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_4329397
_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         'C50 H33 Mo N4 O4 S'
_chemical_formula_sum            'C50 H33 Mo N4 O4 S'
_chemical_formula_weight         881.80
_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                90.000(5)
_cell_angle_beta                 103.875(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   13.516(5)
_cell_length_b                   12.576(5)
_cell_length_c                   23.980(5)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.24
_cell_volume                     3957(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_sigmaI/netI    0.1076
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20800
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.427
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         7334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.2158
_reflns_number_gt                4636
_reflns_number_total             7334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3008377_si_001_4.cif
_cod_data_source_block           2apram
_cod_database_code               4329397