Enhanced Photosensitive Schottky Diode Behavior of Pyrazine over 2-Aminopyrimidine Ligand in Copper(II)-Phthalate MOFs: Experimental and Theoretical Rationalization.
Hossain, Anowar; Dey, Arka; Seth, Saikat Kumar; Ray, Partha Pratim; Ballester, Pablo; Pritchard, Robin G.; Ortega-Castro, Joaquín; Frontera, Antonio; Mukhopadhyay, Subrata; ACS omega 3 (2018) 9160–9171; doi:10.1021/acsomega.8b01111

data_4515923
_publ_section_title
;
 Enhanced Photosensitive Schottky Diode Behavior of Pyrazine over
 2-Aminopyrimidine Ligand in Copper(II)-Phthalate MOFs: Experimental and
 Theoretical Rationalization.
;
_journal_issue                   8
_journal_name_full               'ACS omega'
_journal_page_first              9160
_journal_page_last               9171
_journal_paper_doi               10.1021/acsomega.8b01111
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C40 H30 Cu2 N6 O16, 2(H2 O)'
_chemical_formula_sum            'C40 H34 Cu2 N6 O18'
_chemical_formula_weight         1013.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.253(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8505(5)
_cell_length_b                   10.4670(4)
_cell_length_c                   18.8893(9)
_cell_measurement_reflns_used    2604
_cell_measurement_temperature    150.03(10)
_cell_measurement_theta_max      26.6090
_cell_measurement_theta_min      3.8420
_cell_volume                     2069.73(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      150.03(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
  1 omega   20.00   84.00   1.0000    1.0650
omega____ theta____ kappa____ phi______ frames
    -       18.8601   57.0000  -60.0000 64

  2 omega   13.00   72.00   1.0000    1.0650
omega____ theta____ kappa____ phi______ frames
    -       18.8601   37.0000  -90.0000 59

  3 omega  -48.00   11.00   1.0000    1.0650
omega____ theta____ kappa____ phi______ frames
    -       18.8601    0.0000  -60.0000 59

  4 omega  -70.00  -30.00   1.0000    1.0650
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  135.0000   90.0000 40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9115
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.856
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         4572
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0357P)^2^+1.6827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3310
_reflns_number_total             4572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b01111_si_003.cif
_cod_data_source_block           argp1017sai
_cod_original_cell_volume        2069.73(16)
_cod_database_code               4515923
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.791
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C14A-C13A \\sim C9-C14 \\sim C14-C13 \\sim C13-C12 \\sim C13A-C12A \\sim
C12A-C11A \\sim C12-C11 ~
 C11A-C10A \\sim C11-C10 \\sim C9-C10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C14 \\sim C14A \\sim C9 \\sim C13 \\sim C13A \\sim C12 \\sim C12A \\sim C11
\\sim C11A \\sim C10A \\sim C10: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
O7 \\sim O8 \\sim C16 \\sim O8A \\sim C16A \\sim O7A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O7, O8, C16, O8A, C16A, O7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C14A, C9, C13, C13A, C12, C12A, C11, C11A, C10A, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O7A)=Sof(C16A)=Sof(O8A)=Sof(H8A)=Sof(O9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=
 Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=
 Sof(H14A)=1-FVAR(1)
 Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=
 Sof(H14)=Sof(O9)=Sof(H9A)=Sof(H9B)=Sof(C16)=Sof(O8)=Sof(H8)=Sof(O7)=FVAR(1)
6.a Free rotating group:
 O9(H9A,H9B), O9A(H9AA,H9AB)
6.b Rotating group:
 N3(H3A,H3B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14),
 C18(H18), C19(H19), C20(H20), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A)
6.d Fitted hexagon refined as free rotating group:
 C9(C10,C11,C12,C13,C14)
6.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O8(H8), O8A(H8A)
;
_shelx_res_checksum              14050
_shelx_hkl_checksum              9477
_olex2_submission_special_instructions 'No special instructions were received'