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_4321546
_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 H26 Co N2 O9'
_chemical_formula_weight         641.48
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.753(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2113(9)
_cell_length_b                   11.0383(8)
_cell_length_c                   18.7484(12)
_cell_measurement_temperature    150.0(1)
_cell_volume                     2709.1(3)
_computing_cell_refinement       'Denzo-SMN (Nonius, 1997)'
_computing_data_collection       'KappaCCD server software'
_computing_data_reduction        'Denzo-SMN (Nonius, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  'Bruker SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f 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  0.102
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17338
_diffrn_reflns_theta_full        26.47
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0011(8)
_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_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         5536
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+2.7127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1363
_reflns_number_gt                3904
_reflns_number_total             5536
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000390q_2.cif
_cod_data_source_block           k98158
_cod_database_code               4321546