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_1552201
_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_formula_moiety         'C68 H68 N4 O Zn, C4 H8 O'
_chemical_formula_sum            'C72 H76 N4 O2 Zn'
_chemical_formula_weight         1094.73
_chemical_name_systematic
'[5,15-bis(4-(tert-butyl)phenyl)-10,20-bis((4-(tert-butyl)phenyl)ethynyl)porphyrinato]zinc(II)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-02
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-16 deposited with the CCDC.    2019-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                96.327(2)
_cell_angle_beta                 113.100(2)
_cell_angle_gamma                102.726(2)
_cell_formula_units_Z            2
_cell_length_a                   14.3919(7)
_cell_length_b                   15.0704(7)
_cell_length_c                   15.2655(8)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    130
_cell_measurement_theta_max      70.21
_cell_measurement_theta_min      3.23
_cell_volume                     2898.5(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36414
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.273
_diffrn_reflns_theta_min         3.226
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0984 before and 0.0562 after correction.
The Ratio of minimum to maximum transmission is 0.8712.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_recrystallization_method
'The material was recrystallised from THF by slow evaporation'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.670
_refine_diff_density_min         -1.730
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         10700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1486P)^2^+1.7482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1869
_refine_ls_wR_factor_ref         0.1997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9867
_reflns_number_total             10700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02497b2.cif
_cod_data_source_block           zwp519_130k_0m
_cod_database_code               1552201
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.852
_shelx_estimated_absorpt_t_min   0.807
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H69C(0.5) H69D(0.5) H69A(0.5) H69B(0.5) H71C(0.5) H71D(0.5)
 H71A(0.5) H71B(0.5) O2(0.5) O3(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C69(H69C,
 H69D), C69(H69A,H69B), C70(H70A,H70B), C71(H71C,H71D), C71(H71A,H71B),
 C72(H72A,H72B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C8(H8), C11(H11), C13(H13), C16(H16), C18(H18), C20(H20),
 C24(H24), C25(H25), C27(H27), C28(H28), C30(H30), C32(H32), C34(H34), C36(H36),
  C37(H37), C38(H38), C39(H39), C45(H45), C46(H46), C47(H47), C55(H55), C58(H58)
3.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C56(H56A,H56B,H56C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,
 H61B,H61C), C62(H62A,H62B,H62C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C68(H68A,H68B,H68C)
;
_shelx_res_checksum              83195
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'