Synthesis and Structures of Polymeric Mn, Co, Cu, and Zn Complexes of 3-Diphenylamino-4-hydroxycyclobut-3-ene-1,2-dione (Diphenylaminosquarate) and of the Salt [Ni(H2O)6][(C6H5)2NC4O3]2.2H2O
Avril R. Williams; Bert D. Alleyne; Lincoln A. Hall; Andrew J. P. White; David J. Williams; Laurence K. Thompson; Inorganic Chemistry 39 (2000) 5265–5270; doi:10.1021/ic000390q

data_4321545
_publ_section_title
;
 Synthesis and Structures of Polymeric Mn, Co, Cu, and Zn Complexes of
 3-Diphenylamino-4-hydroxycyclobut-3-ene-1,2-dione (Diphenylaminosquarate)
 and of the Salt [Ni(H2O)6][(C6H5)2NC4O3]2.2H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5265
_journal_page_last               5270
_journal_paper_doi               10.1021/ic000390q
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C32 H24 Cu N2 O8'
_chemical_formula_weight         628.07
_chemical_name_systematic
; 
 ? 
;
_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                 98.178(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2091(7)
_cell_length_b                   10.8984(5)
_cell_length_c                   9.3291(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      21
_cell_volume                     1329.34(12)
_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       'Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3318
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       plates
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.074
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3012
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.164
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_obs          0.0347
_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^)+(0.0517P)^2^+0.7157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1159
_refine_ls_wR_factor_obs         0.0943
_reflns_number_observed          2562
_reflns_number_total             3318
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000390q_1.cif
_cod_data_source_block           LHCAN993
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.7157P] 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^)+(0.0517P)^2^+0.7157P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C32 H24 N2 O8 Cu'
_cod_database_code               4321545