#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:25:19 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178650 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/61/4076153.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4076153
loop_
_publ_author_name
'Vicente, José'
'Chicote, María-Teresa'
'Alvarez-Falcón, Miguel M.'
'Jones, Peter G.'
_publ_section_title
;
 Gold(I) Complexes Derived from C6Me3(C⋮CH)3-1,3,5,
 C6Me4(C⋮CH)2-1,4, and MeC6H4C⋮CH-4§
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5956
_journal_paper_doi               10.1021/om050665f
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C66 H56 Au N P2'
_chemical_formula_weight         1122.02
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 133.930(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.829(2)
_cell_length_b                   12.7529(11)
_cell_length_c                   19.8249(14)
_cell_measurement_reflns_used    7817
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.7
_cell_volume                     5067.1(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'ω- & φ-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39441
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    3.010
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            amber
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.451
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment
'acetylenic H free with SADI, rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         7397
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0367P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                6272
_reflns_number_total             7397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050665fsi20050802_013525.cif
_cod_data_source_block           bernie
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (15
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (23 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5067.2(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4076153
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Au Au 0.5000 0.705368(10) 0.2500 0.02573(4) Uani 1 2 d S
C1 C 0.43833(13) 0.6967(2) 0.26762(17) 0.0315(5) Uani 1 1 d U
C2 C 0.40485(12) 0.6763(2) 0.28396(16) 0.0304(5) Uani 1 1 d U
C3 C 0.36922(11) 0.6454(2) 0.30927(15) 0.0278(5) Uani 1 1 d U
C4 C 0.38675(11) 0.5515(2) 0.35824(15) 0.0282(5) Uani 1 1 d U
C5 C 0.35341(11) 0.5210(2) 0.38553(15) 0.0279(5) Uani 1 1 d U
C6 C 0.30061(11) 0.5830(2) 0.35983(15) 0.0280(5) Uani 1 1 d U
C7 C 0.28373(11) 0.6749(2) 0.31004(16) 0.0295(5) Uani 1 1 d U
C8 C 0.31832(12) 0.7097(2) 0.28592(16) 0.0295(5) Uani 1 1 d U
C9 C 0.44037(11) 0.4844(2) 0.37975(17) 0.0318(5) Uani 1 1 d U
H9A H 0.4276 0.4652 0.3212 0.038 Uiso 1 1 calc R
H9B H 0.4460 0.4206 0.4123 0.038 Uiso 1 1 calc R
H9C H 0.4824 0.5235 0.4198 0.038 Uiso 1 1 calc R
C10 C 0.37380(11) 0.4284(2) 0.44140(16) 0.0297(5) Uani 1 1 d U
C11 C 0.39164(14) 0.3541(2) 0.48995(19) 0.0372(6) Uani 1 1 d DU
H11 H 0.4077(18) 0.298(2) 0.530(2) 0.055(10) Uiso 1 1 d D
C12 C 0.26243(12) 0.5509(2) 0.38516(17) 0.0350(6) Uani 1 1 d U
H12A H 0.2643 0.6075 0.4203 0.042 Uiso 1 1 calc R
H12B H 0.2825 0.4874 0.4237 0.042 Uiso 1 1 calc R
H12C H 0.2158 0.5369 0.3278 0.042 Uiso 1 1 calc R
C13 C 0.22841(13) 0.7370(2) 0.28008(18) 0.0340(5) Uani 1 1 d U
C14 C 0.18135(16) 0.7842(3) 0.2505(2) 0.0444(7) Uani 1 1 d DU
H14 H 0.1426(16) 0.824(3) 0.219(3) 0.071(12) Uiso 1 1 d D
C15 C 0.30013(14) 0.8115(2) 0.2359(2) 0.0382(6) Uani 1 1 d U
H15A H 0.3349 0.8316 0.2375 0.046 Uiso 1 1 calc R
H15B H 0.2961 0.8658 0.2667 0.046 Uiso 1 1 calc R
H15C H 0.2575 0.8040 0.1707 0.046 Uiso 1 1 calc R
P P 0.54629(2) 0.11567(4) 0.35318(3) 0.01789(10) Uani 1 1 d .
N N 0.5000 0.0707(2) 0.2500 0.0217(5) Uani 1 2 d S
C21 C 0.58030(11) 0.24409(18) 0.37057(14) 0.0211(4) Uani 1 1 d DU
C22 C 0.63578(12) 0.2540(2) 0.38311(17) 0.0291(5) Uani 1 1 d DU
H22 H 0.6587 0.1934 0.3899 0.035 Uiso 1 1 calc R
C23 C 0.65764(14) 0.3537(2) 0.38574(19) 0.0385(6) Uani 1 1 d DU
H23 H 0.6959 0.3610 0.3952 0.046 Uiso 1 1 calc R
C24 C 0.62380(13) 0.4421(2) 0.37467(17) 0.0364(6) Uani 1 1 d DU
H24 H 0.6384 0.5096 0.3751 0.044 Uiso 1 1 calc R
C25 C 0.56918(13) 0.4326(2) 0.36299(16) 0.0332(5) Uani 1 1 d DU
H25 H 0.5467 0.4936 0.3565 0.040 Uiso 1 1 calc R
C26 C 0.54685(12) 0.33401(19) 0.36072(15) 0.0265(5) Uani 1 1 d DU
H26 H 0.5090 0.3275 0.3525 0.032 Uiso 1 1 calc R
C31 C 0.50371(10) 0.12076(17) 0.39162(13) 0.0205(4) Uani 1 1 d DU
C32 C 0.44594(11) 0.06147(19) 0.34418(15) 0.0267(5) Uani 1 1 d DU
H32 H 0.4280 0.0223 0.2902 0.032 Uiso 1 1 calc R
C33 C 0.41466(12) 0.0601(2) 0.37674(17) 0.0320(5) Uani 1 1 d DU
H33 H 0.3750 0.0203 0.3443 0.038 Uiso 1 1 calc R
C34 C 0.44067(12) 0.1156(2) 0.45522(16) 0.0295(5) Uani 1 1 d DU
H34 H 0.4190 0.1138 0.4768 0.035 Uiso 1 1 calc R
C35 C 0.49809(12) 0.1743(2) 0.50310(17) 0.0305(5) Uani 1 1 d DU
H35 H 0.5158 0.2127 0.5573 0.037 Uiso 1 1 calc R
C36 C 0.52990(11) 0.17688(19) 0.47158(15) 0.0267(5) Uani 1 1 d DU
H36 H 0.5695 0.2169 0.5045 0.032 Uiso 1 1 calc R
C41 C 0.61568(10) 0.02677(17) 0.43016(14) 0.0210(4) Uani 1 1 d DU
C42 C 0.66757(10) 0.05034(19) 0.52566(14) 0.0261(5) Uani 1 1 d DU
H42 H 0.6669 0.1140 0.5499 0.031 Uiso 1 1 calc R
C43 C 0.71992(11) -0.0196(2) 0.58458(16) 0.0327(5) Uani 1 1 d DU
H43 H 0.7548 -0.0043 0.6495 0.039 Uiso 1 1 calc R
C44 C 0.72163(12) -0.1115(2) 0.54929(17) 0.0355(6) Uani 1 1 d DU
H44 H 0.7582 -0.1583 0.5899 0.043 Uiso 1 1 calc R
C45 C 0.67023(13) -0.1360(2) 0.45491(18) 0.0345(5) Uani 1 1 d DU
H45 H 0.6715 -0.1995 0.4311 0.041 Uiso 1 1 calc R
C46 C 0.61693(11) -0.06695(19) 0.39550(15) 0.0269(5) Uani 1 1 d DU
H46 H 0.5813 -0.0839 0.3311 0.032 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Au C1 173.56(15) 2_655 y
C2 C1 Au 170.0(2) . y
C1 C2 C3 175.1(3) . y
C4 C3 C8 120.9(2) . y
C4 C3 C2 118.8(2) . y
C8 C3 C2 120.3(2) . y
C3 C4 C5 119.7(2) . y
C3 C4 C9 119.0(2) . y
C5 C4 C9 121.4(2) . y
C4 C5 C6 120.1(2) . y
C4 C5 C10 120.4(2) . y
C6 C5 C10 119.5(2) . y
C7 C6 C5 118.9(2) . y
C7 C6 C12 119.7(2) . y
C5 C6 C12 121.4(2) . y
C6 C7 C8 122.2(2) . y
C6 C7 C13 119.6(2) . y
C8 C7 C13 118.2(2) . y
C3 C8 C7 118.2(2) . y
C3 C8 C15 121.7(2) . y
C7 C8 C15 120.1(2) . y
C11 C10 C5 177.9(3) . y
C14 C13 C7 175.8(3) . y
N P C31 112.01(7) . ?
N P C21 115.10(11) . ?
C31 P C21 107.39(10) . ?
N P C41 107.39(10) . ?
C31 P C41 107.28(9) . ?
C21 P C41 107.31(10) . ?
P N P 137.63(18) 2_655 ?
C22 C21 C26 119.9(2) . ?
C22 C21 P 119.26(19) . ?
C26 C21 P 120.45(17) . ?
C21 C22 C23 119.5(2) . ?
C24 C23 C22 120.3(2) . ?
C25 C24 C23 120.4(2) . ?
C24 C25 C26 120.2(2) . ?
C25 C26 C21 119.8(2) . ?
C32 C31 C36 119.54(19) . ?
C32 C31 P 118.97(16) . ?
C36 C31 P 121.33(16) . ?
C31 C32 C33 119.4(2) . ?
C34 C33 C32 120.6(2) . ?
C33 C34 C35 120.5(2) . ?
C34 C35 C36 119.8(2) . ?
C35 C36 C31 120.2(2) . ?
C46 C41 C42 119.7(2) . ?
C46 C41 P 120.07(16) . ?
C42 C41 P 120.19(17) . ?
C43 C42 C41 119.7(2) . ?
C44 C43 C42 120.3(2) . ?
C43 C44 C45 120.5(2) . ?
C44 C45 C46 119.6(2) . ?
C41 C46 C45 120.2(2) . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au C1 1.978(3) . y
Au C1 1.978(3) 2_655 ?
C1 C2 1.208(4) . y
C2 C3 1.442(3) . y
C3 C4 1.400(4) . y
C3 C8 1.408(3) . y
C4 C5 1.415(3) . y
C4 C9 1.503(3) . y
C5 C6 1.417(3) . y
C5 C10 1.438(4) . y
C6 C7 1.387(4) . y
C6 C12 1.513(3) . y
C7 C8 1.411(3) . y
C7 C13 1.442(4) . y
C8 C15 1.493(4) . y
C10 C11 1.187(4) . y
C13 C14 1.165(4) . y
P N 1.5862(11) . ?
P C31 1.801(2) . ?
P C21 1.801(2) . ?
P C41 1.804(2) . ?
N P 1.5862(11) 2_655 ?
C21 C22 1.389(3) . ?
C21 C26 1.403(3) . ?
C22 C23 1.394(4) . ?
C23 C24 1.385(4) . ?
C24 C25 1.375(4) . ?
C25 C26 1.389(3) . ?
C31 C32 1.394(3) . ?
C31 C36 1.397(3) . ?
C32 C33 1.398(3) . ?
C33 C34 1.373(3) . ?
C34 C35 1.382(3) . ?
C35 C36 1.394(3) . ?
C41 C46 1.391(3) . ?
C41 C42 1.402(3) . ?
C42 C43 1.386(3) . ?
C43 C44 1.383(4) . ?
C44 C45 1.390(3) . ?
C45 C46 1.393(3) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C11 H11 Au 0.92(3) 3.18(3) 3.831(3) 130(3) 5_666
