[<i>N</i>,<i>N</i>,<i>N</i>'-Tris(3-aminopropyl)ethylenediamine-κ^5^<i>N</i>]nickel bis(perchlorate)
Xu, Tong-Tao; Xu, Xing-You; Wang, Da-Qi; Gao, Jian; Lu, Lu-De; Acta Crystallographica Section E 62 (2006) m1713–m1715; doi:10.1107/S1600536806024330

data_2209694
_publ_section_title
;[<i>N</i>,<i>N</i>,<i>N</i>'-Tris(3-aminopropyl)ethylenediamine-\k^5^<i>N</i>]nickel
 bis(perchlorate)
;
_journal_coeditor_code           WW2017
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1713
_journal_page_last               m1715
_journal_paper_doi               10.1107/S1600536806024330
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ni (C11 H29 N5)] (Cl O4)2'
_chemical_formula_moiety         'C11 H29 N5 Ni 2+, 2Cl O4 -'
_chemical_formula_sum            'C11 H29 Cl2 N5 Ni O8'
_chemical_formula_weight         489.00
_chemical_name_systematic
;
[N,N,N'-Tris(3-aminopropyl)ethylenediamine-\k^5^N]nickel 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                 90.285(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.454(4)
_cell_length_b                   14.589(7)
_cell_length_c                   14.477(7)
_cell_measurement_reflns_used    882
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      15.898
_cell_measurement_theta_min      2.567
_cell_volume                     1996.7(16)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.1202
_diffrn_reflns_av_sigmaI/netI    0.1834
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10278
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.288
_exptl_absorpt_correction_T_max  0.7919
_exptl_absorpt_correction_T_min  0.6138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue--purple
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.407
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3526
_refine_ls_number_restraints     655
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1944
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                1216
_reflns_number_total             3526
_reflns_threshold_expression     I>\s(I)
_cod_data_source_file            ww2017.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1996.6(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2209694
_cod_database_fobs_code          2209694