Shape-selective one-step synthesis of branched gold nanoparticles on the crystal surface of redox-active Pd<sup>II</sup>-macrocycles.
Yamashita, Yutaro; Tashiro, Shohei; Ishii, Yoshiki; Uchihashi, Takayuki; Matsushita, Nobuyuki; Kubota, Ryou; Shionoya, Mitsuhiko; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1318–1324; doi:10.1039/d1dt03973c

data_7709114
_publ_section_title
;
 Shape-selective one-step synthesis of branched gold nanoparticles on the
 crystal surface of redox-active Pd<sup>II</sup>-macrocycles.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1318
_journal_page_last               1324
_journal_paper_doi               10.1039/d1dt03973c
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C42 H42 Cl4 N6 Pd2, 0.5(C4 H6 N2), 0.5(O)'
_chemical_formula_sum            'C44 H45 Cl4 N7 O0.5 Pd2'
_chemical_formula_weight         1034.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-06-15
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-02 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2066(2)
_cell_length_b                   23.2676(4)
_cell_length_c                   14.0442(3)
_cell_measurement_reflns_used    5943
_cell_measurement_temperature    93
_cell_measurement_theta_max      72.6390
_cell_measurement_theta_min      3.6620
_cell_volume                     4315.58(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (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)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_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    -19.00   8.00   0.50    0.50    --    0.00  38.00-180.00   54
  2  \w     25.00  88.00   0.50    0.50    --    0.00  38.00-180.00  126
  3  \w     42.00  89.00   0.50    0.50    --    0.00  38.00 -90.00   94
  4  \w     74.00 122.00   0.50    1.89    --   98.20 -45.00-150.00   96
  5  \w     14.00  57.00   0.50    1.89    --   98.20 -45.00-150.00   86
  6  \w     12.00  55.00   0.50    1.89    --   98.20 -30.00   0.00   86
  7  \w     70.00 127.00   0.50    1.89    --   98.20 -30.00   0.00  114
  8  \w     12.00  96.00   0.50    1.89    --   98.20 -45.00   0.00  168
  9  \w     88.00 187.00   0.50    1.89    --   98.20  77.00 -30.00  198
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0296449000
_diffrn_orient_matrix_UB_12      -0.0408072000
_diffrn_orient_matrix_UB_13      0.0817470000
_diffrn_orient_matrix_UB_21      0.0623410000
_diffrn_orient_matrix_UB_22      -0.0366237000
_diffrn_orient_matrix_UB_23      -0.0701142000
_diffrn_orient_matrix_UB_31      0.0940519000
_diffrn_orient_matrix_UB_32      0.0371130000
_diffrn_orient_matrix_UB_33      0.0207305000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13527
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.407
_diffrn_reflns_theta_min         3.676
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.334
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       plate
_exptl_crystal_F_000             2088
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.212
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4336
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0685
_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^)+(0.1332P)^2^+8.0473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2022
_refine_ls_wR_factor_ref         0.2127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3555
_reflns_number_total             4336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03973c5.cif
_cod_data_source_block           Pd2LCl4
_cod_depositor_comments          'Adding full bibliography for 7709114.cif.'
_cod_original_formula_sum        'C44 H45 Cl4 N7 O0.50 Pd2'
_cod_database_code               7709114
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHNClPdO
_reflns_odcompleteness_completeness 99.93
_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, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-C3 \\sim C2-C1
 with sigma of 0.02
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H2SA(0.5) H2SB(0.5) H2SC(0.5) O1W(0.25)
4.a Ternary CH refined with riding coordinates:
 N3(H3), N2(H2)
4.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C18(H18A,H18B), C11(H11A,H11B), C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C13(H13), C10(H10), C14(H14), C9(H9), C7(H7), C16(H16),
 C15(H15), C6(H6), C2(H2A), C1(H1)
4.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              44971
_shelx_hkl_checksum              56367
_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 2.612
_oxdiff_exptl_absorpt_empirical_full_min 0.567