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_4329394
_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 Mo N4 O3'
_chemical_formula_sum            'C51 H33 Mo N4 O3'
_chemical_formula_weight         845.75
_chemical_name_systematic
;
 ?
;
_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                87.880(5)
_cell_angle_beta                 79.550(5)
_cell_angle_gamma                77.144(5)
_cell_formula_units_Z            2
_cell_length_a                   10.300(5)
_cell_length_b                   11.185(5)
_cell_length_c                   17.380(5)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.21
_cell_volume                     1919.7(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 0.980
_diffrn_measured_fraction_theta_max 0.977
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.1187
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10342
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.394
_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            green
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       cubic
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.550
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0805
_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^)+(0.1182P)^2^+0.2551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2490
_reflns_number_gt                4914
_reflns_number_total             7003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3008377_si_001_1.cif
_cod_data_source_block           25decam
_cod_database_code               4329394