Lanthanide Complexes of 3-Diphenylamino-4-hydroxycyclobut-3-ene-1,2-dione (Diphenylaminosquarate)
Bert D. Alleyne; Leonard St. Bernard; Hema Jaggernauth; Lincoln A. Hall; Ian Baxter; Andrew J. P. White; David J. Williams; Inorganic Chemistry 38 (1999) 3774–3778; doi:10.1021/ic990200f

data_4322216
_publ_section_title
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 Lanthanide Complexes of 3-Diphenylamino-4-hydroxycyclobut-3-ene-1,2-dione
 (Diphenylaminosquarate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3774
_journal_page_last               3778
_journal_paper_doi               10.1021/ic990200f
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C16 H13 N O4'
_chemical_formula_weight         283.27
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.062(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7460(7)
_cell_length_b                   26.450(2)
_cell_length_c                   6.9099(6)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      10.58
_cell_volume                     1414.8(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2280
_diffrn_reflns_theta_max         63.99
_diffrn_reflns_theta_min         3.34
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5329
_exptl_absorpt_correction_type   'Lamina [0 0 1]'
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       plates
_exptl_crystal_F_000             592
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0046(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.063
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1961
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.076
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_obs          0.0608
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1164P)^2^+0.3468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1918
_refine_ls_wR_factor_obs         0.1754
_reflns_number_observed          1687
_reflns_number_total             2089
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990200f_5.cif
_cod_data_source_block           LH9804
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1164P)^2^+0.3468P] 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^)+(0.1164P)^2^+0.3468P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322216