Stereochemistry and Solid-State Structure of an Intrinsically Chiral Meso-Patterned Porphyrin: Case Study by NMR and Single-Crystal X-ray Diffraction Analysis
Liguo Yang; Yang Zhou; Mengliang Zhu; Luyang Zhao; Liye Wei; Yongzhong Bian; Journal of Organic Chemistry 78 (2013) 9949–9955; doi:10.1021/jo401825k

data_4028656
_publ_section_title
;
 Stereochemistry and Solid-State Structure of an Intrinsically Chiral
 Meso-Patterned Porphyrin: Case Study by NMR and Single-Crystal X-ray
 Diffraction Analysis
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9949
_journal_page_last               9955
_journal_paper_doi               10.1021/jo401825k
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C52 H39 N5 O4 Zn, C H Cl3'
_chemical_formula_sum            'C53 H40 Cl3 N5 O4 Zn'
_chemical_formula_weight         982.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.365(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.721(3)
_cell_length_b                   13.4029(11)
_cell_length_c                   20.590(3)
_cell_measurement_reflns_used    3152
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3574
_cell_measurement_theta_min      2.8901
_cell_volume                     4668.3(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1375
_diffrn_reflns_av_sigmaI/netI    0.2518
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18407
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.8346
_exptl_absorpt_correction_T_min  0.8007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1194
_refine_ls_number_reflns         8587
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.1872
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1661
_reflns_number_gt                3633
_reflns_number_total             8587
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo401825k_si_002.cif
_cod_data_source_block           12
_cod_original_cell_volume        4668.4(10)
_cod_original_sg_symbol_Hall     P2yb
_cod_database_code               4028656