Synthesis and Crystal Structure of (μ-Malonanilide-O,O')bis[bis(dibenzoylmethanato)dioxouranium(VI)]: A New Coordination Mode of the Malonamide Ligand
Shanmugaperumal Kannan; George Ferguson; Inorganic Chemistry 36 (1997) 1724–1725; doi:10.1021/ic960626j

data_4323368
_publ_section_title
;
 Synthesis and Crystal Structure of
 (\m-Malonanilide-O,O')bis[bis(dibenzoylmethanato)dioxouranium(VI)]: A New
 Coordination Mode of the Malonamide Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1724
_journal_page_last               1725
_journal_paper_doi               10.1021/ic960626j
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C75 H58 N2 O14 U2 . C H Cl3 '
_chemical_formula_sum            'C76 H59 Cl3 N2 O14 U2'
_chemical_formula_weight         1806.66
_chemical_name_systematic
;
Bis[uranylbis(dibenzoylmethanato)]malonyldianilide 
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_date             'May 7, 1996'
_audit_creation_method
'from NRCVAX CIF routine and SHELXL93 with Word-Perfect Macro PREPSHEL'
_audit_update_record             '   May 7, 1996  Assembled, pass-1'
_cell_angle_alpha                102.467(12)
_cell_angle_beta                 90.700(11)
_cell_angle_gamma                91.701(8)
_cell_formula_units_Z            2
_cell_length_a                   10.5801(8)
_cell_length_b                   17.732(2)
_cell_length_c                   19.309(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(1)
_cell_measurement_theta_max      14.20
_cell_measurement_theta_min      10.25
_cell_volume                     3534.9(9)
_computing_cell_refinement       'Enraf-Nonius SET4 and CELDIM'
_computing_data_collection       'Enraf-Nonius CAD4 (Enraf-Nonius 1992)'
_computing_data_reduction
'DATRD2 in NRCVAX94 (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_molecular_graphics
'NRCVAX94, PLATON (Spek, 1994a) and PLUTON (Spek 1994b)'
_computing_publication_material  'NRCVAX94, SHELXL93  and WordPerfect'
_computing_structure_refinement  'NRCVAX94 and SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'Patterson Heavy-atom Method'
_diffrn_ambient_temperature      294(1)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.1523
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12391
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        3.1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.755
_exptl_absorpt_correction_T_max  0.4818
_exptl_absorpt_correction_T_min  0.2217
_exptl_absorpt_correction_type   'integration from crystal shape'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       plate
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
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_refine_diff_density_min         -0.760
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment
'riding (SHELXL defaults, C-H 0.93 to 0.98, N-H 0.86\%A)'
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_refine_ls_number_parameters     873
_refine_ls_number_reflns         12391
_refine_ls_number_restraints     486
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_refine_ls_restrained_S_obs      1.141
_refine_ls_R_factor_all          0.1436
_refine_ls_R_factor_obs          0.0558
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1095
_refine_ls_wR_factor_obs         0.0936
_reflns_number_observed          5830
_reflns_number_total             12391
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ic960626j.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0366P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3534.8(8)
_cod_database_code               4323368