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_4329395
_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         'C51 H33 N4 O3 W'
_chemical_formula_sum            'C51 H33 N4 O3 W'
_chemical_formula_weight         933.66
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                87.777(5)
_cell_angle_beta                 79.837(5)
_cell_angle_gamma                77.322(5)
_cell_formula_units_Z            2
_cell_length_a                   10.341(5)
_cell_length_b                   11.124(5)
_cell_length_c                   17.438(5)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      1.88
_cell_volume                     1926.3(14)
_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 0.979
_diffrn_measured_fraction_theta_max 0.975
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10316
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    3.051
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       Needle
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.154
_refine_diff_density_min         -1.689
_refine_diff_density_rms         0.355
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0588
_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^)+(0.1052P)^2^+4.8701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1805
_reflns_number_gt                6087
_reflns_number_total             7008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3008377_si_001_2.cif
_cod_data_source_block           12mardm
_cod_database_code               4329395