Synthesis and Properties of Cobalt(III) Complexes of 4-Substituted Pyridine-Capped Dioxocyclams
Angela L. Reiff; Eva M. Garcia-Frutos; Jun Mo Gil; Oren P. Anderson; Louis S. Hegedus; Inorganic Chemistry 44 (2005) 9162–9174; doi:10.1021/ic050200h

data_4310142
_publ_section_title
;
Synthesis and Properties of Cobalt(III) Complexes of 4-Substituted
Pyridine-Capped Dioxocyclams
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9162
_journal_page_last               9174
_journal_paper_doi               10.1021/ic050200h
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C62 H98 Co2 N12 O24 Rh2'
_chemical_formula_weight         1719.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   39.481(8)
_cell_length_b                   39.481(8)
_cell_length_c                   14.574(4)
_cell_measurement_temperature    273(2)
_cell_volume                     19674(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1121
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37724
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.8877
_exptl_absorpt_correction_T_min  0.7367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plates
_exptl_crystal_F_000             8010
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.00043(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         5367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.400
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1186P)^2^+113.7272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1885
_refine_ls_wR_factor_ref         0.2167
_reflns_number_gt                3572
_reflns_number_total             5367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050200hsi20050204_103054_4.cif
_cod_data_source_block           lsh144m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
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 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4310142