Core-Modified, meso-Alkylidenyl Porphyrins and Their Expanded Analogues: A New Family of Nonplanar Porphyrinoids
Seung-Doo Jeong; Seong-Jin Hong; Kee Jong Park; Sihyun Ham; Jonathan L. Sessler; Vincent Lynch; Chang-Hee Lee; Journal of Organic Chemistry 72 (2007) 6232–6240; doi:10.1021/jo070872k

data_4024094
_publ_section_title
;
 Core-Modified, meso-Alkylidenyl Porphyrins and Their Expanded Analogues:
 A New Family of Nonplanar Porphyrinoids
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6232
_journal_page_last               6240
_journal_paper_doi               10.1021/jo070872k
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety         'C96 H84 N4 O18, C H2 Cl2'
_chemical_formula_sum            'C97 H86 Cl2 N4 O18'
_chemical_formula_weight         1666.68
_chemical_name_systematic
; 
 ? 
;
_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                66.749(1)
_cell_angle_beta                 85.227(1)
_cell_angle_gamma                63.118(1)
_cell_formula_units_Z            2
_cell_length_a                   16.3542(3)
_cell_length_b                   17.9863(3)
_cell_length_c                   18.0871(4)
_cell_measurement_reflns_used    13298
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     4330.46(14)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0735
_diffrn_reflns_av_sigmaI/netI    0.1652
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25745
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0028(4)
_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   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1134
_refine_ls_number_reflns         14809
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1919
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.1540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1834
_reflns_number_gt                6616
_reflns_number_total             14809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo070872ksi20070427_112258.cif
_cod_data_source_block           oxbzph
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4024094