Tris(1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')nickel(II) hexaoxido-μ-peroxido-disulfate(VI) <i>N</i>,<i>N</i>-dimethylformamide disolvate monohydrate
Harvey, Miguel Angel; Suarez, Sebastián; Doctorovich, Fabio; Baggio, Ricardo; Acta Crystallographica Section E 69 (2013) m63–m64; doi:10.1107/S1600536812050775

data_2237116
_publ_section_title
;
 Tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')nickel(II)
 hexaoxido-\m-peroxido-disulfate(VI) <i>N</i>,<i>N</i>-dimethylformamide
 disolvate monohydrate
;
_journal_coeditor_code           BR2216
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m63
_journal_page_last               m64
_journal_paper_doi               10.1107/S1600536812050775
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Ni (C12 H8 N2)3] (S2 O8), 2C3 H7 N O, H2 O'
_chemical_formula_moiety
'C36 H24 N6 Ni, (S2 O8), 2(N C3 H7 O), (H2 O)'
_chemical_formula_sum            'C42 H40 N8 Ni O11 S2'
_chemical_formula_weight         955.65
_chemical_name_systematic
;
Tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')nickel(II)
hexaoxido-\m-peroxido-disulfate(VI)
<i>N</i>,<i>N</i>-dimethylformamide disolvate monohydrate
;
_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-97
_cell_angle_alpha                79.691(3)
_cell_angle_beta                 76.725(3)
_cell_angle_gamma                76.190(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4832(3)
_cell_length_b                   12.2221(4)
_cell_length_c                   18.0044(6)
_cell_measurement_reflns_used    11752
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.8281
_cell_measurement_theta_min      3.6907
_cell_volume                     2161.41(12)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'Oxford Diffraction Gemini CCD S Ultra'
_diffrn_measurement_method       '\w scans, thick slices'
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31646
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.89
_diffrn_reflns_theta_min         3.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2009)'
_exptl_crystal_colour            light_brown
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.728
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         10070
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.318
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0960P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                6165
_reflns_number_total             10070
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br2216.cif
_cod_data_source_block           I
_cod_database_code               2237116
_cod_database_fobs_code          2237116