#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:07:11 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178595 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/06/4070653.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_4070653
loop_
_publ_author_name
'Vicente, José'
'Gil-Rubio, Juan'
'Barquero, Natalia'
'Jones, Peter G.'
'Bautista, Delia'
_publ_section_title
;
 Synthesis of Luminescent Alkynyl Gold Metalaligands Containing
 2,2′-Bipyridine-5-yl and
 2,2′:6′,2′′-Terpyridine-4-yl Donor Groups
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              646
_journal_paper_doi               10.1021/om7009123
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C60 H44 Au N5 P2'
_chemical_formula_weight         1093.91
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.802(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.492(3)
_cell_length_b                   12.3916(12)
_cell_length_c                   15.1409(15)
_cell_measurement_reflns_used    5039
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.18
_cell_volume                     4644.7(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       ω-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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25052
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    3.284
_exptl_absorpt_correction_T_max  0.8530
_exptl_absorpt_correction_T_min  0.4940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.462
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.254
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4752
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0211P)²+22.7639P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0808
_reflns_number_gt                4629
_reflns_number_total             4752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7009123-file007.cif
_cod_data_source_block           1nba235as
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4070653
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
Au1 Au 0.0000 0.508470(17) 0.2500 0.01780(7) Uani 1 2 d S
N1 N 0.21515(15) 0.5727(3) 0.0648(3) 0.0277(8) Uani 1 1 d DU
N2 N 0.24300(15) 0.4984(3) -0.1472(2) 0.0268(8) Uani 1 1 d DU
N3 N 0.0000 0.9757(4) 0.7500 0.0161(10) Uani 1 2 d SU
P1 P 0.05696(4) 0.93345(8) 0.80658(6) 0.0138(2) Uani 1 1 d U
C1 C 0.05465(18) 0.5090(3) 0.1768(3) 0.0238(9) Uani 1 1 d U
C2 C 0.08697(19) 0.5124(3) 0.1300(3) 0.0261(9) Uani 1 1 d U
C3 C 0.12532(18) 0.5212(3) 0.0748(3) 0.0250(9) Uani 1 1 d DU
C4 C 0.1131(2) 0.4947(4) -0.0179(3) 0.0299(10) Uani 1 1 d DU
H4 H 0.0783 0.4678 -0.0467 0.036 Uiso 1 1 calc R
C5 C 0.15159(19) 0.5076(3) -0.0672(3) 0.0280(10) Uani 1 1 d DU
H5 H 0.1436 0.4902 -0.1301 0.034 Uiso 1 1 calc R
C6 C 0.20197(17) 0.5463(3) -0.0240(3) 0.0213(9) Uani 1 1 d DU
C7 C 0.17758(19) 0.5596(4) 0.1122(3) 0.0289(10) Uani 1 1 d DU
H7 H 0.1869 0.5775 0.1750 0.035 Uiso 1 1 calc R
C8 C 0.24425(17) 0.5635(3) -0.0749(3) 0.0212(9) Uani 1 1 d DU
C9 C 0.28112(18) 0.5149(4) -0.1941(3) 0.0274(10) Uani 1 1 d DU
H9 H 0.2809 0.4704 -0.2453 0.033 Uiso 1 1 calc R
C10 C 0.32044(18) 0.5936(4) -0.1713(3) 0.0279(10) Uani 1 1 d DU
H10 H 0.3467 0.6025 -0.2060 0.034 Uiso 1 1 calc R
C11 C 0.32101(18) 0.6590(4) -0.0974(3) 0.0257(9) Uani 1 1 d DU
H11 H 0.3474 0.7141 -0.0806 0.031 Uiso 1 1 calc R
C12 C 0.28282(17) 0.6433(3) -0.0485(3) 0.0222(9) Uani 1 1 d DU
H12 H 0.2828 0.6869 0.0032 0.027 Uiso 1 1 calc R
C21 C 0.09415(16) 0.8528(3) 0.7434(3) 0.0173(8) Uani 1 1 d DU
C22 C 0.08484(16) 0.8667(3) 0.6499(3) 0.0188(8) Uani 1 1 d DU
H22 H 0.0568 0.9134 0.6194 0.023 Uiso 1 1 calc R
C23 C 0.11625(17) 0.8129(3) 0.6008(3) 0.0215(9) Uani 1 1 d DU
H23 H 0.1094 0.8221 0.5368 0.026 Uiso 1 1 calc R
C24 C 0.15746(18) 0.7458(3) 0.6451(3) 0.0247(9) Uani 1 1 d DU
H24 H 0.1794 0.7099 0.6117 0.030 Uiso 1 1 calc R
C25 C 0.16678(19) 0.7310(4) 0.7379(3) 0.0283(10) Uani 1 1 d DU
H25 H 0.1950 0.6846 0.7682 0.034 Uiso 1 1 calc R
C26 C 0.13509(18) 0.7836(3) 0.7872(3) 0.0240(9) Uani 1 1 d DU
H26 H 0.1414 0.7724 0.8509 0.029 Uiso 1 1 calc R
C31 C 0.09788(16) 1.0519(3) 0.8423(2) 0.0158(8) Uani 1 1 d DU
C32 C 0.07797(17) 1.1551(3) 0.8183(3) 0.0208(9) Uani 1 1 d DU
H32 H 0.0411 1.1640 0.7876 0.025 Uiso 1 1 calc R
C33 C 0.11083(17) 1.2447(3) 0.8381(3) 0.0245(9) Uani 1 1 d DU
H33 H 0.0966 1.3145 0.8209 0.029 Uiso 1 1 calc R
C34 C 0.16477(17) 1.2326(3) 0.8835(3) 0.0228(9) Uani 1 1 d DU
H34 H 0.1877 1.2939 0.8966 0.027 Uiso 1 1 calc R
C35 C 0.18486(16) 1.1303(3) 0.9093(3) 0.0226(9) Uani 1 1 d DU
H35 H 0.2214 1.1221 0.9417 0.027 Uiso 1 1 calc R
C36 C 0.15216(16) 1.0403(3) 0.8884(3) 0.0184(8) Uani 1 1 d DU
H36 H 0.1665 0.9705 0.9054 0.022 Uiso 1 1 calc R
C41 C 0.05130(15) 0.8580(3) 0.9053(2) 0.0161(8) Uani 1 1 d DU
C42 C 0.03605(16) 0.7500(3) 0.8964(3) 0.0201(8) Uani 1 1 d DU
H42 H 0.0355 0.7125 0.8414 0.024 Uiso 1 1 calc R
C43 C 0.02163(17) 0.6972(3) 0.9682(3) 0.0220(9) Uani 1 1 d DU
H43 H 0.0104 0.6239 0.9618 0.026 Uiso 1 1 calc R
C44 C 0.02359(17) 0.7514(3) 1.0489(3) 0.0223(9) Uani 1 1 d DU
H44 H 0.0144 0.7149 1.0983 0.027 Uiso 1 1 calc R
C45 C 0.03891(17) 0.8585(3) 1.0577(3) 0.0210(9) Uani 1 1 d DU
H45 H 0.0398 0.8955 1.1130 0.025 Uiso 1 1 calc R
C46 C 0.05299(16) 0.9123(3) 0.9863(3) 0.0173(8) Uani 1 1 d DU
H46 H 0.0637 0.9859 0.9927 0.021 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
C1 Au1 C1 179.6(2) 2
C7 N1 C6 117.8(4) .
C9 N2 C8 117.0(4) .
P1 N3 P1 141.5(3) 2_556
N3 P1 C41 112.06(15) .
N3 P1 C21 115.20(15) .
C41 P1 C21 108.04(18) .
N3 P1 C31 106.4(2) .
C41 P1 C31 109.19(18) .
C21 P1 C31 105.67(18) .
C2 C1 Au1 177.5(4) .
C1 C2 C3 177.6(5) .
C7 C3 C4 116.6(4) .
C7 C3 C2 120.3(4) .
C4 C3 C2 123.1(4) .
C5 C4 C3 119.8(4) .
C4 C5 C6 119.1(4) .
N1 C6 C5 122.7(4) .
N1 C6 C8 116.4(4) .
C5 C6 C8 120.9(4) .
N1 C7 C3 123.9(4) .
N2 C8 C12 122.5(4) .
N2 C8 C6 117.1(4) .
C12 C8 C6 120.4(4) .
N2 C9 C10 123.1(4) .
C11 C10 C9 119.0(4) .
C12 C11 C10 118.9(4) .
C11 C12 C8 119.5(4) .
C22 C21 C26 119.3(4) .
C22 C21 P1 119.2(3) .
C26 C21 P1 121.3(3) .
C23 C22 C21 120.4(4) .
C24 C23 C22 119.9(4) .
C25 C24 C23 120.1(4) .
C24 C25 C26 120.3(4) .
C25 C26 C21 120.1(4) .
C32 C31 C36 118.7(4) .
C32 C31 P1 121.3(3) .
C36 C31 P1 119.8(3) .
C33 C32 C31 121.2(4) .
C32 C33 C34 119.9(4) .
C35 C34 C33 119.5(4) .
C36 C35 C34 120.7(4) .
C35 C36 C31 120.1(4) .
C46 C41 C42 120.0(4) .
C46 C41 P1 119.3(3) .
C42 C41 P1 119.7(3) .
C41 C42 C43 119.8(4) .
C44 C43 C42 120.0(4) .
C45 C44 C43 120.1(4) .
C44 C45 C46 120.4(4) .
C45 C46 C41 119.6(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Au1 C1 1.976(4) .
Au1 C1 1.976(4) 2
N1 C7 1.337(6) .
N1 C6 1.346(6) .
N2 C9 1.349(6) .
N2 C8 1.354(5) .
N3 P1 1.5883(18) .
N3 P1 1.5883(18) 2_556
P1 C41 1.797(4) .
P1 C21 1.802(4) .
P1 C31 1.807(4) .
C1 C2 1.209(6) .
C2 C3 1.434(6) .
C3 C7 1.401(6) .
C3 C4 1.402(6) .
C4 C5 1.377(6) .
C5 C6 1.380(6) .
C6 C8 1.483(6) .
C8 C12 1.385(6) .
C9 C10 1.382(7) .
C10 C11 1.379(6) .
C11 C12 1.370(6) .
C21 C22 1.389(5) .
C21 C26 1.390(5) .
C22 C23 1.387(5) .
C23 C24 1.381(6) .
C24 C25 1.380(6) .
C25 C26 1.386(6) .
C31 C32 1.392(5) .
C31 C36 1.401(5) .
C32 C33 1.380(6) .
C33 C34 1.391(5) .
C34 C35 1.387(6) .
C35 C36 1.383(5) .
C41 C46 1.390(5) .
C41 C42 1.391(5) .
C42 C43 1.392(5) .
C43 C44 1.386(5) .
C44 C45 1.380(6) .
C45 C46 1.389(5) .
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
C4 H4 Au1 0.95 3.26 3.978(5) 134.1 5_565
C33 H33 Au1 0.95 3.28 4.162(4) 154.9 5_576
C42 H42 Au1 0.95 3.10 3.879(4) 139.9 5_566
