#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:20:39 +0100 (lun 21 de mar de 2016) $
#$Revision: 178809 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/63/4106346.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_4106346
loop_
_publ_author_name
'Sang Ho Lim'
'Marilyn M. Olmstead'
'Alan L. Balch'
_publ_section_title
;
 Molecular Accordion: Vapoluminescence and Molecular Flexibility in the
 Orange and Green Luminescent Crystals of the Dimer,
 Au2(μ-bis-(diphenylphosphino)ethane)2Br2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10229
_journal_page_last               10238
_journal_paper_doi               10.1021/ja2026807
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C52 H48 Au2 Br2 P4, 2(C3 H7 N O)'
_chemical_formula_sum            'C58 H62 Au2 Br2 N2 O2 P4'
_chemical_formula_weight         1496.73
_chemical_name_common            '[AuBr(dppe)]2.2(DMF)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.357(2)
_cell_angle_beta                 101.085(2)
_cell_angle_gamma                109.337(2)
_cell_formula_units_Z            1
_cell_length_a                   11.0206(10)
_cell_length_b                   11.6968(11)
_cell_length_c                   12.2211(11)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.486
_cell_measurement_theta_min      3.492
_cell_volume                     1382.9(2)
_computing_cell_refinement       SAINT
_computing_data_collection       'SMART 5.054 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45A (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21118
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         31.35
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    6.902
_exptl_absorpt_correction_T_max  0.501
_exptl_absorpt_correction_T_min  0.326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.083
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         8277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0244P)²+0.2920P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0488
_reflns_number_gt                7427
_reflns_number_total             8277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2026807_si_007.cif
_cod_data_source_block           dr90
_cod_database_code               4106346
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.621731(8) 0.459013(8) 0.445893(8) 0.01400(3) Uani 1 1 d .
Br1 Br 0.59843(2) 0.41301(2) 0.66439(2) 0.01658(5) Uani 1 1 d .
P1 P 0.47551(6) 0.27148(5) 0.30110(5) 0.01155(10) Uani 1 1 d .
P2 P 0.79283(5) 0.65910(5) 0.52815(5) 0.01192(11) Uani 1 1 d .
O1 O 0.1249(2) 0.94961(18) 0.06621(17) 0.0312(5) Uani 1 1 d .
N1 N -0.0061(2) 0.7372(2) 0.0115(2) 0.0277(5) Uani 1 1 d .
C1 C 0.4900(2) 0.2693(2) 0.15445(19) 0.0137(4) Uani 1 1 d .
C2 C 0.4516(2) 0.1549(2) 0.0639(2) 0.0188(5) Uani 1 1 d .
H2A H 0.4118 0.0754 0.0765 0.023 Uiso 1 1 calc R
C3 C 0.4715(3) 0.1573(3) -0.0444(2) 0.0223(5) Uani 1 1 d .
H3A H 0.4466 0.0793 -0.1053 0.027 Uiso 1 1 calc R
C4 C 0.5277(3) 0.2733(3) -0.0644(2) 0.0214(5) Uani 1 1 d .
H4A H 0.5419 0.2747 -0.1384 0.026 Uiso 1 1 calc R
C5 C 0.5628(3) 0.3865(2) 0.0244(2) 0.0206(5) Uani 1 1 d .
H5A H 0.5995 0.4658 0.0105 0.025 Uiso 1 1 calc R
C6 C 0.5448(2) 0.3851(2) 0.1337(2) 0.0190(5) Uani 1 1 d .
H6A H 0.5699 0.4633 0.1943 0.023 Uiso 1 1 calc R
C7 C 0.4997(2) 0.1313(2) 0.32332(19) 0.0122(4) Uani 1 1 d .
C8 C 0.6310(2) 0.1429(2) 0.3687(2) 0.0169(4) Uani 1 1 d .
H8A H 0.7042 0.2222 0.3867 0.020 Uiso 1 1 calc R
C9 C 0.6546(2) 0.0387(2) 0.3876(2) 0.0210(5) Uani 1 1 d .
H9A H 0.7444 0.0458 0.4149 0.025 Uiso 1 1 calc R
C10 C 0.5480(2) -0.0759(2) 0.3667(2) 0.0171(4) Uani 1 1 d .
H10A H 0.5646 -0.1458 0.3830 0.020 Uiso 1 1 calc R
C11 C 0.4173(2) -0.0881(2) 0.3220(2) 0.0171(4) Uani 1 1 d .
H11A H 0.3442 -0.1665 0.3077 0.021 Uiso 1 1 calc R
C12 C 0.3928(2) 0.0142(2) 0.2981(2) 0.0156(4) Uani 1 1 d .
H12A H 0.3034 0.0045 0.2645 0.019 Uiso 1 1 calc R
C13 C 0.2979(2) 0.2378(2) 0.28744(19) 0.0131(4) Uani 1 1 d .
H13A H 0.2771 0.3093 0.2710 0.016 Uiso 1 1 calc R
H13B H 0.2417 0.1594 0.2202 0.016 Uiso 1 1 calc R
C14 C 0.7377(2) 0.7805(2) 0.6002(2) 0.0137(4) Uani 1 1 d .
H14A H 0.8102 0.8660 0.6206 0.016 Uiso 1 1 calc R
H14B H 0.6579 0.7775 0.5443 0.016 Uiso 1 1 calc R
C15 C 0.9382(2) 0.6732(2) 0.6379(2) 0.0149(4) Uani 1 1 d .
C16 C 1.0286(2) 0.7919(2) 0.7171(2) 0.0204(5) Uani 1 1 d .
H16A H 1.0132 0.8668 0.7155 0.025 Uiso 1 1 calc R
C17 C 1.1416(2) 0.8005(3) 0.7984(2) 0.0256(6) Uani 1 1 d .
H17A H 1.2027 0.8813 0.8526 0.031 Uiso 1 1 calc R
C18 C 1.1647(3) 0.6923(3) 0.8004(2) 0.0281(6) Uani 1 1 d .
H18A H 1.2417 0.6988 0.8563 0.034 Uiso 1 1 calc R
C19 C 1.0768(3) 0.5742(3) 0.7218(3) 0.0292(6) Uani 1 1 d .
H19A H 1.0942 0.5000 0.7226 0.035 Uiso 1 1 calc R
C20 C 0.9622(3) 0.5643(3) 0.6409(2) 0.0219(5) Uani 1 1 d .
H20A H 0.9006 0.4831 0.5880 0.026 Uiso 1 1 calc R
C21 C 0.8618(2) 0.7306(2) 0.4249(2) 0.0142(4) Uani 1 1 d .
C22 C 0.9984(2) 0.7754(2) 0.4336(2) 0.0211(5) Uani 1 1 d .
H22A H 1.0588 0.7621 0.4912 0.025 Uiso 1 1 calc R
C23 C 1.0463(3) 0.8393(3) 0.3585(2) 0.0255(6) Uani 1 1 d .
H23A H 1.1396 0.8696 0.3651 0.031 Uiso 1 1 calc R
C24 C 0.9601(3) 0.8594(3) 0.2742(2) 0.0258(6) Uani 1 1 d .
H24A H 0.9944 0.9060 0.2251 0.031 Uiso 1 1 calc R
C25 C 0.8228(3) 0.8113(3) 0.2614(2) 0.0245(5) Uani 1 1 d .
H25A H 0.7629 0.8232 0.2022 0.029 Uiso 1 1 calc R
C26 C 0.7733(2) 0.7459(2) 0.3353(2) 0.0203(5) Uani 1 1 d .
H26A H 0.6792 0.7115 0.3252 0.024 Uiso 1 1 calc R
C27 C -0.1379(3) 0.6352(3) -0.0466(3) 0.0455(9) Uani 1 1 d .
H27A H -0.2028 0.6715 -0.0714 0.068 Uiso 1 1 calc R
H27B H -0.1659 0.5896 0.0080 0.068 Uiso 1 1 calc R
H27C H -0.1340 0.5757 -0.1156 0.068 Uiso 1 1 calc R
C28 C 0.0991(3) 0.7025(3) 0.0662(3) 0.0343(7) Uani 1 1 d .
H28A H 0.1859 0.7751 0.0904 0.051 Uiso 1 1 calc R
H28B H 0.1018 0.6293 0.0099 0.051 Uiso 1 1 calc R
H28C H 0.0807 0.6796 0.1353 0.051 Uiso 1 1 calc R
C29 C 0.0183(3) 0.8589(3) 0.0160(2) 0.0271(6) Uani 1 1 d .
H29A H -0.0541 0.8754 -0.0233 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'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.0060 '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'
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_1
P2 Au1 P1 157.80(2) .
P2 Au1 Br1 96.582(16) .
P1 Au1 Br1 105.099(16) .
C7 P1 C1 105.86(10) .
C7 P1 C13 105.30(10) .
C1 P1 C13 104.45(10) .
C7 P1 Au1 113.17(7) .
C1 P1 Au1 113.15(8) .
C13 P1 Au1 114.06(7) .
C15 P2 C21 104.77(11) .
C15 P2 C14 105.09(10) .
C21 P2 C14 100.50(10) .
C15 P2 Au1 116.29(8) .
C21 P2 Au1 115.61(8) .
C14 P2 Au1 112.85(8) .
C29 N1 C28 121.0(2) .
C29 N1 C27 122.1(3) .
C28 N1 C27 116.9(3) .
C6 C1 C2 119.3(2) .
C6 C1 P1 118.82(18) .
C2 C1 P1 121.83(18) .
C3 C2 C1 120.1(2) .
C3 C2 H2A 120.0 .
C1 C2 H2A 120.0 .
C2 C3 C4 120.4(2) .
C2 C3 H3A 119.8 .
C4 C3 H3A 119.8 .
C5 C4 C3 119.5(2) .
C5 C4 H4A 120.2 .
C3 C4 H4A 120.2 .
C4 C5 C6 120.5(2) .
C4 C5 H5A 119.8 .
C6 C5 H5A 119.8 .
C5 C6 C1 120.1(2) .
C5 C6 H6A 119.9 .
C1 C6 H6A 119.9 .
C8 C7 C12 119.3(2) .
C8 C7 P1 117.93(17) .
C12 C7 P1 122.78(17) .
C9 C8 C7 120.1(2) .
C9 C8 H8A 120.0 .
C7 C8 H8A 120.0 .
C8 C9 C10 120.4(2) .
C8 C9 H9A 119.8 .
C10 C9 H9A 119.8 .
C11 C10 C9 119.9(2) .
C11 C10 H10A 120.1 .
C9 C10 H10A 120.1 .
C10 C11 C12 120.1(2) .
C10 C11 H11A 119.9 .
C12 C11 H11A 119.9 .
C11 C12 C7 120.1(2) .
C11 C12 H12A 119.9 .
C7 C12 H12A 119.9 .
C14 C13 P1 111.98(15) 2_666
C14 C13 H13A 109.2 2_666
P1 C13 H13A 109.2 .
C14 C13 H13B 109.2 2_666
P1 C13 H13B 109.2 .
H13A C13 H13B 107.9 .
C13 C14 P2 113.09(15) 2_666
C13 C14 H14A 109.0 2_666
P2 C14 H14A 109.0 .
C13 C14 H14B 109.0 2_666
P2 C14 H14B 109.0 .
H14A C14 H14B 107.8 .
C20 C15 C16 119.4(2) .
C20 C15 P2 119.43(18) .
C16 C15 P2 121.17(18) .
C17 C16 C15 120.1(2) .
C17 C16 H16A 120.0 .
C15 C16 H16A 120.0 .
C18 C17 C16 120.1(2) .
C18 C17 H17A 119.9 .
C16 C17 H17A 119.9 .
C17 C18 C19 120.6(2) .
C17 C18 H18A 119.7 .
C19 C18 H18A 119.7 .
C18 C19 C20 119.7(3) .
C18 C19 H19A 120.1 .
C20 C19 H19A 120.1 .
C15 C20 C19 120.2(2) .
C15 C20 H20A 119.9 .
C19 C20 H20A 119.9 .
C22 C21 C26 118.8(2) .
C22 C21 P2 123.04(19) .
C26 C21 P2 118.06(17) .
C21 C22 C23 120.2(2) .
C21 C22 H22A 119.9 .
C23 C22 H22A 119.9 .
C24 C23 C22 120.8(2) .
C24 C23 H23A 119.6 .
C22 C23 H23A 119.6 .
C23 C24 C25 119.8(2) .
C23 C24 H24A 120.1 .
C25 C24 H24A 120.1 .
C26 C25 C24 120.0(2) .
C26 C25 H25A 120.0 .
C24 C25 H25A 120.0 .
C25 C26 C21 120.2(2) .
C25 C26 H26A 119.9 .
C21 C26 H26A 119.9 .
N1 C27 H27A 109.5 .
N1 C27 H27B 109.5 .
H27A C27 H27B 109.5 .
N1 C27 H27C 109.5 .
H27A C27 H27C 109.5 .
H27B C27 H27C 109.5 .
N1 C28 H28A 109.5 .
N1 C28 H28B 109.5 .
H28A C28 H28B 109.5 .
N1 C28 H28C 109.5 .
H28A C28 H28C 109.5 .
H28B C28 H28C 109.5 .
O1 C29 N1 125.7(3) .
O1 C29 H29A 117.2 .
N1 C29 H29A 117.2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Au1 P2 2.3032(6) .
Au1 P1 2.3041(6) .
Au1 Br1 2.8848(3) .
P1 C7 1.816(2) .
P1 C1 1.825(2) .
P1 C13 1.830(2) .
P2 C15 1.813(2) .
P2 C21 1.818(2) .
P2 C14 1.833(2) .
O1 C29 1.216(3) .
N1 C29 1.343(4) .
N1 C28 1.447(4) .
N1 C27 1.450(4) .
C1 C6 1.393(3) .
C1 C2 1.398(3) .
C2 C3 1.388(3) .
C2 H2A 0.9500 .
C3 C4 1.392(4) .
C3 H3A 0.9500 .
C4 C5 1.384(4) .
C4 H4A 0.9500 .
C5 C6 1.391(3) .
C5 H5A 0.9500 .
C6 H6A 0.9500 .
C7 C8 1.395(3) .
C7 C12 1.398(3) .
C8 C9 1.387(3) .
C8 H8A 0.9500 .
C9 C10 1.388(3) .
C9 H9A 0.9500 .
C10 C11 1.385(3) .
C10 H10A 0.9500 .
C11 C12 1.391(3) .
C11 H11A 0.9500 .
C12 H12A 0.9500 .
C13 C14 1.540(3) 2_666
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 C13 1.540(3) 2_666
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C20 1.390(3) .
C15 C16 1.396(3) .
C16 C17 1.394(3) .
C16 H16A 0.9500 .
C17 C18 1.376(4) .
C17 H17A 0.9500 .
C18 C19 1.383(4) .
C18 H18A 0.9500 .
C19 C20 1.398(4) .
C19 H19A 0.9500 .
C20 H20A 0.9500 .
C21 C22 1.393(3) .
C21 C26 1.407(3) .
C22 C23 1.387(4) .
C22 H22A 0.9500 .
C23 C24 1.379(4) .
C23 H23A 0.9500 .
C24 C25 1.391(4) .
C24 H24A 0.9500 .
C25 C26 1.389(4) .
C25 H25A 0.9500 .
C26 H26A 0.9500 .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
C29 H29A 0.9500 .
