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_4505763
_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         'C44 H46 N4'
_chemical_formula_sum            'C44 H46 N4'
_chemical_formula_weight         630.85
_chemical_name_systematic
; 
 5,15-diphenyl-2,8,12,18-tetraethyl-3,7,13,17-tetramethylporphyrin, alpha form 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 104.238(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.6155(5)
_cell_length_b                   15.7605(10)
_cell_length_c                   13.1152(9)
_cell_measurement_reflns_used    1481
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.64
_cell_measurement_theta_min      2.68
_cell_volume                     1726.14(19)
_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      180(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'Thin slice \w-scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS, Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6904
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5919
_diffrn_reflns_theta_full        28.94
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         2.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.9986
_exptl_absorpt_correction_T_min  0.9958
_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    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1028P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1474
_reflns_number_gt                1801
_reflns_number_total             2361
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg010029u.cif
_cod_data_source_block           cam132
_cod_original_sg_symbol_H-M      I2/m
_cod_database_code               4505763