Di-μ-chloro-bis{[tris(2-pyridylmethyl)amine-κ^4^<i>N</i>]nickel(II)} bis(triethylammonium) tetraperchlorate
Bing Tong; Richard E. Norman; Shih-Chi Chang; Acta Crystallographica Section C 55 (1999) 1236–1238; doi:10.1107/S010827019900596X

data_2008785
_publ_section_title
;
 Di-\m-chloro-bis{[tris(2-pyridylmethyl)amine-\k^4^<i>N</i>]nickel(II)}
 bis(triethylammonium) tetraperchlorate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1236
_journal_page_last               1238
_journal_paper_doi               10.1107/S010827019900596X
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac
'(C6 H16 N)2 [Ni2 Cl4 (C18 H18 N4)2] (Cl O4)4'
_chemical_formula_moiety         'C36 H36 Cl2 N8 Ni2 4(Cl O4) 2(C6 H16 N)'
_chemical_formula_sum            'C48 H68 Cl6 N10 Ni2 O16'
_chemical_formula_weight         1371.24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 107.71(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.511(4)
_cell_length_b                   22.022(3)
_cell_length_c                   12.521(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      20.0
_cell_volume                     3023.6(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1988)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1997)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'PATTY in DIRDIF92 (Beurskens et al., 1992)'
_diffrn_ambient_temperature      294.2
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.080
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9991
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        1.25
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.672
_refine_ls_goodness_of_fit_ref   1.960
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5429
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.097
_refine_ls_R_factor_gt           0.045
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00013|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.060
_refine_ls_wR_factor_ref         0.054
_reflns_number_gt                5429
_reflns_number_total             9210
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fr1198.cif
_cod_data_source_block           FR1198
_cod_depositor_comments
;

2017-04-24
Formula fixed to be consistent with Z value and molecular weight.
                 miguel
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_cod_original_formula_sum            'C24 H34 Cl3 N5 Ni O8'
_cod_original_cell_volume        3024.0(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2008785