Quantifying the Exfoliation Ease Level of 2D Materials via Mechanical Anisotropy
Ji, Li-Jun; Qin, Yan; Gui, Di; Li, Wei; Li, Yanchun; Li, Xiaodong; Lu, Peixiang; Chemistry of Materials 30 (2018) 8732–; doi:10.1021/acs.chemmater.8b01082

data_4003089
_publ_section_title
;
 Quantifying the Exfoliation Ease Level of 2D Materials via Mechanical
 Anisotropy
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              8732
_journal_paper_doi               10.1021/acs.chemmater.8b01082
_journal_volume                  30
_journal_year                    2018
_chemical_formula_moiety         'C4 Cu N7 O3, C12 H28 N'
_chemical_formula_sum            'C16 H28 Cu N8 O3'
_chemical_formula_weight         444.00
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-12-01
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.141(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9601(4)
_cell_length_b                   13.1817(4)
_cell_length_c                   16.0836(4)
_cell_measurement_reflns_used    6996
_cell_measurement_temperature    300
_cell_measurement_theta_max      27.1590
_cell_measurement_theta_min      2.9420
_cell_volume                     2271.67(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7a (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9446
_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    -74.00 119.00   1.00   25.00    --   30.00  54.00 -60.00  193
  2  \w     65.00  91.00   1.00   25.00    --   30.00  54.00 -60.00   26
  3  \w    -63.00 119.00   1.00   25.00    --   30.00  54.00-120.00  182
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0461310000
_diffrn_orient_matrix_UB_12      0.0369551000
_diffrn_orient_matrix_UB_13      -0.0157087000
_diffrn_orient_matrix_UB_21      -0.0466035000
_diffrn_orient_matrix_UB_22      -0.0382040000
_diffrn_orient_matrix_UB_23      -0.0059771000
_diffrn_orient_matrix_UB_31      -0.0089369000
_diffrn_orient_matrix_UB_32      0.0083949000
_diffrn_orient_matrix_UB_33      0.0418757000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15494
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4451
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0531P)^2^+2.7842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3674
_reflns_number_total             4451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm8b01082_si_002.cif
_cod_data_source_block           ljj-1
_cod_original_cell_volume        2271.65(11)
_cod_database_code               4003089
_chemical_oxdiff_formula         'C H N Cu'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim C1A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C2 \\sim C2A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C4 \\sim C4A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C5 \\sim C5A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C7 \\sim C7A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C8 \\sim C8A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C10 \\sim C10A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C11 \\sim C11A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C3 \\sim C3A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C6 \\sim C6A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C9 \\sim C9A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C12 \\sim C12A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(N7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H3C)=FVAR(1)
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(H6AC)=1-FVAR(2)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=FVAR(2)
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(H9AC)=1-FVAR(3)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(H9C)=FVAR(3)
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=
 Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(4)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=FVAR(4)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C1A(H1AA,H1AB), C2A(H2AA,H2AB), C4(H4A,H4B), C5(H5A,
 H5B), C4A(H4AA,H4AB), C5A(H5AA,H5AB), C7(H7A,H7B), C8(H8A,H8B), C7A(H7AA,H7AB),
  C8A(H8AA,H8AB), C10(H10A,H10B), C11(H11A,H11B), C10A(H10C,H10D), C11A(H11C,
 H11D)
4.b Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C6(H6A,H6B,H6C), C6A(H6AA,H6AB,H6AC),
 C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC), C12(H12A,H12B,H12C), C12A(H12D,H12E,H12F)
;
_shelx_res_checksum              31884
_shelx_hkl_checksum              10288
_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 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.881