Microwave Assisted Stereoselective Synthesis of Cis-Substituted TinIV Phthalocyanine Dicarboxylates. Application as Corrosion Inhibitors
Hiram I. Beltrán; Raquel Esquivel; Arturo Sosa-Sánchez; Jose L. Sosa-Sánchez; Herbert Höpfl; Victor Barba; Norberto Farfán; Mónica Galicia García; Octavio Olivares-Xometl; Luis S. Zamudio-Rivera; Inorganic Chemistry 43 (2004) 3555–3557; doi:10.1021/ic049634n

data_4311104
_publ_contact_author_address
;
Programa de Ingenier\'ia Molecular, Instituto Mexicano del Petr\'oleo,
Eje Central L\'azaro C\'ardenas 152, Col. San Bartolo Atepehuacan,
C. P. 07730, M\'exico, D. F.
;
_publ_contact_author_fax         (52)91756239
_publ_contact_author_name        'Hiram Isaac Beltr\'an Conde'
_publ_contact_author_phone       (52)91757399
_publ_section_title
;
 Microwave Assisted Stereoselective Synthesis of Cis-Substituted TinIV
 Phthalocyanine Dicarboxylates. Application as Corrosion Inhibitors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3555
_journal_page_last               3557
_journal_paper_doi               10.1021/ic049634n
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C60 H70 N8 O4 Sn1'
_chemical_formula_structural     'C60 H70 N8 O4 SN1'
_chemical_formula_sum            'C60 H70 N8 O4 Sn'
_chemical_formula_weight         1085.93
_chemical_name_common            'Compound 3b'
_chemical_name_systematic
;
Phthalocyaninato tinIV bis(tetradecanoate)2
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-04-24T17:30:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                81.983(5)
_cell_angle_beta                 89.708(5)
_cell_angle_gamma                73.359(5)
_cell_formula_units_Z            2
_cell_length_a                   9.559(5)
_cell_length_b                   11.670(5)
_cell_length_c                   25.913(5)
_cell_measurement_reflns_used    6622
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      3.183
_cell_measurement_wavelength     0.71073
_cell_volume                     2740.7(19)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.104117
_diffrn_orient_matrix_UB_12      0.237434E-1
_diffrn_orient_matrix_UB_13      0.103985E-1
_diffrn_orient_matrix_UB_21      -0.186868E-1
_diffrn_orient_matrix_UB_22      0.77812E-1
_diffrn_orient_matrix_UB_23      -0.242322E-1
_diffrn_orient_matrix_UB_31      -0.27369E-1
_diffrn_orient_matrix_UB_32      -0.393634E-1
_diffrn_orient_matrix_UB_33      -0.287316E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.072
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            13839
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         3.2
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.52
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         9026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+7.0956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1582
_reflns_number_gt                6663
_reflns_number_total             9026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049634nsi20040412_065142.cif
_cod_data_source_block           nfhb71
_cod_original_sg_symbol_H-M      'P 1'
_cod_original_formula_sum        'C60 H70 N8 O4 Sn1'
_cod_database_code               4311104