Synthesis and Electrochemical Properties of Transition Metal Complexes of 2,2':6',2''-Terpyridine 1,1''-Dioxide
Kaname Ito; Toshi Nagata; Koji Tanaka; Inorganic Chemistry 40 (2001) 6331–6333; doi:10.1021/ic010883a

data_4320621
_publ_section_title
;
 Synthesis and Electrochemical Properties of Transition Metal Complexes of
 2,2':6',2''-Terpyridine 1,1''-Dioxide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6331
_journal_page_last               6333
_journal_paper_doi               10.1021/ic010883a
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C30 H22 Cl2 N6 Ni O12'
_chemical_formula_weight         788.14
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Tue Jan 24 01:18:27 2001'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 97.27(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.304(2)
_cell_length_b                   10.065(2)
_cell_length_c                   19.783(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      17.3
_cell_measurement_theta_min      15.1
_cell_volume                     3022.8(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.02777
_diffrn_orient_matrix_UB_12      -0.03150
_diffrn_orient_matrix_UB_13      -0.04025
_diffrn_orient_matrix_UB_21      -0.05973
_diffrn_orient_matrix_UB_22      -0.01567
_diffrn_orient_matrix_UB_23      -0.02564
_diffrn_orient_matrix_UB_31      -0.00065
_diffrn_orient_matrix_UB_32      0.09291
_diffrn_orient_matrix_UB_33      -0.01796
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  3.43
_diffrn_reflns_av_sigmaI/netI    0.081
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6083
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        -1.17
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1608.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.58
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.803
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     460
_refine_ls_number_reflns         3430
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0584
_refine_ls_shift/esd_max         0.0003
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00226|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1050
_reflns_number_observed          3430
_reflns_number_total             5816
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ic010883a_2.cif
_cod_data_source_block           Ni(terpyO2)2.(ClO4)2
_cod_depositor_comments
;
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 'w = 1/[\s^2^(Fo) +
0.00226|Fo|^2^]' 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) + 0.00226|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3022.9(8)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C30 H22 Cl2 N6 O12 Ni '
_cod_database_code               4320621