Synthesis and Structure of Self-Assembled Pd2Au23(PPh3)10Br7 Nanocluster: Exploiting Factors That Promote Assembly of Icosahedral Nano-Building-Blocks
Kang, Xi; Xiang, Ji; Lv, Ying; Du, Wenjun; Yu, Haizhu; Wang, Shuxin; Zhu, Manzhou; Chemistry of Materials  (2017) –; doi:10.1021/acs.chemmater.7b02015

data_4002836
_publ_section_title
;
 Synthesis and Structure of Self-Assembled Pd2Au23(PPh3)10Br7 Nanocluster:
 Exploiting Factors That Promote Assembly of Icosahedral
 Nano-Building-Blocks
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.7b02015
_journal_year                    2017
_chemical_formula_moiety         'C180 H150 Au23 Br7 P10 Pd2'
_chemical_formula_sum            'C180 H150 Au23 Br7 P10 Pd2'
_chemical_formula_weight         7925.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.950(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.475(4)
_cell_length_b                   24.378(5)
_cell_length_c                   29.610(6)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.19
_cell_volume                     11590(4)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2236
_diffrn_reflns_av_unetI/netI     0.2352
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            83850
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.411
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.954
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1448 before and 0.0747 after correction.
The Ratio of minimum to maximum transmission is 0.6151.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_description       cube
_exptl_crystal_F_000             7068
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.160
_refine_diff_density_max         2.764
_refine_diff_density_min         -2.872
_refine_diff_density_rms         0.397
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         21461
_refine_ls_number_restraints     3267
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0809
_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^)+(0.0611P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9497
_reflns_number_total             21461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b02015_si_002.cif
_cod_data_source_block           ixing83
_cod_database_code               4002836
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C26 \\sim C53 \\sim C44 \\sim C37 \\sim C54 \\sim C50 \\sim C27 \\sim C30 \\sim
C31 \\sim C47 \\sim C77 \\sim C58 \\sim C28 \\sim C42 \\sim C82 \\sim C39 \\sim
C59 \\sim C56 \\sim C29 \\sim C33 \\sim C43 \\sim C36 \\sim C48 \\sim C34 \\sim
C35 \\sim C106 \\sim C76 \\sim C75 \\sim C69 \\sim C55 \\sim C38 \\sim C71
\\sim C45 \\sim C65 \\sim C57 \\sim C78 \\sim C60 \\sim C5AA \\sim C6AA \\sim
C40 \\sim C7AA \\sim C68 \\sim C61 \\sim C100 \\sim C70 \\sim C86 \\sim C157
\\sim C171 \\sim C62 \\sim C64 \\sim C52 \\sim C66 \\sim C4AA \\sim C3AA \\sim
C79 \\sim C102 \\sim C8AA \\sim C9AA \\sim C95 \\sim C107 \\sim C91 \\sim C205
\\sim C261 \\sim C0AA \\sim C49 \\sim C63 \\sim C94 \\sim C190 \\sim C166 \\sim
C110 \\sim C2AA \\sim C1AA \\sim C109 \\sim C0BA \\sim C154 \\sim C72 \\sim
C2BA \\sim C1BA \\sim C5BA \\sim C6BA \\sim C7BA \\sim C8BA \\sim C9BA \\sim
C0CA \\sim C32 \\sim C4BA \\sim C1CA \\sim C108 \\sim C3BA \\sim C161: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C53(H53), C44(H44), C37(H37), C54(H54), C50(H50), C30(H30), C31(H31),
 C47(H47), C77(H77), C58(H58), C42(H42), C82(H82), C39(H39), C59(H59), C56(H56),
  C33(H33), C43(H43), C36(H36), C48(H48), C34(H34), C106(H106), C76(H76),
 C75(H75), C69(H69), C55(H55), C71(H71), C45(H45), C65(H65), C57(H57), C78(H78),
  C5AA(H5AA), C6AA(H6AA), C40(H40), C7AA(H7AA), C68(H68), C100(H100), C70(H70),
 C86(H86), C157(H157), C171(H171), C64(H64), C52(H52), C66(H66), C4AA(H4AA),
 C3AA(H3AA), C102(H102), C8AA(H8AA), C9AA(H9AA), C95(H95), C107(H107),
 C205(H205), C261(H261), C0AA(H0AA), C49(H49), C63(H63), C190(H190), C166(H166),
  C110(H110), C2AA(H2AA), C1AA(H1AA), C0BA(H0BA), C154(H154), C72(H72),
 C2BA(H2BA), C1BA(H1BA), C6BA(H6BA), C7BA(H7BA), C8BA(H8BA), C9BA(H9BA),
 C0CA(H0CA), C4BA(H4BA), C1CA(H1CA), C108(H108), C3BA(H3BA), C161(H161)
4.b Fitted hexagon refined as free rotating group:
 C26(C53,C44,C37,C54,C50), C27(C30,C31,C47,C77,C58), C28(C42,C82,C39,C59,C56),
 C29(C33,C43,C36,C48,C34), C35(C106,C76,C75,C69,C55), C38(C71,C45,C65,C57,C78),
 C60(C5AA,C6AA,C40,C7AA,C68), C61(C100,C70,C86,C157,C171), C62(C64,C52,C66,C4AA,
 C3AA), C79(C102,C8AA,C9AA,C95,C107), C91(C205,C261,C0AA,C49,C63), C94(C190,
 C166,C110,C2AA,C1AA), C109(C0BA,C154,C72,C2BA,C1BA), C5BA(C6BA,C7BA,C8BA,C9BA,
 C0CA), C32(C4BA,C1CA,C108,C3BA,C161)
;
_shelx_res_checksum              94984
_shelx_hkl_checksum              46872
_shelx_fab_checksum              2545
_olex2_submission_special_instructions 'No special instructions were received'