1,4-Diazoniabicyclo[2.2.2]octane triaquatrichloronickelate(II) chloride monohydrate
Bremner, Colin A.; Harrison, William T. A.; Acta Crystallographica Section E 59 (2003) m797–m799; doi:10.1107/S1600536803018555

data_2202300
_publ_section_title
;
 1,4-Diazoniabicyclo[2.2.2]octane triaquatrichloronickelate(II)
 chloride monohydrate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m797
_journal_page_last               m799
_journal_paper_doi               10.1107/S1600536803018555
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '(C6 H14 N2) [Ni Cl3 (H2 O)3] Cl, H2 O'
_chemical_formula_moiety         'C6 H14 N2 2+, Cl3 H6 Ni O3 1-, H2 O, Cl 1-'
_chemical_formula_sum            'C6 H22 Cl4 N2 Ni O4'
_chemical_formula_weight         386.77
_chemical_name_systematic        ?
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   'difmap (O-H) and geom (N-H and C-H)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.70190(10)
_cell_length_b                   11.9573(2)
_cell_length_c                   18.0923(4)
_cell_measurement_reflns_used    6654
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1449.86(5)
_computing_cell_refinement       COLLECT
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        COLLECT
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and ATOMS (Shape software, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f'
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10211
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.24
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.079
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            'bright green'
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.780
_refine_ls_abs_structure_details 'Flack (1983), 1395 Friedel pairs'
_refine_ls_abs_structure_Flack   0.478(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0414P)^2^+0.3311P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                3224
_reflns_number_total             3303
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br6114.cif
_cod_data_source_block           I
_cod_database_code               2202300
_cod_database_fobs_code          2202300