Beta-Octakis(methylthio)porphycenes: synthesis, characterisation and third order nonlinear optical studies
Anup Rana; Sangsu Lee; Dongho Kim; Pradeepta K. Panda; Chem.Commun. 51 (2015) 7705–; doi:10.1039/C5cc02279G

data_7117050
_publ_section_title
;
 Beta-Octakis(methylthio)porphycenes: synthesis, characterisation and
 third order nonlinear optical studies
;
_journal_name_full               Chem.Commun.
_journal_page_first              7705
_journal_paper_doi               10.1039/C5cc02279G
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C28 H28 N4 S8, O'
_chemical_formula_sum            'C28 H28 N4 O S8'
_chemical_formula_weight         693.02
_chemical_name_common            porphycene
_chemical_name_systematic
; 
 2,3,6,7,12,13,16,17-octa(methylthio)porphycene 
;
_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
_audit_update_record
;
2015-03-04 deposited with the CCDC.
2015-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.92(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8402(17)
_cell_length_b                   14.927(3)
_cell_length_c                   23.777(5)
_cell_measurement_reflns_used    1486
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.9440
_cell_measurement_theta_min      3.1950
_cell_volume                     3114.7(11)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.30a (release 13-01-2014 CrysAlis171 .NET)
(compiled Jan 13 2014,18:40:09)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.30a (release 13-01-2014 CrysAlis171 .NET)
(compiled Jan 13 2014,18:40:09)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.30a (release 13-01-2014 CrysAlis171 .NET)
(compiled Jan 13 2014,18:40:09)
;
_computing_molecular_graphics
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_sigmaI/netI    0.1513
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12561
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.30a (release 13-01-2014 CrysAlis171 .NET)
(compiled Jan 13 2014,18:40:09)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'blue purple'
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1676
_refine_ls_R_factor_gt           0.0752
_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^)+(0.0473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1793
_reflns_number_gt                2547
_reflns_number_total             5515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc02279g2.cif
_cod_data_source_block           OTMPo
_cod_original_cell_volume        3114.9(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7117050