Uranium(III) Coordination Chemistry and Oxidation in a Flexible Small-Cavity Macrocycle
Arnold, Polly L.; Farnaby, Joy H.; Gardiner, Michael G.; Love, Jason B.; Organometallics 34 (2015) 2114–; doi:10.1021/om5012193

data_4085359
_publ_section_title
;
 Uranium(III) Coordination Chemistry and Oxidation in a Flexible
 Small-Cavity Macrocycle
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2114
_journal_paper_doi               10.1021/om5012193
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C56 H40 B2 F20 N2 U, C7 H8'
_chemical_formula_sum            'C63 H48 B2 F20 N2 U'
_chemical_formula_weight         1472.68
_chemical_name_systematic
;
 ?
;
_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   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                76.775(4)
_cell_angle_beta                 76.666(4)
_cell_angle_gamma                66.029(3)
_cell_formula_units_Z            2
_cell_length_a                   12.5995(5)
_cell_length_b                   14.4004(5)
_cell_length_c                   17.7411(9)
_cell_measurement_reflns_used    3237
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      22.1150
_cell_measurement_theta_min      3.5120
_cell_volume                     2828.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    ortep
_computing_publication_material  mercury
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 16.1042
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.1523
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27382
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.908
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.5507
_exptl_crystal_size_mid          0.1057
_exptl_crystal_size_min          0.0426
_refine_diff_density_max         2.200
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         12953
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.001
_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^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8784
_reflns_number_total             12953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5012193_si_001.cif
_cod_data_source_block           p13171a
_cod_depositor_comments
'Adding full bibliography for 4085357--4085359.cif.'
_cod_database_code               4085359
_shelx_estimated_absorpt_t_min   0.93840
_shelx_estimated_absorpt_t_max   1.00000
_shelxl_version_number           2014-3
_shelx_res_checksum              10721
_shelx_hkl_checksum              99886