Precise Implantation of an Archimedean Ag@Cu<sub>12</sub> Cuboctahedron into a Platonic Cu<sub>4</sub>Bis(diphenylphosphino)hexane<sub>6</sub> Tetrahedron.
Han, Bao-Liang; Wang, Zhi; Gupta, Rakesh Kumar; Feng, Lei; Wang, Suna; Kurmoo, Mohamedally; Gao, Zhi-Yong; Schein, Stan; Tung, Chen-Ho; Sun, Di; ACS nano  (2021) –; doi:10.1021/acsnano.1c00942

data_4518644
_publ_section_title
;
 Precise Implantation of an Archimedean Ag@Cu<sub>12</sub> Cuboctahedron
 into a Platonic Cu<sub>4</sub>Bis(diphenylphosphino)hexane<sub>6</sub>
 Tetrahedron.
;
_journal_name_full               'ACS nano'
_journal_paper_doi               10.1021/acsnano.1c00942
_journal_year                    2021
_chemical_formula_moiety         'C180 H192 Ag Cu16 P12 S8'
_chemical_formula_sum            'C180 H192 Ag Cu16 P12 S8'
_chemical_formula_weight         4107.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-12-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.506(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.1664(7)
_cell_length_b                   17.0909(6)
_cell_length_c                   22.9344(7)
_cell_measurement_reflns_used    13387
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      25.7540
_cell_measurement_theta_min      3.2490
_cell_volume                     9861.1(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.99(10)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  20.00   1.00  120.00    --   -5.62  57.00  90.00   39
  2  \w     43.00  73.00   1.00  120.00    --   -5.62  29.00 109.00   30
  3  \w     41.00  68.00   1.00  120.00    --   -5.62  57.00  90.00   27
  4  \w    -25.00  24.00   1.00  120.00    --   -5.62  29.00 109.00   49
  5  \w    -25.00  32.00   1.00  120.00    --   -5.62 -99.00 -60.00   57
  6  \w    -63.00  27.00   1.00  120.00    --    6.79 -57.00-150.00   90
  7  \w    -66.00  33.00   1.00  120.00    --    6.79 -77.00 -60.00   99
  8  \w    -80.00 -16.00   1.00  120.00    --   -5.62 -29.00 -52.00   64
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0218705000
_diffrn_orient_matrix_UB_12      0.0244123000
_diffrn_orient_matrix_UB_13      0.0076447000
_diffrn_orient_matrix_UB_21      -0.0108271000
_diffrn_orient_matrix_UB_22      0.0301062000
_diffrn_orient_matrix_UB_23      -0.0179691000
_diffrn_orient_matrix_UB_31      -0.0141072000
_diffrn_orient_matrix_UB_32      0.0147978000
_diffrn_orient_matrix_UB_33      0.0240176000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            57642
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         3.202
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.008
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             4182
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 4795 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         16798
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+13.9217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.907
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                13360
_reflns_number_total             16798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nn1c00942_si_002.cif
_cod_data_source_block           SD/AgCu16a
_cod_database_code               4518644
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CuCNP
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.906
_diffrn_oxdiff_ac3_digest_frames
;
01120ec8ecd7e95015821c8fba860770900045592dd
;
_diffrn_oxdiff_ac3_digest_hkl
;
010af54f5e9dca917de7c247f83a346d51fd10
;
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C76-C75
 1.55 with sigma of 0.01
 H57-H83A
 1.9 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
Uanis(C53) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
4.a Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,
 H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B),
 C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B),
  C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
  C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38),
  C39(H39), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47),
 C48(H48), C51(H51), C52(H52), C53(H53), C54(H54), C49(H49), C55(H55), C56(H56),
  C57(H57), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C67(H67), C69(H69), C70(H70), C71(H71), C72(H72)
4.c Fitted hexagon refined as free rotating group:
 C51(C52,C53,C54,C49,C50)
;
_shelx_res_checksum              80348
_shelx_hkl_checksum              31670
_shelx_fab_checksum              8278
_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 1.422
_oxdiff_exptl_absorpt_empirical_full_min 0.678