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_4131021
_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
'C204 H198 Ag12 Cu3 P6, C188 H182 Ag8 Cu4 P6, 3(F6 P), 6(C4 O), 2(O)'
_chemical_formula_sum            'C416 H440 Ag20 Cu7 F18 O8 P15'
_chemical_formula_weight         8976.41
_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             2016-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                78.6710(10)
_cell_angle_beta                 71.197(2)
_cell_angle_gamma                75.6150(10)
_cell_formula_units_Z            1
_cell_length_a                   19.3944(14)
_cell_length_b                   19.4536(13)
_cell_length_c                   29.451(2)
_cell_measurement_reflns_used    9116
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.78
_cell_measurement_theta_min      2.17
_cell_volume                     10106.4(12)
_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 0.999
_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  0.0948
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            158483
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.16
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  0.6747
_exptl_absorpt_correction_T_min  0.5363
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4530
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.602
_refine_diff_density_min         -4.435
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2047
_refine_ls_number_reflns         36569
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1397P)^2^+43.9066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2047
_refine_ls_wR_factor_ref         0.2390
_reflns_number_gt                26655
_reflns_number_total             36569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b08674_si_002.cif
_cod_data_source_block           9
_cod_original_cell_volume        10106.5(12)
_cod_database_code               4131021
_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
 P7-F1 = P7-F2 = P7-F3 = P7-F4 = P7-F5 = P7-F6
 1.58 with sigma of 0.01
 P8-F7 = P8-F8 = P8-F10 = P8-F11 = P8-F12
 1.58 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: P8(0.5) F7(0.5) F8(0.5) F10(0.5) F11(0.5) F12(0.5) F9(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C184(H18A,H18B)
5.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C108(H10A,H10B,
 H10C), C109(H10D,H10E,H10F), C110(H11A,H11B,H11C), C116(H11D,H11E,H11F),
 C117(H11G,H11H,H11I), C118(H11J,H11K,H11L), C124(H12A,H12B,H12C), C125(H12D,
 H12E,H12F), C126(H12G,H12H,H12I), C132(H13A,H13B,H13C), C133(H13D,H13E,H13F),
 C134(H13G,H13H,H13I), C140(H14D,H14E,H14F), C141(H14G,H14H,H14I), C142(H14J,
 H14K,H14L)
5.c Aromatic/amide H refined with riding coordinates:
 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), 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), C162(H162), C163(H163),
 C164(H164), C165(H165), C166(H166), C168(H168), C169(H169), C170(H170),
 C171(H171), C172(H172), C174(H174), C175(H175), C176(H176), C177(H177),
 C178(H178), C180(H180), C181(H181), C182(H182), C183(H183), C186(H186),
 C187(H187), C188(H188), C189(H189), C190(H190), C192(H192), C193(H193),
 C194(H194), C195(H195), C196(H196)
;
_olex2_submission_special_instructions 'No special instructions were received'