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_4505769
_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 H76 N6, 2(C H Cl3)'
_chemical_formula_sum            'C64 H78 Cl6 N6'
_chemical_formula_weight         1144.02
_chemical_name_systematic
; 
 5,15-bis(4-cyanophenyl)-2,8,12,18-tetrahexyl-3,7,13,17-tetramethylporphyrin,
 chloroform solvate (1/2)
;
_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                107.095(3)
_cell_angle_beta                 98.703(4)
_cell_angle_gamma                92.845(4)
_cell_formula_units_Z            1
_cell_length_a                   6.9810(3)
_cell_length_b                   14.874(1)
_cell_length_c                   15.408(1)
_cell_measurement_reflns_used    7042
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.91
_cell_volume                     1504.08(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics    'XP (Sheldrick, 1993)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_sigmaI/netI    0.1031
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8074
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.53
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5249
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1547
_refine_ls_R_factor_gt           0.0967
_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^)+(0.0940P)^2^+4.2616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2142
_refine_ls_wR_factor_ref         0.2482
_reflns_number_gt                3235
_reflns_number_total             5249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg010029u.cif
_cod_data_source_block           js0019
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4505769