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_4518645
_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_absolute_configuration syn
_chemical_formula_moiety         'C180 H184 Ag1 Cu16 P12 S8, F6 P1'
_chemical_formula_sum            'C180 H184 Ag Cu16 F6 P13 S8'
_chemical_formula_weight         4244.86
_space_group_crystal_system      cubic
_space_group_IT_number           219
_space_group_name_Hall           'F -4a 2 3'
_space_group_name_H-M_alt        'F -4 3 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.2120(3)
_cell_length_b                   33.2120(3)
_cell_length_c                   33.2120(3)
_cell_measurement_reflns_used    4858
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      71.7680
_cell_measurement_theta_min      5.2800
_cell_volume                     36634.1(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_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     33.00 117.00   1.00  230.00    --  104.28 -10.00 -90.00   84
  2  \w   -100.00 -74.00   1.00  230.00    --  -86.25  10.00  83.00   26
  3  \w    -70.00 -38.00   1.00   64.00    --  -48.45 -38.00  90.00   32
  4  \w   -120.00 -74.00   1.00   64.00    --  -48.45 -38.00  90.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0284011000
_diffrn_orient_matrix_UB_12      -0.0235927000
_diffrn_orient_matrix_UB_13      0.0281407000
_diffrn_orient_matrix_UB_21      -0.0187870000
_diffrn_orient_matrix_UB_22      0.0212961000
_diffrn_orient_matrix_UB_23      0.0366674000
_diffrn_orient_matrix_UB_31      -0.0315228000
_diffrn_orient_matrix_UB_32      -0.0338095000
_diffrn_orient_matrix_UB_33      0.0034625000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10837
_diffrn_reflns_point_group_measured_fraction_full 0.850
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        66.590
_diffrn_reflns_theta_max         66.590
_diffrn_reflns_theta_min         2.661
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
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    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             17216
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 675 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2304
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0690
_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^)+(0.1377P)^2^+259.8337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2244
_refine_ls_wR_factor_ref         0.2351
_reflns_Friedel_coverage         0.611
_reflns_Friedel_fraction_full    0.688
_reflns_Friedel_fraction_max     0.687
_reflns_number_gt                1966
_reflns_number_total             2304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nn1c00942_si_002.cif
_cod_data_source_block           SD/AgCu16b
_cod_original_cell_volume        36634.1(10)
_cod_original_sg_symbol_Hall     'F -4c 2 3'
_cod_database_code               4518645
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CuCP
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.715
_reflns_odcompleteness_completeness 99.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C8-C6
 1.5 with sigma of 0.01
 C9-C8
 1.55 with sigma of 0.001
 C6-C9
 2.3 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C7: within 2A with sigma of 0.004
and sigma for terminal atoms of 0.008
C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008
P1 \\sim C6 \\sim C8 \\sim C9: within 2A with sigma of 0.004 and sigma for
terminal atoms of 0.008
4. Others
 Fixed Sof: H11(0.33333)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15)
5.c Fitted hexagon refined as free rotating group:
 C10(C11,C12,C13,C14,C15)
;
_shelx_res_checksum              32544
_shelx_hkl_checksum              70426
_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 1.323
_oxdiff_exptl_absorpt_empirical_full_min 0.667