Octakis(dimethylammonium) hexa-μ~2~-chlorido-hexachloridotrinickelate(II) dichloride: a linear trinickel complex with asymmetric bridging
Gerdes, Allison; Bond, Marcus R.; Acta Crystallographica Section C 65 (2009) m398–m400; doi:10.1107/S0108270109036853

data_2017321
_publ_section_title
;
 Octakis(dimethylammonium)
 hexa-\m~2~-chlorido-hexachloridotrinickelate(II) dichloride: a linear
 trinickel complex with asymmetric bridging
;
_journal_coeditor_code           DN3125
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m398
_journal_page_last               m400
_journal_paper_doi               10.1107/S0108270109036853
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '(C2 H8 N)8 [Ni3 Cl12] Cl2'
_chemical_formula_moiety         '8(C2 H8 N +), Cl12 Ni3 6-, 2(Cl -)'
_chemical_formula_sum            'C16 H64 Cl14 N8 Ni3'
_chemical_formula_weight         1041.18
_chemical_name_systematic
;
Octakis(dimethylammonium) hexa-\m~2~-chlorido-hexachloridotrinickelate(II)
dichloride
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.4640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0058(2)
_cell_length_b                   20.0564(4)
_cell_length_c                   10.9787(2)
_cell_measurement_reflns_used    18336
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.294
_cell_measurement_theta_min      2.91
_cell_volume                     2201.17(7)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
HKL DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and ORTEPIII (Burnett & Johnson,
1996)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34160
_diffrn_reflns_reduction_process
;
Scaled and merged with HKL Denzo and Scalepack
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology,
Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr
& R. M. Sweet, pp. 307-326. New York: Academic Press.
;
_diffrn_reflns_theta_full        45.29
_diffrn_reflns_theta_max         45.29
_diffrn_reflns_theta_min         4.16
_exptl_absorpt_coefficient_mu    2.143
_exptl_absorpt_correction_T_max  0.635
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.764
_refine_ls_extinction_coef       0.00392(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         18194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0077P)^2^+0.5877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.047
_refine_ls_wR_factor_ref         0.0519
_reflns_number_gt                13786
_reflns_number_total             18194
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn3125.cif
_cod_data_source_block           I
_cod_database_code               2017321
_cod_database_fobs_code          2017321