Synthesis, Spectral, and Structural Studies of Porphyrins Having Sterically Hindered [η5-CpCo(η4-C4Ph4)] Cobalt Sandwich Units at the Meso Positions
Karunesh Keshav; Dheeraj Kumar; Anil J. Elias; Inorganic Chemistry 52 (2013) 12351–12366; doi:10.1021/ic401099c

data_4336514
_publ_contact_author_address
;DEPARTMENT OF CHEMISTRY
INDIAN INSTITUTE OF TECHNOLOGY DELHI
HAUZ KHAS, NEW DELHI 110016
INDIA
;
_publ_contact_author_email       elias@chemistry.iitd.ac.in
_publ_contact_author_fax         +91-11-26581504
_publ_contact_author_name        'Prof.Anil J. Elias'
_publ_contact_author_phone       +91-11-26591504
_publ_section_title
;
 Synthesis, Spectral, and Structural Studies of Porphyrins Having
 Sterically Hindered [\h5-CpCo(\h4-C4Ph4)] Cobalt Sandwich Units at the
 Meso Positions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12351
_journal_page_last               12366
_journal_paper_doi               10.1021/ic401099c
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C63 H45 Co Fe N4'
_chemical_formula_sum            'C63 H45 Co Fe N4'
_chemical_formula_weight         972.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.541(10)
_cell_angle_beta                 89.485(11)
_cell_angle_gamma                76.647(10)
_cell_formula_units_Z            2
_cell_length_a                   11.483(5)
_cell_length_b                   12.921(5)
_cell_length_c                   19.322(8)
_cell_measurement_temperature    293(2)
_cell_volume                     2741(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0840
_diffrn_reflns_av_sigmaI/netI    0.2548
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13474
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       block
_exptl_crystal_F_000             1008.0
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.165
_platon_squeeze_details
;
;
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         9506
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.2161
_refine_ls_R_factor_gt           0.1257
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3082
_refine_ls_wR_factor_ref         0.3542
_reflns_number_gt                3607
_reflns_number_total             9640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401099c_si_002_7.cif
_cod_data_source_block           9
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4336514