Polynuclear Complexes of the Pendent-Arm Ligand 1,4,7-Tris(acetophenoneoxime)-1,4,7-triazacyclononane
Vitaly Pavlishchuk; Frank Birkelbach; Thomas Weyhermüller; Karl Wieghardt; Phalguni Chaudhuri; Inorganic Chemistry 41 (2002) 4405–4416; doi:10.1021/ic011322m

data_4318362
_publ_section_title
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 Polynuclear Complexes of the Pendent-Arm Ligand
 1,4,7-Tris(acetophenoneoxime)-1,4,7-triazacyclononane
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4405
_journal_page_last               4416
_journal_paper_doi               10.1021/ic011322m
_journal_volume                  41
_journal_year                    2002
_chemical_formula_structural     '[C90 H102 N18 Ni4 O9]2+, 2 (ClO4)-, 3 H2O'
_chemical_formula_sum            'C90 H108 Cl2 N18 Ni4 O20'
_chemical_formula_weight         2067.68
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.248(3)
_cell_length_b                   21.248(3)
_cell_length_c                   21.248(3)
_cell_measurement_reflns_used    4432
_cell_measurement_temperature    100(2)
_cell_volume                     9593(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '83 frames a 1 deg./w and 600 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating Mo-anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16100
_diffrn_reflns_theta_max         24.65
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.432
_exptl_absorpt_correction_type   'DELREFABS, Platon99, A.L. Spek, Utrecht, NL'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             4320
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         5411
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.100
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_obs          0.0697
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+16.4751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2040
_refine_ls_wR_factor_obs         0.1745
_reflns_number_observed          4333
_reflns_number_total             5434
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011322m_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+16.4751P] 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^)+(0.1050P)^2^+16.4751P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4318362