Cobalt Coordination Induced Functionalized Molecular Clefts: Isolation of {CoIII-ZnII} Heterometallic Complexes and Their Applications in Beckmann Rearrangement Reactions
Anurag Mishra; Afsar Ali; Shailesh Upreti; Rajeev Gupta; Inorganic Chemistry 47 (2008) 154–161; doi:10.1021/ic7016424

data_4304181
_publ_contact_author_address
;
Department of Chemistry 
University of Delhi
Delhi - 110 007
INDIA
;
_publ_contact_author_email       'rgupta@chemistry.du.ac.in '
_publ_contact_author_fax         '91 11 2766 6605'
_publ_contact_author_name        'Dr. Rajeev Gupta'
_publ_contact_author_phone       '91 11 2666 7624'
_publ_section_title
;
Cobalt Coordination Induced Functionalized Molecular Clefts: Isolation of
{CoIII-ZnII} Heterometallic Complexes and Their Applications in Beckmann
Rearrangement Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              154
_journal_page_last               161
_journal_paper_doi               10.1021/ic7016424
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C33 H24 Co N9 O3, C3 H7 N O'
_chemical_formula_sum            'C36 H31 Co N10 O4'
_chemical_formula_weight         726.64
_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                 90.567(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.808(5)
_cell_length_b                   14.788(5)
_cell_length_c                   25.216(5)
_cell_measurement_reflns_used    3918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.41
_cell_volume                     3284(2)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0759
_diffrn_reflns_av_sigmaI/netI    0.1043
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21871
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS;Bruker-2000
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.109
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1792
_refine_ls_wR_factor_ref         0.1946
_reflns_number_gt                5321
_reflns_number_total             8083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7016424-file005_1.cif
_cod_data_source_block           Complex1
_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.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed to
'constr' 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      'P 21/n'
_cod_database_code               4304181