Assembly of Heterometallic Silver(I)-Copper(I) Alkyl-1,3-diynyl Clusters via Inner-Core Expansion.
Hau, Sam C. K.; Yeung, Margaret C.-L.; Yam, Vivian W.-W.; Mak, Thomas C. W.; Journal of the American Chemical Society 138 (2016) 13732–13739; doi:10.1021/jacs.6b08674

data_4131014
_publ_section_title
;
 Assembly of Heterometallic Silver(I)-Copper(I) Alkyl-1,3-diynyl Clusters
 via Inner-Core Expansion.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13732
_journal_page_last               13739
_journal_paper_doi               10.1021/jacs.6b08674
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C129 H111 Ag3 Cu P6, 2(F3 P0.5)'
_chemical_formula_sum            'C129 H111 Ag3 Cu F6 P7'
_chemical_formula_weight         2379.12
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                94.708(2)
_cell_angle_beta                 90.237(2)
_cell_angle_gamma                111.692(2)
_cell_formula_units_Z            2
_cell_length_a                   13.6648(14)
_cell_length_b                   15.9205(18)
_cell_length_c                   27.740(3)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.28
_cell_volume                     5584.7(10)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1379
_diffrn_reflns_av_unetI/netI     0.1186
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            81763
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         0.74
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.7811
_exptl_absorpt_correction_T_min  0.6712
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2428
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.353
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1318
_refine_ls_number_reflns         20074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.2005
_reflns_number_gt                13796
_reflns_number_total             20074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b08674_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        5584.6(11)
_cod_database_code               4131014
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C12(H12), C19(H19)
2.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39),
  C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48),
 C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66),
 C67(H67), C68(H68), C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
  C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C83(H83), C84(H84),
 C85(H85), C86(H86), C87(H87), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93),
  C95(H95), C96(H96), C97(H97), C98(H98), C99(H99), C101(H101), C102(H102),
 C103(H103), C104(H104), C105(H105), C107(H107), C108(H108), C109(H109),
 C110(H110), C111(H111), C113(H113), C114(H114), C115(H115), C116(H116),
 C117(H117), C119(H119), C120(H120), C121(H121), C122(H122), C123(H123),
 C125(H125), C126(H126), C127(H127), C128(H128), C129(H129)
;
_olex2_submission_special_instructions 'No special instructions were received'