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_4322212
_publ_section_title
;
 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            'C48 H52 La N3 O20'
_chemical_formula_weight         1129.84
_chemical_name_systematic
; 
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                95.145(13)
_cell_angle_beta                 97.282(10)
_cell_angle_gamma                92.32(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2791(13)
_cell_length_b                   13.371(3)
_cell_length_c                   20.137(3)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      19.89
_cell_measurement_theta_min      2.23
_cell_volume                     2464.9(8)
_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      203(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  0.0623
_diffrn_reflns_av_sigmaI/netI    0.1059
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7841
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        34.78
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.404
_exptl_absorpt_correction_T_max  0.147
_exptl_absorpt_correction_T_min  0.066
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            'Pale blue/green'
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       needles
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.270
_refine_diff_density_min         -2.262
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.0014(2)
_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   1.082
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         7309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_obs          0.0819
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1116P)^2^+9.2708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2248
_refine_ls_wR_factor_obs         0.1982
_reflns_number_observed          5633
_reflns_number_total             7316
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990200f_1.cif
_cod_data_source_block           LH9703
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1116P)^2^+9.2708P] 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^)+(0.1116P)^2^+9.2708P] 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        2464.8(8)
_cod_original_formula_sum        'C48 H52 N3 O20 La'
_cod_database_code               4322212