Predesigned Metal-Anchored Building Block for In Situ Generation of Pd Nanoparticles in Porous Covalent Organic Framework: Application in Heterogeneous Tandem Catalysis.
Bhadra, Mohitosh; Sasmal, Himadri Sekhar; Basu, Arghya; Midya, Siba P.; Kandambeth, Sharath; Pachfule, Pradip; Balaraman, Ekambaram; Banerjee, Rahul; ACS applied materials & interfaces 9 (2017) 13785–13792; doi:10.1021/acsami.7b02355

data_4514098
_publ_contact_author
;
Dr. Rahul Banerjee

Scientist
Physical/Materials Chemistry Division  
National Chemical Laboratory
Dr. Homi Bhaba Road
Pune 411008, India
;
_publ_section_title
;
 Predesigned Metal-Anchored Building Block for In Situ Generation of Pd
 Nanoparticles in Porous Covalent Organic Framework: Application in
 Heterogeneous Tandem Catalysis.
;
_journal_issue                   15
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              13785
_journal_page_last               13792
_journal_paper_doi               10.1021/acsami.7b02355
_journal_volume                  9
_journal_year                    2017
_chemical_formula_moiety         'C10 H10 Cl2 N4 Pd'
_chemical_formula_sum            'C10 H10 Cl2 N4 Pd'
_chemical_formula_weight         363.52
_chemical_name_common            Bpy-PdCl2
_chemical_name_systematic        Bpy-PdCl2
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.382(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0173(2)
_cell_length_b                   8.6586(2)
_cell_length_c                   13.7906(3)
_cell_measurement_reflns_used    2725
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5470
_cell_measurement_theta_min      3.0060
_cell_volume                     1180.14(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.640
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    8.00   66.00   1.0000    2.0700
omega____ theta____ kappa____ phi______ frames
    -       19.7469   77.0000 -120.0000 58

  2 omega   -2.00   50.00   1.0000    2.0700
omega____ theta____ kappa____ phi______ frames
    -       19.7469   57.0000 -150.0000 52

  3 omega   41.00   95.00   1.0000    2.0700
omega____ theta____ kappa____ phi______ frames
    -       19.7469  178.0000 -180.0000 54

  4 omega  -63.00  -12.00   1.0000    2.0700
omega____ theta____ kappa____ phi______ frames
    -      -19.7469  -57.0000  -60.0000 51

  5 omega   61.00   86.00   1.0000    2.0700
omega____ theta____ kappa____ phi______ frames
    -       19.7469  178.0000  150.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0524965000
_diffrn_orient_matrix_UB_12      -0.0146346000
_diffrn_orient_matrix_UB_13      0.0401127000
_diffrn_orient_matrix_UB_21      0.0158352000
_diffrn_orient_matrix_UB_22      -0.0697959000
_diffrn_orient_matrix_UB_23      -0.0225524000
_diffrn_orient_matrix_UB_31      0.0463063000
_diffrn_orient_matrix_UB_32      0.0402708000
_diffrn_orient_matrix_UB_33      -0.0245312000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4732
_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         26.372
_diffrn_reflns_theta_min         2.994
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.005
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0203P)^2^+0.0406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2055
_reflns_number_total             2410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am7b02355_si_002.cif
_cod_data_source_block           Bpy-PdCl2
_cod_original_cell_volume        1180.14(5)
_cod_database_code               4514098
_chemical_oxdiff_formula         'C12 H10 N6 O5 Pd3 Cl6 S7'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Rotating group:
 N4(H4A), N7(H7A)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C15(H15)
;
_shelx_res_checksum              60327
_shelx_hkl_checksum              40520
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'