Hydronium tris(oxamide dioxime-κ^2^<i>N</i>,<i>N</i>')nickel(II) triiodide
M. Bélombé, Michel; Nenwa, Justin; Kammoe, Astride L.; Poudeu, Pierre F. P.; Acta Crystallographica Section E 62 (2006) m2583–m2585; doi:10.1107/S160053680603621X

data_2210754
_publ_section_title
;
 Hydronium tris(oxamide dioxime-\k^2^<i>N</i>,<i>N</i>')nickel(II)
 triiodide
;
_journal_coeditor_code           OM2032
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2583
_journal_page_last               m2585
_journal_paper_doi               10.1107/S160053680603621X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(H3 O) [Ni (C2 H6 N2 O2)3] I3'
_chemical_formula_moiety         'H3 O +, C6 H18 N12 Ni O6 2+, 3I -'
_chemical_formula_sum            'C6 H21 I3 N12 Ni O7'
_chemical_formula_weight         812.76
_chemical_name_systematic
;
Hydronium tris(oxamide dioxime-\k^2^N,N')nickel(II) triiodide
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   16.105(2)
_cell_length_b                   16.105(2)
_cell_length_c                   14.488(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.08
_cell_measurement_theta_min      2.03
_cell_volume                     3254.3(9)
_computing_cell_refinement       'RECIPE (Stoe & Cie, 2002)'
_computing_data_collection       'WinXpose (Stoe & Cie, 2002)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 and DIAMOND'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Stoe IPDS-II'
_diffrn_measurement_method       \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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13652
_diffrn_reflns_theta_full        35.08
_diffrn_reflns_theta_max         35.08
_diffrn_reflns_theta_min         4.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0.8
_diffrn_standards_interval_time  3
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.218
_exptl_absorpt_correction_T_max  0.678
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[X-RED32 (Stoe & Cie, 2001);
crystal description using FACEIT (Stoe & Cie, 2002);
optimization using equivalent reflections
(X-SHAPE; Stoe & Cie, 1999)]
;
_exptl_crystal_colour            pink--red
_exptl_crystal_density_diffrn    2.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Hexagonal
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.490
_refine_diff_density_min         -1.193
_refine_ls_extinction_coef       0.00016(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         1557
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0275
_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-exp(-10(sin\q/\l)^2^)]/
[\s^2^(Fo^2^)+30.9996*P+(0.0144P)^2^]
where P = (Fo^2^ + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0587
_reflns_number_gt                1461
_reflns_number_total             1557
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2032.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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 'Trigonal' changed to 'trigonal'
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        3254.4(9)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C6 H21 I3 N12 Ni1 O7'
_cod_database_code               2210754
_cod_database_fobs_code          2210754