Controlling conformations and physical properties of meso-tetrakis(phenylethynyl)porphyrins by ring fusion: synthesis, properties and structural characterizations
Shen, Zhen; Uno, Hidemitsu; Shimizu, Yusuke; Ono, Noboru; Organic & Biomolecular Chemistry 2 (2004) 3442–3447; doi:10.1039/b412688b

data_7153544
_publ_section_title
;
 Controlling conformations and physical properties of
 meso-tetrakis(phenylethynyl)porphyrins by ring fusion: synthesis,
 properties and structural characterizations
;
_journal_issue                   23
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              3442
_journal_page_last               3447
_journal_paper_doi               10.1039/b412688b
_journal_volume                  2
_journal_year                    2004
_chemical_formula_moiety         'C78 H60 N4 O2 Zn '
_chemical_formula_sum            'C78 H60 N4 O2 Zn'
_chemical_formula_weight         1150.74
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 117.893(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.864(8)
_cell_length_b                   11.647(2)
_cell_length_c                   18.709(5)
_cell_measurement_reflns_used    6770
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     5944(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  'SHELXL-97 and PLATON SQUEEZE'
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.9834
_diffrn_measured_fraction_theta_max 0.9834
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       w
_diffrn_radiation_type           'Mo Ka'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0667
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29851
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  0.9681
_exptl_absorpt_correction_T_min  0.8352
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Higashi, T. (1999). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6725
_refine_ls_number_restraints     368
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1429
_refine_ls_R_factor_gt           0.1022
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[s^2^(Fo^2^)+(0.1857P)^2^+3.2778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2950
_refine_ls_wR_factor_ref         0.3209
_reflns_number_gt                3899
_reflns_number_total             6725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b412688bsup1.cif
_cod_data_source_block           '__Zn-1/2MeOH'
_cod_original_cell_volume        5944(3)
_cod_original_sg_symbol_Hall     -c_2yc
_cod_original_sg_symbol_H-M      c_1_2/c_1
_cod_original_formula_sum        'C78 H60 N4 O2 Zn '
_cod_database_code               7153544