Syntheses, structures and theoretical investigations of [Au10S2(PPh2)2(dppma2)4(dppma3)]·[Au6S2(dppma2)2(dppma3)].
Yu, Wen; Guggolz, Lukas; Fuhr, Olaf; Fenske, Dieter; Dehnen, Stefanie; Dalton transactions (Cambridge, England : 2003) 44 (2015) 9363–9366; doi:10.1039/c5dt01360g

data_7035063
_publ_section_title
;
 Syntheses, structures and theoretical investigations of
 [Au10S2(PPh2)2(dppma2)4(dppma3)]&#x00B7;[Au6S2(dppma2)2(dppma3)].
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9363
_journal_page_last               9366
_journal_paper_doi               10.1039/c5dt01360g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C116 H82 Au10 O15 P8 S6, C60 H42 Au6 O9 P4 S4, 8(C H2 Cl2), C7 H16'
_chemical_formula_sum            'C191 H156 Au16 Cl16 O24 P12 S10'
_chemical_formula_weight         7246.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-03-13 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                92.1940(10)
_cell_angle_beta                 91.0980(10)
_cell_angle_gamma                93.1300(10)
_cell_formula_units_Z            2
_cell_length_a                   15.4644(3)
_cell_length_b                   25.0982(5)
_cell_length_c                   27.0905(4)
_cell_measurement_reflns_used    143373
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      30.71
_cell_measurement_theta_min      1.50
_cell_volume                     10488.8(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
 2001 frames, detector distance = 80 mm
;
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'Stoe StadiVari Mo'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.3 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_laue_measured_fraction_full 0.983
_diffrn_reflns_laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            79203
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.100
_diffrn_reflns_theta_min         1.505
_diffrn_source                   'Mo GeniX 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            Cu
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.596
_exptl_absorpt_correction_T_max  0.3416
_exptl_absorpt_correction_T_min  0.0237
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.294
_exptl_crystal_description       needle
_exptl_crystal_F_000             6740
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.411
_refine_diff_density_min         -3.994
_refine_diff_density_rms         0.397
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2266
_refine_ls_number_reflns         40454
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1327P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31663
_reflns_number_total             40454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01360g2.cif
_cod_data_source_block           wen477_neu
_cod_depositor_comments          'Adding full bibliography for 7035063.cif.'
_cod_database_code               7035063
_shelxl_version_number           2013-4
_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
 Cl15-C184 = Cl16-C184
 1.76 with sigma of 0.02
 C185-C186 = C186-C187 = C187-C188 = C188-C189 = C189-C190 = C190-C191
 1.54 with sigma of 0.02
 C185-C187 = C186-C188 = C187-C189 = C188-C190 = C189-C191
 2.51 with sigma of 0.02
3. Others
 Fixed Sof: C74A(0.5) H74A(0.5) C74B(0.5) H74B(0.5) C75A(0.5) H75A(0.5)
 C75B(0.5) H75B(0.5) C76A(0.5) H76A(0.5) C76B(0.5) H76B(0.5) H77A(0.5) H77B(0.5)
4.a Ternary CH refined with riding coordinates:
 C57(H57), C60(H60), C129(H129), C132(H132)
4.b Secondary CH2 refined with riding coordinates:
 C178(H17A,H17B), C177(H17C,H17D), C179(H17E,H17F), C180(H18N,H18O), C181(H18P,
 H18Q), C182(H18R,H18S), C183(H18L,H18M), C184(H18T,H18U), C186(H18D,H18E),
 C187(H18F,H18G), C188(H18H,H18I), C189(H18J,H18K), C190(H19A,H19B)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68),
  C69(H69), C70(H70), C71(H71), C72(H72), C74A(H74A), C74B(H74B), C75A(H75A),
 C75B(H75B), C76A(H76A), C76B(H76B), C77(H77A), C77(H77B), C78(H78), C80(H80),
 C81(H81), C82(H82), C83(H83), C84(H84), C90(H90), C91(H91), C92(H92), C93(H93),
  C94(H94), C96(H96), C97(H97), C98(H98), C99(H99), C100(H100), C106(H106),
 C107(H107), C108(H108), C109(H109), C110(H110), C112(H112), C113(H113),
 C114(H114), C115(H115), C116(H116), C118(H118), C119(H119), C120(H120),
 C121(H121), C122(H122), C124(H124), C125(H125), C126(H126), C127(H127),
 C128(H128), C134(H134), C135(H135), C136(H136), C137(H137), C138(H138),
 C140(H140), C141(H141), C142(H142), C143(H143), C144(H144), C150(H150),
 C151(H151), C152(H152), C153(H153), C154(H154), C156(H156), C157(H157),
 C158(H158), C159(H159), C160(H160), C166(H166), C167(H167), C168(H168),
 C169(H169), C170(H170), C172(H172), C173(H173), C174(H174), C175(H175),
 C176(H176)
4.d Idealised Me refined as rotating group:
 C185(H18A,H18B,H18C), C191(H19C,H19D,H19E)
;
_olex2_submission_special_instructions 'No special instructions were received'