Polypyridyl-functionalizated alkynyl gold(I) metallaligands supported by tri- and tetradentate phosphanes
Ferrer, Montserrat; Giménez, Leticia; Gutiérrez, Albert; Lima, J. C. Carlos; Rodriguez, Laura; Martinez, Manuel; Martín, Avelino; Puttreddy, Rakesh; Rissanen, Kari; Dalton Trans.  (2017) –; doi:10.1039/C7DT02732J

data_7044235
_publ_section_title
;
 Polypyridyl-functionalizated alkynyl gold(I) metallaligands supported by
 tri- and tetradentate phosphanes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02732J
_journal_year                    2017
_chemical_formula_moiety         '4(C101 H76 Au4 N8 P4), 7(C H2 Cl2)'
_chemical_formula_sum            'C411 H318 Au16 Cl14 N32 P16'
_chemical_formula_weight         9848.24
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-07-13 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.877(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   33.1673(9)
_cell_length_b                   17.3472(5)
_cell_length_c                   34.8570(14)
_cell_measurement_reflns_used    22386
_cell_measurement_temperature    120
_cell_measurement_theta_max      76.0630
_cell_measurement_theta_min      3.2850
_cell_volume                     19290.2(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -49.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176   37.0000    0.0000 82

  2 omega -107.00  -14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  -57.0000 -150.0000 93

  3 omega   55.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1176 -125.0000 -180.0000 38

  4 omega   36.00   93.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  150.0000 57

  5 omega   29.00   60.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   30.0000 31

  6 omega   65.00  109.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   30.0000 44

  7 omega   86.00  174.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -90.0000 88

  8 omega   39.00   90.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   90.0000 51

  9 omega   39.00   94.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  150.0000 55

 10 omega   39.00   99.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000    0.0000 60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0281350000
_diffrn_orient_matrix_UB_12      -0.0182585000
_diffrn_orient_matrix_UB_13      0.0421274000
_diffrn_orient_matrix_UB_21      -0.0392933000
_diffrn_orient_matrix_UB_22      -0.0121176000
_diffrn_orient_matrix_UB_23      0.0148078000
_diffrn_orient_matrix_UB_31      -0.0004002000
_diffrn_orient_matrix_UB_32      -0.0859393000
_diffrn_orient_matrix_UB_33      -0.0109366000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            60809
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.749
_diffrn_reflns_theta_max         66.749
_diffrn_reflns_theta_min         3.260
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.090
_exptl_absorpt_correction_T_max  0.305
_exptl_absorpt_correction_T_min  0.144
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       block
_exptl_crystal_F_000             9500
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         8.516
_refine_diff_density_min         -3.241
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1777
_refine_ls_number_reflns         33966
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.1094
_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^)+(0.0815P)^2^+761.0872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2547
_refine_ls_wR_factor_ref         0.2650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27931
_reflns_number_total             33966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02732j2.cif
_cod_data_source_block           tetraphosbipy
_cod_original_cell_volume        19290.2(12)
_cod_database_code               7044235
_chemical_oxdiff_formula         'C101 H200 N8 P4 Au4'
_shelx_estimated_absorpt_t_max   0.281
_shelx_estimated_absorpt_t_min   0.153
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C3S-Cl5S
 1.7 with sigma of 0.02
 Cl6S-C3S
 1.7 with sigma of 0.02
 C4S-Cl8S
 1.79 with sigma of 0.02
 C4S-Cl7S
 1.79 with sigma of 0.02
 C2S-Cl3S
 1.79 with sigma of 0.02
 Cl4S-C2S
 1.79 with sigma of 0.02
 C7A-C8A
 1.54 with sigma of 0.01
 C44A-C43A
 1.5 with sigma of 0.01
 Au2-C1C
 1.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1S) \\sim Ueq, Uanis(C1S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl10) \\sim Ueq, Uanis(C5S) \\sim Ueq, Uanis(Cl9S) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3A) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(C6A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C6A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C3A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C45A) \\sim Ueq, Uanis(C44A) \\sim Ueq, Uanis(N8A) \\sim Ueq, Uanis(C48A)
\\sim Ueq, Uanis(C47A) \\sim Ueq, Uanis(C46A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C43A) \\sim Ueq, Uanis(C42A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.01
Uanis(C39A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C2S) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C1C) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C24A) = Uanis(C23A) = Uanis(C22A) = Uanis(C21A) = Uanis(C20A)
Uanis(C91A) = Uanis(C94A)
Uanis(C96A) = Uanis(C95A) = Uanis(C93A) = Uanis(C92A)
Uanis(Cl8S) = Uanis(C4S) = Uanis(Cl7S)
Uanis(Cl6S) = Uanis(C3S) = Uanis(Cl5S)
Uanis(C4A) = Uanis(C7A)
Uanis(C6A) = Uanis(C5A) = Uanis(C4A) = Uanis(C3A) = Uanis(N1A) = Uanis(C7A)
Uanis(C4A) = Uanis(C2A) = Uanis(C1A) = Uanis(C9A) = Uanis(C10A) = Uanis(C11A) =
Uanis(C12A) = Uanis(N2A) = Uanis(C8A)
Uanis(C41A) = Uanis(C42A) = Uanis(N7A) = Uanis(C39A)
Uanis(C44A) = Uanis(N8A) = Uanis(C48A) = Uanis(C45A) = Uanis(C46A) = Uanis(C47A)
Uanis(C67) = Uanis(C70)
Uanis(C68) = Uanis(C69) = Uanis(C71) = Uanis(C72)
Uanis(C49) = Uanis(C52)
Uanis(C54) = Uanis(C53) = Uanis(C51) = Uanis(C50)
Uanis(C23) = Uanis(C20) = Uanis(C19) = Uanis(C16)
Uanis(C21) = Uanis(C22) = Uanis(C24) = Uanis(N4) = Uanis(C17)
Uanis(C56) = Uanis(C55) = Uanis(C60) = Uanis(C59) = Uanis(C58) = Uanis(C57)
Uanis(C74) = Uanis(C75) = Uanis(C77) = Uanis(C78)
Uanis(C18) = Uanis(C17)
Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(N3)
Uanis(C4) = Uanis(C2) = Uanis(C1)
Uanis(C85) = Uanis(C88)
Uanis(C86) = Uanis(C90)
Uanis(C87) = Uanis(C89)
Uanis(C80) = Uanis(C84)
Uanis(C83) = Uanis(C81)
Uanis(C82) = Uanis(C79)
4. Others
 Fixed Sof: Cl1S(0.5) Cl2S(0.5) Cl3S(0.5) Cl4S(0.5) Cl5S(0.5) Cl6S(0.5)
 Cl7S(0.5) Cl8S(0.5) Cl9S(0.5) Cl10(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) C2S(0.5)
 H2SA(0.5) H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5)
 C5S(0.5) H5SA(0.5) H5SB(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,
 H5SB), C6S(H6SA,H6SB), C13(H13A,H13B), C14(H14A,H14B), C98(H98A,H98B),
 C98A(H98C,H98D), C99(H99A,H99B), C99A(H99C,H99D), C100(H10B,H10C), C101(H10D,
 H10E)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C3A(H3A), C5A(H5A), C6A(H6A), C5(H5), C6(H6), C9A(H9A), C10A(H10A),
 C11A(H11A), C12A(H12A), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15),
 C17(H17), C18(H18), C15A(H15A), C17A(H17A), C18A(H18A), C21(H21), C22(H22),
 C23(H23), C24(H24), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C27(H27),
 C27A(H27A), C29(H29), C29A(H29A), C30(H30), C30A(H30A), C33(H33), C33A(H33A),
 C34(H34), C34A(H34A), C35(H35), C35A(H35A), C36(H36), C36A(H36A), C39(H39),
 C39A(H39A), C42A(H42A), C41A(H41A), C41(H41), C42(H42), C45A(H45A), C46A(H46A),
  C47A(H47A), C48A(H48A), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50),
 C50A(H50A), C51(H51), C51A(H51A), C52(H52), C52A(H52A), C53(H53), C53A(H53A),
 C54(H54), C54A(H54A), C56(H56), C56A(H56A), C57(H57), C57A(H57A), C58(H58),
 C58A(H58A), C59(H59), C59A(H59A), C60(H60), C60A(H60A), C62(H62), C62A(H62A),
 C63(H63), C63A(H63A), C64(H64), C64A(H64A), C65(H65), C65A(H65A), C66(H66),
 C66A(H66A), C68(H68), C68A(H68A), C69(H69), C69A(H69A), C70(H70), C70A(H70A),
 C71(H71), C71A(H71A), C72(H72), C72A(H72A), C74A(H74A), C75A(H75A), C76A(H76A),
  C77A(H77A), C78(H78), C74(H74), C75(H75), C76(H76), C77(H77), C78A(H78A),
 C80(H80), C80A(H80A), C81(H81), C81A(H81A), C82(H82), C82A(H82A), C83(H83),
 C83A(H83A), C84(H84), C84A(H84A), C86(H86), C86A(H86A), C87(H87), C87A(H87A),
 C88(H88), C88A(H88A), C89(H89), C89A(H89A), C90(H90), C90A(H90A), C92(H92),
 C92A(H92A), C93(H93), C93A(H93A), C94(H94), C94A(H94A), C95(H95), C95A(H95A),
 C96(H96), C96A(H96A)
5.c Fitted hexagon refined as free rotating group:
 C3A(C4A,C5A,C6A,C7A,N1A), C8A(C9A,C10A,C11A,C12A,N2A), C15(C16,C17,C18,C19,
 N3), C20(C21,C22,C23,C24,N4), C40A(C39A,N7A,C43A,C42A,C41A), C44A(C45A,C46A,
 C47A,C48A,N8A), C78(C73,C74,C75,C76,C77)
;
_shelx_res_checksum              26002
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'