Synthesis and Characterization of Azobenzene-Confined Porphyrins
Maike V. Peters; Richard Goddard; Stefan Hecht; Journal of Organic Chemistry 71 (2006) 7846–7849; doi:10.1021/jo0612877

data_4021988
_publ_section_title
;
 Synthesis and Characterization of Azobenzene-Confined Porphyrins
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7846
_journal_page_last               7849
_journal_paper_doi               10.1021/jo0612877
_journal_volume                  71
_journal_year                    2006
_chemical_compound_source        acetonitrile
_chemical_formula_moiety         'C67 H57 N9 O9 Zn, 2.25(C2 H3 N)'
_chemical_formula_sum            'C71.5 H63.75 N11.25 O9 Zn'
_chemical_formula_weight         1289.96
_chemical_melting_point          ?
_chemical_name_systematic
; 
 5-(2,6-di(phenylazo)-phenyl)-10,15,20-tri(2,4,6-
 trimethoxyphenyl)-porphyrin-acetonitrile-zinc(ii) 
 acetonitrile solute
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0
_cell_angle_beta                 103.509(6)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   16.481(2)
_cell_length_b                   27.466(4)
_cell_length_c                   14.888(2)
_cell_measurement_reflns_used    1815
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.90
_cell_measurement_theta_min      3.19
_cell_volume                     6552.8(17)
_computing_cell_refinement       'PROTEUM2 (Bruker AXS, 2004)'
_computing_data_collection       'PROTEUM2 (Bruker AXS, 2004)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker AXS X8 Proteum'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'focusing multilayer optic'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1404
_diffrn_reflns_av_sigmaI/netI    0.1102
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19323
_diffrn_reflns_theta_full        35.24
_diffrn_reflns_theta_max         35.24
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.669297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker AXS (2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             2694
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00045(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         2746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1676
_refine_ls_R_factor_gt           0.0953
_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^)+(0.1526P)^2^+46.9169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2339
_refine_ls_wR_factor_ref         0.2852
_reflns_number_gt                1609
_reflns_number_total             2746
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo0612877si20060622_085501.cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'unknown' was changed to '?' - the
value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 21/c'
_cod_original_formula_sum        'C71.50 H63.75 N11.25 O9 Zn'
_cod_database_code               4021988