Enhanced charge transport via d(δ)-p(π) conjugation in Mo<sub>2</sub>-integrated single-molecule junctions.
Meng, Miao; Tang, Zheng; Mallick, Suman; Luo, Ming Hui; Tan, Zhibing; Liu, Jun-Yang; Shi, Jia; Yang, Yang; Liu, Chun Y.; Hong, Wenjing; Nanoscale 12 (2020) 10320–10327; doi:10.1039/d0nr00195c

data_1557783
_publ_section_title
;
 Enhanced charge transport via d(\d)-p(\p) conjugation in
 Mo<sub>2</sub>-integrated single-molecule junctions.
;
_journal_issue                   18
_journal_name_full               Nanoscale
_journal_page_first              10320
_journal_page_last               10327
_journal_paper_doi               10.1039/d0nr00195c
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         '2(C42 H39.5 Mo2 N6 O8), 2(C H2 Cl2)'
_chemical_formula_sum            'C86 H83 Cl4 Mo4 N12 O16'
_chemical_formula_weight         2066.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-12-04 deposited with the CCDC.	2020-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.726(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.1713(5)
_cell_length_b                   14.8958(4)
_cell_length_c                   22.0423(12)
_cell_measurement_reflns_used    6170
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.1120
_cell_measurement_theta_min      3.0190
_cell_volume                     4770.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -14.00  21.00   0.50    4.00    --    0.00 -57.00 150.00   70
  2  \w    -19.00  88.00   0.50    4.00    --    0.00  57.00-150.00  214
  3  \w    -83.00 -50.00   0.50    4.00    --    0.00 -57.00   0.00   66
  4  \w     -1.00  26.00   0.50    4.00    --    0.00  19.00-180.00   54
  5  \w    -34.00  -7.00   0.50    4.00    --    0.00 -57.00   0.00   54
  6  \w     76.00 116.00   0.50   35.00    --   95.20 -61.00  30.00   80
  7  \w     77.00 159.00   0.50   35.00    --   95.20  45.00   0.00  164
  8  \w      6.00 110.00   0.50   35.00    --   95.20 -45.00-150.00  208
  9  \w    122.00 184.00   0.50   35.00    --   95.20  45.00 -30.00  124
 10  \w     77.00 104.00   0.50   35.00    --   95.20  45.00 120.00   54
 11  \w     33.00 109.00   0.50   35.00    --   95.20 -45.00  60.00  152
 12  \w     76.00 185.00   0.50   35.00    --   95.20  45.00  90.00  218
 13  \w     22.00 102.00   0.50   35.00    --   95.20 -30.00  90.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0635353000
_diffrn_orient_matrix_UB_12      -0.0399079000
_diffrn_orient_matrix_UB_13      -0.0615738000
_diffrn_orient_matrix_UB_21      -0.0846174000
_diffrn_orient_matrix_UB_22      0.0358008000
_diffrn_orient_matrix_UB_23      0.0176216000
_diffrn_orient_matrix_UB_31      0.0054716000
_diffrn_orient_matrix_UB_32      0.0884957000
_diffrn_orient_matrix_UB_33      -0.0350434000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26351
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.212
_diffrn_reflns_theta_min         3.041
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.789
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       plate
_exptl_crystal_F_000             1047
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.586
_refine_diff_density_min         -1.490
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         9419
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.1024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1154P)^2^+40.0567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2697
_refine_ls_wR_factor_ref         0.2860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6841
_reflns_number_total             9419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nr00195c2.cif
_cod_data_source_block           Mo2_INA
_cod_depositor_comments
'Adding full bibliography for 1557783--1557784.cif.'
_cod_database_code               1557783
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-C1S = Cl2-C1S = Cl3-C2S = Cl4-C2S
 1.78 with sigma of 0.02
 Cl1-Cl2 = Cl3-Cl4
 2.78 with sigma of 0.02
 C14-O1 = C14-O1A
 1.35 with sigma of 0.02
 O1-C17 = O1A-C17A
 1.42 with sigma of 0.02
 C14-C17 = C14-C17A
 2.35 with sigma of 0.02
3. Rigid bond restraints
 C14, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl4, Cl5
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Cl4 \\sim Cl5: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
: with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Same fragment restrains
{Cl1, C1S, Cl2} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl3, C2S, Cl4}
{Cl1, C1S, Cl2} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl5, C3S, Cl6}
{Cl1, C1S, Cl2} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl7, C4S, Cl8}
6. Others
 Fixed Sof: O1(0.5) C17(0.5) H17D(0.5) H17E(0.5) H17F(0.5) O1A(0.5) C17A(0.5)
 Cl1(0.25) C1S(0.25) H1SA(0.25) H1SB(0.25) Cl2(0.25) Cl3(0.25) C2S(0.25)
 H2SA(0.25) H2SB(0.25) Cl4(0.25) Cl5(0.25) C3S(0.25) H3SA(0.25) H3SB(0.25)
 Cl6(0.25) Cl7(0.25) C4S(0.25) H4SA(0.25) H4SB(0.25) Cl8(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB)
7.b Me refined with riding coordinates:
 C17(H17D,H17E,H17F), C17A(H17A,H17B,H17C)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15),
 C16(H16), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C30(H30), C32(H32),
  C33(H33), C35(H35), C36(H36), C40(H40), C42(H42), C43(H43), C45(H45),
 C46(H46), C50(H50)
7.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              177
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.973
_oxdiff_exptl_absorpt_empirical_full_min 0.692