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_4131015
_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         'C160 H149 Ag7 Cu P5, F7 P, 1.5(C4 H10 O)'
_chemical_formula_sum            'C166 H166 Ag7 Cu F7 O1.5 P6'
_chemical_formula_weight         3322.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 93.844(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.290(2)
_cell_length_b                   22.473(2)
_cell_length_c                   38.287(4)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      2.66
_cell_volume                     14843(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0983
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            158946
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.05
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  0.7206
_exptl_absorpt_correction_T_min  0.5925
_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    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6740
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         3.603
_refine_diff_density_min         -2.082
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1595
_refine_ls_number_reflns         26818
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.1373
_refine_ls_R_factor_gt           0.0988
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1180P)^2^+252.4499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2460
_refine_ls_wR_factor_ref         0.2964
_reflns_number_gt                19532
_reflns_number_total             26818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b08674_si_002.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C166 H166 Ag7 Cu F7 O1.50 P6'
_cod_database_code               4131015
_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. Restrained distances
 C64-C65
 1.47 with sigma of 0.01
 C16-C17 = C17-C18 = C18-C19 = C19-C20
 1.53 with sigma of 0.01
 O1-C161
 1.46 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Ag3A)=1-FVAR(1)
 Sof(Ag3)=FVAR(1)
 Fixed Sof: O1(0.5) C161(0.5) H16C(0.5) H16D(0.5) C162(0.5) H16E(0.5)
 H16F(0.5) H16G(0.5) C163(0.5) H16H(0.5) H16I(0.5) C164(0.5) H16J(0.5)
 H16K(0.5) H16L(0.5)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C25(H25), C35(H35), C45(H45), C55(H55)
5.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), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,
 H40B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B),
 C50(H50A,H50B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
  C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,
 H70B), C161(H16C,H16D), C163(H16H,H16I), C165(H16M,H16N), C167(H16R,H16S)
5.c Me refined with riding coordinates:
 C162(H16E,H16F,H16G), C164(H16J,H16K,H16L), C166(H16O,H16P,H16Q), C168(H16T,
 H16U,H16V)
5.d Aromatic/amide H refined with riding coordinates:
 C60(H60), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C78(H78),
 C79(H79), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C86(H86), C87(H87),
  C88(H88), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96),
 C97(H97), C98(H98), C99(H99), C100(H100), C102(H102), C103(H103), C104(H104),
 C105(H105), C106(H106), C108(H108), C109(H109), C110(H110), C111(H111),
 C112(H112), C114(H114), C115(H115), C116(H116), C117(H117), C118(H118),
 C120(H120), C121(H121), C122(H122), C123(H123), C124(H124), C126(H126),
 C127(H127), C128(H128), C129(H129), C130(H130), C132(H132), C133(H133),
 C134(H134), C135(H135), C136(H136), C138(H138), C139(H139), C140(H140),
 C141(H141), C142(H142), C144(H144), C145(H145), C146(H146), C147(H147),
 C148(H148), C150(H150), C151(H151), C152(H152), C153(H153), C154(H154),
 C156(H156), C157(H157), C158(H158), C159(H159), C160(H160)
;
_olex2_submission_special_instructions 'No special instructions were received'