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_8000393
_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         'C216 H180 Au Cu24 P12'
_chemical_formula_sum            'C216 H180 Au Cu24 P12'
_chemical_formula_weight         4869.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-05 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            8
_cell_length_a                   33.3830(9)
_cell_length_b                   38.6374(11)
_cell_length_c                   39.1118(10)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    161
_cell_measurement_theta_max      23.949
_cell_measurement_theta_min      2.171
_cell_volume                     50448(2)
_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      161
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1260
_diffrn_reflns_av_unetI/netI     0.1011
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            252022
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         0.960
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.669
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1182 before and 0.0793 after correction. The Ratio of minimum to maximum transmission is 0.5731. 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    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             19448
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.470
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       0.000115(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1847
_refine_ls_number_reflns         43772
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0671P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25972
_reflns_number_total             43772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz9b02297_si_002.cif
_cod_data_source_block           20181229c_0m
_cod_database_code               8000393
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.776
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
P6 \\sim C058 \\sim C078 \\sim C07G \\sim C06L \\sim C05S \\sim C04C: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C01D(H01D), C026(H026), C02B(H02B), C02E(H02E), C02C(H02C), C023(H023),
 C04H(H04H), C03R(H03R), C03P(H03P), C02N(H02N), C030(H030), C02I(H02I),
 C02X(H02X), C046(H046), C03K(H03K), C01E(H01E), C03F(H03F), C01Z(H01Z),
 C02M(H02M), C01B(H01B), C05A(H05A), C05T(H05T), C05K(H05K), C062(H062),
 C04P(H04P), C020(H020), C06F(H06F), C065(H065), C03I(H03I), C01M(H01M),
 C01K(H01K), C03M(H03M), C02Y(H02Y), C029(H029), C022(H022), C03T(H03T),
 C03N(H03N), C035(H035), C04B(H04B), C01L(H01L), C02V(H02V), C03Y(H03Y),
 C04D(H04D), C01N(H01N), C01O(H01O), C021(H021), C02Z(H02Z), C032(H032),
 C04T(H04T), C03J(H03J), C02K(H02K), C03X(H03X), C04S(H04S), C04X(H04X),
 C03S(H03S), C02H(H02H), C04J(H04J), C061(H061), C04W(H04W), C03A(H03A),
 C02D(H02D), C02G(H02G), C027(H027), C03O(H03O), C02F(H02F), C037(H037),
 C02W(H02W), C04M(H04M), C05R(H05R), C02U(H02U), C04O(H04O), C05I(H05I),
 C04Q(H04Q), C043(H043), C039(H039), C01T(H01T), C03G(H03G), C04Z(H04Z),
 C05Z(H05Z), C04K(H04K), C02J(H02J), C052(H052), C051(H051), C04G(H04G),
 C053(H053), C04Y(H04Y), C060(H060), C03H(H03H), C044(H044), C047(H047),
 C05L(H05L), C05M(H05M), C040(H040), C02O(H02O), C01I(H01I), C056(H056),
 C05Y(H05Y), C069(H069), C06B(H06B), C05C(H05C), C057(H057), C05P(H05P),
 C04E(H04E), C03E(H03E), C033(H033), C01S(H01S), C04A(H04A), C04U(H04U),
 C01Y(H01Y), C01X(H01X), C04I(H04I), C05E(H05E), C03V(H03V), C04R(H04R),
 C02S(H02S), C054(H054), C05D(H05D), C05O(H05O), C06K(H06K), C06A(H06A),
 C02Q(H02Q), C03D(H03D), C049(H049), C06J(H06J), C05W(H05W), C06S(H06S),
 C06E(H06E), C048(H048), C05V(H05V), C05N(H05N), C03U(H03U), C04V(H04V),
 C066(H066), C05B(H05B), C045(H045), C06N(H06N), C076(H076), C06I(H06I),
 C063(H063), C05H(H05H), C06R(H06R), C06X(H06X), C06T(H06T), C06Y(H06Y),
 C06G(H06G), C036(H036), C055(H055), C04N(H04N), C04L(H04L), C03L(H03L),
 C05J(H05J), C05X(H05X), C067(H067), C06H(H06H), C06M(H06M), C03C(H03C),
 C041(H041), C05F(H05F), C050(H050), C038(H038), C05Q(H05Q), C06Q(H06Q),
 C071(H071), C068(H068), C06C(H06C), C04C(H04C), C05S(H05S), C06L(H06L),
 C07G(H07G), C078(H078), C06O(H06O), C072(H072), C074(H074), C06P(H06P),
 C064(H064), C06D(H06D), C042(H042), C02L(H02L), C05U(H05U), C070(H070)
3.b Fitted hexagon refined as free rotating group:
 C012(C01D,C026,C02B,C02E,C02C), C013(C023,C04H,C03R,C03P,C02N), C014(C030,
 C02I,C02X,C046,C03K), C015(C01E,C03F,C01Z,C02M,C01B), C016(C05A,C05T,C05K,C062,
 C04P), C017(C020,C06F,C065,C03I,C01M), C018(C01K,C03M,C02Y,C029,C022),
 C019(C03T,C03N,C035,C04B,C01L), C01A(C02V,C03Y,C04D,C01N,C01O), C01C(C021,C02Z,
 C032,C04T,C03J), C01F(C02K,C03X,C04S,C04X,C03S), C01G(C02H,C04J,C061,C04W,
 C03A), C01H(C02D,C02G,C027,C03O,C02F), C01J(C037,C02W,C04M,C05R,C02U),
 C01P(C04O,C05I,C04Q,C043,C039), C01R(C01T,C03G,C04Z,C05Z,C04K), C01U(C02J,C052,
 C051,C04G,C053), C01V(C04Y,C060,C03H,C044,C047), C01W(C05L,C05M,C040,C02O,
 C01I), C024(C056,C05Y,C069,C06B,C05C), C025(C057,C05P,C04E,C03E,C033),
 C028(C01S,C04A,C04U,C01Y,C01X), C02A(C04I,C05E,C03V,C04R,C02S), C02P(C054,C05D,
 C05O,C06K,C06A), C02Q(C02T,C03D,C049,C06J,C05W), C02R(C06S,C06E,C048,C05V,
 C05N), C031(C03U,C04V,C066,C05B,C045), C034(C06N,C076,C06I,C063,C05H),
 C03B(C06R,C06X,C06T,C06Y,C06G), C03Q(C036,C055,C04N,C04L,C03L), C03W(C05J,C05X,
 C067,C06H,C06M), C03Z(C03C,C041,C05F,C050,C038), C04F(C05Q,C06Q,C071,C068,
 C06C), C058(C04C,C05S,C06L,C07G,C078), C059(C06O,C072,C074,C06P,C064),
 C06D(C01Q,C042,C02L,C05U,C070)
;
_shelx_res_checksum              11689
_shelx_hkl_checksum              76312
_shelx_fab_checksum              78249
_olex2_submission_special_instructions 'No special instructions were received'