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_2007088
_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          '[Pd (C11 H26 N4)] [I3]2'
_chemical_formula_moiety         'C11 H26 N4 Pd 2+, 2I3 -'
_chemical_formula_sum            'C11 H26 I6 N4 Pd'
_chemical_formula_weight         1082.2
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                99.03(9)
_cell_angle_beta                 101.14(9)
_cell_angle_gamma                107.43(10)
_cell_formula_units_Z            1
_cell_length_a                   7.787(7)
_cell_length_b                   9.173(9)
_cell_length_c                   9.382(6)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    150
_cell_measurement_theta_max      16.5
_cell_measurement_theta_min      13.0
_cell_volume                     610.6(11)
_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, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measurement_device
;
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    0.0225
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2146
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.84
_diffrn_standards_decay_%        4.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.346
_exptl_absorpt_correction_T_max  0.392
_exptl_absorpt_correction_T_min  0.204
_exptl_absorpt_correction_type   '\y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.943
_exptl_crystal_density_meas      ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         '1.51 (0.83\%A from I1)'
_refine_diff_density_min         '-1.84 (0.84\%A from I1)'
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.154
_refine_ls_goodness_of_fit_obs   1.145
_refine_ls_hydrogen_treatment    'H atoms placed using riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2146
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.154
_refine_ls_restrained_S_obs      1.143
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_obs          .0503
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.032P)^2^+11.04P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1133
_refine_ls_wR_factor_obs         .1044
_reflns_number_observed          1863
_reflns_number_total             2146
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ha1203.cif
_cod_data_source_block           2
_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 (4 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^)+(0.032P)^2^+11.04P] 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^)+(0.032P)^2^+11.04P] 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        610.6(9)
_cod_database_code               2007088