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_4131013
_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         'C138 H122 Ag3 Cu P6, F6 P, 2(C4 H10 O)'
_chemical_formula_sum            'C146 H142 Ag3 Cu F6 O2 P7'
_chemical_formula_weight         2646.54
_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   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                90.00
_cell_angle_beta                 93.058(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.876(2)
_cell_length_b                   24.260(3)
_cell_length_c                   29.799(4)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.22
_cell_volume                     12905(3)
_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_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1461
_diffrn_reflns_av_unetI/netI     0.0972
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            139174
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.14
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.8044
_exptl_absorpt_correction_T_min  0.7029
_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    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5452
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.846
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1445
_refine_ls_number_reflns         23345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+107.9697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.2006
_reflns_number_gt                15045
_reflns_number_total             23345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b08674_si_002.cif
_cod_data_source_block           1
_cod_database_code               4131013
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Ag2(0.7) Ag2'(0.3)
3.a Ternary CH refined with riding coordinates:
 C5(H5), C15(H15), C25(H25)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C139(H13A,
 H13B), C141(H14D,H14E), C143(H14I,H14J), C145(H14N,H14O)
3.c Me refined with riding coordinates:
 C140(H14A,H14B,H14C), C142(H14F,H14G,H14H), C144(H14K,H14L,H14M), C146(H14P,
 H14Q,H14R)
3.d Aromatic/amide H refined with riding coordinates:
 C27(H27), 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), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C128(H128), C129(H129),
 C130(H130), C131(H131), C132(H132), C134(H134), C135(H135), C136(H136),
 C137(H137), C138(H138)
;
_olex2_submission_special_instructions 'No special instructions were received'