[Cu23(PhSe)16(Ph3P)8(H)6]·BF4: Atomic-Level Insights into Cuboidal Polyhydrido Copper Nanoclusters and Their Quasi-simple Cubic Self-Assembly
Huang, Ren-Wu; Yin, Jun; Dong, Chunwei; Maity, Partha; Hedhili, Mohamed Nejib; Nematulloev, Saidkhodzha; Alamer, Badriah; Ghosh, Atanu; Mohammed, Omar F.; Bakr, Osman M.; ACS Materials Letters  (2020) 90–99; doi:10.1021/acsmaterialslett.0c00513

data_4518388
_publ_section_title
;
 [Cu23(PhSe)16(Ph3P)8(H)6]&#x00B7;BF4: Atomic-Level Insights into Cuboidal
 Polyhydrido Copper Nanoclusters and Their Quasi-simple Cubic
 Self-Assembly
;
_journal_name_full               'ACS Materials Letters'
_journal_page_first              90
_journal_page_last               99
_journal_paper_doi               10.1021/acsmaterialslett.0c00513
_journal_year                    2020
_chemical_formula_moiety         'C240 H200 Cu23 P8 Se16'
_chemical_formula_sum            'C240 H200 Cu23 P8 Se16'
_chemical_formula_weight         6056.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-03
_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            4
_cell_length_a                   23.5776(9)
_cell_length_b                   45.6755(17)
_cell_length_c                   25.9902(9)
_cell_measurement_reflns_used    9689
_cell_measurement_temperature    107(2)
_cell_measurement_theta_max      58.995
_cell_measurement_theta_min      3.536
_cell_volume                     27989.3(18)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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      106.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            139877
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        59.026
_diffrn_reflns_theta_max         59.026
_diffrn_reflns_theta_min         2.709
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.953
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.2767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             11884
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.700
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.263
_refine_ls_extinction_coef       0.000008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1440
_refine_ls_number_reflns         19895
_refine_ls_number_restraints     1155
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1362
_refine_ls_R_factor_gt           0.1269
_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^)+(0.0001P)^2^+1952.9143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2741
_refine_ls_wR_factor_ref         0.2790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17632
_reflns_number_total             19895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz0c00513_si_002.cif
_cod_data_source_block           cu23se16_100k
_cod_database_code               4518388
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.383
_shelx_estimated_absorpt_t_min   0.269
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C14-C13 \\sim C14-C15 \\sim C16-C15 \\sim C16-C17 \\sim C18-C17 \\sim C18-C13
 with sigma of 0.01
 C14-C18 \\sim C17-C15
 with sigma of 0.01
 C13-C16 \\sim C17-C14 \\sim C15-C18
 with sigma of 0.01
 Se7-C9B \\sim Se7-C13
 with sigma of 0.01
 C9B-C14B \\sim C9B-C10B \\sim C14-C13 \\sim C18-C13 \\sim C18-C17 \\sim
C14B-C13B \\sim C16-C17 ~
 C13B-C12B \\sim C16-C15 \\sim C14-C15 \\sim C10B-C11B \\sim C11B-C12B
 with sigma of 0.01
 C88-C87 \\sim C89-C88 \\sim C89-C90 \\sim C90-C85 \\sim C87-C86 \\sim C86-C85
 with sigma of 0.01
 C6-C1 \\sim C6-C5 \\sim C5B-C4B \\sim C4-C5 \\sim C3B-C4B \\sim C3-C4 \\sim
C3B-C2B \\sim C3-C2 \\sim C2-C1 ~
 C1-C1B \\sim C2B-C1B
 with sigma of 0.01
 C20-C19 \\sim C19-C15B \\sim C16B-C15B \\sim C21-C20 \\sim C22B-C16B \\sim
C22-C21 \\sim C23-C22B ~
 C23-C22 \\sim C24-C23 \\sim C24-C19
 with sigma of 0.01
 C94-C95 \\sim C94-C93 \\sim C95-C96 \\sim C96-C91 \\sim C92-C91 \\sim C93-C92
 with sigma of 0.01
 C6B-C7 \\sim C8-C7 \\sim C7B-C6B \\sim C8-C9 \\sim C9-C10 \\sim C7B-C8B \\sim
C10-C11 \\sim C8B-C11 \\sim C7-
 C12 \\sim C11-C12
 with sigma of 0.01
3. Restrained planarity
 C6B, C7, C7B, C8B, C11, C12
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C9B \\sim C10B \\sim C11B \\sim C12B \\sim C13 \\sim C13B \\sim C14 \\sim C14B
\\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C1B \\sim C2 \\sim C2B \\sim C3 \\sim C3B \\sim C4 \\sim C4B \\sim C5 \\sim C5B
\\sim C6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C15B \\sim C16B \\sim C20 \\sim C21 \\sim C22 \\sim C22B \\sim C23 \\sim C24:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C6B \\sim C7B \\sim C8 \\sim C8B \\sim C9 \\sim C10 \\sim C11: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C1B, C2, C2B, C3, C3B, C4, C4B, C5, C5B, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C24, C23, C22, C22B, C21, C16B, C15B, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C92, C96, C95, C94, C93, C91
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C97, C98, C99, C100, C101, C102
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C67, C72, C71, C70, C69, C68
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C80, C79, C84, C83, C82, C81
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C38, C37, C39, C40, C41, C42
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C43, C44, C45, C46, C47, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C85, C90, C89, C88, C87, C86
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C7, C6B, C8, C9, C7B, C11, C8B, C10, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=Sof(H11a)=1-FVAR(1)
 Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(H11)=FVAR(1)
 Sof(H23a)=Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16B)=Sof(C22B)=Sof(H22B)=1-FVAR(2)
 Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(H23)=FVAR(2)
 Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=
 Sof(C5B)=Sof(H5B)=1-FVAR(3)
 Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=
 Sof(H6)=FVAR(3)
 Sof(C9B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11B)=Sof(C12B)=Sof(H12B)=
 Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14B)=1-FVAR(4)
 Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=
 Sof(H17)=Sof(C18)=Sof(H18)=FVAR(4)
7.a Aromatic/amide H refined with riding coordinates:
 C1B(H1B), C2(H2), C2B(H2B), C3(H3), C3B(H3B), C4(H4), C4B(H4B), C5(H5),
 C5B(H5B), C6(H6), C6B(H6B), C7B(H7B), C8(H8), C8B(H8B), C9(H9), C10(H10),
 C10B(H10B), C11(H11), C11(H11a), C11B(H11B), C12(H12), C12B(H12B), C13B(H13B),
 C14(H14), C14B(H14B), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20),
 C21(H21), C22(H22), C23(H23a), C23(H23), C24(H24), C15B(H15B), C16B(H16B),
 C22B(H22B), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50),
 C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59),
  C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68),
 C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C86(H86),
 C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93), C94(H94), C95(H95),
  C96(H96), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C104(H104),
 C105(H105), C106(H106), C107(H107), C108(H108), C110(H110), C111(H111),
 C112(H112), C113(H113), C114(H114), C116(H116), C117(H117), C118(H118),
 C119(H119), C120(H120)
7.b Fitted hexagon refined as free rotating group:
 C23(C24,C19,C15B,C16B,C22B)
;
_olex2_submission_special_instructions 'No special instructions were received'