Chemistry of Constrained Dioxocyclam Ligands with Co(III): Unusual Examples of C-H and C-N Bond Cleavage
Chuanjiang Hu; Robert M. Chin; Thoi D. Nguyen; Khoi T. Nguyen; Paul S. Wagenknecht; Lawrence C. Nathan; Inorganic Chemistry 42 (2003) 7602–7607; doi:10.1021/ic0302027

data_4312471
_publ_contact_author_address
;
         Department of Chemistry
         San Jose State University
         San Jose, CA 95192
;
_publ_contact_author_email       pwagen@jupiter.sjsu.edu
_publ_contact_author_fax         408-924-4945
_publ_contact_author_name        'Paul S. Wagenknecht'
_publ_contact_author_phone       408-924-5008
_publ_section_title
;
 Chemistry of Constrained Dioxocyclam Ligands with Co(III): Unusual
 Examples of C-H and C-N Bond Cleavage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7602
_journal_page_last               7607
_journal_paper_doi               10.1021/ic0302027
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C13 H23 Co N4 O3, 3 (H2 O), 2 (H O0.50)'
_chemical_formula_sum            'C13 H31 Co N4 O7'
_chemical_formula_weight         414.35
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           'Siemens SHELXTL v. 5.03 1994'
_cell_angle_alpha                90.00
_cell_angle_beta                 105.115(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.824(2)
_cell_length_b                   9.189(2)
_cell_length_c                   11.3108(13)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    298
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      4.92
_cell_volume                     1788.4(5)
_computing_cell_refinement       'Siemens XSCANS v. 2.2 1995'
_computing_data_collection       'Siemens XSCANS v. 2.2 1995'
_computing_data_reduction        'Siemens XSCANS v. 2.2 1995'
_computing_molecular_graphics    'Siemens SHELXTL v. 5.03 1994'
_computing_publication_material  'Siemens SHELXTL v. 5.03 1994'
_computing_structure_refinement  'Siemens SHELXTL v. 5.03 1994'
_computing_structure_solution    'Siemens SHELXTL v. 5.03 1994'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Siemens Bruker AXS P4'
_diffrn_measurement_method       '\w 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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2088
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
' S.Parkin,et.al.,J.Appl.Crystallog.,1995,28,53-56'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       pillar
_exptl_crystal_F_000             880.0
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0028(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     ' SHELXL v. 5.03  1994'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1679
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+2.0112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                1466
_reflns_number_total             1679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0302027_1.cif
_cod_data_source_block           1
_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 
;
_cod_database_code               4312471