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_4318361
_publ_section_title
;
 Polynuclear Complexes of the Pendent-Arm Ligand
 1,4,7-Tris(acetophenoneoxime)-1,4,7-triazacyclononane
;
_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_analytical
'[C60 H68 N12 O6 Co3]2+,(ClO4)2-,H2O,EtO2,C3H5O'
_chemical_formula_sum            'C67 H86 Cl2 Co3 N12 O18'
_chemical_formula_weight         1595.17
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 104.57(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.442(2)
_cell_length_b                   17.302(2)
_cell_length_c                   17.263(2)
_cell_measurement_reflns_used    42637
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.00
_cell_volume                     6776.6(13)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius Kappa-CCD'
_diffrn_measurement_method       '\w-scan,129 imagesa 1.0 deg/240 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  0.0951
_diffrn_reflns_av_sigmaI/netI    0.1222
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18081
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_type   'MulScanAbs,Platon Program Suite 1999'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       opaque
_exptl_crystal_F_000             3324
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.017
_refine_ls_goodness_of_fit_obs   1.112
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         6562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_restrained_S_obs      1.112
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_obs          0.0630
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+25.6999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1449
_refine_ls_wR_factor_obs         0.1192
_reflns_number_observed          4043
_reflns_number_total             6619
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011322m_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0432P)^2^+25.6999P] 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^)+(0.0432P)^2^+25.6999P] 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               4318361