Solid-State Synthesis of Molybdenum and Tungsten Porphyrins and Aerial Oxidation of Coordinated Benzenethiolate to Benzenesulfonate
Goutam Nandi; Sabyasachi Sarkar; Inorganic Chemistry 51 (2012) 6412–6420; doi:10.1021/ic3008377

data_4329396
_publ_contact_author_address
;Department of Chemistry
Indian Institute of Technology Kanpur
Kanpur, U.P.
India - 208016
;
_publ_contact_author_email       abya@iitk.ac.in
_publ_contact_author_fax         915122597265
_publ_contact_author_name        'Sabyasachi Sarkar'
_publ_contact_author_phone       915122597265
_publ_section_title
;
 Solid-State Synthesis of Molybdenum and Tungsten Porphyrins and Aerial
 Oxidation of Coordinated Benzenethiolate to Benzenesulfonate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6412
_journal_page_last               6420
_journal_paper_doi               10.1021/ic3008377
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C44 H28 Mo N4 O'
_chemical_formula_sum            'C44 H28 Mo N4 O'
_chemical_formula_weight         724.64
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   13.328(5)
_cell_length_b                   13.328(5)
_cell_length_c                   9.624(5)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      2.16
_cell_volume                     1709.6(13)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'Diamond 3.1e'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       '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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4549
_diffrn_reflns_theta_full        25.46
_diffrn_reflns_theta_max         25.46
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       Block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.424
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.424
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+8.8167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1428
_reflns_number_gt                833
_reflns_number_total             848
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3008377_si_001_3.cif
_cod_data_source_block           20novbm
_cod_database_code               4329396