From thioether substituted porphyrins to sulfur linked porphyrin dimers: an unusual S/NΑr via thiolate displacement?
Aoife A. Ryan; Shane Plunkett; Aoife Casey; Thomas McCabe; Mathias O. Senge; Chem.Commun. 50 (2014) 353–; doi:10.1039/c3cc46828c

data_7110189
_publ_section_title
;
 From thioether substituted porphyrins to sulfur linked porphyrin dimers:
 an unusual S/N\Ar via thiolate displacement?
;
_journal_name_full               Chem.Commun.
_journal_page_first              353
_journal_paper_doi               10.1039/c3cc46828c
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C79.5 H56 N8 O2.5 S Zn2'
_chemical_formula_weight         1326.12
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Bis{Methanol(10,15,20-triphenylporphyrinato-5-
yl)zinc(II)}sulfide 
;
_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                99.9990(10)
_cell_angle_beta                 103.4040(10)
_cell_angle_gamma                93.3760(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2362(6)
_cell_length_b                   15.0184(7)
_cell_length_c                   17.9322(9)
_cell_measurement_reflns_used    8591
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      2.32
_cell_volume                     3140.0(3)
_computing_cell_refinement       'SAINT v7.12 (Bruker, 2005)'
_computing_data_collection       'Apex2 v1.0-27 (Bruker, 2005)'
_computing_data_reduction        'SAINT v7.12 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL 5.1, XP (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      104(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26768
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  0.7894
_exptl_absorpt_correction_T_min  0.7258
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program SADABS (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1370
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         5.992
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         10863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0855
_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^)+(0.0980P)^2^+24.5641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2093
_refine_ls_wR_factor_ref         0.2226
_reflns_number_gt                8742
_reflns_number_total             10863
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc46828c.txt
_cod_data_source_block           ms551c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'n/d' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/d' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C79.50 H56 N8 O2.50 S Zn2'
_cod_database_code               7110189