Molecular Conformation and Intermolecular Interactions in the Crystal Structures of Free-Base 5,15-Diarylporphyrins
Bond, Andrew D.; Feeder, Neil; Redman, James E.; Teat, Simon J.; Sanders, Jeremy K. M.; Crystal Growth & Design 2 (2002) 27–; doi:10.1021/cg010029u

data_4505768
_publ_section_title
;
 Molecular Conformation and Intermolecular Interactions in the Crystal
 Structures of Free-Base 5,15-Diarylporphyrins
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              27
_journal_paper_doi               10.1021/cg010029u
_journal_volume                  2
_journal_year                    2002
_chemical_formula_moiety         'C62 H82 N4 O2'
_chemical_formula_sum            'C62 H82 N4 O2'
_chemical_formula_weight         915.32
_chemical_name_systematic
; 
 5,15-bis(3-methoxyphenyl)-2,8,12,18-tetrahexyl-3,7,13,17-tetramethylporphyrin 
;
_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
_cell_angle_alpha                81.20(1)
_cell_angle_beta                 75.28(1)
_cell_angle_gamma                86.76(1)
_cell_formula_units_Z            1
_cell_length_a                   7.998(1)
_cell_length_b                   12.450(1)
_cell_length_c                   14.476(1)
_cell_measurement_reflns_used    7435
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.59
_cell_measurement_theta_min      3.67
_cell_volume                     1377.5(2)
_computing_cell_refinement       'Bruker SAINT (Bruker AXS, 1994)'
_computing_data_collection       'Bruker SMART (Bruker AXS, 1994)'
_computing_data_reduction        'Bruker SAINT (Bruker AXS, 1994)'
_computing_molecular_graphics    'XP (Sheldrick, 1993)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.816
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'Thin slice \w-scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Beamline ID11, ESRF'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.5062
_diffrn_reflns_av_R_equivalents  0.1417
_diffrn_reflns_av_sigmaI/netI    0.1841
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11789
_diffrn_reflns_theta_full        19.59
_diffrn_reflns_theta_max         19.59
_diffrn_reflns_theta_min         3.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.9996
_exptl_absorpt_correction_T_min  0.9957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Correction applied by SADABS - note that the transmission factors are
 not real since they include corrections for beam decay and possibly
 crystal decay (the two cannot be distinguished).

 The numbers listed in the CIF are those calculated by SHELXL. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1344
_refine_ls_R_factor_gt           0.0866
_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^)+(0.1134P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2102
_refine_ls_wR_factor_ref         0.2270
_reflns_number_gt                3105
_reflns_number_total             5478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg010029u.cif
_cod_data_source_block           js9921
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4505768