Gram-Scale Preparation of Stable Hydride M@Cu<sub>24</sub> (M = Au/Cu) Nanoclusters.
Chen, Along; Kang, Xi; Jin, Shan; Du, Wenjun; Wang, Shuxin; Zhu, Manzhou; The journal of physical chemistry letters 10 (2019) 6124–6128; doi:10.1021/acs.jpclett.9b02297

data_8000391
_publ_section_title
;
 Gram-Scale Preparation of Stable Hydride M@Cu<sub>24</sub> (M = Au/Cu)
 Nanoclusters.
;
_journal_issue                   20
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              6124
_journal_page_last               6128
_journal_paper_doi               10.1021/acs.jpclett.9b02297
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         '2(C108 H72 Cu12.5 F18 P6)'
_chemical_formula_sum            'C216 H144 Cu25 F36 P12'
_chemical_formula_weight         5383.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           30
_space_group_name_Hall           'P 2 -2bc'
_space_group_name_H-M_alt        'P n c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-24 deposited with the CCDC.	2019-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.557(3)
_cell_length_b                   22.3796(19)
_cell_length_c                   32.859(3)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    160
_cell_measurement_theta_max      24.485
_cell_measurement_theta_min      2.202
_cell_volume                     25412(4)
_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      160
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1316
_diffrn_reflns_av_unetI/netI     0.1736
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            68031
_diffrn_reflns_point_group_measured_fraction_full 0.752
_diffrn_reflns_point_group_measured_fraction_max 0.752
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.084
_exptl_absorpt_coefficient_mu    2.185
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1273 before and 0.0898 after correction. The Ratio of minimum to maximum transmission is 0.5829. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             10676
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.789
_refine_diff_density_min         -1.701
_refine_diff_density_rms         0.220
_refine_ls_abs_structure_details
;
 Flack x determined using 4487 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.037(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2171
_refine_ls_number_reflns         33679
_refine_ls_number_restraints     4897
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1692
_refine_ls_R_factor_gt           0.0956
_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^)+(0.1604P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2458
_refine_ls_wR_factor_ref         0.2819
_reflns_Friedel_coverage         0.477
_reflns_Friedel_fraction_full    0.495
_reflns_Friedel_fraction_max     0.495
_reflns_number_gt                19048
_reflns_number_total             33679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz9b02297_si_004.cif
_cod_data_source_block           20190123b_0m
_cod_original_cell_volume        25413(3)
_cod_database_code               8000391
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.811
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C019 \\sim C01T \\sim C01N \\sim C050 \\sim C06X \\sim C057 \\sim C01A \\sim
C01J \\sim C06Z \\sim C05C \\sim C04M \\sim C021 \\sim C01B \\sim C02G \\sim
C025 \\sim C045 \\sim C04R \\sim C01G \\sim C01D \\sim C03D \\sim C04X \\sim
C059 \\sim C02F \\sim C05A \\sim C01M \\sim C03W \\sim C051 \\sim C07X \\sim
C07T \\sim C04S \\sim C01R \\sim C03R \\sim C068 \\sim C071 \\sim C065 \\sim
C043 \\sim C01W \\sim C080 \\sim C08C \\sim C07A \\sim C06U \\sim C033 \\sim
C024 \\sim C01H \\sim C03S \\sim C03H \\sim C03N \\sim C01Z \\sim C026 \\sim
C04Y \\sim C05M \\sim C07Z \\sim C05W \\sim C042 \\sim C02C \\sim C02L \\sim
C06B \\sim C07K \\sim C04N \\sim C062 \\sim C03E \\sim C02Q \\sim C05H \\sim
C06C \\sim C069 \\sim C06A \\sim C072 \\sim C02U \\sim C04I \\sim C075 \\sim
C05Q \\sim C05S \\sim C06Q \\sim C02V \\sim C058 \\sim C05D \\sim C06N \\sim
C06P \\sim C06W \\sim C02W \\sim C07E \\sim C07R \\sim C078 \\sim C07O \\sim
C05L \\sim C02X \\sim C056 \\sim C06R \\sim C04D \\sim C03L \\sim C03C \\sim
C02Z \\sim C05J \\sim C074 \\sim C066 \\sim C06V \\sim C07N \\sim C030 \\sim
C02B \\sim C040 \\sim C06K \\sim C07P \\sim C04G \\sim C031 \\sim C032 \\sim
C03J \\sim C05K \\sim C06S \\sim C06D \\sim C046 \\sim C03A \\sim C02J \\sim
C02R \\sim C07V \\sim C05Z \\sim C02S \\sim C03B \\sim C082 \\sim C06L \\sim
C05Y \\sim C07H \\sim C05B \\sim C03G \\sim C01Q \\sim C03Y \\sim C07G \\sim
C07I \\sim C07Q \\sim C03I \\sim C05O \\sim C076 \\sim C07W \\sim C06G \\sim
C04B \\sim C03M \\sim C06F \\sim C05N \\sim C04W \\sim C05U \\sim C04F \\sim
C03O \\sim C035 \\sim C028 \\sim C05P \\sim C06E \\sim C05G \\sim C03P \\sim
C02H \\sim C01X \\sim C03U \\sim C03K \\sim C05I \\sim C03V \\sim C04U \\sim
C05T \\sim C04T \\sim C037 \\sim C02D \\sim C03X \\sim C041 \\sim C06I \\sim
C08B \\sim C067 \\sim C03Q \\sim C01O \\sim C048 \\sim C044 \\sim C07M \\sim
C053 \\sim C01P \\sim C036 \\sim C04A \\sim C060 \\sim C06M \\sim C081 \\sim
C05F \\sim C038 \\sim C04C \\sim C04Z \\sim C04O \\sim C07J \\sim C07L \\sim
C063 \\sim C04E \\sim C055 \\sim C02P \\sim C05X \\sim C6 \\sim C05E \\sim C04H
\\sim C073 \\sim C07B \\sim C07F \\sim C06J \\sim C052 \\sim C04K \\sim C083
\\sim C07D \\sim C07S \\sim C06O \\sim C04Q \\sim C04L \\sim C05R \\sim C06T
\\sim C07C \\sim C085 \\sim C064 \\sim C04P \\sim C04V \\sim C05V \\sim C061
\\sim C04J \\sim C06Y \\sim C06H \\sim C034 \\sim C03Z: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(F018) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F01F) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F047) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 F018
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F01F
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F047
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 C01T(H01T), C01N(H01N), C06X(H06X), C057(H057), C01J(H01J), C06Z(H06Z),
 C04M(H04M), C021(H021), C02G(H02G), C025(H025), C04R(H04R), C01G(H01G),
 C03D(H03D), C04X(H04X), C02F(H02F), C05A(H05A), C03W(H03W), C051(H051),
 C07T(H07T), C04S(H04S), C03R(H03R), C068(H068), C065(H065), C043(H043),
 C080(H080), C08C(H08C), C06U(H06U), C033(H033), C01H(H01H), C03S(H03S),
 C03N(H03N), C01Z(H01Z), C04Y(H04Y), C05M(H05M), C05W(H05W), C042(H042),
 C06B(H06B), C07K(H07K), C062(H062), C03E(H03E), C05H(H05H), C06C(H06C),
 C06A(H06A), C072(H072), C04I(H04I), C075(H075), C05S(H05S), C06Q(H06Q),
 C058(H058), C05D(H05D), C06P(H06P), C06W(H06W), C07E(H07E), C07R(H07R),
 C07O(H07O), C05L(H05L), C056(H056), C06R(H06R), C03L(H03L), C03C(H03C),
 C05J(H05J), C074(H074), C06V(H06V), C07N(H07N), C02B(H02B), C040(H040),
 C07P(H07P), C04G(H04G), C03J(H03J), C05K(H05K), C06D(H06D), C046(H046),
 C02J(H02J), C02R(H02R), C05Z(H05Z), C02S(H02S), C082(H082), C06L(H06L),
 C07H(H07H), C05B(H05B), C01Q(H01Q), C03Y(H03Y), C07I(H07I), C07Q(H07Q),
 C05O(H05O), C076(H076), C06G(H06G), C04B(H04B), C06F(H06F), C05N(H05N),
 C05U(H05U), C04F(H04F), C035(H035), C028(H028), C06E(H06E), C05G(H05G),
 C02H(H02H), C01X(H01X), C03K(H03K), C05I(H05I), C04U(H04U), C05T(H05T),
 C037(H037), C02D(H02D), C06I(H06I), C08B(H08B), C03Q(H03Q), C01O(H01O),
 C044(H044), C07M(H07M), C01P(H01P), C036(H036), C060(H060), C06M(H06M),
 C05F(H05F), C038(H038), C04Z(H04Z), C04O(H04O), C07L(H07L), C063(H063),
 C055(H055), C02P(H02P), C6(H6), C05E(H05E), C073(H073), C07B(H07B), C06J(H06J),
  C052(H052), C083(H083), C07D(H07D), C06O(H06O), C04Q(H04Q), C05R(H05R),
 C06T(H06T), C085(H085), C064(H064), C02C(H02C), C031(H031), C05V(H05V),
 C04V(H04V), C04J(H04J), C06Y(H06Y), C034(H034), C03Z(H03Z)
4.b Fitted hexagon refined as free rotating group:
 C019(C01T,C01N,C050,C06X,C057), C01A(C01J,C06Z,C05C,C04M,C021), C01B(C02G,
 C025,C045,C04R,C01G), C01D(C03D,C04X,C059,C02F,C05A), C01M(C03W,C051,C07X,C07T,
 C04S), C01R(C03R,C068,C071,C065,C043), C01W(C080,C08C,C07A,C06U,C033),
 C024(C01H,C03S,C03H,C03N,C01Z), C026(C04Y,C05M,C07Z,C05W,C042), C02L(C06B,C07K,
 C04N,C062,C03E), C02Q(C05H,C06C,C069,C06A,C072), C02U(C04I,C075,C05Q,C05S,
 C06Q), C02V(C058,C05D,C06N,C06P,C06W), C02W(C07E,C07R,C078,C07O,C05L),
 C02X(C056,C06R,C04D,C03L,C03C), C02Z(C05J,C074,C066,C06V,C07N), C030(C02B,C040,
 C06K,C07P,C04G), C032(C03J,C05K,C06S,C06D,C046), C03A(C02J,C02R,C07V,C05Z,
 C02S), C03B(C082,C06L,C05Y,C07H,C05B), C03G(C01Q,C03Y,C07G,C07I,C07Q),
 C03I(C05O,C076,C07W,C06G,C04B), C03M(C06F,C05N,C04W,C05U,C04F), C03O(C035,C028,
 C05P,C06E,C05G), C03P(C02H,C01X,C03U,C03K,C05I), C03V(C04U,C05T,C04T,C037,
 C02D), C041(C06I,C08B,C067,C03Q,C01O), C048(C044,C07M,C053,C01P,C036),
 C04A(C060,C06M,C081,C05F,C038), C04C(C04Z,C04O,C07J,C07L,C063), C04E(C055,C02P,
 C05X,C6,C05E), C04H(C073,C07B,C07F,C06J,C052), C04K(C083,C07D,C07S,C06O,C04Q),
 C04L(C05R,C06T,C07C,C085,C064), C04P(C02C,C031,C03X,C05V,C04V), C061(C04J,C06Y,
 C06H,C034,C03Z)
;
_shelx_res_checksum              466
_shelx_hkl_checksum              31671
_olex2_submission_special_instructions 'No special instructions were received'