Bis(tri-2-pyridylamine)nickel(II) bis(perchlorate)
Wang, Shi; He, Wenrui; Huang, Wei; Acta Crystallographica Section E 67 (2011) m78–; doi:10.1107/S1600536810051627

data_2228832
_publ_section_title
;
 Bis(tri-2-pyridylamine)nickel(II) bis(perchlorate)
;
_journal_coeditor_code           NK2079
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m78
_journal_paper_doi               10.1107/S1600536810051627
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni (C15 H12 N4)2] (Cl O4)2'
_chemical_formula_moiety         'C30 H24 N8 Ni 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C30 H24 Cl2 N8 Ni O8'
_chemical_formula_weight         754.18
_chemical_name_systematic
;
Bis(tri-2-pyridylamine)nickel(II) bis(perchlorate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.542(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.360(4)
_cell_length_b                   17.570(8)
_cell_length_c                   11.165(5)
_cell_measurement_reflns_used    7662
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.8955
_cell_measurement_theta_min      2.1845
_cell_volume                     1617.3(13)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14055
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0415P)^2^+0.1545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                2611
_reflns_number_total             3895
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            nk2079.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2228832
_cod_database_fobs_code          2228832