma of 0.01
 U1-H1
 3.48 with sigma of 0.02
 As1-H1
 1.54 with sigma of 0.005
 Si2-C15 sim Si2-C12
 with sigma of 0.02
 C16-C15 sim C13-C12
 with sigma of 0.02
 Si1-C7 sim Si1-C4 sim Si1-C1
 with sigma of 0.02
 C3-C1 sim C5-C4 sim C6-C4 sim C8-C7
 with sigma of 0.02
 C3-C1 sim C2-C1 sim C8-C7 sim C9-C7 sim C6-C4 sim C5-C4
 with sigma of 0.02
 C13-C12 sim C14-C12
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.0025 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.0025 and sigma
for terminal atoms of 0.005
5. Others
 Fixed Sof: C17(0.5) H17A(0.5) H17B(0.5) H18A(0.5) H18B(0.5)
6.a Ternary CH refined with riding coordinates:
 C1(H1A), C4(H4), C7(H7), C12(H12), C15(H15)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C17(H17A,H17B), C18(H18A,H18B)
6.c Me refined with riding coordinates:
 C3(H3A,H3B,H3C)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
;