Diaquadibenzoatobis[2-(4-pyridyl-κ<i>N</i>)-4,4,5,5-tetramethylimidazoline-1-oxyl 3-oxide]nickel(II)
Qihua Zhao; Xiaofeng Wang; Ruibin Fang; Tiekink, Edward R. T.; Acta Crystallographica Section E 59 (2003) m719–m721; doi:10.1107/S160053680301585X

data_2202689
_publ_section_title
;Diaquadibenzoatobis[2-(4-pyridyl-\k<i>N</i>)-4,4,5,5-tetramethylimidazoline-1-oxyl
 3-oxide]nickel(II)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m719
_journal_page_last               m721
_journal_paper_doi               10.1107/S160053680301585X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ni (C7 H5 O2)2 (C12 H16 N3 O2)2 (H2 O1)2]'
_chemical_formula_moiety         'C38 H46 N6 Ni O10'
_chemical_formula_sum            'C38 H46 N6 Ni O10'
_chemical_formula_weight         805.52
_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                86.319(2)
_cell_angle_beta                 87.290(2)
_cell_angle_gamma                79.486(2)
_cell_formula_units_Z            1
_cell_length_a                   6.7001(3)
_cell_length_b                   11.3354(6)
_cell_length_c                   12.8740(6)
_cell_measurement_reflns_used    2446
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      2.4
_cell_volume                     958.73(8)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHEXLTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'PATTY in DIRDIF92 (Beurskens et al., 1992)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker AXS SMART CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_sigmaI/netI    0.054
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8055
_diffrn_reflns_theta_full        30.0
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000; Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         5468
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.062
_refine_ls_R_factor_gt           0.049
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0644P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.116
_refine_ls_wR_factor_ref         0.123
_reflns_number_gt                4462
_reflns_number_total             5468
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6086.cif
_cod_data_source_block           I
_cod_database_code               2202689
_cod_database_fobs_code          2202689