[Cu32(PET)24H8Cl2](PPh4)2: A Copper Hydride Nanocluster with a Bisquare Antiprismatic Core.
Lee, Sanghwa; Bootharaju, Megalamane S.; Deng, Guocheng; Malola, Sami; Baek, Woonhyuk; Häkkinen, Hannu; Zheng, Nanfeng; Hyeon, Taeghwan; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c06577

data_4135126
_publ_section_title
;
 [Cu32(PET)24H8Cl2](PPh4)2: A Copper Hydride Nanocluster with a Bisquare
 Antiprismatic Core.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c06577
_journal_year                    2020
_chemical_formula_moiety         'C192 H224 Cl2 Cu32 S24, 2(C24 H20 P)'
_chemical_formula_sum            'C240 H264 Cl2 Cu32 P2 S24'
_chemical_formula_weight         6084.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                116.547(4)
_cell_angle_beta                 103.456(3)
_cell_angle_gamma                104.134(4)
_cell_formula_units_Z            1
_cell_length_a                   18.5763(7)
_cell_length_b                   19.8786(8)
_cell_length_c                   20.7652(7)
_cell_measurement_reflns_used    9634
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      64.6470
_cell_measurement_theta_min      4.3670
_cell_volume                     6113.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.783
_diffrn_measured_fraction_theta_max 0.954
_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   -107.00 -68.00   1.00    6.00    --  -41.13-134.00 146.00   39
  2  \w   -113.00 -17.00   1.00    6.00    --  -41.13 -57.00  30.00   96
  3  \w    -67.00  25.00   1.00    6.00    --  -41.13  57.00-180.00   92
  4  \w     39.00  83.00   1.00    6.00    --   41.13-135.00 -33.00   44
  5  \w     56.00 111.00   1.00   15.00    --   89.91-125.00  30.00   55
  6  \w     92.00 117.00   1.00   15.00    --   89.91-125.00 -90.00   25
  7  \w     75.00 164.00   1.00   15.00    --   89.91  30.00 120.00   89
  8  \w     72.00 135.00   1.00   15.00    --   89.91  30.00-150.00   63
  9  \w     38.00 114.00   1.00   15.00    --   89.91 -30.00 150.00   76
 10  \w     45.00 106.00   1.00   15.00    --   89.91-125.00 150.00   61
 11  \w    108.00 162.00   1.00   15.00    --   89.91 125.00  60.00   54
 12  \w     15.00 106.00   1.00   15.00    --   89.91 -30.00 -60.00   91
 13  \w    125.00 150.00   1.00   15.00    --   89.91 125.00 150.00   25
 14  \w     94.00 163.00   1.00   15.00    --   89.91 125.00-180.00   69
 15  \w     12.00 124.00   1.00   15.00    --   89.91 -77.00 150.00  112
 16  \w    -91.00 -65.00   1.00    6.00    --  -41.13 125.00-150.00   26
 17  \w   -107.00 -81.00   1.00    6.00    --  -41.13 -37.00-180.00   26
 18  \w   -111.00 -85.00   1.00    6.00    --  -41.13 -37.00 120.00   26
 19  \w     84.00 110.00   1.00   15.00    --   89.91 -94.00 -30.00   26
 20  \w    119.00 145.00   1.00   15.00    --   89.91 125.00  30.00   26
 21  \w     72.00  98.00   1.00   15.00    --   89.91-125.00-180.00   26
 22  \w     31.00  57.00   1.00   15.00    --   89.91 -94.00 -30.00   26
 23  \w    129.00 169.00   1.00   15.00    --   89.91  77.00-150.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0748401000
_diffrn_orient_matrix_UB_12      0.0084864000
_diffrn_orient_matrix_UB_13      -0.0408072000
_diffrn_orient_matrix_UB_21      -0.0508434000
_diffrn_orient_matrix_UB_22      -0.0913947000
_diffrn_orient_matrix_UB_23      -0.0358066000
_diffrn_orient_matrix_UB_31      -0.0217268000
_diffrn_orient_matrix_UB_32      0.0226162000
_diffrn_orient_matrix_UB_33      0.0720759000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.783
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35992
_diffrn_reflns_point_group_measured_fraction_full 0.783
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         59.998
_diffrn_reflns_theta_min         3.652
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.501
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (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    1.653
_exptl_crystal_description       block
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.252
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.282
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1243
_refine_ls_number_reflns         17321
_refine_ls_number_restraints     880
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.2482
_refine_ls_R_factor_gt           0.1726
_refine_ls_shift/su_max          2.601
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.4500P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4704
_refine_ls_wR_factor_ref         0.6203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9764
_reflns_number_total             17321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c06577_si_002.cif
_cod_data_source_block           Cu32
_cod_original_cell_volume        6113.6(5)
_cod_database_code               4135126
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 94.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C10-C9
 1.45 with sigma of 0.01
 C10_$1-C9_$1
 1.46 with sigma of 0.01
 C83-C82
 1.55 with sigma of 0.01
 C82-C84
 2.55 with sigma of 0.01
 C88-C82
 2.55 with sigma of 0.01
 Cu8_$1-H
 2 with sigma of 0.01
 Cu14-H
 1.65 with sigma of 0.01
 Cu13-HA
 1.8 with sigma of 0.01
 Cu6_$1-H
 1.65 with sigma of 0.01
 Cu7_$1-HA
 1.8 with sigma of 0.01
 Cu6_$1-HA
 1.7 with sigma of 0.01
 Cu3_$1-HA
 2 with sigma of 0.01
 Cu6_$1-HC_$1
 2.2 with sigma of 0.01
 HC_$1-Cu6
 2.2 with sigma of 0.01
 C9-C10
 1.5 with sigma of 0.01
 Cu13_$1-H0AA_$1
 1.6 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Cu1A)=1-FVAR(1)
 Sof(Cu1)=FVAR(1)
 Sof(Cu2A)=1-FVAR(2)
 Sof(Cu2)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B), C17(H17A,H17B),
 C18(H18A,H18B), C25(H25A,H25B), C26(H26A,H26B), C41(H41A,H41B), C42(H42A,H42B),
  C49(H49A,H49B), C50(H50A,H50B), C57(H57A,H57B), C58(H58A,H58B), C65(H65A,
 H65B), C66(H66A,H66B), C73(H73A,H73B), C74(H74A,H74B), C81(H81A,H81B),
 C82(H82A,H82B), C89(H89A,H89B), C90(H90A,H90B), C97(H97A,H97B), C98(H98A,H98B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C6(H6), C5(H5), C4(H4), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C32(H32),
  C31(H31), C30(H30), C29(H29), C28(H28), C44(H44), C45(H45), C46(H46),
 C47(H47), C48(H48), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C60(H60),
  C61(H61), C62(H62), C63(H63), C64(H64), C68(H68), C69(H69), C70(H70),
 C71(H71), C72(H72), C80(H80), C76(H76), C77(H77), C78(H78), C79(H79), C88(H88),
  C87(H87), C86(H86), C85(H85), C84(H84), C92(H92), C93(H93), C94(H94),
 C95(H95), C96(H96), C104(H104), C103(H103), C102(H102), C101(H101), C100(H100),
  C106(H106), C107(H107), C108(H108), C109(H109), C110(H110), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C117(H117), C122(H122),
 C121(H121), C120(H120), C119(H119), C128(H128), C124(H124), C125(H125),
 C126(H126), C127(H127)
5.c Fitted hexagon refined as free rotating group:
 C8(C7,C6,C5,C4,C3), C11(C12,C13,C14,C15,C16), C20(C21,C22,C23,C24,C19),
 C27(C32,C31,C30,C29,C28), C80(C75,C76,C77,C78,C79), C83(C88,C87,C86,C85,C84),
 C91(C92,C93,C94,C95,C96), C99(C104,C103,C102,C101,C100), C106(C105,C107,C108,
 C109,C110), C111(C112,C113,C114,C115,C116), C117(C118,C122,C121,C120,C119),
 C128(C123,C124,C125,C126,C127)
;
_olex2_date_sample_data_collection 2019-10-11
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.183
_oxdiff_exptl_absorpt_empirical_full_min 0.290