Synthesis and Characterization of Uranyl Compounds with Iminodiacetate and Oxydiacetate Displaying Variable Denticity
J. Jiang; M. J. Sarsfield; J. C. Renshaw; F. R. Livens; D. Collison; J. M. Charnock; M. Helliwell; H. Eccles; Inorganic Chemistry 41 (2002) 2799–2806; doi:10.1021/ic020121v

data_4317988
_publ_section_title
;
 Synthesis and Characterization of Uranyl Compounds with Iminodiacetate
 and Oxydiacetate Displaying Variable Denticity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2799
_journal_page_last               2806
_journal_paper_doi               10.1021/ic020121v
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C10 H22 N4 O9 U'
_chemical_formula_weight         580.33
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_cell_angle_alpha                90
_cell_angle_beta                 107.75(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.024(9)
_cell_length_b                   7.462(4)
_cell_length_c                   12.467(6)
_cell_measurement_reflns_used    1
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      38.2
_cell_measurement_theta_min      38.2
_cell_volume                     1685.5(15)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00600
_diffrn_orient_matrix_UB_12      -0.01408
_diffrn_orient_matrix_UB_13      -0.07652
_diffrn_orient_matrix_UB_21      -0.05483
_diffrn_orient_matrix_UB_22      0.00383
_diffrn_orient_matrix_UB_23      -0.03448
_diffrn_orient_matrix_UB_31      0.00203
_diffrn_orient_matrix_UB_32      0.13322
_diffrn_orient_matrix_UB_33      -0.00703
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.02558
_diffrn_reflns_av_sigmaI/netI    0.040
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            1923
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         79.73
_diffrn_reflns_theta_min         3.72
_diffrn_standards_decay_%        -0.86
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    28.047
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.287
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1096.00
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.85
_refine_diff_density_min         -3.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.622
_refine_ls_goodness_of_fit_obs   2.741
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1606
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_obs          0.0442
_refine_ls_shift/esd_max         0.0010
_refine_ls_shift/esd_mean        0.0180
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0492
_refine_ls_wR_factor_obs         0.0475
_reflns_number_observed          1606
_reflns_number_total             1868
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic020121v_4.cif
_cod_data_source_block           C10H22N4O9U
_cod_depositor_comments
;
 Correcting the data name order in the GEOM_TORSION loop.

 Antanas Vaitkus,
 2018-08-08

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00002|Fo|^2^]' 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) + 0.00002|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1685(1)
_cod_original_sg_symbol_H-M      'C 2/m      '
_cod_original_formula_sum        'C10 H22 N4 O9 U '
_cod_database_code               4317988