Magnetic communication and reactivity of a stable homometallic cation–cation trimer of pentavalent uranyl
Chatelain, Lucile; Mougel, Victor; Pécaut, Jacques; Mazzanti, Marinella; Chemical Science 3 (2012) 1075–; doi:10.1039/c2sc00782g

data_1515022
_publ_section_title
;
 Magnetic communication and reactivity of a stable homometallic
 cation--cation trimer of pentavalent uranyl
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1075
_journal_paper_doi               10.1039/c2sc00782g
_journal_volume                  3
_journal_year                    2012
_chemical_formula_sum            'C90 H77 N12 O7 U3'
_chemical_formula_weight         2152.73
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.954(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7294(13)
_cell_length_b                   16.6323(7)
_cell_length_c                   29.5917(11)
_cell_measurement_reflns_used    1722
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.8274
_cell_measurement_theta_min      3.3962
_cell_volume                     8232.7(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_details
;
1 omega -45.00 51.00 1.0000 300.0000
omega____ theta____ kappa____ phi______ frames
- -18.7175 77.0000 -120.0000 96

2 omega -40.00 -9.00 1.0000 300.0000
omega____ theta____ kappa____ phi______ frames
- -18.7175 77.0000 -30.0000 31

3 omega -9.00 77.00 1.0000 300.0000
omega____ theta____ kappa____ phi______ frames
- 16.9988 37.0000 120.0000 86

4 omega 11.00 45.00 1.0000 300.0000
omega____ theta____ kappa____ phi______ frames
- 16.9988 77.0000 -90.0000 34

5 omega -12.00 77.00 1.0000 300.0000
omega____ theta____ kappa____ phi______ frames
- 16.9988 77.0000 120.0000 89

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1477
_diffrn_reflns_av_sigmaI/netI    0.1378
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            53639
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    5.949
_exptl_absorpt_correction_T_max  0.9056
_exptl_absorpt_correction_T_min  0.4771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4132
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.454
_refine_diff_density_min         -1.579
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1016
_refine_ls_number_reflns         15282
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0768
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1614
_reflns_number_gt                9181
_reflns_number_total             15282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc00782g.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1515022