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_4310143
_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            'C88 H114 Co2 N20 O12 Ru'
_chemical_formula_weight         1862.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.127(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0984(12)
_cell_length_b                   11.8549(12)
_cell_length_c                   29.740(3)
_cell_measurement_reflns_used    3126
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.78
_cell_measurement_theta_min      2.42
_cell_volume                     4211.5(7)
_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      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0874
_diffrn_reflns_av_sigmaI/netI    0.0842
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            34284
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.8931
_exptl_absorpt_correction_T_min  0.7832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       rods
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.0047(4)
_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   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         8598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1327
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.868
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+29.5213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1855
_refine_ls_wR_factor_ref         0.2090
_reflns_number_gt                5609
_reflns_number_total             8598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050200hsi20050204_103054_5.cif
_cod_data_source_block           lsh146m
_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 
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_cod_database_code               4310143