Bis(acetonitrile-<i>N</i>)(1,4,8,12-tetraazacyclopentadecane)nickel(II) Bis(triiodide) and (1,4,8,12-Tetraazacyclopentadecane)palladium(II) Bis(triiodide)
Blake, Alexander J.; Li, Wan-Sheung; Lippolis, Vito; Schröder, Martin; Acta Crystallographica Section C 54 (1998) 299–302; doi:10.1107/S0108270197014200

data_2007087
_publ_section_title
;
 Bis(acetonitrile-<i>N</i>)(1,4,8,12-tetraazacyclopentadecane)nickel(II)
 Bis(triiodide) and (1,4,8,12-Tetraazacyclopentadecane)palladium(II)
 Bis(triiodide)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              299
_journal_page_last               302
_journal_paper_doi               10.1107/S0108270197014200
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[Ni (C2 H3 N)2 (C11 H26 N4)] (I3)2'
_chemical_formula_moiety         'C15 H32 N6 Ni 2+, 2I3 -'
_chemical_formula_sum            'C15 H32 I6 N6 Ni'
_chemical_formula_weight         1116.58
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.05(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.885(6)
_cell_length_b                   18.689(4)
_cell_length_c                   9.452(3)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    150
_cell_measurement_theta_max      20.1
_cell_measurement_theta_min      13.5
_cell_volume                     2975.3(16)
_computing_cell_refinement       STADI4
_computing_data_collection       'STADI4 (Stoe & Cie, 1996a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1995)'
_computing_publication_material  SHELXL96
_computing_structure_refinement  'SHELXL96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measurement_device_type
;
Stoe Stadi-4 four-circle diffractometer with Oxford Cryosystems open-flow
cryostat (Cosier & Glazer, 1986)
;
_diffrn_measurement_method       \w/\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2631
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        'variation +- 2'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.892
_exptl_absorpt_correction_T_max  0.305
_exptl_absorpt_correction_T_min  0.103
_exptl_absorpt_correction_type   '\y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.493
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.15
_refine_diff_density_max         '1.37 (0.92\%A from I3)'
_refine_diff_density_min         '-1.21 (0.94\%A from I1)'
_refine_ls_abs_structure_details 'Flack  (1983)'
_refine_ls_abs_structure_Flack   0.12(12)
_refine_ls_extinction_coef       0.000310(15)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         2631
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.042P)^2^+43.4P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                2413
_reflns_number_total             2631
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ha1203.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (11 times).

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.042P)^2^+43.4P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.042P)^2^+43.4P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2975.2(13)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2007087