Two 2,5-Dihydroxy-1,4-benzoquinonate-<i>O</i>,<i>O</i>'-Containing Mononuclear Complexes: [Cu(C~6~H~2~O~4~)(C~8~H~6~N~4~)(H~2~O)].5H~2~O and [Ni(C~6~H~2~O~4~)(C~12~H~12~N~2~)~2~].H~2~O (C~8~H~6~N~4~ = 2,2'-Bipyrimidine, C~12~H~12~N~2~ = 4,4'-Dimethyl-2,2'-bipyridine)
Decurtins, S.; Schmalle, H. W.; Schneuwly, P.; Zheng, L.-M.; Acta Crystallographica Section C 52 (1996) 561–566; doi:10.1107/S0108270195010298

data_2004579
_publ_section_title
;
 Two 2,5-Dihydroxy-1,4-benzoquinonate-<i>O</i>,<i>O</i>'-Containing
 Mononuclear Complexes: [Cu(C~6~H~2~O~4~)(C~8~H~6~N~4~)(H~2~O)].5H~2~O
 and [Ni(C~6~H~2~O~4~)(C~12~H~12~N~2~)~2~].H~2~O (C~8~H~6~N~4~ =
 2,2'-Bipyrimidine, C~12~H~12~N~2~ = 4,4'-Dimethyl-2,2'-bipyridine)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              561
_journal_page_last               566
_journal_paper_doi               10.1107/S0108270195010298
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Ni (C6 H2 O4) (C12 H12 N2)2] , H2 O'
_chemical_formula_moiety         'C30 H26 N4 Ni O4,H2 O1'
_chemical_formula_sum            'C30 H28 N4 Ni O5'
_chemical_formula_weight         583.27
_chemical_name_systematic
;bis(4,4'-dimethyl-2,2'-bipyridine-N,N')(4,5-dihydroxy-1,2-benzoquinonate-O,O')-
nickel(II)
 monohydrate
;
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.942(3)
_cell_length_b                   12.942(3)
_cell_length_c                   29.326(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      16.9
_cell_measurement_theta_min      4.1
_cell_volume                     4253.9(16)
_computing_cell_refinement       'Enraf-Nonius CAD-4 software'
_computing_data_collection       'Enraf-Nonius CAD-4 software'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971), SCHAKAL (Keller)'
_computing_publication_material  'CIF (Hall et al., 1991)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \w-2\q
_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  0.1022
_diffrn_reflns_av_sigmaI/netI    0.0881
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            '9041 including 168 standards'
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        -1.1
_diffrn_standards_interval_count 400
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.8575
_exptl_absorpt_correction_T_min  0.6987
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_meas      1.36
_exptl_crystal_density_method    'flotation in ?'
_exptl_crystal_description       'hexagonal bipyramide'
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.55
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.516
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_coef       0.0016(7)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.233
_refine_ls_goodness_of_fit_obs   1.215
_refine_ls_hydrogen_treatment    'H atoms refined with a riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         2835
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.239
_refine_ls_restrained_S_obs      1.215
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_obs          0.0521
_refine_ls_shift/esd_max         -0.110
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0853P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1812
_refine_ls_wR_factor_obs         0.1259
_reflns_number_observed          1596
_reflns_number_total             2837
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bk1126.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0853P)^2^] 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^)+(0.0853P)^2^]
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        4253.9(13)
_cod_database_code               2004579