Crystal structure of tris(ethylenediamine)nickel(II) diperchlorate 2-(4-pyridyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide solvate monohydrate, [Ni(C~2~H~8~N~2~)~3~][ClO~4~]~2~ · C~12~H~16~N~3~O~2~ · H~2~O
Wang, Yu-Fang; Liu, Yuan-Ying; Zeitschrift für Kristallographie - New Crystal Structures 222 (2007) 439–441; doi:

data_8102223
_publ_section_title
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Crystal structure of tris(ethylenediamine)nickel(II) diperchlorate 
2-(4-pyridyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide solvate 
monohydrate, [Ni(C~2~H~8~N~2~)~3~][ClO~4~]~2~ &#x00B7; C~12~H~16~N~3~O~2~ 
&#x00B7; H~2~O
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_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              439
_journal_page_last               441
_journal_volume                  222
_journal_year                    2007
_chemical_formula_structural
'[Ni(en)3][ClO4]2 &#x00B7; NITpPy &#x00B7; H~2~O'
_chemical_formula_sum            'C18 H42 Cl2 N9 Ni O11'
_chemical_formula_weight         690.22
_chemical_name_systematic
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tris(ethylenediamine)nickel(II) diperchlorate 
2-(4-pyridyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide 
solvate monohydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 99.292(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.897(2)
_cell_length_b                   15.461(4)
_cell_length_c                   10.407(2)
_cell_measurement_reflns_used    3743
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.47
_cell_volume                     1571.6(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       phi/omega
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9662
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.8944
_exptl_absorpt_correction_T_min  0.7909
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.779
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         6757
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0728
_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^)+(0.1323P)^2^+0.6071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.2037
_reflns_number_gt                5195
_reflns_number_total             6757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2161.cff
_cod_data_source_block           a
_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 1555 2011-01-17 13:19:09Z saulius 
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_cod_original_sg_symbol_H-M      P12(1)1
_cod_database_code               8102223