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_4304183
_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         '2(C33 H24 Cl2 Co N9 O3 Zn), C2 H3 N'
_chemical_formula_sum            'C68 H51 Cl4 Co2 N19 O6 Zn2'
_chemical_formula_weight         1620.72
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 129.8370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.283(3)
_cell_length_b                   14.2505(13)
_cell_length_c                   22.139(2)
_cell_measurement_reflns_used    6381
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.84
_cell_measurement_theta_min      2.34
_cell_volume                     7578.5(12)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35634
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    1.258
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS;Bruker-2000
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.099
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         6723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1222P)^2^+24.0756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2082
_refine_ls_wR_factor_ref         0.2225
_reflns_number_gt                5892
_reflns_number_total             6744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7016424-file005_3.cif
_cod_data_source_block           Complex3
_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               4304183