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_1515024
_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            'C57.5 H44.25 N8.75 O5 U2'
_chemical_formula_weight         1413.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.531(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   27.1234(13)
_cell_length_b                   27.3660(13)
_cell_length_c                   28.2322(16)
_cell_measurement_reflns_used    5782
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.2618
_cell_measurement_theta_min      3.3157
_cell_volume                     20954.7(18)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
1 omega 60.00 101.00 1.0000 160.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 179.0000 -120.0000 41

2 omega -48.00 93.00 1.0000 160.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 0.0000 30.0000 141

3 omega 61.00 101.00 1.0000 160.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 179.0000 -30.0000 40

4 omega 1.00 44.00 1.0000 160.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 0.0000 120.0000 43

;
_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  0.0764
_diffrn_reflns_av_sigmaI/netI    0.1138
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            42381
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    6.232
_exptl_absorpt_correction_T_max  0.8908
_exptl_absorpt_correction_T_min  0.2743
_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            black
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             10792
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.369
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1321
_refine_ls_number_reflns         17778
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+853.3683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1722
_reflns_number_gt                11780
_reflns_number_total             17778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc00782g.txt
_cod_data_source_block           3
_cod_original_cell_volume        20954.7(19)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C57.50 H44.25 N8.75 O5 U2'
_cod_database_code               1515024