Unravelling the conductance path through single-porphyrin junctions
El Abbassi, Maria; Zwick, Patrick; Rates, Alfredo; Stefani, Davide; Prescimone, Alessandro; Mayor, Marcel; van der Zant, Herre S. J.; Dulić, Diana; Chemical Science  (2019) –; doi:10.1039/C9SC02497B

data_1552205
_publ_section_title
;
 Unravelling the conductance path through single-porphyrin junctions
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02497B
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_compound_source        'Patrick Zwick'
_chemical_formula_moiety         'C52 H58 N5 Si2'
_chemical_formula_sum            'C52 H58 N5 Si2'
_chemical_formula_weight         809.24
_chemical_name_systematic
5,15-dimesityl-10,20-bis((trimethylsilyl)ethynyl)porphyrin
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2018-05-04
_audit_creation_method           CRYSTALS_ver_14.61_build_6720
_audit_update_record
;
2019-04-16 deposited with the CCDC.    2019-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.887(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2455(5)
_cell_length_b                   14.4419(6)
_cell_length_c                   14.4390(6)
_cell_measurement_reflns_used    8255
_cell_measurement_temperature    123
_cell_measurement_theta_max      68
_cell_measurement_theta_min      3
_cell_volume                     2310.16(17)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11091
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         67.680
_diffrn_reflns_theta_min         3.107
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             866
_exptl_crystal_recrystallization_method
; 
THF / MeOH
;
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.10
_refine_diff_density_min         -0.47
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 1766 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.491(17)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9484
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         6075
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.0004387
_refine_ls_shift/su_mean         0.0000251
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 3.44 4.45 1.18 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1446
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1446
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              10
_reflns_limit_k_min              -16
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                5607
_reflns_number_total             6115
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0641
_oxford_refine_ls_scale          0.13945(7)
_oxford_reflns_number_all        6075
_oxford_structure_analysis_title 'ZWP403_123K_0m in P2(1)'
_cod_data_source_file            c9sc02497b2.cif
_cod_data_source_block           ZWP403_123K
_cod_original_sg_symbol_H-M      'P 21 '
_cod_database_code               1552205
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_hooft_y                  0.488(19)
_oxford_bijvoet_difference       0.491(17)
_oxford_refined_flack_x          0.43(4)