Large-scale synthesis, mechanism, and application of a luminescent copper hydride nanocluster.
Xu, Tingting; Wang, Endong; Liu, Shuai; Wei, Zhezhen; Yin, Peiqun; Sun, Jianan; Xu, Wen Wu; Song, Yongbo; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt02595k

data_7714554
_publ_section_title
;
 Large-scale synthesis, mechanism, and application of a luminescent copper
 hydride nanocluster.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt02595k
_journal_year                    2023
_chemical_formula_moiety         'C68 H57 Cl2 Cu4 N4 P4, C24 H20 B'
_chemical_formula_sum            'C92 H77 B Cl2 Cu4 N4 P4'
_chemical_formula_weight         1698.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-28 deposited with the CCDC.	2023-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.903(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0437(3)
_cell_length_b                   30.6258(7)
_cell_length_c                   18.2015(4)
_cell_measurement_reflns_used    25804
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      69.95
_cell_measurement_theta_min      4.21
_cell_volume                     8858.4(3)
_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      120(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34146
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        62.494
_diffrn_reflns_theta_max         62.494
_diffrn_reflns_theta_min         4.209
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    2.661
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2310
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       block
_exptl_crystal_F_000             3484
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.799
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         13781
_refine_ls_number_restraints     1080
_refine_ls_restrained_S_all      0.808
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0460
_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^)+(0.1228P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10498
_reflns_number_total             13781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02595k2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7714554
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C52 \\sim C63 \\sim C46 \\sim C28 \\sim C18 \\sim C57 \\sim C51 \\sim C58 \\sim
C1 \\sim C23 \\sim C56 \\sim C53 \\sim C68 \\sim C62 \\sim C47 \\sim C40 \\sim
C6 \\sim C55 \\sim C41 \\sim C35 \\sim C27 \\sim C5 \\sim C74 \\sim C50 \\sim
C54 \\sim C67 \\sim C86 \\sim C22 \\sim C12 \\sim C2 \\sim C70 \\sim C66 \\sim
C71 \\sim C45 \\sim C26 \\sim C19 \\sim C29 \\sim C3 \\sim C49 \\sim C4 \\sim
C43 \\sim C44 \\sim C73 \\sim C69 \\sim C59 \\sim C80 \\sim C75 \\sim C61 \\sim
C24 \\sim C64 \\sim C36 \\sim C72 \\sim C39 \\sim C7 \\sim C48 \\sim C60 \\sim
C87 \\sim C65 \\sim C13 \\sim C25 \\sim C21 \\sim C88 \\sim C42 \\sim C85 \\sim
C17 \\sim C79 \\sim C76 \\sim C8 \\sim C77 \\sim C38 \\sim C20 \\sim C11 \\sim
C37 \\sim C15 \\sim C81 \\sim C14 \\sim C16 \\sim C78 \\sim C92 \\sim C82 \\sim
C89 \\sim C9 \\sim C10 \\sim C83 \\sim C84 \\sim C90 \\sim C91 \\sim C30 \\sim
C34 \\sim C32 \\sim C31 \\sim C33: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C52) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C51) \\sim Ueq,
Uanis(C58) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C62) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C66)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C73) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C80)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C64) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C60) \\sim Ueq,
Uanis(C87) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C85) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C76)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C78) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C89)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C83) \\sim Ueq,
Uanis(C84) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C51(H51), C58(H58), C56(H56), C53(H53), C68(H68), C62(H62),
 C47(H47), C55(H55), C41(H41), C27(H27), C5(H5), C74(H74), C50(H50), C54(H54),
 C67(H67), C22(H22), C2(H2), C70(H70), C66(H66), C71(H71), C45(H45), C26(H26),
 C19(H19), C3(H3), C49(H49), C4(H4), C43(H43), C44(H44), C73(H73), C59(H59),
 C80(H80), C61(H61), C24(H24), C64(H64), C36(H36), C72(H72), C39(H39), C7(H7),
 C48(H48), C60(H60), C65(H65), C13(H13), C25(H25), C21(H21), C88(H88), C42(H42),
  C85(H85), C17(H17), C79(H79), C76(H76), C8(H8), C77(H77), C38(H38), C20(H20),
 C11(H11), C37(H37), C15(H15), C81(H81), C14(H14), C16(H16), C78(H78), C92(H92),
  C82(H82), C89(H89), C9(H9), C10(H10), C83(H83), C84(H84), C90(H90), C91(H91),
 C30(H30), C34(H34), C32(H32), C31(H31), C33(H33)
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_shelx_res_checksum              83838
_shelx_fab_checksum              52824
_olex2_submission_special_instructions 'No special instructions were received'