Tris(1,10-phenanthroline)nickel(II) di-μ-iodo-bis(diiodomercurate) <i>N</i>,<i>N</i>-dimethylformamide solvate monohydrate
Hua Fang; Xuya Dai; Acta Crystallographica Section E 62 (2006) m3565–m3566; doi:10.1107/S160053680605032X

data_2211339
_publ_section_title
;
 Tris(1,10-phenanthroline)nickel(II) di-\m-iodo-bis(diiodomercurate)
 <i>N</i>,<i>N</i>-dimethylformamide solvate monohydrate
;
_journal_coeditor_code           CI2216
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3565
_journal_page_last               m3566
_journal_paper_doi               10.1107/S160053680605032X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ni (C12 H8 N2)3] [Hg2 I6], C3 H7 N O, H2 O'
_chemical_formula_moiety
'C36 H24 N6 Ni 2+, Hg2 I6 2-, C3 H7 N O, H2 O'
_chemical_formula_sum            'C39 H33 Hg2 I6 N7 Ni O2'
_chemical_formula_weight         1853.01
_chemical_name_systematic
;
Tris(1,10-phenanthroline)nickel(II) di-iodo-bis(diiodomercurate)
N,N'-dimethylformamide monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.846(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6312(17)
_cell_length_b                   18.756(3)
_cell_length_c                   20.197(3)
_cell_measurement_reflns_used    6415
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.17
_cell_volume                     4750.8(12)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30627
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.62
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.779
_exptl_absorpt_correction_T_max  0.2471
_exptl_absorpt_correction_T_min  0.1299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.808
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         10830
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0408
_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/[\s^2^(Fo^2^)+(0.0404P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                7281
_reflns_number_total             10830
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2216.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        4750.8(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2211339
_cod_database_fobs_code          2211339