Crystal structure of 5,10,15-triphenyl-20-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)porphyrin
Senge, Mathias O.; Eckhardt, Hans-Georg; Acta Crystallographica Section E 70 (2014) o1085–o1086; doi:10.1107/S1600536814019680

data_2239970
_publ_section_title
;
 Crystal structure of
 5,10,15-triphenyl-20-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)porphyrin
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1085
_journal_page_last               o1086
_journal_paper_doi               10.1107/S1600536814019680
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C44 H37 B N4 O2'
_chemical_formula_moiety         'C44 H37 B N4 O2'
_chemical_formula_sum            'C44 H37 B N4 O2'
_chemical_formula_weight         664.59
_chemical_name_systematic
;
5,10,15-Triphenyl-20-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)porphyrin
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.353(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0758(5)
_cell_length_b                   10.5245(4)
_cell_length_c                   27.1358(10)
_cell_measurement_reflns_used    9566
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.76
_cell_measurement_theta_min      4.05
_cell_volume                     3501.2(2)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2005)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2005)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2005)'
_computing_molecular_graphics
;
<i>XP</i> in <i>SHELXTL</i> (Sheldrick, 2008) and
<i>DIAMOND</i> (Brandenburg, 1998)
;
_computing_publication_material  '<i>SHELXTL-Plus</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25108
_diffrn_reflns_theta_full        66.78
_diffrn_reflns_theta_max         66.78
_diffrn_reflns_theta_min         4.04
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.8154
_exptl_absorpt_correction_T_min  0.7508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2005)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triangle
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.271
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0402P)^2^+2.0737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                5788
_reflns_number_total             5993
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lx2293sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2239970
_cod_database_fobs_code          2239970