Bis{bis[5-<i>tert</i>-butyl-2-oxido-3-(1-pyridiniomethyl)phenyl]methane}dioxouranium bis(trifluoromethanesulfonate) pyridine disolvate: a uranyl bis(diphenoxide) complex resulting from homooxacalixarene cleavage
Salmon, Lionel; Thuéry, Pierre; Ephritikhine, Michel; Masci, Bernardo; Acta Crystallographica Section C 60 (2004) m27–m29; doi:10.1107/S0108270103027513

data_2013754
_publ_section_title
;Bis{bis[5-<i>tert</i>-butyl-2-oxido-3-(1-pyridiniomethyl)phenyl]methane}dioxouranium
 bis(trifluoromethanesulfonate) pyridine disolvate: a uranyl bis(diphenoxide)
 complex resulting from homooxacalixarene cleavage
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m27
_journal_page_last               m29
_journal_paper_doi               10.1107/S0108270103027513
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac
'[U O2 (C33 H38 N2 O2)2] (C F3 O3 S)2 , 2C5 H5 N'
_chemical_formula_moiety         'C66 H76 N4 O6 U 2+ ,2C F3 O3 S - , 2C5 H5 N'
_chemical_formula_sum            'C78 H86 F6 N6 O12 S2 U'
_chemical_formula_weight         1715.68
_chemical_name_systematic
;
Bis{bis[5-tert-butyl-2-oxido-3-(1-pyridiniomethyl)phenyl]methane}dioxouranium
bis(trifluoromethanesulfonate) pyridine disolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                102.472(6)
_cell_angle_beta                 106.903(6)
_cell_angle_gamma                94.800(6)
_cell_formula_units_Z            1
_cell_length_a                   10.7189(9)
_cell_length_b                   11.1479(13)
_cell_length_c                   17.0975(16)
_cell_measurement_reflns_used    13391
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.54
_cell_volume                     1885.0(3)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'EvalCCD (Duisenberg et al., 2003)'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.089
_diffrn_reflns_av_sigmaI/netI    0.149
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13391
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.288
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.54
_refine_diff_density_min         -2.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         6934
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.087
_refine_ls_R_factor_gt           0.051
_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^)+(0.0328P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.087
_refine_ls_wR_factor_ref         0.096
_reflns_number_gt                5444
_reflns_number_total             6934
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa1040.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               2013754
_cod_database_fobs_code          2013754