# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pb3p98
_database_code_depnum_ccdc_archive 'CCDC 834016'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_date             2011-05-20T12:02:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H18 N4, 2(H2 O), 2(Br)'
_chemical_formula_sum            'C16 H22 Br2 N4 O2'
_chemical_formula_weight         462.2

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P_21_21_21
_symmetry_space_group_name_Hall  'P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.1485(6)
_cell_length_b                   14.5332(12)
_cell_length_c                   15.4360(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1828.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    7674
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      20.8

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        SADABS; Sheldrick, 1996

;
_exptl_absorpt_correction_T_min  .80
_exptl_absorpt_correction_T_max  1


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.48595
_diffrn_radiation_type           synchrotron
_diffrn_radiation_monochromator  diamond
_diffrn_measurement_device_type  
;
        CCD area detector
;
_diffrn_measurement_method       'φ and ω scans'
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_number            26940
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         0.9
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_full        19
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.812
_reflns_number_total             5197
_reflns_number_gt                4806
_reflns_threshold_expression     I>2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'


#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

Water molecule hydrogen atoms geometries were restrained to ideal values.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0269P)²+0.6734P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5197
_refine_ls_number_parameters     231
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0635
_refine_ls_wR_factor_gt          0.0618
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(2)
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.099

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.001 0.001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.27 1.287 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.002 0.001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.004 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.82512(3) 0.648097(16) 0.195939(15) 0.01865(6) Uani 1 1 d . . .
Br2 Br 0.14625(3) 0.527971(15) 0.550808(14) 0.01694(6) Uani 1 1 d . . .
C1 C 0.1453(3) 0.49632(15) 0.30193(16) 0.0166(4) Uani 1 1 d . . .
H1A H 0.0495 0.4997 0.2626 0.02 Uiso 1 1 calc R . .
H1B H 0.1047 0.4846 0.3613 0.02 Uiso 1 1 calc R . .
N21 N 0.2355(3) 0.58397(12) 0.29979(13) 0.0123(4) Uani 1 1 d . . .
C22 C 0.3259(3) 0.61582(15) 0.36631(14) 0.0125(4) Uani 1 1 d . . .
H22 H 0.3195 0.5954 0.4247 0.015 Uiso 1 1 calc R . .
N23 N 0.4255(3) 0.68061(13) 0.33647(13) 0.0114(4) Uani 1 1 d . . .
C24 C 0.3964(3) 0.69235(16) 0.24876(15) 0.0150(5) Uani 1 1 d . . .
H24 H 0.4489 0.7353 0.2116 0.018 Uiso 1 1 calc R . .
C25 C 0.2792(3) 0.63128(16) 0.22608(15) 0.0157(5) Uani 1 1 d . . .
H25 H 0.235 0.6226 0.1697 0.019 Uiso 1 1 calc R . .
C2 C 0.5586(3) 0.72755(15) 0.38493(15) 0.0135(4) Uani 1 1 d . . .
H2A H 0.5311 0.7936 0.3906 0.016 Uiso 1 1 calc R . .
H2B H 0.6618 0.7229 0.3513 0.016 Uiso 1 1 calc R . .
C31 C 0.6731(3) 0.60640(15) 0.49068(15) 0.0132(4) Uani 1 1 d . . .
C32 C 0.5863(3) 0.68782(15) 0.47411(15) 0.0117(4) Uani 1 1 d . . .
C33 C 0.5267(3) 0.73918(15) 0.54393(16) 0.0147(4) Uani 1 1 d . . .
H33 H 0.4671 0.7942 0.5331 0.018 Uiso 1 1 calc R . .
C34 C 0.5529(3) 0.71143(17) 0.62870(16) 0.0172(5) Uani 1 1 d . . .
H34 H 0.5111 0.7469 0.6754 0.021 Uiso 1 1 calc R . .
C35 C 0.6407(3) 0.63145(16) 0.64488(14) 0.0169(5) Uani 1 1 d . . .
H35 H 0.6597 0.6122 0.7028 0.02 Uiso 1 1 calc R . .
C36 C 0.7006(3) 0.57971(16) 0.57647(15) 0.0162(5) Uani 1 1 d . . .
H36 H 0.7613 0.5253 0.588 0.019 Uiso 1 1 calc R . .
C3 C 0.7399(3) 0.54343(16) 0.42061(16) 0.0154(5) Uani 1 1 d . . .
H3A H 0.7699 0.5802 0.369 0.018 Uiso 1 1 calc R . .
H3B H 0.8398 0.512 0.4419 0.018 Uiso 1 1 calc R . .
N41 N 0.6137(3) 0.47399(13) 0.39674(13) 0.0147(4) Uani 1 1 d . . .
C42 C 0.5311(3) 0.47317(16) 0.32256(15) 0.0157(5) Uani 1 1 d . . .
H42 H 0.5579 0.5078 0.2723 0.019 Uiso 1 1 calc R . .
N43 N 0.4033(3) 0.41507(13) 0.33032(13) 0.0154(4) Uani 1 1 d . . .
C44 C 0.4080(4) 0.37714(16) 0.41255(16) 0.0179(5) Uani 1 1 d . . .
H44 H 0.3326 0.3338 0.4357 0.021 Uiso 1 1 calc R . .
C45 C 0.5394(3) 0.41302(16) 0.45380(17) 0.0184(5) Uani 1 1 d . . .
H45 H 0.5744 0.3992 0.511 0.022 Uiso 1 1 calc R . .
C4 C 0.2588(3) 0.41761(16) 0.27360(16) 0.0168(5) Uani 1 1 d . . .
H4A H 0.1993 0.3583 0.2771 0.02 Uiso 1 1 calc R . .
H4B H 0.2936 0.4271 0.2128 0.02 Uiso 1 1 calc R . .
O1 O 1.0923(3) 0.82557(15) 0.14083(15) 0.0342(5) Uani 1 1 d D . .
H1AO H 1.112(5) 0.811(3) 0.0889(14) 0.051 Uiso 1 1 d D . .
H1BO H 1.033(5) 0.782(2) 0.157(2) 0.051 Uiso 1 1 d D . .
O2 O 0.5589(3) 0.66163(15) 0.03628(14) 0.0349(5) Uani 1 1 d D . .
H2AO H 0.620(4) 0.653(3) 0.0810(19) 0.052 Uiso 1 1 d D . .
H2BO H 0.493(4) 0.617(2) 0.039(3) 0.052 Uiso 1 1 d D . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
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
C1 N21 1.471(3) . ?
C1 C4 1.534(3) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
N21 C22 1.346(3) . ?
N21 C25 1.376(3) . ?
C22 N23 1.326(3) . ?
C22 H22 0.95 . ?
N23 C24 1.385(3) . ?
N23 C2 1.484(3) . ?
C24 C25 1.350(4) . ?
C24 H24 0.95 . ?
C25 H25 0.95 . ?
C2 C32 1.510(3) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C31 C36 1.398(3) . ?
C31 C32 1.402(3) . ?
C31 C3 1.518(3) . ?
C32 C33 1.398(3) . ?
C33 C34 1.386(4) . ?
C33 H33 0.95 . ?
C34 C35 1.387(4) . ?
C34 H34 0.95 . ?
C35 C36 1.385(3) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C3 N41 1.487(3) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
N41 C42 1.328(3) . ?
N41 C45 1.388(3) . ?
C42 N43 1.346(3) . ?
C42 H42 0.95 . ?
N43 C44 1.384(3) . ?
N43 C4 1.468(3) . ?
C44 C45 1.351(4) . ?
C44 H44 0.95 . ?
C45 H45 0.95 . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
O1 H1AO 0.846(18) . ?
O1 H1BO 0.831(18) . ?
O2 H2AO 0.860(18) . ?
O2 H2BO 0.848(18) . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N21 C1 C4 109.8(2) . . ?
N21 C1 H1A 109.7 . . ?
C4 C1 H1A 109.7 . . ?
N21 C1 H1B 109.7 . . ?
C4 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C22 N21 C25 108.5(2) . . ?
C22 N21 C1 123.65(19) . . ?
C25 N21 C1 125.5(2) . . ?
N23 C22 N21 108.31(19) . . ?
N23 C22 H22 125.8 . . ?
N21 C22 H22 125.8 . . ?
C22 N23 C24 108.8(2) . . ?
C22 N23 C2 126.8(2) . . ?
C24 N23 C2 124.2(2) . . ?
C25 C24 N23 107.1(2) . . ?
C25 C24 H24 126.5 . . ?
N23 C24 H24 126.5 . . ?
C24 C25 N21 107.3(2) . . ?
C24 C25 H25 126.4 . . ?
N21 C25 H25 126.4 . . ?
N23 C2 C32 113.14(19) . . ?
N23 C2 H2A 109 . . ?
C32 C2 H2A 109 . . ?
N23 C2 H2B 109 . . ?
C32 C2 H2B 109 . . ?
H2A C2 H2B 107.8 . . ?
C36 C31 C32 119.2(2) . . ?
C36 C31 C3 116.8(2) . . ?
C32 C31 C3 124.0(2) . . ?
C33 C32 C31 119.0(2) . . ?
C33 C32 C2 116.5(2) . . ?
C31 C32 C2 124.4(2) . . ?
C34 C33 C32 121.3(2) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C33 C34 C35 119.6(2) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C36 C35 C34 120.0(2) . . ?
C36 C35 H35 120 . . ?
C34 C35 H35 120 . . ?
C35 C36 C31 121.0(2) . . ?
C35 C36 H36 119.5 . . ?
C31 C36 H36 119.5 . . ?
N41 C3 C31 109.8(2) . . ?
N41 C3 H3A 109.7 . . ?
C31 C3 H3A 109.7 . . ?
N41 C3 H3B 109.7 . . ?
C31 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C42 N41 C45 108.7(2) . . ?
C42 N41 C3 124.7(2) . . ?
C45 N41 C3 125.3(2) . . ?
N41 C42 N43 108.7(2) . . ?
N41 C42 H42 125.6 . . ?
N43 C42 H42 125.6 . . ?
C42 N43 C44 108.0(2) . . ?
C42 N43 C4 123.5(2) . . ?
C44 N43 C4 125.4(2) . . ?
C45 C44 N43 107.5(2) . . ?
C45 C44 H44 126.3 . . ?
N43 C44 H44 126.3 . . ?
C44 C45 N41 107.0(2) . . ?
C44 C45 H45 126.5 . . ?
N41 C45 H45 126.5 . . ?
N43 C4 C1 109.39(19) . . ?
N43 C4 H4A 109.8 . . ?
C1 C4 H4A 109.8 . . ?
N43 C4 H4B 109.8 . . ?
C1 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
H1AO O1 H1BO 102(2) . . ?
H2AO O2 H2BO 103(2) . . ?

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
C22 H22 Br2 0.95 2.6 3.447(2) 149.2 .
C42 H42 Br1 0.95 3.21 4.003(2) 142.5 .
O1 H1AO O2 0.846(18) 2.02(3) 2.754(3) 145(4) 3_565
O1 H1BO Br1 0.831(18) 2.652(19) 3.481(2) 175(4) .
O2 H2AO Br1 0.860(18) 2.438(18) 3.289(2) 170(3) .
O2 H2BO Br2 0.848(18) 2.39(2) 3.231(2) 169(4) 2_564

#===END
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p3394
_database_code_depnum_ccdc_archive 'CCDC 834017'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_date             2011-05-24T08:13:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C17 H20 N4, C3 H6 O, 2(Br), H2 O'
_chemical_formula_sum            'C20 H28 Br2 N4 O2'
_chemical_formula_weight         516.28

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P_-1
_symmetry_space_group_name_Hall  '-p 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2891(14)
_cell_length_b                   11.4501(17)
_cell_length_c                   11.666(2)
_cell_angle_alpha                104.754(2)
_cell_angle_beta                 111.067(2)
_cell_angle_gamma                92.096(2)
_cell_volume                     1108.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2945
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      28.15

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       cuboid
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             524
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
       SADABS; Sheldrick, 1996

;
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_T_max  1


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
        Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_number            10429
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.889
_reflns_number_total             5339
_reflns_number_gt                3858
_reflns_threshold_expression     I>2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'


#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

The acetone solvent molecule was modelled as being disordered over
two sets of sites with site occupancies of the two components refined to
0.668(5) and its complement.
Water molecule hydrogen geometries were restrained to ideal values.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0451P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5339
_refine_ls_number_parameters     290
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.0968
_refine_ls_wR_factor_gt          0.0876
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.105

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.15294(4) 0.67493(3) 0.67428(3) 0.02670(10) Uani 1 1 d . . .
Br2 Br 0.26641(4) 0.90318(3) 0.31606(3) 0.03010(11) Uani 1 1 d . . .
C0 C 0.7168(4) 0.6059(3) 0.4900(3) 0.0260(7) Uani 1 1 d . . .
H0A H 0.7213 0.5668 0.5575 0.031 Uiso 1 1 calc R . .
H0B H 0.8031 0.5822 0.4622 0.031 Uiso 1 1 calc R . .
C1 C 0.5635(4) 0.5541(3) 0.3762(3) 0.0274(7) Uani 1 1 d . . .
H1A H 0.5499 0.4639 0.355 0.033 Uiso 1 1 calc R . .
H1B H 0.4765 0.5828 0.4006 0.033 Uiso 1 1 calc R . .
N21 N 0.5561(3) 0.5897(2) 0.2618(3) 0.0226(6) Uani 1 1 d . . .
C22 C 0.4689(4) 0.6688(3) 0.2145(3) 0.0234(7) Uani 1 1 d . . .
H22 H 0.3917 0.7039 0.2423 0.028 Uiso 1 1 calc R . .
N23 N 0.5075(3) 0.6909(2) 0.1218(2) 0.0217(6) Uani 1 1 d . . .
C24 C 0.6227(4) 0.6227(3) 0.1086(3) 0.0233(7) Uani 1 1 d . . .
H24 H 0.6715 0.6207 0.0493 0.028 Uiso 1 1 calc R . .
C25 C 0.6535(4) 0.5592(3) 0.1959(3) 0.0243(7) Uani 1 1 d . . .
H25 H 0.7278 0.5042 0.2094 0.029 Uiso 1 1 calc R . .
C2 C 0.4399(4) 0.7787(3) 0.0501(3) 0.0249(7) Uani 1 1 d . . .
H2A H 0.3929 0.8373 0.0997 0.03 Uiso 1 1 calc R . .
H2B H 0.3564 0.7342 -0.033 0.03 Uiso 1 1 calc R . .
C31 C 0.6694(4) 0.9463(3) 0.1197(3) 0.0228(7) Uani 1 1 d . . .
C32 C 0.5646(4) 0.8481(3) 0.0263(3) 0.0217(7) Uani 1 1 d . . .
C33 C 0.5655(4) 0.8136(3) -0.0965(3) 0.0289(8) Uani 1 1 d . . .
H33 H 0.4922 0.7475 -0.1605 0.035 Uiso 1 1 calc R . .
C34 C 0.6720(4) 0.8744(3) -0.1262(3) 0.0336(8) Uani 1 1 d . . .
H34 H 0.6717 0.8501 -0.2104 0.04 Uiso 1 1 calc R . .
C35 C 0.7784(4) 0.9700(3) -0.0342(3) 0.0316(8) Uani 1 1 d . . .
H35 H 0.8525 1.0114 -0.0543 0.038 Uiso 1 1 calc R . .
C36 C 0.7772(4) 1.0055(3) 0.0878(3) 0.0280(8) Uani 1 1 d . . .
H36 H 0.8511 1.0716 0.1512 0.034 Uiso 1 1 calc R . .
C3 C 0.6708(4) 0.9958(3) 0.2526(3) 0.0250(7) Uani 1 1 d . . .
H3A H 0.7263 1.0803 0.2901 0.03 Uiso 1 1 calc R . .
H3B H 0.5623 0.9984 0.2473 0.03 Uiso 1 1 calc R . .
N41 N 0.7474(3) 0.9211(2) 0.3377(2) 0.0218(6) Uani 1 1 d . . .
C42 C 0.6856(4) 0.8809(3) 0.4093(3) 0.0220(7) Uani 1 1 d . . .
H42 H 0.59 0.8989 0.4172 0.026 Uiso 1 1 calc R . .
N43 N 0.7794(3) 0.8114(2) 0.4681(2) 0.0224(6) Uani 1 1 d . . .
C44 C 0.9087(4) 0.8104(3) 0.4356(3) 0.0255(7) Uani 1 1 d . . .
H44 H 0.9954 0.769 0.4649 0.031 Uiso 1 1 calc R . .
C45 C 0.8887(4) 0.8793(3) 0.3545(3) 0.0245(7) Uani 1 1 d . . .
H45 H 0.9587 0.8959 0.3162 0.029 Uiso 1 1 calc R . .
C4 C 0.7460(4) 0.7436(3) 0.5496(3) 0.0285(8) Uani 1 1 d . . .
H4A H 0.6532 0.77 0.566 0.034 Uiso 1 1 calc R . .
H4B H 0.8352 0.7642 0.6331 0.034 Uiso 1 1 calc R . .
C101 C 1.059(4) 0.533(3) 0.214(4) 0.0418(17) Uani 0.668(5) 1 d P A 1
H10A H 1.0331 0.6135 0.2059 0.063 Uiso 0.668(5) 1 calc PR A 1
H10B H 1.1694 0.5302 0.2303 0.063 Uiso 0.668(5) 1 calc PR A 1
H10C H 1.0371 0.5183 0.2861 0.063 Uiso 0.668(5) 1 calc PR A 1
C102 C 0.9633(6) 0.4385(5) 0.0950(5) 0.0309(13) Uani 0.668(5) 1 d P A 1
O102 O 0.8377(4) 0.4552(3) 0.0241(3) 0.0324(10) Uani 0.668(5) 1 d P A 1
C103 C 1.0020(19) 0.315(2) 0.055(2) 0.044(3) Uani 0.668(5) 1 d P A 1
H10D H 0.9955 0.2696 0.1135 0.065 Uiso 0.668(5) 1 calc PR A 1
H10E H 1.108 0.3211 0.0556 0.065 Uiso 0.668(5) 1 calc PR A 1
H10F H 0.9281 0.2729 -0.0325 0.065 Uiso 0.668(5) 1 calc PR A 1
C201 C 1.067(8) 0.539(6) 0.219(8) 0.0418(17) Uani 0.332(5) 1 d P A 2
H20A H 1.1446 0.6122 0.2516 0.063 Uiso 0.332(5) 1 calc PR A 2
H20B H 1.0645 0.5106 0.2905 0.063 Uiso 0.332(5) 1 calc PR A 2
H20C H 0.9637 0.5597 0.1736 0.063 Uiso 0.332(5) 1 calc PR A 2
C202 C 1.1079(12) 0.4404(11) 0.1272(12) 0.039(3) Uani 0.332(5) 1 d P A 2
O202 O 1.2286(10) 0.4545(8) 0.1115(9) 0.057(3) Uani 0.332(5) 1 d P A 2
C203 C 1.036(5) 0.326(5) 0.081(4) 0.044(3) Uani 0.332(5) 1 d P A 2
H20D H 0.9237 0.3264 0.0598 0.065 Uiso 0.332(5) 1 calc PR A 2
H20E H 1.077 0.2823 0.145 0.065 Uiso 0.332(5) 1 calc PR A 2
H20F H 1.0531 0.2855 0.003 0.065 Uiso 0.332(5) 1 calc PR A 2
O1 O 0.3766(4) 0.7325(3) 0.5211(3) 0.0521(8) Uani 1 1 d D . .
H1AO H 0.313(5) 0.714(4) 0.548(5) 0.080(19) Uiso 1 1 d D . .
H1BO H 0.337(5) 0.776(4) 0.477(4) 0.072(18) Uiso 1 1 d D . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
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
C0 C4 1.522(5) . ?
C0 C1 1.523(4) . ?
C0 H0A 0.99 . ?
C0 H0B 0.99 . ?
C1 N21 1.472(4) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
N21 C22 1.330(4) . ?
N21 C25 1.385(4) . ?
C22 N23 1.331(4) . ?
C22 H22 0.95 . ?
N23 C24 1.377(4) . ?
N23 C2 1.485(4) . ?
C24 C25 1.353(4) . ?
C24 H24 0.95 . ?
C25 H25 0.95 . ?
C2 C32 1.525(4) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C31 C32 1.390(4) . ?
C31 C36 1.396(4) . ?
C31 C3 1.504(4) . ?
C32 C33 1.389(4) . ?
C33 C34 1.379(5) . ?
C33 H33 0.95 . ?
C34 C35 1.374(5) . ?
C34 H34 0.95 . ?
C35 C36 1.381(5) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C3 N41 1.481(4) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
N41 C42 1.327(4) . ?
N41 C45 1.378(4) . ?
C42 N43 1.327(4) . ?
C42 H42 0.95 . ?
N43 C44 1.384(4) . ?
N43 C4 1.475(4) . ?
C44 C45 1.347(4) . ?
C44 H44 0.95 . ?
C45 H45 0.95 . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C101 C102 1.47(4) . ?
C101 H10A 0.98 . ?
C101 H10B 0.98 . ?
C101 H10C 0.98 . ?
C102 O102 1.219(6) . ?
C102 C103 1.47(3) . ?
C103 H10D 0.98 . ?
C103 H10E 0.98 . ?
C103 H10F 0.98 . ?
C201 C202 1.51(7) . ?
C201 H20A 0.98 . ?
C201 H20B 0.98 . ?
C201 H20C 0.98 . ?
C202 O202 1.210(13) . ?
C202 C203 1.33(5) . ?
C203 H20D 0.98 . ?
C203 H20E 0.98 . ?
C203 H20F 0.98 . ?
O1 H1AO 0.810(19) . ?
O1 H1BO 0.811(19) . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 C0 C1 116.5(3) . . ?
C4 C0 H0A 108.2 . . ?
C1 C0 H0A 108.2 . . ?
C4 C0 H0B 108.2 . . ?
C1 C0 H0B 108.2 . . ?
H0A C0 H0B 107.3 . . ?
N21 C1 C0 112.8(3) . . ?
N21 C1 H1A 109 . . ?
C0 C1 H1A 109 . . ?
N21 C1 H1B 109 . . ?
C0 C1 H1B 109 . . ?
H1A C1 H1B 107.8 . . ?
C22 N21 C25 108.4(3) . . ?
C22 N21 C1 125.6(3) . . ?
C25 N21 C1 125.5(3) . . ?
N21 C22 N23 108.8(3) . . ?
N21 C22 H22 125.6 . . ?
N23 C22 H22 125.6 . . ?
C22 N23 C24 108.6(3) . . ?
C22 N23 C2 124.5(3) . . ?
C24 N23 C2 126.8(3) . . ?
C25 C24 N23 107.2(3) . . ?
C25 C24 H24 126.4 . . ?
N23 C24 H24 126.4 . . ?
C24 C25 N21 107.0(3) . . ?
C24 C25 H25 126.5 . . ?
N21 C25 H25 126.5 . . ?
N23 C2 C32 110.8(2) . . ?
N23 C2 H2A 109.5 . . ?
C32 C2 H2A 109.5 . . ?
N23 C2 H2B 109.5 . . ?
C32 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C32 C31 C36 118.5(3) . . ?
C32 C31 C3 124.0(3) . . ?
C36 C31 C3 117.5(3) . . ?
C33 C32 C31 120.0(3) . . ?
C33 C32 C2 117.2(3) . . ?
C31 C32 C2 122.7(3) . . ?
C34 C33 C32 120.5(3) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C35 C34 C33 120.1(3) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C34 C35 C36 119.6(3) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
C35 C36 C31 121.2(3) . . ?
C35 C36 H36 119.4 . . ?
C31 C36 H36 119.4 . . ?
N41 C3 C31 112.2(3) . . ?
N41 C3 H3A 109.2 . . ?
C31 C3 H3A 109.2 . . ?
N41 C3 H3B 109.2 . . ?
C31 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C42 N41 C45 108.7(3) . . ?
C42 N41 C3 124.0(3) . . ?
C45 N41 C3 127.3(3) . . ?
N43 C42 N41 108.7(3) . . ?
N43 C42 H42 125.6 . . ?
N41 C42 H42 125.6 . . ?
C42 N43 C44 108.4(3) . . ?
C42 N43 C4 125.0(3) . . ?
C44 N43 C4 126.6(3) . . ?
C45 C44 N43 107.1(3) . . ?
C45 C44 H44 126.5 . . ?
N43 C44 H44 126.5 . . ?
C44 C45 N41 107.0(3) . . ?
C44 C45 H45 126.5 . . ?
N41 C45 H45 126.5 . . ?
N43 C4 C0 113.1(3) . . ?
N43 C4 H4A 109 . . ?
C0 C4 H4A 109 . . ?
N43 C4 H4B 109 . . ?
C0 C4 H4B 109 . . ?
H4A C4 H4B 107.8 . . ?
O102 C102 C103 113.9(7) . . ?
O102 C102 C101 121.2(15) . . ?
C103 C102 C101 124.8(15) . . ?
C202 C201 H20A 109.5 . . ?
C202 C201 H20B 109.5 . . ?
H20A C201 H20B 109.5 . . ?
C202 C201 H20C 109.5 . . ?
H20A C201 H20C 109.5 . . ?
H20B C201 H20C 109.5 . . ?
O202 C202 C203 115(3) . . ?
O202 C202 C201 121(3) . . ?
C203 C202 C201 123(4) . . ?
C202 C203 H20D 109.5 . . ?
C202 C203 H20E 109.5 . . ?
H20D C203 H20E 109.5 . . ?
C202 C203 H20F 109.5 . . ?
H20D C203 H20F 109.5 . . ?
H20E C203 H20F 109.5 . . ?
H1AO O1 H1BO 106(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
O1 H1AO Br1 0.810(19) 2.54(2) 3.334(3) 169(5) .
O1 H1BO Br2 0.811(19) 2.58(2) 3.370(3) 166(5) .
C22 H22 Br2 0.95 2.69 3.535(3) 149 .
C42 H42 Br2 0.95 2.81 3.685(3) 152.8 .

#===END
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lw1b39

_database_code_depnum_ccdc_archive 'CCDC 834018'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_date             2015-01-20T07:57:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C18 H22 Br2 N4'
_chemical_formula_moiety         'C18 H22 N4, 2(Br)'
_chemical_formula_weight         454.21

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.1040(4)
_cell_length_b                   12.7208(6)
_cell_length_c                   15.8340(10)
_cell_angle_alpha                90
_cell_angle_beta                 101.216(5)
_cell_angle_gamma                90
_cell_volume                     1798.72(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    22520
_cell_measurement_theta_min      2.6113
_cell_measurement_theta_max      30.0398

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.677
_exptl_crystal_F_000             912
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_size_max          .39
_exptl_crystal_size_mid          .37
_exptl_crystal_size_min          .22
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            colourless


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_absorpt_correction_T_min  0.73697
_exptl_absorpt_correction_T_max  1.21416

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.0009
_diffrn_orient_matrix_ub_11      -0.0733690577
_diffrn_orient_matrix_ub_12      0.0102673969
_diffrn_orient_matrix_ub_13      -0.0231672811
_diffrn_orient_matrix_ub_21      -0.0266769165
_diffrn_orient_matrix_ub_22      0.0010805667
_diffrn_orient_matrix_ub_23      0.0391167158
_diffrn_orient_matrix_ub_31      0.0143342175
_diffrn_orient_matrix_ub_32      0.0547292613
_diffrn_orient_matrix_ub_33      0.003586299
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_number            40296
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.787
_diffrn_reflns_theta_max         30.136
_diffrn_reflns_theta_full        29
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.95
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.95
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.95
_reflns_number_total             5046
_reflns_number_gt                4002
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#


_computing_data_collection       
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinement       
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction        
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;

_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0533P)²+0.6256P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5046
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0837
_refine_ls_wR_factor_gt          0.0808
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.64
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.104

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.05008(2) 0.27957(2) 0.50094(2) 0.01824(7) Uani 1 d . .
Br2 Br 0.54733(3) 0.36053(2) 0.24535(2) 0.03021(8) Uani 1 d . .
C0 C 0.3647(2) 0.12038(18) 0.48210(14) 0.0189(4) Uani 1 d . .
H0A H 0.2963 0.1747 0.4973 0.023 Uiso 1 calc . .
H0B H 0.4002 0.0771 0.534 0.023 Uiso 1 calc . .
C1 C 0.2776(3) 0.05017(18) 0.41085(14) 0.0211(5) Uani 1 d . .
H1A H 0.3455 -0.0037 0.3945 0.025 Uiso 1 calc . .
H1B H 0.1962 0.0135 0.4323 0.025 Uiso 1 calc . .
N21 N 0.2138(2) 0.11407(15) 0.33514(12) 0.0170(4) Uani 1 d . .
C22 C 0.1158(2) 0.19196(17) 0.33473(13) 0.0167(4) Uani 1 d . .
H22 H 0.0689 0.2108 0.3812 0.02 Uiso 1 calc . .
N23 N 0.0948(2) 0.23880(14) 0.25813(11) 0.0149(4) Uani 1 d . .
C24 C 0.1825(3) 0.18917(18) 0.20800(14) 0.0194(4) Uani 1 d . .
H24 H 0.1895 0.2068 0.1506 0.023 Uiso 1 calc . .
C25 C 0.2562(3) 0.11102(19) 0.25589(14) 0.0203(4) Uani 1 d . .
H25 H 0.3245 0.0629 0.2385 0.024 Uiso 1 calc . .
C2 C -0.0067(2) 0.32882(17) 0.23168(14) 0.0172(4) Uani 1 d . .
H2A H -0.0696 0.3403 0.2753 0.021 Uiso 1 calc . .
H2B H -0.0739 0.3123 0.1762 0.021 Uiso 1 calc . .
C31 C 0.1342(2) 0.49744(16) 0.28952(14) 0.0152(4) Uani 1 d . .
C32 C 0.0798(2) 0.42839(17) 0.22190(14) 0.0154(4) Uani 1 d . .
C33 C 0.1037(2) 0.45269(18) 0.13942(14) 0.0185(4) Uani 1 d . .
H33 H 0.0672 0.4066 0.0929 0.022 Uiso 1 calc . .
C34 C 0.1801(3) 0.54310(17) 0.12468(14) 0.0203(5) Uani 1 d . .
H34 H 0.1937 0.559 0.0681 0.024 Uiso 1 calc . .
C35 C 0.2367(3) 0.61044(18) 0.19210(15) 0.0204(5) Uani 1 d . .
H35 H 0.291 0.6715 0.1824 0.024 Uiso 1 calc . .
C36 C 0.2128(2) 0.58726(18) 0.27367(14) 0.0184(4) Uani 1 d . .
H36 H 0.2507 0.6334 0.3199 0.022 Uiso 1 calc . .
C3 C 0.1074(2) 0.48198(18) 0.37958(14) 0.0175(4) Uani 1 d . .
H3A H 0.0709 0.5487 0.4003 0.021 Uiso 1 calc . .
H3B H 0.0285 0.4282 0.3787 0.021 Uiso 1 calc . .
N41 N 0.2446(2) 0.44836(14) 0.44016(11) 0.0163(4) Uani 1 d . .
C42 C 0.3430(2) 0.37809(17) 0.42325(14) 0.0187(4) Uani 1 d . .
H42 H 0.3473 0.3503 0.3681 0.022 Uiso 1 calc . .
N43 N 0.4351(2) 0.35304(16) 0.49738(12) 0.0195(4) Uani 1 d . .
C44 C 0.3943(3) 0.4115(2) 0.56267(14) 0.0223(5) Uani 1 d . .
H44 H 0.4415 0.4103 0.6217 0.027 Uiso 1 calc . .
C45 C 0.2753(3) 0.47069(19) 0.52714(14) 0.0217(5) Uani 1 d . .
H45 H 0.2226 0.5186 0.5564 0.026 Uiso 1 calc . .
C4 C 0.5526(3) 0.2715(2) 0.50911(17) 0.0255(5) Uani 1 d . .
H4A H 0.5793 0.252 0.5707 0.031 Uiso 1 calc . .
H4B H 0.6434 0.2999 0.4916 0.031 Uiso 1 calc . .
C5 C 0.4993(2) 0.17454(19) 0.45583(15) 0.0212(5) Uani 1 d . .
H5A H 0.583 0.1237 0.4615 0.025 Uiso 1 calc . .
H5B H 0.4719 0.1951 0.3945 0.025 Uiso 1 calc . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C0 C5 1.532(3) . ?
C0 C1 1.533(3) . ?
C0 H0A 0.99 . ?
C0 H0B 0.99 . ?
C1 N21 1.471(3) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
N21 C22 1.332(3) . ?
N21 C25 1.383(3) . ?
C22 N23 1.331(3) . ?
C22 H22 0.95 . ?
N23 C24 1.383(3) . ?
N23 C2 1.480(3) . ?
C24 C25 1.348(3) . ?
C24 H24 0.95 . ?
C25 H25 0.95 . ?
C2 C32 1.515(3) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C31 C36 1.397(3) . ?
C31 C32 1.399(3) . ?
C31 C3 1.506(3) . ?
C32 C33 1.400(3) . ?
C33 C34 1.387(3) . ?
C33 H33 0.95 . ?
C34 C35 1.387(3) . ?
C34 H34 0.95 . ?
C35 C36 1.382(3) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C3 N41 1.483(3) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
N41 C42 1.329(3) . ?
N41 C45 1.381(3) . ?
C42 N43 1.341(3) . ?
C42 H42 0.95 . ?
N43 C44 1.382(3) . ?
N43 C4 1.475(3) . ?
C44 C45 1.349(3) . ?
C44 H44 0.95 . ?
C45 H45 0.95 . ?
C4 C5 1.520(3) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 C0 C1 112.86(19) . . ?
C5 C0 H0A 109 . . ?
C1 C0 H0A 109 . . ?
C5 C0 H0B 109 . . ?
C1 C0 H0B 109 . . ?
H0A C0 H0B 107.8 . . ?
N21 C1 C0 110.09(18) . . ?
N21 C1 H1A 109.6 . . ?
C0 C1 H1A 109.6 . . ?
N21 C1 H1B 109.6 . . ?
C0 C1 H1B 109.6 . . ?
H1A C1 H1B 108.2 . . ?
C22 N21 C25 108.74(18) . . ?
C22 N21 C1 124.94(19) . . ?
C25 N21 C1 126.01(19) . . ?
N23 C22 N21 108.34(19) . . ?
N23 C22 H22 125.8 . . ?
N21 C22 H22 125.8 . . ?
C22 N23 C24 108.78(18) . . ?
C22 N23 C2 125.11(19) . . ?
C24 N23 C2 126.11(18) . . ?
C25 C24 N23 107.08(19) . . ?
C25 C24 H24 126.5 . . ?
N23 C24 H24 126.5 . . ?
C24 C25 N21 107.1(2) . . ?
C24 C25 H25 126.5 . . ?
N21 C25 H25 126.5 . . ?
N23 C2 C32 111.53(17) . . ?
N23 C2 H2A 109.3 . . ?
C32 C2 H2A 109.3 . . ?
N23 C2 H2B 109.3 . . ?
C32 C2 H2B 109.3 . . ?
H2A C2 H2B 108 . . ?
C36 C31 C32 119.6(2) . . ?
C36 C31 C3 117.40(19) . . ?
C32 C31 C3 122.98(19) . . ?
C31 C32 C33 118.6(2) . . ?
C31 C32 C2 124.08(19) . . ?
C33 C32 C2 117.28(19) . . ?
C34 C33 C32 120.9(2) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C33 C34 C35 120.4(2) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C36 C35 C34 119.0(2) . . ?
C36 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
C35 C36 C31 121.4(2) . . ?
C35 C36 H36 119.3 . . ?
C31 C36 H36 119.3 . . ?
N41 C3 C31 112.27(17) . . ?
N41 C3 H3A 109.2 . . ?
C31 C3 H3A 109.2 . . ?
N41 C3 H3B 109.2 . . ?
C31 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C42 N41 C45 109.03(19) . . ?
C42 N41 C3 125.44(18) . . ?
C45 N41 C3 124.57(18) . . ?
N41 C42 N43 108.34(19) . . ?
N41 C42 H42 125.8 . . ?
N43 C42 H42 125.8 . . ?
C42 N43 C44 108.28(19) . . ?
C42 N43 C4 126.3(2) . . ?
C44 N43 C4 125.30(19) . . ?
C45 C44 N43 107.4(2) . . ?
C45 C44 H44 126.3 . . ?
N43 C44 H44 126.3 . . ?
C44 C45 N41 106.9(2) . . ?
C44 C45 H45 126.5 . . ?
N41 C45 H45 126.5 . . ?
N43 C4 C5 110.81(18) . . ?
N43 C4 H4A 109.5 . . ?
C5 C4 H4A 109.5 . . ?
N43 C4 H4B 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C4 C5 C0 113.6(2) . . ?
C4 C5 H5A 108.8 . . ?
C0 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
C0 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?

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
C22 H22 Br1 0.95 2.52 3.463(2) 174.3 .
C42 H42 Br2 0.95 2.91 3.672(2) 137.7 .

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lw12a

_database_code_depnum_ccdc_archive 'CCDC 834019'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_date             2010-05-12T10:01:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C25 H24 N4, C2 H6 O, 2(Br)'
_chemical_formula_sum            'C27 H30 Br2 N4 O'
_chemical_formula_weight         586.37

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  -p_2ybc

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.578(2)
_cell_length_b                   22.0948(17)
_cell_length_c                   13.560(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.175(17)
_cell_angle_gamma                90
_cell_volume                     2869.6(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    19051
_cell_measurement_theta_min      2.5977
_cell_measurement_theta_max      31.8664

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
         CrysAlis RED, Oxford Diffraction Ltd.,
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_absorpt_correction_T_min  0.5136
_exptl_absorpt_correction_T_max  1


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measurement_device_type  
;
 Oxford Diffraction Xcalibur diffractometer

;
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_av_unetI/netI     0.049
_diffrn_reflns_number            51143
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.6
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_full        27.5
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             6588
_reflns_number_gt                4907
_reflns_threshold_expression     I>2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_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_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_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    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'



#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

All crystals of this compound were found to be merohedrally twinned. After 
application  of the twin law given in the cif, the structure was solved and 
refined.

One bromine atom was modelled as being disordered over two sites
with occupancies refined to 0.806(3) and its complement. It is possible 
that this apparent disorder is due to further unresolved twinning.

One solvent ethanol molecule is disordered about an inversion centre.

The geometries of the solvents were restrained to ideal values.

ADP's of the solvent molecules, the phenimidazolylidene and phenyl rings
  were restrained to reasonable values.

Ethanol hydroxyl hydrogen atoms were not included in the model.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1483P)²+5.5620P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6588
_refine_ls_number_parameters     346
_refine_ls_number_restraints     289
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0804
_refine_ls_wR_factor_ref         0.2403
_refine_ls_wR_factor_gt          0.228
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.353
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.145

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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
_atom_site_disorder_assembly
_atom_site_disorder_group
C0 C 0.2057(11) 0.1745(4) 0.6185(8) 0.064(3) Uani 1 1 d . . .
H0A H 0.2085 0.2184 0.6041 0.077 Uiso 1 1 calc R . .
H0B H 0.1073 0.1638 0.6323 0.077 Uiso 1 1 calc R . .
C1 C 0.2912(11) 0.1631(4) 0.7124(7) 0.054(3) Uani 1 1 d . . .
H1A H 0.2393 0.1784 0.7703 0.065 Uiso 1 1 calc R . .
H1B H 0.3053 0.119 0.7211 0.065 Uiso 1 1 calc R . .
N21 N 0.4219(9) 0.1921(3) 0.7072(4) 0.0454(16) Uani 1 1 d U . .
C22 C 0.5435(11) 0.1625(3) 0.6938(5) 0.0474(19) Uani 1 1 d U . .
H22 H 0.5515 0.1197 0.6892 0.057 Uiso 1 1 calc R . .
N23 N 0.6483(8) 0.1995(3) 0.6881(5) 0.0438(16) Uani 1 1 d U . .
C23A C 0.5965(9) 0.2577(3) 0.7019(5) 0.0373(15) Uani 1 1 d U . .
C24 C 0.6702(11) 0.3132(4) 0.7024(7) 0.0488(19) Uani 1 1 d U . .
H24 H 0.7678 0.3153 0.6908 0.059 Uiso 1 1 calc R . .
C25 C 0.5921(10) 0.3631(3) 0.7206(5) 0.0406(17) Uani 1 1 d U . .
H25 H 0.6369 0.4014 0.7247 0.049 Uiso 1 1 calc R . .
C26 C 0.4496(10) 0.3599(3) 0.7333(5) 0.0416(17) Uani 1 1 d U . .
H26 H 0.3996 0.3963 0.7449 0.05 Uiso 1 1 calc R . .
C27 C 0.3759(11) 0.3059(4) 0.7299(6) 0.0461(19) Uani 1 1 d U . .
H27 H 0.2775 0.3046 0.7387 0.055 Uiso 1 1 calc R . .
C27A C 0.4537(9) 0.2540(3) 0.7130(5) 0.0340(15) Uani 1 1 d U . .
C2 C 0.8020(10) 0.1847(4) 0.6617(9) 0.061(3) Uani 1 1 d . . .
H2A H 0.8272 0.2071 0.6011 0.073 Uiso 1 1 calc R . .
H2B H 0.8632 0.1995 0.7155 0.073 Uiso 1 1 calc R . .
C31 C 0.8014(10) 0.0891(4) 0.5556(7) 0.0471(19) Uani 1 1 d U . .
C32 C 0.8298(11) 0.1202(4) 0.6460(7) 0.058(2) Uani 1 1 d U . .
C33 C 0.8759(13) 0.0870(5) 0.7268(8) 0.064(2) Uani 1 1 d U . .
H33 H 0.8896 0.1066 0.7884 0.076 Uiso 1 1 calc R . .
C34 C 0.9026(15) 0.0248(5) 0.7184(9) 0.077(3) Uani 1 1 d U . .
H34 H 0.9379 0.003 0.7734 0.092 Uiso 1 1 calc R . .
C35 C 0.8779(14) -0.0043(5) 0.6319(7) 0.074(3) Uani 1 1 d DU . .
H35 H 0.8915 -0.0468 0.6274 0.088 Uiso 1 1 calc R . .
C36 C 0.8333(11) 0.0276(4) 0.5510(7) 0.055(2) Uani 1 1 d DU . .
H36 H 0.8239 0.0071 0.4898 0.065 Uiso 1 1 calc R . .
C3 C 0.7574(9) 0.1236(4) 0.4636(8) 0.051(2) Uani 1 1 d . . .
H3A H 0.827 0.1556 0.4503 0.061 Uiso 1 1 calc R . .
H3B H 0.7575 0.0955 0.4068 0.061 Uiso 1 1 calc R . .
N41 N 0.6203(7) 0.1511(3) 0.4714(5) 0.0314(13) Uani 1 1 d U . .
C42 C 0.5035(7) 0.1200(3) 0.4885(4) 0.0261(13) Uani 1 1 d U . .
H42 H 0.4997 0.0774 0.4983 0.031 Uiso 1 1 calc R . .
N43 N 0.3917(6) 0.1569(2) 0.4898(4) 0.0283(12) Uani 1 1 d U . .
C43A C 0.4385(8) 0.2159(3) 0.4729(5) 0.0289(13) Uani 1 1 d U . .
C44 C 0.3661(10) 0.2714(3) 0.4675(6) 0.0405(17) Uani 1 1 d U . .
H44 H 0.2678 0.2744 0.4748 0.049 Uiso 1 1 calc R . .
C45 C 0.4527(9) 0.3223(3) 0.4503(5) 0.0413(17) Uani 1 1 d DU . .
H45 H 0.4106 0.3612 0.4467 0.05 Uiso 1 1 calc RD . .
C46 C 0.5981(8) 0.3178(3) 0.4382(6) 0.0414(17) Uani 1 1 d DU . .
H46 H 0.6512 0.3535 0.4274 0.05 Uiso 1 1 calc R . .
C47 C 0.6646(9) 0.2629(3) 0.4418(7) 0.0434(18) Uani 1 1 d DU . .
H47 H 0.7624 0.2598 0.4313 0.052 Uiso 1 1 calc R . .
C47A C 0.5848(9) 0.2122(3) 0.4612(5) 0.0299(13) Uani 1 1 d U . .
C4 C 0.2520(8) 0.1396(4) 0.5231(8) 0.050(2) Uani 1 1 d . . .
H4A H 0.2507 0.0956 0.5366 0.06 Uiso 1 1 calc R . .
H4B H 0.184 0.1478 0.4696 0.06 Uiso 1 1 calc R . .
O101 O 0.588(2) 0.0414(7) 0.8798(11) 0.087(5) Uani 0.5 1 d PDU . .
C102 C 0.633(4) -0.0049(12) 0.942(2) 0.096(6) Uani 0.5 1 d PDU . .
H10A H 0.7364 -0.0042 0.9466 0.115 Uiso 0.5 1 calc PR . .
H10B H 0.6051 -0.0445 0.9141 0.115 Uiso 0.5 1 calc PR . .
C103 C 0.571(4) 0.0019(13) 1.0461(19) 0.109(7) Uani 0.5 1 d PDU . .
H10C H 0.5826 0.0437 1.0686 0.164 Uiso 0.5 1 calc PR . .
H10D H 0.6191 -0.0255 1.0916 0.164 Uiso 0.5 1 calc PR . .
H10E H 0.4713 -0.0082 1.0441 0.164 Uiso 0.5 1 calc PR . .
O201 O 0.021(3) 0.3537(13) 0.562(2) 0.154(8) Uani 0.5 1 d PDU . .
C202 C 0.100(5) 0.397(2) 0.534(4) 0.170(12) Uani 0.5 1 d PDU . .
H20A H 0.0435 0.4346 0.5295 0.204 Uiso 0.5 1 calc PR . .
H20B H 0.1348 0.3879 0.4672 0.204 Uiso 0.5 1 calc PR . .
C203 C 0.224(5) 0.410(2) 0.599(4) 0.185(14) Uani 0.5 1 d PDU . .
H20C H 0.1934 0.4128 0.668 0.278 Uiso 0.5 1 calc PR . .
H20D H 0.267 0.4484 0.5795 0.278 Uiso 0.5 1 calc PR . .
H20E H 0.2922 0.3773 0.5927 0.278 Uiso 0.5 1 calc PRD . .
Br1 Br 0.01982(12) 0.22774(5) 0.34567(9) 0.0706(4) Uani 1 1 d . . .
Br2 Br 0.43590(13) 0.00944(3) 0.66098(8) 0.0426(3) Uani 0.806(3) 1 d P A 1
Br2' Br 0.5967(6) 0.00792(15) 0.6569(3) 0.0480(16) Uani 0.194(3) 1 d P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.




;
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
C0 C1 1.533(15) . ?
C0 C4 1.571(14) . ?
C0 H0A 0.99 . ?
C0 H0B 0.99 . ?
C1 N21 1.408(12) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
N21 C22 1.348(12) . ?
N21 C27A 1.403(9) . ?
C22 N23 1.298(12) . ?
C22 H22 0.95 . ?
N23 C23A 1.390(9) . ?
N23 C2 1.551(13) . ?
C23A C27A 1.379(12) . ?
C23A C24 1.415(11) . ?
C24 C25 1.357(12) . ?
C24 H24 0.95 . ?
C25 C26 1.378(13) . ?
C25 H25 0.95 . ?
C26 C27 1.387(12) . ?
C26 H26 0.95 . ?
C27 C27A 1.388(11) . ?
C27 H27 0.95 . ?
C2 C32 1.464(12) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C31 C36 1.394(12) . ?
C31 C32 1.431(13) . ?
C31 C3 1.520(12) . ?
C32 C33 1.390(14) . ?
C33 C34 1.403(15) . ?
C33 H33 0.95 . ?
C34 C35 1.358(16) . ?
C34 H34 0.95 . ?
C35 C36 1.371(8) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C3 N41 1.451(11) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
N41 C42 1.335(9) . ?
N41 C47A 1.398(8) . ?
C42 N43 1.346(9) . ?
C42 H42 0.95 . ?
N43 C43A 1.398(8) . ?
N43 C4 1.464(10) . ?
C43A C44 1.410(10) . ?
C43A C47A 1.413(11) . ?
C44 C45 1.417(11) . ?
C44 H44 0.95 . ?
C45 C46 1.406(8) . ?
C45 H45 0.95 . ?
C46 C47 1.371(8) . ?
C46 H46 0.95 . ?
C47 C47A 1.382(10) . ?
C47 H47 0.95 . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
O101 C102 1.40(3) . ?
C102 C103 1.54(3) . ?
C102 H10A 0.99 . ?
C102 H10B 0.99 . ?
C103 H10C 0.98 . ?
C103 H10D 0.98 . ?
C103 H10E 0.98 . ?
O201 C202 1.29(3) . ?
C202 C203 1.50(3) . ?
C202 H20A 0.99 . ?
C202 H20B 0.99 . ?
C203 H20C 0.98 . ?
C203 H20D 0.98 . ?
C203 H20E 0.98 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C0 C4 116.8(7) . . ?
C1 C0 H0A 108.1 . . ?
C4 C0 H0A 108.1 . . ?
C1 C0 H0B 108.1 . . ?
C4 C0 H0B 108.1 . . ?
H0A C0 H0B 107.3 . . ?
N21 C1 C0 110.8(7) . . ?
N21 C1 H1A 109.5 . . ?
C0 C1 H1A 109.5 . . ?
N21 C1 H1B 109.5 . . ?
C0 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C22 N21 C27A 107.0(7) . . ?
C22 N21 C1 123.6(7) . . ?
C27A N21 C1 129.3(8) . . ?
N23 C22 N21 111.8(6) . . ?
N23 C22 H22 124.1 . . ?
N21 C22 H22 124.1 . . ?
C22 N23 C23A 107.4(7) . . ?
C22 N23 C2 127.9(7) . . ?
C23A N23 C2 124.5(7) . . ?
C27A C23A N23 108.3(7) . . ?
C27A C23A C24 123.1(8) . . ?
N23 C23A C24 128.6(8) . . ?
C25 C24 C23A 115.5(9) . . ?
C25 C24 H24 122.2 . . ?
C23A C24 H24 122.2 . . ?
C24 C25 C26 121.8(8) . . ?
C24 C25 H25 119.1 . . ?
C26 C25 H25 119.1 . . ?
C25 C26 C27 123.0(7) . . ?
C25 C26 H26 118.5 . . ?
C27 C26 H26 118.5 . . ?
C26 C27 C27A 116.3(9) . . ?
C26 C27 H27 121.8 . . ?
C27A C27 H27 121.8 . . ?
C23A C27A C27 120.2(7) . . ?
C23A C27A N21 105.5(7) . . ?
C27 C27A N21 134.3(8) . . ?
C32 C2 N23 114.4(8) . . ?
C32 C2 H2A 108.7 . . ?
N23 C2 H2A 108.7 . . ?
C32 C2 H2B 108.7 . . ?
N23 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C36 C31 C32 117.8(8) . . ?
C36 C31 C3 120.8(8) . . ?
C32 C31 C3 120.8(8) . . ?
C33 C32 C31 118.7(9) . . ?
C33 C32 C2 117.2(9) . . ?
C31 C32 C2 123.9(9) . . ?
C32 C33 C34 120.8(10) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
C35 C34 C33 120.2(10) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C34 C35 C36 120.0(10) . . ?
C34 C35 H35 120 . . ?
C36 C35 H35 120 . . ?
C35 C36 C31 122.2(9) . . ?
C35 C36 H36 118.9 . . ?
C31 C36 H36 118.9 . . ?
N41 C3 C31 113.6(7) . . ?
N41 C3 H3A 108.8 . . ?
C31 C3 H3A 108.8 . . ?
N41 C3 H3B 108.8 . . ?
C31 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
C42 N41 C47A 108.1(6) . . ?
C42 N41 C3 123.7(6) . . ?
C47A N41 C3 128.2(6) . . ?
N41 C42 N43 110.9(5) . . ?
N41 C42 H42 124.6 . . ?
N43 C42 H42 124.6 . . ?
C42 N43 C43A 107.9(6) . . ?
C42 N43 C4 125.0(6) . . ?
C43A N43 C4 126.0(6) . . ?
N43 C43A C44 131.4(7) . . ?
N43 C43A C47A 106.4(6) . . ?
C44 C43A C47A 122.2(7) . . ?
C43A C44 C45 114.3(8) . . ?
C43A C44 H44 122.9 . . ?
C45 C44 H44 122.9 . . ?
C46 C45 C44 122.9(7) . . ?
C46 C45 H45 118.5 . . ?
C44 C45 H45 118.5 . . ?
C47 C46 C45 121.2(7) . . ?
C47 C46 H46 119.4 . . ?
C45 C46 H46 119.4 . . ?
C46 C47 C47A 117.8(8) . . ?
C46 C47 H47 121.1 . . ?
C47A C47 H47 121.1 . . ?
C47 C47A N41 131.8(7) . . ?
C47 C47A C43A 121.5(6) . . ?
N41 C47A C43A 106.6(6) . . ?
N43 C4 C0 112.7(8) . . ?
N43 C4 H4A 109 . . ?
C0 C4 H4A 109 . . ?
N43 C4 H4B 109 . . ?
C0 C4 H4B 109 . . ?
H4A C4 H4B 107.8 . . ?
O101 C102 C103 111(2) . . ?
O101 C102 H10A 109.4 . . ?
C103 C102 H10A 109.4 . . ?
O101 C102 H10B 109.4 . . ?
C103 C102 H10B 109.4 . . ?
H10A C102 H10B 108 . . ?
C102 C103 H10C 109.5 . . ?
C102 C103 H10D 109.5 . . ?
H10C C103 H10D 109.5 . . ?
C102 C103 H10E 109.5 . . ?
H10C C103 H10E 109.5 . . ?
H10D C103 H10E 109.5 . . ?
O201 C202 C203 116(3) . . ?
O201 C202 H20A 108.3 . . ?
C203 C202 H20A 108.3 . . ?
O201 C202 H20B 108.3 . . ?
C203 C202 H20B 108.4 . . ?
H20A C202 H20B 107.4 . . ?
C202 C203 H20C 109.5 . . ?
C202 C203 H20D 109.5 . . ?
H20C C203 H20D 109.5 . . ?
C202 C203 H20E 109.5 . . ?
H20C C203 H20E 109.5 . . ?
H20D C203 H20E 109.5 . . ?

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
C22 H22 Br2 0.95 2.7 3.563(7) 150.8 .
C42 H42 Br2 0.95 2.74 3.444(6) 131.6 .
C22 H22 Br2' 0.95 2.55 3.489(8) 171.9 .
C42 H42 Br2' 0.95 2.8 3.483(7) 129.7 .

_diffrn_reflns_twin_matrix       
;
-1.00  0.00  0.00 0.00 -1.00  0.00 0.00  0.00 1.00 
;
_refine_ls_twin_fraction         0.47


#===END
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lw1p55

_database_code_depnum_ccdc_archive 'CCDC 834020'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_vrf_PLAT934_lw1p55              
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          3 Check
RESPONSE:  six reflections with poor agreement were omitted from the refinement.
;

_vrf_PLAT931_lw1p55              
;
PROBLEM: Found Twin Law ( 1 0  0)[       ] Estimated BASF       0.09 Check
        
RESPONSE:  Twin law appled with twin component fraction refined to 0.024.
;


_audit_creation_date             2015-01-20T10:02:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C26 H26 Br2 N4'
_chemical_formula_moiety         'C26 H26 N4, 2(Br)'
_chemical_formula_weight         554.33

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6464(10)
_cell_length_b                   13.5603(10)
_cell_length_c                   13.6869(10)
_cell_angle_alpha                90
_cell_angle_beta                 97.140(9)
_cell_angle_gamma                90
_cell_volume                     2329.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25290
_cell_measurement_theta_min      2.5476
_cell_measurement_theta_max      31.5043

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             1120

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
      CrysAlis RED, Oxford Diffraction Ltd.,
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_absorpt_correction_T_min  0.58181
_exptl_absorpt_correction_T_max  1.2228

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.0009
_diffrn_orient_matrix_ub_11      0.0165628717
_diffrn_orient_matrix_ub_12      -0.022263186
_diffrn_orient_matrix_ub_13      0.0461459159
_diffrn_orient_matrix_ub_21      0.0185386037
_diffrn_orient_matrix_ub_22      0.0463002825
_diffrn_orient_matrix_ub_23      0.0191818794
_diffrn_orient_matrix_ub_31      -0.0507001308
_diffrn_orient_matrix_ub_32      0.0095546301
_diffrn_orient_matrix_ub_33      0.0148495623
_diffrn_measurement_device_type  
;
 Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       'ω scans'

_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_number            64688
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.556
_diffrn_reflns_theta_max         31.581
_diffrn_reflns_theta_full        30.75
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.94
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.94
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.94
_reflns_number_total             7480
_reflns_number_gt                5078
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinement       
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction        
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'


#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 The central two carbon atoms of the C4 alkyl chain were modelled as being 
disordered over two sets of sites with occupancies set at 0.5 after trial 
refinement.
Refined as a 2-component twin.
six reflections with poor agreement were omitted from the refinement.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0535P)²+16.7251P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7480
_refine_ls_number_parameters     308
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1562
_refine_ls_wR_factor_gt          0.145
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.049
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.23

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.34053(3) 0.36035(3) 0.03931(4) 0.02480(12) Uani 1 d . .
Br2 Br 0.36967(4) 0.35911(4) 0.53475(3) 0.02556(12) Uani 1 d . .
C11 C 0.2118(8) 0.1273(8) 0.1409(7) 0.028(2) Uani 0.5 d A 1
H11A H 0.141 0.1476 0.1079 0.034 Uiso 0.5 calc A 1
H11B H 0.2469 0.1862 0.1729 0.034 Uiso 0.5 calc A 1
C12 C 0.1973(7) 0.0502(8) 0.2190(8) 0.027(2) Uani 0.5 d A 1
H12A H 0.2441 -0.0071 0.2114 0.033 Uiso 0.5 calc A 1
H12B H 0.1225 0.0269 0.2111 0.033 Uiso 0.5 calc A 1
C11' C 0.1982(7) 0.0590(6) 0.1433(7) 0.0192(16) Uani 0.5 d A 2
H11C H 0.1274 0.0443 0.1068 0.023 Uiso 0.5 calc A 2
H11D H 0.2252 -0.0026 0.1765 0.023 Uiso 0.5 calc A 2
C12' C 0.1839(7) 0.1369(7) 0.2232(7) 0.0212(16) Uani 0.5 d A 2
H12C H 0.2224 0.198 0.2094 0.025 Uiso 0.5 calc A 2
H12D H 0.1073 0.1532 0.2212 0.025 Uiso 0.5 calc A 2
C1 C 0.2767(4) 0.0895(4) 0.0661(4) 0.0261(9) Uani 1 d . .
H1A H 0.2462 0.0261 0.0401 0.031 Uiso 0.5 calc A 1
H1B H 0.2727 0.1368 0.0107 0.031 Uiso 0.5 calc A 1
H1C H 0.2598 0.0499 0.0054 0.031 Uiso 0.5 calc A 2
H1D H 0.2652 0.1598 0.0484 0.031 Uiso 0.5 calc A 2
N21 N 0.3888(3) 0.0744(3) 0.1054(3) 0.0205(7) Uani 1 d . .
C22 C 0.4582(3) 0.1458(4) 0.1391(3) 0.0235(9) Uani 1 d . .
H22 H 0.4411 0.2139 0.1424 0.028 Uiso 1 calc . .
N23 N 0.5536(3) 0.1075(3) 0.1671(3) 0.0187(7) Uani 1 d . .
C23A C 0.5494(3) 0.0060(3) 0.1495(3) 0.0193(8) Uani 1 d . .
C24 C 0.6266(4) -0.0671(4) 0.1629(3) 0.0255(9) Uani 1 d . .
H24 H 0.698 -0.0528 0.1893 0.031 Uiso 1 calc . .
C25 C 0.5945(4) -0.1622(4) 0.1358(4) 0.0297(10) Uani 1 d . .
H25 H 0.6448 -0.2145 0.1448 0.036 Uiso 1 calc . .
C26 C 0.4894(4) -0.1828(4) 0.0955(4) 0.0272(10) Uani 1 d . .
H26 H 0.4707 -0.2487 0.077 0.033 Uiso 1 calc . .
C27 C 0.4121(4) -0.1103(4) 0.0819(3) 0.0230(9) Uani 1 d . .
H27 H 0.341 -0.1247 0.0548 0.028 Uiso 1 calc . .
C27A C 0.4442(3) -0.0144(3) 0.1100(3) 0.0191(8) Uani 1 d . .
C2 C 0.6507(3) 0.1626(3) 0.2086(3) 0.0231(9) Uani 1 d . .
H2A H 0.7054 0.1569 0.163 0.028 Uiso 1 calc . .
H2B H 0.6799 0.1324 0.2721 0.028 Uiso 1 calc . .
C31 C 0.5967(3) 0.3058(3) 0.3132(3) 0.0220(8) Uani 1 d . .
C32 C 0.6279(3) 0.2699(4) 0.2246(3) 0.0240(9) Uani 1 d . .
C33 C 0.6362(4) 0.3349(4) 0.1475(4) 0.0313(11) Uani 1 d . .
H33 H 0.6569 0.3106 0.0876 0.038 Uiso 1 calc . .
C34 C 0.6149(4) 0.4352(4) 0.1564(4) 0.0365(12) Uani 1 d . .
H34 H 0.6197 0.4785 0.1025 0.044 Uiso 1 calc . .
C35 C 0.5868(4) 0.4710(4) 0.2438(4) 0.0338(12) Uani 1 d . .
H35 H 0.5741 0.5396 0.2509 0.041 Uiso 1 calc . .
C36 C 0.5768(4) 0.4066(3) 0.3222(4) 0.0274(10) Uani 1 d . .
H36 H 0.5563 0.4316 0.382 0.033 Uiso 1 calc . .
C3 C 0.5874(4) 0.2414(3) 0.4016(3) 0.0213(8) Uani 1 d . .
H3A H 0.6565 0.2081 0.4212 0.026 Uiso 1 calc . .
H3B H 0.572 0.2835 0.4573 0.026 Uiso 1 calc . .
N41 N 0.5031(3) 0.1661(3) 0.3830(3) 0.0194(7) Uani 1 d . .
C42 C 0.3998(4) 0.1866(4) 0.3628(3) 0.0238(9) Uani 1 d . .
H42 H 0.3701 0.251 0.3598 0.029 Uiso 1 calc . .
N43 N 0.3439(3) 0.1032(3) 0.3471(3) 0.0225(7) Uani 1 d . .
C43A C 0.4141(3) 0.0234(3) 0.3585(3) 0.0201(8) Uani 1 d . .
C44 C 0.3968(4) -0.0775(4) 0.3514(3) 0.0236(9) Uani 1 d . .
H44 H 0.3276 -0.1045 0.3347 0.028 Uiso 1 calc . .
C45 C 0.4867(4) -0.1367(3) 0.3700(3) 0.0234(8) Uani 1 d . .
H45 H 0.4794 -0.2063 0.3646 0.028 Uiso 1 calc . .
C46 C 0.5888(4) -0.0953(3) 0.3967(3) 0.0233(9) Uani 1 d . .
H46 H 0.6483 -0.1381 0.4097 0.028 Uiso 1 calc . .
C47 C 0.6049(4) 0.0042(3) 0.4044(3) 0.0203(8) Uani 1 d . .
H47 H 0.6737 0.0313 0.4232 0.024 Uiso 1 calc . .
C47A C 0.5153(3) 0.0639(3) 0.3833(3) 0.0184(8) Uani 1 d . .
C4 C 0.2268(4) 0.0983(5) 0.3266(4) 0.0355(12) Uani 1 d . .
H4A H 0.196 0.1653 0.3282 0.043 Uiso 0.5 calc A 1
H4B H 0.1977 0.0575 0.3769 0.043 Uiso 0.5 calc A 1
H4C H 0.1953 0.1377 0.3766 0.043 Uiso 0.5 calc A 2
H4D H 0.2038 0.0291 0.3327 0.043 Uiso 0.5 calc A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C11 C1 1.480(11) . ?
C11 C12 1.523(14) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C12 C4 1.612(12) . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
C11' C12' 1.548(12) . ?
C11' C1 1.591(10) . ?
C11' H11C 0.99 . ?
C11' H11D 0.99 . ?
C12' C4 1.543(10) . ?
C12' H12C 0.99 . ?
C12' H12D 0.99 . ?
C1 N21 1.466(6) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C1 H1C 0.99 . ?
C1 H1D 0.99 . ?
N21 C22 1.349(6) . ?
N21 C27A 1.392(6) . ?
C22 N23 1.326(6) . ?
C22 H22 0.95 . ?
N23 C23A 1.398(6) . ?
N23 C2 1.488(5) . ?
C23A C24 1.387(6) . ?
C23A C27A 1.400(6) . ?
C24 C25 1.389(7) . ?
C24 H24 0.95 . ?
C25 C26 1.402(7) . ?
C25 H25 0.95 . ?
C26 C27 1.382(7) . ?
C26 H26 0.95 . ?
C27 C27A 1.402(6) . ?
C27 H27 0.95 . ?
C2 C32 1.505(7) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C31 C32 1.407(7) . ?
C31 C36 1.399(6) . ?
C31 C3 1.510(6) . ?
C32 C33 1.389(7) . ?
C33 C34 1.395(8) . ?
C33 H33 0.95 . ?
C34 C35 1.378(9) . ?
C34 H34 0.95 . ?
C35 C36 1.402(7) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C3 N41 1.476(6) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
N41 C42 1.331(6) . ?
N41 C47A 1.393(6) . ?
C42 N43 1.337(6) . ?
C42 H42 0.95 . ?
N43 C43A 1.396(6) . ?
N43 C4 1.474(6) . ?
C43A C44 1.387(7) . ?
C43A C47A 1.395(6) . ?
C44 C45 1.389(7) . ?
C44 H44 0.95 . ?
C45 C46 1.413(7) . ?
C45 H45 0.95 . ?
C46 C47 1.367(6) . ?
C46 H46 0.95 . ?
C47 C47A 1.394(6) . ?
C47 H47 0.95 . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C4 H4C 0.99 . ?
C4 H4D 0.99 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C11 C12 111.9(8) . . ?
C1 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
C1 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 C4 109.2(7) . . ?
C11 C12 H12A 109.8 . . ?
C4 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
C4 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
C12' C11' C1 115.4(7) . . ?
C12' C11' H11C 108.4 . . ?
C1 C11' H11C 108.4 . . ?
C12' C11' H11D 108.4 . . ?
C1 C11' H11D 108.4 . . ?
H11C C11' H11D 107.5 . . ?
C4 C12' C11' 111.0(7) . . ?
C4 C12' H12C 109.4 . . ?
C11' C12' H12C 109.4 . . ?
C4 C12' H12D 109.4 . . ?
C11' C12' H12D 109.4 . . ?
H12C C12' H12D 108 . . ?
N21 C1 C11 112.9(5) . . ?
N21 C1 C11' 112.0(5) . . ?
N21 C1 H1A 109 . . ?
C11 C1 H1A 109 . . ?
N21 C1 H1B 109 . . ?
C11 C1 H1B 109 . . ?
H1A C1 H1B 107.8 . . ?
N21 C1 H1C 109.2 . . ?
C11' C1 H1C 109.2 . . ?
N21 C1 H1D 109.2 . . ?
C11' C1 H1D 109.2 . . ?
H1C C1 H1D 107.9 . . ?
C22 N21 C27A 107.6(4) . . ?
C22 N21 C1 125.7(4) . . ?
C27A N21 C1 126.6(4) . . ?
N23 C22 N21 110.4(4) . . ?
N23 C22 H22 124.8 . . ?
N21 C22 H22 124.8 . . ?
C22 N23 C23A 108.8(4) . . ?
C22 N23 C2 126.3(4) . . ?
C23A N23 C2 124.9(4) . . ?
C24 C23A C27A 121.9(4) . . ?
C24 C23A N23 132.1(4) . . ?
C27A C23A N23 106.0(4) . . ?
C23A C24 C25 116.8(4) . . ?
C23A C24 H24 121.6 . . ?
C25 C24 H24 121.6 . . ?
C24 C25 C26 121.4(5) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C27 C26 C25 122.1(5) . . ?
C27 C26 H26 119 . . ?
C25 C26 H26 119 . . ?
C26 C27 C27A 116.5(4) . . ?
C26 C27 H27 121.7 . . ?
C27A C27 H27 121.7 . . ?
N21 C27A C23A 107.2(4) . . ?
N21 C27A C27 131.6(4) . . ?
C23A C27A C27 121.2(4) . . ?
N23 C2 C32 112.1(4) . . ?
N23 C2 H2A 109.2 . . ?
C32 C2 H2A 109.2 . . ?
N23 C2 H2B 109.2 . . ?
C32 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C32 C31 C36 119.2(4) . . ?
C32 C31 C3 123.3(4) . . ?
C36 C31 C3 117.5(4) . . ?
C33 C32 C31 119.3(5) . . ?
C33 C32 C2 118.0(4) . . ?
C31 C32 C2 122.7(4) . . ?
C32 C33 C34 121.3(5) . . ?
C32 C33 H33 119.4 . . ?
C34 C33 H33 119.4 . . ?
C35 C34 C33 119.5(5) . . ?
C35 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
C34 C35 C36 120.2(5) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C35 C36 C31 120.4(5) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
N41 C3 C31 112.9(4) . . ?
N41 C3 H3A 109 . . ?
C31 C3 H3A 109 . . ?
N41 C3 H3B 109 . . ?
C31 C3 H3B 109 . . ?
H3A C3 H3B 107.8 . . ?
C42 N41 C47A 108.3(4) . . ?
C42 N41 C3 124.1(4) . . ?
C47A N41 C3 127.6(4) . . ?
N41 C42 N43 110.0(4) . . ?
N41 C42 H42 125 . . ?
N43 C42 H42 125 . . ?
C42 N43 C43A 108.8(4) . . ?
C42 N43 C4 124.5(4) . . ?
C43A N43 C4 126.6(4) . . ?
C44 C43A N43 131.6(4) . . ?
C44 C43A C47A 122.5(4) . . ?
N43 C43A C47A 105.8(4) . . ?
C45 C44 C43A 116.0(4) . . ?
C45 C44 H44 122 . . ?
C43A C44 H44 122 . . ?
C44 C45 C46 121.2(4) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 H45 119.4 . . ?
C47 C46 C45 122.4(4) . . ?
C47 C46 H46 118.8 . . ?
C45 C46 H46 118.8 . . ?
C46 C47 C47A 116.6(4) . . ?
C46 C47 H47 121.7 . . ?
C47A C47 H47 121.7 . . ?
C47 C47A C43A 121.3(4) . . ?
C47 C47A N41 131.7(4) . . ?
C43A C47A N41 107.1(4) . . ?
N43 C4 C12' 113.0(5) . . ?
N43 C4 C12 107.8(5) . . ?
N43 C4 H4A 110.1 . . ?
C12 C4 H4A 110.1 . . ?
N43 C4 H4B 110.1 . . ?
C12 C4 H4B 110.1 . . ?
H4A C4 H4B 108.5 . . ?
N43 C4 H4C 109 . . ?
C12' C4 H4C 109 . . ?
N43 C4 H4D 109 . . ?
C12' C4 H4D 109 . . ?
H4C C4 H4D 107.8 . . ?

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
C22 H22 Br1 0.95 2.67 3.470(5) 142.7 .
C42 H42 Br2 0.95 2.81 3.374(5) 119.1 .

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lw1193

_database_code_depnum_ccdc_archive 'CCDC 834021'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_date             2007-02-15T14:18:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C36 H46 Au2 Br Cl N8 O3'
_chemical_formula_moiety         'C36 H40 Au2 N8, Br, Cl, 3(H2 O) '
_chemical_formula_weight         1148.1
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P m c 21'
_symmetry_space_group_name_Hall  p_2c_-2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, z'
'x, -y, z+1/2'

_cell_length_a                   14.5133(5)
_cell_length_b                   7.1167(2)
_cell_length_c                   19.1502(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1977.96(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7925
_cell_measurement_theta_min      2.8609
_cell_measurement_theta_max      31.8741

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    8.532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.37824
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.0009
_diffrn_orient_matrix_ub_11      0.0900927503
_diffrn_orient_matrix_ub_12      0.0155848649
_diffrn_orient_matrix_ub_13      0.0108343836
_diffrn_orient_matrix_ub_21      0.0261718794
_diffrn_orient_matrix_ub_22      0.0065498841
_diffrn_orient_matrix_ub_23      -0.035474174
_diffrn_orient_matrix_ub_31      -0.0342133457
_diffrn_orient_matrix_ub_32      0.0458630631
_diffrn_orient_matrix_ub_33      0.0013249575
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.1177
_diffrn_reflns_number            27729
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         31.96
_diffrn_reflns_theta_full        31
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  
;
 Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       'ω scans'

_reflns_number_total             6523
_reflns_number_gt                4368
_reflns_threshold_expression     I>2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinement       
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction        
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'


#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

The anionic sites were modelled as being occupied partially by Cl- and Br- 
ions (for site (1)), or Br- and H2O (site (2)), or Cl- and H2O (site (3))
 with occupancies set at 0.5 after trial refinement.  Other peaks in the 
difference maps were modelled as being water molecules with occupancies 
set at either 1.0 or 0.5 after trial refinement and considerations of 
molecular interactions. Anisotropic displacement parameters were employed 
for the non-hydrogen atoms. Water molecule hydrogen atoms were not located. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0750P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6523
_refine_ls_number_parameters     239
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1462
_refine_ls_wR_factor_gt          0.1367
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.003
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.062(19)
_refine_diff_density_max         4.257
_refine_diff_density_min         -1.768
_refine_diff_density_rms         0.283

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.006 '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'

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0 0.51253(6) 0.499988(18) 0.03169(10) Uani 1 2 d S . .
Au2 Au 0 0.95796(5) 0.545569(16) 0.02787(9) Uani 1 2 d S . .
Br1 Br 0 0.8349(3) 0.28087(9) 0.0521(6) Uani 0.5 2 d SP . .
Cl1 Cl 0 0.8349(3) 0.28087(9) 0.0521(6) Uani 0.5 2 d SP . .
O2 O 0.5 0.597(5) 0.6880(15) 0.1615(17) Uani 0.5 2 d SP . .
Br2 Br 0.5 0.6259(10) 0.6681(2) 0.1615(17) Uani 0.5 2 d SP . .
O3 Cl 0.5 0.3094(15) 0.6039(5) 0.091(3) Uiso 0.5 2 d SP . .
CL3 O 0.5 0.197(4) 0.6042(13) 0.091(3) Uiso 0.5 2 d SP . .
C11 C 0.1213(6) 0.5599(12) 0.6671(4) 0.041(2) Uani 1 1 d . . .
H11A H 0.0774 0.6296 0.6372 0.049 Uiso 1 1 calc R . .
H11B H 0.0857 0.5073 0.7066 0.049 Uiso 1 1 calc R . .
C12 C 0.1900(6) 0.6989(11) 0.6961(4) 0.038(2) Uani 1 1 d . . .
H12A H 0.2524 0.6653 0.6795 0.046 Uiso 1 1 calc R . .
H12B H 0.1899 0.6905 0.7477 0.046 Uiso 1 1 calc R . .
C1 C 0.1599(7) 0.3948(10) 0.6243(4) 0.040(2) Uani 1 1 d . . .
H1A H 0.2114 0.3364 0.6503 0.048 Uiso 1 1 calc R . .
H1B H 0.1112 0.2988 0.6184 0.048 Uiso 1 1 calc R . .
N21 N 0.1928(5) 0.4528(8) 0.5555(4) 0.0345(16) Uani 1 1 d . . .
C22 C 0.1352(6) 0.5080(10) 0.5021(5) 0.0359(19) Uani 1 1 d . . .
N23 N 0.1958(4) 0.5540(9) 0.4490(4) 0.0336(17) Uani 1 1 d . . .
C24 C 0.2902(6) 0.5320(11) 0.4711(6) 0.047(3) Uani 1 1 d . . .
H24 H 0.3439 0.5573 0.4444 0.056 Uiso 1 1 calc R . .
C25 C 0.2868(7) 0.4673(11) 0.5384(5) 0.045(2) Uani 1 1 d . . .
H25 H 0.3376 0.4382 0.5676 0.054 Uiso 1 1 calc R . .
C2 C 0.1702(6) 0.6221(12) 0.3789(4) 0.037(2) Uani 1 1 d . . .
H2A H 0.1079 0.6781 0.3813 0.044 Uiso 1 1 calc R . .
H2B H 0.1672 0.5134 0.3467 0.044 Uiso 1 1 calc R . .
C31 C 0.2347(5) 0.9535(10) 0.3681(4) 0.0311(18) Uani 1 1 d . . .
C32 C 0.2358(5) 0.7657(11) 0.3491(3) 0.033(2) Uani 1 1 d . . .
C33 C 0.3015(6) 0.7002(16) 0.3001(3) 0.037(2) Uani 1 1 d . . .
H33 H 0.3028 0.5709 0.2877 0.045 Uiso 1 1 calc R . .
C34 C 0.3629(6) 0.8217(15) 0.2705(5) 0.052(3) Uani 1 1 d . . .
H34 H 0.4054 0.7769 0.2366 0.063 Uiso 1 1 calc R . .
C35 C 0.3641(6) 1.0187(18) 0.2902(4) 0.043(3) Uani 1 1 d . . .
H35 H 0.4067 1.1048 0.2704 0.052 Uiso 1 1 calc R . .
C36 C 0.3005(6) 1.0737(12) 0.3388(4) 0.037(2) Uani 1 1 d . . .
H36 H 0.301 1.2011 0.3536 0.045 Uiso 1 1 calc R . .
C3 C 0.1694(5) 1.0307(10) 0.4200(4) 0.0301(19) Uani 1 1 d . . .
H3A H 0.1626 1.1674 0.412 0.036 Uiso 1 1 calc R . .
H3B H 0.1083 0.9718 0.4129 0.036 Uiso 1 1 calc R . .
N41 N 0.1986(4) 0.9994(8) 0.4919(4) 0.0270(15) Uani 1 1 d . . .
C42 C 0.1412(5) 0.9655(8) 0.5466(5) 0.0238(15) Uani 1 1 d . . .
N43 N 0.1989(5) 0.9406(8) 0.6019(3) 0.0261(16) Uani 1 1 d . . .
C44 C 0.2863(6) 0.9632(10) 0.5828(4) 0.0258(19) Uani 1 1 d . . .
H44 H 0.3386 0.9527 0.6123 0.031 Uiso 1 1 calc R . .
C45 C 0.2874(5) 1.0028(11) 0.5156(4) 0.0253(18) Uani 1 1 d . . .
H45 H 0.3406 1.0291 0.4884 0.03 Uiso 1 1 calc R . .
C4 C 0.1683(7) 0.9009(12) 0.6744(4) 0.033(2) Uani 1 1 d . . .
H4A H 0.1011 0.9225 0.678 0.04 Uiso 1 1 calc R . .
H4B H 0.1994 0.9888 0.7068 0.04 Uiso 1 1 calc R . .
O4 O 0.5 0.123(2) 0.4486(8) 0.044(4) Uiso 0.5 2 d SP A 3
O5 O 0.5 0.727(3) 0.4627(10) 0.069(6) Uiso 0.5 2 d SP B 4
O6 O 0 0.2890(7) 0.3220(3) 0.0085(11) Uiso 1 2 d S C 5



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Au1 C22 1.963(9) 3 ?
Au1 C22 1.963(9) . ?
Au1 Au2 3.2880(6) . ?
Au2 C42 2.051(7) 3 ?
Au2 C42 2.051(7) . ?
C11 C12 1.511(11) . ?
C11 C1 1.538(12) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C12 C4 1.529(11) . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
C1 N21 1.460(11) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
N21 C22 1.379(11) . ?
N21 C25 1.406(12) . ?
C22 N23 1.384(11) . ?
N23 C24 1.443(11) . ?
N23 C2 1.473(11) . ?
C24 C25 1.369(14) . ?
C24 H24 0.95 . ?
C25 H25 0.95 . ?
C2 C32 1.509(11) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C31 C32 1.386(11) . ?
C31 C36 1.398(11) . ?
C31 C3 1.479(11) . ?
C32 C33 1.417(11) . ?
C33 C34 1.365(13) . ?
C33 H33 0.95 . ?
C34 C35 1.452(16) . ?
C34 H34 0.95 . ?
C35 C36 1.368(12) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C3 N41 1.459(10) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
N41 C42 1.359(11) . ?
N41 C45 1.366(9) . ?
C42 N43 1.362(10) . ?
N43 C44 1.330(11) . ?
N43 C4 1.485(9) . ?
C44 C45 1.317(11) . ?
C44 H44 0.95 . ?
C45 H45 0.95 . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22 Au1 C22 177.0(5) 3 . ?
C22 Au1 Au2 90.6(2) 3 . ?
C22 Au1 Au2 90.6(2) . . ?
C42 Au2 C42 176.8(4) 3 . ?
C42 Au2 Au1 91.59(17) 3 . ?
C42 Au2 Au1 91.59(17) . . ?
C12 C11 C1 117.1(7) . . ?
C12 C11 H11A 108 . . ?
C1 C11 H11A 108 . . ?
C12 C11 H11B 108 . . ?
C1 C11 H11B 108 . . ?
H11A C11 H11B 107.3 . . ?
C11 C12 C4 112.3(7) . . ?
C11 C12 H12A 109.1 . . ?
C4 C12 H12A 109.1 . . ?
C11 C12 H12B 109.1 . . ?
C4 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
N21 C1 C11 112.6(6) . . ?
N21 C1 H1A 109.1 . . ?
C11 C1 H1A 109.1 . . ?
N21 C1 H1B 109.1 . . ?
C11 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C22 N21 C25 113.2(7) . . ?
C22 N21 C1 123.4(7) . . ?
C25 N21 C1 123.3(7) . . ?
N21 C22 N23 103.1(7) . . ?
N21 C22 Au1 128.8(7) . . ?
N23 C22 Au1 128.0(7) . . ?
C22 N23 C24 111.2(7) . . ?
C22 N23 C2 126.0(7) . . ?
C24 N23 C2 122.8(7) . . ?
C25 C24 N23 106.2(9) . . ?
C25 C24 H24 126.9 . . ?
N23 C24 H24 126.9 . . ?
C24 C25 N21 106.2(8) . . ?
C24 C25 H25 126.9 . . ?
N21 C25 H25 126.9 . . ?
N23 C2 C32 114.1(6) . . ?
N23 C2 H2A 108.7 . . ?
C32 C2 H2A 108.7 . . ?
N23 C2 H2B 108.7 . . ?
C32 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C32 C31 C36 118.5(7) . . ?
C32 C31 C3 122.8(7) . . ?
C36 C31 C3 118.7(7) . . ?
C31 C32 C33 119.9(8) . . ?
C31 C32 C2 123.2(7) . . ?
C33 C32 C2 116.9(8) . . ?
C34 C33 C32 120.4(10) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 120.7(8) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 H34 119.6 . . ?
C36 C35 C34 116.5(9) . . ?
C36 C35 H35 121.8 . . ?
C34 C35 H35 121.8 . . ?
C35 C36 C31 123.9(9) . . ?
C35 C36 H36 118 . . ?
C31 C36 H36 118 . . ?
N41 C3 C31 113.1(6) . . ?
N41 C3 H3A 109 . . ?
C31 C3 H3A 109 . . ?
N41 C3 H3B 109 . . ?
C31 C3 H3B 109 . . ?
H3A C3 H3B 107.8 . . ?
C42 N41 C45 109.0(7) . . ?
C42 N41 C3 125.2(6) . . ?
C45 N41 C3 125.8(7) . . ?
N41 C42 N43 104.2(6) . . ?
N41 C42 Au2 127.6(6) . . ?
N43 C42 Au2 128.2(6) . . ?
C44 N43 C42 110.8(6) . . ?
C44 N43 C4 124.5(7) . . ?
C42 N43 C4 124.6(7) . . ?
C45 C44 N43 107.9(7) . . ?
C45 C44 H44 126.1 . . ?
N43 C44 H44 126.1 . . ?
C44 C45 N41 108.0(7) . . ?
C44 C45 H45 126 . . ?
N41 C45 H45 126 . . ?
N43 C4 C12 111.8(7) . . ?
N43 C4 H4A 109.3 . . ?
C12 C4 H4A 109.3 . . ?
N43 C4 H4B 109.3 . . ?
C12 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?

#===END 
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lw1194

_database_code_depnum_ccdc_archive 'CCDC 834022'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_date             2007-02-06T09:08:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C40 H60 Au2 Br0.75 Cl1.25 N8 O6'
_chemical_formula_moiety         
;
C36 H40 Au2 N8, 0.75(Br),1.25(Cl),4(C H4 O), 2(H2 O)
;
_chemical_formula_weight         1247.14

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P_-1
_symmetry_space_group_name_Hall  -p_1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1215(5)
_cell_length_b                   11.4030(10)
_cell_length_c                   11.959(3)
_cell_angle_alpha                84.260(10)
_cell_angle_beta                 82.030(10)
_cell_angle_gamma                78.157(7)
_cell_volume                     1070.5(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    24757
_cell_measurement_theta_min      2.5722
_cell_measurement_theta_max      37.3237

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             610
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    7.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.40154
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.0009
_diffrn_orient_matrix_ub_11      -0.0074624361
_diffrn_orient_matrix_ub_12      0.0093408434
_diffrn_orient_matrix_ub_13      -0.0586639224
_diffrn_orient_matrix_ub_21      -0.0171457445
_diffrn_orient_matrix_ub_22      -0.0585100624
_diffrn_orient_matrix_ub_23      0.0003461148
_diffrn_orient_matrix_ub_31      -0.0878230697
_diffrn_orient_matrix_ub_32      0.0232320473
_diffrn_orient_matrix_ub_33      0.0123185507
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_number            49142
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.58
_diffrn_reflns_theta_max         37.45
_diffrn_reflns_theta_full        36.5
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  
;
 Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       'ω scans'

_reflns_number_total             10859
_reflns_number_gt                8807
_reflns_threshold_expression     I>2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinement       
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction        
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'


#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 The CH3OH and water molecule H atoms were located in the difference map. The 
 CH3OH hydroxyl H atoms were refined as parts of riding models. The 
geometries of the water molecule H atoms were restrained to ideal values.
The halide site was refined as being occupied part by Br and part Cl, 
the occupancies refining to Cl 0.624(2), Br 1-0.624(2). 

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0156P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         10859
_refine_ls_number_parameters     275
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.032
_refine_ls_R_factor_gt           0.0227
_refine_ls_wR_factor_ref         0.0416
_refine_ls_wR_factor_gt          0.0403
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_diff_density_max         4.395
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.148

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.342036(8) 0.557298(6) 0.437033(6) 0.01191(2) Uani 1 1 d . . .
Cl1 Cl 0.72373(4) 0.86294(3) 0.87936(3) 0.01813(9) Uani 0.6236(16) 1 d P . .
Br1 Br 0.72373(4) 0.86294(3) 0.87936(3) 0.01813(9) Uani 0.3764(16) 1 d P . .
C0 C 0.3407(2) 0.76043(16) 0.64775(15) 0.0157(3) Uani 1 1 d . . .
H0A H 0.3666 0.8399 0.619 0.019 Uiso 1 1 calc R . .
H0B H 0.4147 0.6997 0.6 0.019 Uiso 1 1 calc R . .
C1 C 0.1562(2) 0.76087(15) 0.63410(16) 0.0159(3) Uani 1 1 d . . .
H1A H 0.0809 0.8131 0.6892 0.019 Uiso 1 1 calc R . .
H1B H 0.1336 0.7952 0.5571 0.019 Uiso 1 1 calc R . .
N21 N 0.11640(18) 0.63982(13) 0.65169(12) 0.0120(3) Uani 1 1 d . . .
C22 C 0.1866(2) 0.54953(15) 0.58416(15) 0.0115(3) Uani 1 1 d . . .
N23 N 0.11723(18) 0.45513(12) 0.63026(12) 0.0111(3) Uani 1 1 d . . .
C24 C 0.0002(2) 0.48653(16) 0.72317(15) 0.0149(3) Uani 1 1 d . . .
H24 H -0.067 0.4364 0.7683 0.018 Uiso 1 1 calc R . .
C25 C 0.0005(2) 0.60267(16) 0.73702(15) 0.0150(3) Uani 1 1 d . . .
H25 H -0.0661 0.6498 0.7943 0.018 Uiso 1 1 calc R . .
C2 C 0.1566(2) 0.33792(15) 0.58021(15) 0.0136(3) Uani 1 1 d . . .
H2A H 0.2702 0.3286 0.5358 0.016 Uiso 1 1 calc R . .
H2B H 0.0733 0.3372 0.5273 0.016 Uiso 1 1 calc R . .
C31 C 0.2945(2) 0.17833(15) 0.72346(14) 0.0120(3) Uani 1 1 d . . .
C32 C 0.1538(2) 0.23257(15) 0.66658(15) 0.0125(3) Uani 1 1 d . . .
C33 C 0.0077(2) 0.18303(16) 0.68720(16) 0.0155(3) Uani 1 1 d . . .
H33 H -0.0875 0.2189 0.6492 0.019 Uiso 1 1 calc R . .
C34 C -0.0016(2) 0.08276(17) 0.76186(16) 0.0175(4) Uani 1 1 d . . .
H34 H -0.1024 0.0509 0.775 0.021 Uiso 1 1 calc R . .
C35 C 0.1369(2) 0.02921(16) 0.81724(16) 0.0182(4) Uani 1 1 d . . .
H35 H 0.1318 -0.0397 0.8683 0.022 Uiso 1 1 calc R . .
C36 C 0.2840(2) 0.07733(15) 0.79736(16) 0.0156(3) Uani 1 1 d . . .
H36 H 0.3789 0.0402 0.8352 0.019 Uiso 1 1 calc R . .
C3 C 0.4586(2) 0.22458(15) 0.70621(15) 0.0131(3) Uani 1 1 d . . .
H3A H 0.5482 0.1628 0.7377 0.016 Uiso 1 1 calc R . .
H3B H 0.4934 0.2383 0.624 0.016 Uiso 1 1 calc R . .
N41 N 0.44338(17) 0.33729(13) 0.76072(12) 0.0111(3) Uani 1 1 d . . .
C42 C 0.5169(2) 0.43032(15) 0.71530(14) 0.0110(3) Uani 1 1 d . . .
N43 N 0.47829(18) 0.51123(13) 0.79486(12) 0.0123(3) Uani 1 1 d . . .
C44 C 0.3830(2) 0.46851(16) 0.88940(15) 0.0142(3) Uani 1 1 d . . .
H44 H 0.3408 0.5087 0.9564 0.017 Uiso 1 1 calc R . .
C45 C 0.3613(2) 0.35909(16) 0.86837(15) 0.0137(3) Uani 1 1 d . . .
H45 H 0.3016 0.3071 0.9176 0.016 Uiso 1 1 calc R . .
C4 C 0.5305(2) 0.62773(15) 0.78666(16) 0.0152(3) Uani 1 1 d . . .
H4A H 0.621 0.6304 0.7224 0.018 Uiso 1 1 calc R . .
H4B H 0.5781 0.6359 0.8567 0.018 Uiso 1 1 calc R . .
C5 C 0.3845(2) 0.73347(16) 0.76974(15) 0.0148(3) Uani 1 1 d . . .
H5A H 0.4135 0.8062 0.7946 0.018 Uiso 1 1 calc R . .
H5B H 0.2823 0.7171 0.8194 0.018 Uiso 1 1 calc R . .
O1 O 0.3640(2) 0.86466(14) 0.04147(14) 0.0250(3) Uani 1 1 d D . .
H1BO H 0.333(3) 0.9375(19) 0.056(2) 0.031(7) Uiso 1 1 d D . .
H1AO H 0.449(3) 0.859(2) 0.000(2) 0.038(8) Uiso 1 1 d D . .
C10 C 0.0642(2) 0.7017(2) 0.03072(17) 0.0233(4) Uani 1 1 d . . .
H10A H 0.0285 0.634 0.0028 0.028 Uiso 1 1 calc R . .
H10B H 0.0776 0.7629 -0.0317 0.028 Uiso 1 1 calc R . .
H10C H -0.0218 0.7365 0.0904 0.028 Uiso 1 1 calc R . .
O10 O 0.21993(17) 0.66095(13) 0.07474(13) 0.0232(3) Uani 1 1 d . . .
H10 H 0.2689 0.719 0.0749 0.035 Uiso 1 1 calc R . .
C20 C 0.7196(3) 0.9580(2) 0.5642(2) 0.0316(5) Uani 1 1 d . . .
H20A H 0.606 1.0028 0.5891 0.038 Uiso 1 1 calc R . .
H20B H 0.7355 0.9579 0.4815 0.038 Uiso 1 1 calc R . .
H20C H 0.8048 0.9964 0.5885 0.038 Uiso 1 1 calc R . .
O20 O 0.7372(2) 0.83903(13) 0.61235(14) 0.0290(3) Uani 1 1 d . . .
H20 H 0.7215 0.8392 0.6833 0.044 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Au1 C42 2.0216(17) 2_666 ?
Au1 C22 2.0239(17) . ?
Au1 Au1 3.1402(4) 2_666 ?
C0 C1 1.528(3) . ?
C0 C5 1.536(3) . ?
C0 H0A 0.99 . ?
C0 H0B 0.99 . ?
C1 N21 1.470(2) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
N21 C22 1.355(2) . ?
N21 C25 1.385(2) . ?
C22 N23 1.351(2) . ?
N23 C24 1.383(2) . ?
N23 C2 1.476(2) . ?
C24 C25 1.351(3) . ?
C24 H24 0.95 . ?
C25 H25 0.95 . ?
C2 C32 1.506(2) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C31 C36 1.390(2) . ?
C31 C32 1.412(2) . ?
C31 C3 1.512(2) . ?
C32 C33 1.398(2) . ?
C33 C34 1.387(3) . ?
C33 H33 0.95 . ?
C34 C35 1.386(3) . ?
C34 H34 0.95 . ?
C35 C36 1.396(3) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C3 N41 1.474(2) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
N41 C42 1.354(2) . ?
N41 C45 1.386(2) . ?
C42 N43 1.352(2) . ?
C42 Au1 2.0216(17) 2_666 ?
N43 C44 1.385(2) . ?
N43 C4 1.465(2) . ?
C44 C45 1.348(2) . ?
C44 H44 0.95 . ?
C45 H45 0.95 . ?
C4 C5 1.527(2) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
O1 H1BO 0.84(2) . ?
O1 H1AO 0.79(2) . ?
C10 O10 1.410(2) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
O10 H10 0.84 . ?
C20 O20 1.407(3) . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?
O20 H20 0.84 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C42 Au1 C22 176.07(7) 2_666 . ?
C42 Au1 Au1 93.36(5) 2_666 2_666 ?
C22 Au1 Au1 90.56(5) . 2_666 ?
C1 C0 C5 114.77(15) . . ?
C1 C0 H0A 108.6 . . ?
C5 C0 H0A 108.6 . . ?
C1 C0 H0B 108.6 . . ?
C5 C0 H0B 108.6 . . ?
H0A C0 H0B 107.6 . . ?
N21 C1 C0 112.34(14) . . ?
N21 C1 H1A 109.1 . . ?
C0 C1 H1A 109.1 . . ?
N21 C1 H1B 109.1 . . ?
C0 C1 H1B 109.1 . . ?
H1A C1 H1B 107.9 . . ?
C22 N21 C25 110.60(14) . . ?
C22 N21 C1 124.10(14) . . ?
C25 N21 C1 125.28(15) . . ?
N23 C22 N21 104.94(14) . . ?
N23 C22 Au1 126.80(12) . . ?
N21 C22 Au1 127.97(12) . . ?
C22 N23 C24 111.07(14) . . ?
C22 N23 C2 122.62(14) . . ?
C24 N23 C2 126.19(14) . . ?
C25 C24 N23 106.47(15) . . ?
C25 C24 H24 126.8 . . ?
N23 C24 H24 126.8 . . ?
C24 C25 N21 106.87(15) . . ?
C24 C25 H25 126.6 . . ?
N21 C25 H25 126.6 . . ?
N23 C2 C32 113.58(14) . . ?
N23 C2 H2A 108.8 . . ?
C32 C2 H2A 108.8 . . ?
N23 C2 H2B 108.8 . . ?
C32 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C36 C31 C32 119.14(16) . . ?
C36 C31 C3 118.17(16) . . ?
C32 C31 C3 122.68(15) . . ?
C33 C32 C31 118.70(16) . . ?
C33 C32 C2 118.27(16) . . ?
C31 C32 C2 122.96(15) . . ?
C34 C33 C32 121.56(17) . . ?
C34 C33 H33 119.2 . . ?
C32 C33 H33 119.2 . . ?
C35 C34 C33 119.72(17) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C34 C35 C36 119.46(17) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C31 C36 C35 121.42(17) . . ?
C31 C36 H36 119.3 . . ?
C35 C36 H36 119.3 . . ?
N41 C3 C31 112.39(13) . . ?
N41 C3 H3A 109.1 . . ?
C31 C3 H3A 109.1 . . ?
N41 C3 H3B 109.1 . . ?
C31 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
C42 N41 C45 110.86(14) . . ?
C42 N41 C3 124.47(14) . . ?
C45 N41 C3 124.54(14) . . ?
N43 C42 N41 104.96(14) . . ?
N43 C42 Au1 127.89(12) . 2_666 ?
N41 C42 Au1 127.13(12) . 2_666 ?
C42 N43 C44 110.66(14) . . ?
C42 N43 C4 126.24(14) . . ?
C44 N43 C4 123.08(15) . . ?
C45 C44 N43 107.01(15) . . ?
C45 C44 H44 126.5 . . ?
N43 C44 H44 126.5 . . ?
C44 C45 N41 106.50(15) . . ?
C44 C45 H45 126.8 . . ?
N41 C45 H45 126.8 . . ?
N43 C4 C5 112.78(15) . . ?
N43 C4 H4A 109 . . ?
C5 C4 H4A 109 . . ?
N43 C4 H4B 109 . . ?
C5 C4 H4B 109 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 C0 115.04(15) . . ?
C4 C5 H5A 108.5 . . ?
C0 C5 H5A 108.5 . . ?
C4 C5 H5B 108.5 . . ?
C0 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
H1BO O1 H1AO 107(2) . . ?
O10 C10 H10A 109.5 . . ?
O10 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O10 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C10 O10 H10 109.5 . . ?
O20 C20 H20A 109.5 . . ?
O20 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O20 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C20 O20 H20 109.5 . . ?


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
O1 H1BO Cl1 0.84(2) 2.41(2) 3.2474(16) 170(2) 2_676
O1 H1AO Cl1 0.79(2) 2.49(2) 3.2721(16) 173(3) 1_554
O10 H10 O1 0.84 1.95 2.779(2) 166.8 .
O20 H20 Cl1 0.84 2.39 3.2168(18) 168.0 .


#===END
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lw2329

_database_code_depnum_ccdc_archive 'CCDC 834023'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_date             2010-06-06T22:21:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C52 H58 Au2 Br2 N8 O5'
_chemical_formula_moiety         'C50 H44 Au2 N8,2(C H4 O),2(Br),3(H2 O)'
_chemical_formula_weight         1428.82

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  -p_1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.9166(3)
_cell_length_b                   14.7735(3)
_cell_length_c                   15.8256(3)
_cell_angle_alpha                114.049(2)
_cell_angle_beta                 95.802(2)
_cell_angle_gamma                109.275(2)
_cell_volume                     2504.04(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    29647
_cell_measurement_theta_min      3.5665
_cell_measurement_theta_max      39.5538

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.34
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1388
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -3 2 0.1074
0 3 -2 0.2302
-3 0 -2 0.171
-1 0 0 0.2071
0 0 -1 0.1948
0 0 1 0.2322
1 0 0 0.1554
-13 3 16 0.3354
-7 18 2 0.3318
7 -19 -1 0.2078
1 2 -3 0.3018
-18 6 -1 0.1918

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    7.504
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro, Oxford Diffraction Ltd.,
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

;
_exptl_absorpt_correction_T_min  0.064
_exptl_absorpt_correction_T_max  0.203

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 10.4738
_diffrn_orient_matrix_ub_11      0.0379764867
_diffrn_orient_matrix_ub_12      0.0128296966
_diffrn_orient_matrix_ub_13      0.042846523
_diffrn_orient_matrix_ub_21      -0.0470023212
_diffrn_orient_matrix_ub_22      -0.0162014786
_diffrn_orient_matrix_ub_23      0.0181795934
_diffrn_orient_matrix_ub_31      -0.0033823553
_diffrn_orient_matrix_ub_32      -0.0537957231
_diffrn_orient_matrix_ub_33      -0.0209647788
_diffrn_measurement_device_type  'Oxford Diffraction Gemini, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_number            67453
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.57
_diffrn_reflns_theta_max         39.64
_diffrn_reflns_theta_full        39
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.963
_reflns_number_total             29220
_reflns_number_gt                19768
_reflns_threshold_expression     I>2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_cell_refinement       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction        
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'



#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

One methanol solvent molecule was found to be disordered over two sets of
 sites with occupancies set to 0.5 after trial refinement. 
 Water molecule hydrogen atoms were not located. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0199P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         29220
_refine_ls_number_parameters     646
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0536
_refine_ls_wR_factor_gt          0.0519
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_restrained_S_all      0.906
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0
_refine_diff_density_max         3.9
_refine_diff_density_min         -2.283
_refine_diff_density_rms         0.169

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.481271(6) 0.838939(5) 0.704031(5) 0.010360(10) Uani 1 1 d . . .
Au2 Au 0.487659(6) 0.624330(5) 0.631382(5) 0.009000(10) Uani 1 1 d . . .
Br1 Br 0.922561(18) 0.701925(19) 0.791678(16) 0.02389(5) Uani 1 1 d . . .
Br2 Br 0.964412(17) 0.288033(16) 0.647073(15) 0.01916(4) Uani 1 1 d . . .
C10 C 0.30094(15) 0.64571(14) 0.39126(13) 0.0127(4) Uani 1 1 d . . .
H10A H 0.3295 0.6592 0.3399 0.015 Uiso 1 1 calc R . .
H10B H 0.2168 0.6085 0.3673 0.015 Uiso 1 1 calc R . .
C11 C 0.33181(15) 0.75536(15) 0.47835(13) 0.0141(4) Uani 1 1 d . . .
H11A H 0.2853 0.7909 0.4629 0.017 Uiso 1 1 calc R . .
H11B H 0.3117 0.7431 0.5327 0.017 Uiso 1 1 calc R . .
N121 N 0.45293(13) 0.82903(12) 0.50896(11) 0.0114(3) Uani 1 1 d . . .
C122 C 0.52748(15) 0.86215(14) 0.59329(13) 0.0111(3) Uani 1 1 d . . .
N123 N 0.63209(13) 0.92043(12) 0.59099(11) 0.0106(3) Uani 1 1 d . . .
C124 C 0.62443(15) 0.93113(14) 0.50749(13) 0.0111(3) Uani 1 1 d . . .
C125 C 0.70436(16) 0.98765(15) 0.47434(14) 0.0154(4) Uani 1 1 d . . .
H125 H 0.7823 1.0282 0.5099 0.018 Uiso 1 1 calc R . .
C126 C 0.66430(17) 0.98167(17) 0.38665(15) 0.0190(4) Uani 1 1 d . . .
H126 H 0.7163 1.0193 0.3617 0.023 Uiso 1 1 calc R . .
C127 C 0.55009(17) 0.92206(16) 0.33417(14) 0.0182(4) Uani 1 1 d . . .
H127 H 0.5268 0.9197 0.2741 0.022 Uiso 1 1 calc R . .
C128 C 0.46920(16) 0.86600(15) 0.36662(14) 0.0155(4) Uani 1 1 d . . .
H128 H 0.3912 0.8259 0.3309 0.019 Uiso 1 1 calc R . .
C129 C 0.50936(15) 0.87212(14) 0.45489(13) 0.0119(3) Uani 1 1 d . . .
C12 C 0.73721(15) 0.96791(15) 0.66905(13) 0.0142(4) Uani 1 1 d . . .
H12A H 0.718 0.9431 0.7171 0.017 Uiso 1 1 calc R . .
H12B H 0.7635 1.0479 0.7014 0.017 Uiso 1 1 calc R . .
C131 C 0.83893(15) 0.83896(15) 0.61357(12) 0.0117(3) Uani 1 1 d . . .
C132 C 0.83527(15) 0.94074(15) 0.63855(12) 0.0115(3) Uani 1 1 d . . .
C133 C 0.92908(16) 1.02297(16) 0.64118(14) 0.0159(4) Uani 1 1 d . . .
H133 H 0.928 1.0923 0.6594 0.019 Uiso 1 1 calc R . .
C134 C 1.02474(16) 1.00679(17) 0.61788(14) 0.0188(4) Uani 1 1 d . . .
H134 H 1.087 1.0637 0.6182 0.023 Uiso 1 1 calc R . .
C135 C 1.02836(16) 0.90757(17) 0.59437(14) 0.0180(4) Uani 1 1 d . . .
H135 H 1.0932 0.8955 0.5784 0.022 Uiso 1 1 calc R . .
C136 C 0.93722(16) 0.82586(16) 0.59412(13) 0.0150(4) Uani 1 1 d . . .
H136 H 0.9416 0.7585 0.5802 0.018 Uiso 1 1 calc R . .
C13 C 0.74296(16) 0.74197(15) 0.60584(13) 0.0138(4) Uani 1 1 d . . .
H13A H 0.7726 0.6879 0.6051 0.017 Uiso 1 1 calc R . .
H13B H 0.7146 0.7649 0.6635 0.017 Uiso 1 1 calc R . .
N141 N 0.64678(12) 0.68976(12) 0.51905(10) 0.0098(3) Uani 1 1 d . . .
C142 C 0.53754(15) 0.64195(14) 0.51961(12) 0.0094(3) Uani 1 1 d . . .
N143 N 0.47063(12) 0.61063(12) 0.43240(11) 0.0105(3) Uani 1 1 d . . .
C144 C 0.53755(15) 0.63616(14) 0.37489(13) 0.0112(3) Uani 1 1 d . . .
C145 C 0.50695(17) 0.61899(15) 0.28057(13) 0.0143(4) Uani 1 1 d . . .
H145 H 0.4296 0.5842 0.2435 0.017 Uiso 1 1 calc R . .
C146 C 0.59540(17) 0.65545(16) 0.24450(14) 0.0174(4) Uani 1 1 d . . .
H146 H 0.5786 0.647 0.1812 0.021 Uiso 1 1 calc R . .
C147 C 0.70980(17) 0.70477(16) 0.29870(14) 0.0170(4) Uani 1 1 d . . .
H147 H 0.7682 0.728 0.2708 0.02 Uiso 1 1 calc R . .
C148 C 0.73959(16) 0.72047(15) 0.39149(13) 0.0142(4) Uani 1 1 d . . .
H148 H 0.8171 0.753 0.4277 0.017 Uiso 1 1 calc R . .
C149 C 0.65056(15) 0.68625(14) 0.42955(12) 0.0103(3) Uani 1 1 d . . .
C14 C 0.34568(15) 0.56804(15) 0.40648(13) 0.0135(4) Uani 1 1 d . . .
H14A H 0.3184 0.5543 0.4581 0.016 Uiso 1 1 calc R . .
H14B H 0.3141 0.4978 0.3467 0.016 Uiso 1 1 calc R . .
C20 C 0.16060(15) 0.60052(15) 0.70593(13) 0.0137(4) Uani 1 1 d . . .
H20A H 0.141 0.5964 0.7635 0.016 Uiso 1 1 calc R . .
H20B H 0.088 0.5675 0.6557 0.016 Uiso 1 1 calc R . .
C21 C 0.22704(15) 0.53025(15) 0.67003(13) 0.0131(4) Uani 1 1 d . . .
H21A H 0.1758 0.4533 0.6472 0.016 Uiso 1 1 calc R . .
H21B H 0.251 0.5367 0.6145 0.016 Uiso 1 1 calc R . .
C22 C 0.63010(15) 0.68421(16) 0.85599(14) 0.0150(4) Uani 1 1 d . . .
H22A H 0.6542 0.7143 0.8121 0.018 Uiso 1 1 calc R . .
H22B H 0.6593 0.6276 0.8464 0.018 Uiso 1 1 calc R . .
N221 N 0.32827(13) 0.56006(12) 0.74365(11) 0.0114(3) Uani 1 1 d . . .
C222 C 0.43732(15) 0.60513(14) 0.74245(12) 0.0108(3) Uani 1 1 d . . .
N223 N 0.50478(13) 0.63274(12) 0.82869(11) 0.0114(3) Uani 1 1 d . . .
C224 C 0.43758(15) 0.59911(15) 0.88306(13) 0.0120(3) Uani 1 1 d . . .
C225 C 0.46400(17) 0.60089(16) 0.97160(13) 0.0168(4) Uani 1 1 d . . .
H225 H 0.5405 0.633 1.0098 0.02 Uiso 1 1 calc R . .
C226 C 0.37344(18) 0.55373(18) 1.00074(14) 0.0204(4) Uani 1 1 d . . .
H226 H 0.3882 0.5532 1.0605 0.024 Uiso 1 1 calc R . .
C227 C 0.26006(18) 0.50647(18) 0.94508(15) 0.0212(4) Uani 1 1 d . . .
H227 H 0.2004 0.4747 0.968 0.025 Uiso 1 1 calc R . .
C228 C 0.23344(16) 0.50511(16) 0.85796(14) 0.0159(4) Uani 1 1 d . . .
H228 H 0.1569 0.4732 0.82 0.019 Uiso 1 1 calc R . .
C229 C 0.32415(15) 0.55266(15) 0.82873(12) 0.0115(3) Uani 1 1 d . . .
C231 C 0.67877(16) 0.87529(16) 0.99213(13) 0.0154(4) Uani 1 1 d . . .
C232 C 0.68454(15) 0.77390(16) 0.95827(13) 0.0145(4) Uani 1 1 d . . .
C233 C 0.75001(17) 0.75647(18) 1.02064(15) 0.0221(4) Uani 1 1 d . . .
H233 H 0.756 0.6886 0.9981 0.027 Uiso 1 1 calc R . .
C234 C 0.80674(19) 0.8359(2) 1.11488(16) 0.0299(5) Uani 1 1 d . . .
H234 H 0.8491 0.8216 1.1569 0.036 Uiso 1 1 calc R . .
C235 C 0.80143(19) 0.9353(2) 1.14719(16) 0.0309(6) Uani 1 1 d . . .
H235 H 0.8411 0.9905 1.2113 0.037 Uiso 1 1 calc R . .
C236 C 0.73834(18) 0.95450(19) 1.08614(15) 0.0239(5) Uani 1 1 d . . .
H236 H 0.7355 1.0236 1.1089 0.029 Uiso 1 1 calc R . .
C23 C 0.61868(16) 0.90732(16) 0.92902(14) 0.0150(4) Uani 1 1 d . . .
H23A H 0.646 0.9874 0.962 0.018 Uiso 1 1 calc R . .
H23B H 0.6418 0.8866 0.8685 0.018 Uiso 1 1 calc R . .
N241 N 0.49292(13) 0.85960(12) 0.90417(11) 0.0121(3) Uani 1 1 d . . .
C242 C 0.42654(16) 0.82361(15) 0.81544(13) 0.0122(4) Uani 1 1 d . . .
N243 N 0.31737(13) 0.78406(13) 0.81690(11) 0.0124(3) Uani 1 1 d . . .
C244 C 0.31230(16) 0.79821(15) 0.90867(13) 0.0134(4) Uani 1 1 d . . .
C245 C 0.21880(17) 0.77635(17) 0.94562(14) 0.0191(4) Uani 1 1 d . . .
H245 H 0.1427 0.744 0.9066 0.023 Uiso 1 1 calc R . .
C246 C 0.24312(19) 0.80445(19) 1.04218(15) 0.0249(5) Uani 1 1 d . . .
H246 H 0.1822 0.7916 1.0708 0.03 Uiso 1 1 calc R . .
C247 C 0.35554(19) 0.85151(19) 1.09883(15) 0.0249(5) Uani 1 1 d . . .
H247 H 0.3685 0.8686 1.1648 0.03 Uiso 1 1 calc R . .
C248 C 0.44808(17) 0.87394(17) 1.06275(13) 0.0180(4) Uani 1 1 d . . .
H248 H 0.524 0.9062 1.102 0.022 Uiso 1 1 calc R . .
C249 C 0.42411(16) 0.84645(15) 0.96458(13) 0.0139(4) Uani 1 1 d . . .
C24 C 0.21809(16) 0.72089(15) 0.73197(13) 0.0139(4) Uani 1 1 d . . .
H24A H 0.2427 0.7265 0.6764 0.017 Uiso 1 1 calc R . .
H24B H 0.1615 0.7531 0.7441 0.017 Uiso 1 1 calc R . .
O1 O 0.89274(12) 0.55791(12) 0.56107(10) 0.0211(3) Uani 1 1 d . . .
O2 O 0.08990(13) 0.64019(12) 0.51409(10) 0.0215(3) Uani 1 1 d . . .
O3 O 0.77562(14) 0.51860(14) 0.85270(11) 0.0315(4) Uani 1 1 d . . .
O40 O 0.81744(12) 0.88792(12) 0.83084(11) 0.0224(3) Uani 1 1 d . . .
H40 H 0.8476 0.8432 0.8172 0.034 Uiso 1 1 calc R . .
C40 C 0.9018(2) 0.9936(2) 0.8924(2) 0.0398(7) Uani 1 1 d . . .
H40A H 0.8984 1.0141 0.9589 0.06 Uiso 1 1 calc R . .
H40B H 0.8883 1.0451 0.8735 0.06 Uiso 1 1 calc R . .
H40C H 0.9773 0.995 0.8874 0.06 Uiso 1 1 calc R . .
O50 O 0.8312(3) 0.3384(3) 0.8117(2) 0.0334(8) Uani 0.5 1 d P A 1
H50 H 0.803 0.3833 0.8158 0.05 Uiso 0.5 1 calc PR A 1
C50 C 0.9270(5) 0.3873(4) 0.8913(4) 0.0358(12) Uani 0.5 1 d P A 1
H50A H 0.97 0.4629 0.9063 0.054 Uiso 0.5 1 calc PR A 1
H50B H 0.9759 0.3476 0.8758 0.054 Uiso 0.5 1 calc PR A 1
H50C H 0.9016 0.3852 0.947 0.054 Uiso 0.5 1 calc PR A 1
O60 O 0.8907(4) 0.2353(4) 0.8120(3) 0.0667(15) Uani 0.5 1 d P B 2
H60 H 0.8983 0.2424 0.7627 0.1 Uiso 0.5 1 calc PRD B 2
C60 C 0.9976(6) 0.2892(7) 0.8804(5) 0.077(3) Uani 0.5 1 d P B 2
H60A H 1.0009 0.3558 0.9331 0.116 Uiso 0.5 1 calc PR B 2
H60B H 1.058 0.3078 0.8499 0.116 Uiso 0.5 1 calc PR B 2
H60C H 1.0083 0.2417 0.9059 0.116 Uiso 0.5 1 calc PR B 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
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
Au1 C122 2.0276(19) . ?
Au1 C242 2.033(2) . ?
Au1 Au2 2.93289(12) . ?
Au2 C142 2.0266(18) . ?
Au2 C222 2.0269(19) . ?
C10 C11 1.525(3) . ?
C10 C14 1.531(3) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
C11 N121 1.470(2) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
N121 C122 1.358(2) . ?
N121 C129 1.390(2) . ?
C122 N123 1.355(2) . ?
N123 C124 1.391(2) . ?
N123 C12 1.479(2) . ?
C124 C125 1.391(3) . ?
C124 C129 1.402(2) . ?
C125 C126 1.388(3) . ?
C125 H125 0.95 . ?
C126 C127 1.393(3) . ?
C126 H126 0.95 . ?
C127 C128 1.388(3) . ?
C127 H127 0.95 . ?
C128 C129 1.396(3) . ?
C128 H128 0.95 . ?
C12 C132 1.516(3) . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
C131 C136 1.392(3) . ?
C131 C132 1.409(3) . ?
C131 C13 1.503(3) . ?
C132 C133 1.387(3) . ?
C133 C134 1.391(3) . ?
C133 H133 0.95 . ?
C134 C135 1.376(3) . ?
C134 H134 0.95 . ?
C135 C136 1.378(3) . ?
C135 H135 0.95 . ?
C136 H136 0.95 . ?
C13 N141 1.478(2) . ?
C13 H13A 0.99 . ?
C13 H13B 0.99 . ?
N141 C142 1.356(2) . ?
N141 C149 1.403(2) . ?
C142 N143 1.357(2) . ?
N143 C144 1.393(2) . ?
N143 C14 1.468(2) . ?
C144 C149 1.392(2) . ?
C144 C145 1.398(3) . ?
C145 C146 1.377(3) . ?
C145 H145 0.95 . ?
C146 C147 1.405(3) . ?
C146 H146 0.95 . ?
C147 C148 1.381(3) . ?
C147 H147 0.95 . ?
C148 C149 1.395(3) . ?
C148 H148 0.95 . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C20 C21 1.531(3) . ?
C20 C24 1.534(3) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 N221 1.468(2) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C22 N223 1.471(2) . ?
C22 C232 1.509(3) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
N221 C222 1.351(2) . ?
N221 C229 1.399(2) . ?
C222 N223 1.364(2) . ?
N223 C224 1.398(2) . ?
C224 C225 1.396(3) . ?
C224 C229 1.399(2) . ?
C225 C226 1.378(3) . ?
C225 H225 0.95 . ?
C226 C227 1.404(3) . ?
C226 H226 0.95 . ?
C227 C228 1.377(3) . ?
C227 H227 0.95 . ?
C228 C229 1.382(3) . ?
C228 H228 0.95 . ?
C231 C236 1.389(3) . ?
C231 C232 1.401(3) . ?
C231 C23 1.515(3) . ?
C232 C233 1.392(3) . ?
C233 C234 1.387(3) . ?
C233 H233 0.95 . ?
C234 C235 1.372(4) . ?
C234 H234 0.95 . ?
C235 C236 1.377(3) . ?
C235 H235 0.95 . ?
C236 H236 0.95 . ?
C23 N241 1.476(2) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
N241 C242 1.355(2) . ?
N241 C249 1.397(3) . ?
C242 N243 1.343(2) . ?
N243 C244 1.392(2) . ?
N243 C24 1.470(2) . ?
C244 C249 1.387(3) . ?
C244 C245 1.394(3) . ?
C245 C246 1.381(3) . ?
C245 H245 0.95 . ?
C246 C247 1.399(3) . ?
C246 H246 0.95 . ?
C247 C248 1.377(3) . ?
C247 H247 0.95 . ?
C248 C249 1.407(3) . ?
C248 H248 0.95 . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
O40 C40 1.413(3) . ?
O40 H40 0.84 . ?
C40 H40A 0.98 . ?
C40 H40B 0.98 . ?
C40 H40C 0.98 . ?
O50 C50 1.411(6) . ?
O50 H50 0.84 . ?
C50 H50A 0.98 . ?
C50 H50B 0.98 . ?
C50 H50C 0.98 . ?
O60 C60 1.407(8) . ?
O60 H60 0.84 . ?
C60 H60A 0.98 . ?
C60 H60B 0.98 . ?
C60 H60C 0.98 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C122 Au1 C242 174.84(8) . . ?
C122 Au1 Au2 94.12(5) . . ?
C242 Au1 Au2 90.25(5) . . ?
C142 Au2 C222 179.44(7) . . ?
C142 Au2 Au1 88.60(5) . . ?
C222 Au2 Au1 91.93(5) . . ?
C11 C10 C14 116.98(15) . . ?
C11 C10 H10A 108.1 . . ?
C14 C10 H10A 108.1 . . ?
C11 C10 H10B 108.1 . . ?
C14 C10 H10B 108.1 . . ?
H10A C10 H10B 107.3 . . ?
N121 C11 C10 113.86(15) . . ?
N121 C11 H11A 108.8 . . ?
C10 C11 H11A 108.8 . . ?
N121 C11 H11B 108.8 . . ?
C10 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C122 N121 C129 109.80(15) . . ?
C122 N121 C11 124.84(16) . . ?
C129 N121 C11 125.33(15) . . ?
N123 C122 N121 107.13(16) . . ?
N123 C122 Au1 128.35(13) . . ?
N121 C122 Au1 124.22(13) . . ?
C122 N123 C124 110.31(14) . . ?
C122 N123 C12 123.57(16) . . ?
C124 N123 C12 126.09(16) . . ?
C125 C124 N123 132.70(16) . . ?
C125 C124 C129 121.33(17) . . ?
N123 C124 C129 105.94(16) . . ?
C126 C125 C124 116.56(17) . . ?
C126 C125 H125 121.7 . . ?
C124 C125 H125 121.7 . . ?
C125 C126 C127 121.9(2) . . ?
C125 C126 H126 119 . . ?
C127 C126 H126 119 . . ?
C128 C127 C126 122.21(19) . . ?
C128 C127 H127 118.9 . . ?
C126 C127 H127 118.9 . . ?
C127 C128 C129 115.92(17) . . ?
C127 C128 H128 122 . . ?
C129 C128 H128 122 . . ?
N121 C129 C128 131.25(17) . . ?
N121 C129 C124 106.68(16) . . ?
C128 C129 C124 122.06(18) . . ?
N123 C12 C132 115.81(15) . . ?
N123 C12 H12A 108.3 . . ?
C132 C12 H12A 108.3 . . ?
N123 C12 H12B 108.3 . . ?
C132 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
C136 C131 C132 118.58(17) . . ?
C136 C131 C13 117.01(17) . . ?
C132 C131 C13 124.41(17) . . ?
C133 C132 C131 118.56(17) . . ?
C133 C132 C12 117.76(17) . . ?
C131 C132 C12 123.56(17) . . ?
C132 C133 C134 121.86(19) . . ?
C132 C133 H133 119.1 . . ?
C134 C133 H133 119.1 . . ?
C135 C134 C133 119.37(19) . . ?
C135 C134 H134 120.3 . . ?
C133 C134 H134 120.3 . . ?
C134 C135 C136 119.55(19) . . ?
C134 C135 H135 120.2 . . ?
C136 C135 H135 120.2 . . ?
C135 C136 C131 122.01(19) . . ?
C135 C136 H136 119 . . ?
C131 C136 H136 119 . . ?
N141 C13 C131 113.40(16) . . ?
N141 C13 H13A 108.9 . . ?
C131 C13 H13A 108.9 . . ?
N141 C13 H13B 108.9 . . ?
C131 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
C142 N141 C149 110.53(14) . . ?
C142 N141 C13 121.57(15) . . ?
C149 N141 C13 127.81(15) . . ?
N141 C142 N143 106.59(15) . . ?
N141 C142 Au2 125.60(12) . . ?
N143 C142 Au2 127.80(13) . . ?
C142 N143 C144 110.30(15) . . ?
C142 N143 C14 124.71(16) . . ?
C144 N143 C14 124.61(15) . . ?
C149 C144 N143 106.81(16) . . ?
C149 C144 C145 122.41(18) . . ?
N143 C144 C145 130.78(17) . . ?
C146 C145 C144 116.12(17) . . ?
C146 C145 H145 121.9 . . ?
C144 C145 H145 121.9 . . ?
C145 C146 C147 121.85(18) . . ?
C145 C146 H146 119.1 . . ?
C147 C146 H146 119.1 . . ?
C148 C147 C146 121.77(19) . . ?
C148 C147 H147 119.1 . . ?
C146 C147 H147 119.1 . . ?
C147 C148 C149 116.85(17) . . ?
C147 C148 H148 121.6 . . ?
C149 C148 H148 121.6 . . ?
C144 C149 C148 120.98(17) . . ?
C144 C149 N141 105.73(15) . . ?
C148 C149 N141 133.29(16) . . ?
N143 C14 C10 112.71(15) . . ?
N143 C14 H14A 109 . . ?
C10 C14 H14A 109 . . ?
N143 C14 H14B 109 . . ?
C10 C14 H14B 109 . . ?
H14A C14 H14B 107.8 . . ?
C21 C20 C24 117.92(16) . . ?
C21 C20 H20A 107.8 . . ?
C24 C20 H20A 107.8 . . ?
C21 C20 H20B 107.8 . . ?
C24 C20 H20B 107.8 . . ?
H20A C20 H20B 107.2 . . ?
N221 C21 C20 113.48(15) . . ?
N221 C21 H21A 108.9 . . ?
C20 C21 H21A 108.9 . . ?
N221 C21 H21B 108.9 . . ?
C20 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
N223 C22 C232 114.77(16) . . ?
N223 C22 H22A 108.6 . . ?
C232 C22 H22A 108.6 . . ?
N223 C22 H22B 108.6 . . ?
C232 C22 H22B 108.6 . . ?
H22A C22 H22B 107.5 . . ?
C222 N221 C229 110.72(15) . . ?
C222 N221 C21 125.26(16) . . ?
C229 N221 C21 123.86(15) . . ?
N221 C222 N223 106.79(16) . . ?
N221 C222 Au2 125.61(13) . . ?
N223 C222 Au2 127.60(13) . . ?
C222 N223 C224 110.01(15) . . ?
C222 N223 C22 123.85(16) . . ?
C224 N223 C22 126.03(16) . . ?
C225 C224 N223 132.87(17) . . ?
C225 C224 C229 120.62(18) . . ?
N223 C224 C229 106.46(16) . . ?
C226 C225 C224 116.56(18) . . ?
C226 C225 H225 121.7 . . ?
C224 C225 H225 121.7 . . ?
C225 C226 C227 122.24(19) . . ?
C225 C226 H226 118.9 . . ?
C227 C226 H226 118.9 . . ?
C228 C227 C226 121.5(2) . . ?
C228 C227 H227 119.3 . . ?
C226 C227 H227 119.3 . . ?
C227 C228 C229 116.40(18) . . ?
C227 C228 H228 121.8 . . ?
C229 C228 H228 121.8 . . ?
C228 C229 C224 122.73(17) . . ?
C228 C229 N221 131.24(16) . . ?
C224 C229 N221 105.91(16) . . ?
C236 C231 C232 119.11(19) . . ?
C236 C231 C23 117.32(19) . . ?
C232 C231 C23 123.37(16) . . ?
C233 C232 C231 118.43(17) . . ?
C233 C232 C22 117.49(19) . . ?
C231 C232 C22 123.96(17) . . ?
C234 C233 C232 121.5(2) . . ?
C234 C233 H233 119.3 . . ?
C232 C233 H233 119.3 . . ?
C235 C234 C233 119.7(2) . . ?
C235 C234 H234 120.2 . . ?
C233 C234 H234 120.2 . . ?
C234 C235 C236 119.6(2) . . ?
C234 C235 H235 120.2 . . ?
C236 C235 H235 120.2 . . ?
C235 C236 C231 121.6(2) . . ?
C235 C236 H236 119.2 . . ?
C231 C236 H236 119.2 . . ?
N241 C23 C231 116.20(17) . . ?
N241 C23 H23A 108.2 . . ?
C231 C23 H23A 108.2 . . ?
N241 C23 H23B 108.2 . . ?
C231 C23 H23B 108.2 . . ?
H23A C23 H23B 107.4 . . ?
C242 N241 C249 109.61(16) . . ?
C242 N241 C23 122.73(16) . . ?
C249 N241 C23 127.63(15) . . ?
N243 C242 N241 107.48(17) . . ?
N243 C242 Au1 125.96(13) . . ?
N241 C242 Au1 126.35(14) . . ?
C242 N243 C244 110.00(15) . . ?
C242 N243 C24 125.29(16) . . ?
C244 N243 C24 124.15(16) . . ?
C249 C244 N243 106.60(17) . . ?
C249 C244 C245 122.87(18) . . ?
N243 C244 C245 130.46(17) . . ?
C246 C245 C244 116.18(19) . . ?
C246 C245 H245 121.9 . . ?
C244 C245 H245 121.9 . . ?
C245 C246 C247 121.4(2) . . ?
C245 C246 H246 119.3 . . ?
C247 C246 H246 119.3 . . ?
C248 C247 C246 122.57(19) . . ?
C248 C247 H247 118.7 . . ?
C246 C247 H247 118.7 . . ?
C247 C248 C249 116.42(18) . . ?
C247 C248 H248 121.8 . . ?
C249 C248 H248 121.8 . . ?
C244 C249 N241 106.25(16) . . ?
C244 C249 C248 120.56(18) . . ?
N241 C249 C248 133.17(17) . . ?
N243 C24 C20 113.49(16) . . ?
N243 C24 H24A 108.9 . . ?
C20 C24 H24A 108.9 . . ?
N243 C24 H24B 108.9 . . ?
C20 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C40 O40 H40 109.5 . . ?
O40 C40 H40A 109.5 . . ?
O40 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
O40 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C60 O60 H60 109.5 . . ?
O60 C60 H60A 109.5 . . ?
O60 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
O60 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?

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
O40 H40 Br1 0.84 2.49 3.3202(16) 171.9 .
O50 H50 O3 0.84 2.01 2.824(4) 164.5 .
O60 H60 Br2 0.84 2.34 3.162(5) 166.4 .

#===END
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lw3235


_database_code_depnum_ccdc_archive 'CCDC 834024'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_date             2010-05-05T16:25:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C52 H48 Au2 N8, 2Br,2(C H4 O)'
_chemical_formula_sum            'C54 H56 Au2 Br2 N8 O2'
_chemical_formula_weight         1402.82

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, 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'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   16.5234(2)
_cell_length_b                   17.3329(2)
_cell_length_c                   33.2686(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9528.08(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30839
_cell_measurement_theta_min      2.5003
_cell_measurement_theta_max      36.9721

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5440
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    7.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_T_max  1


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measurement_device_type  
;
 Oxford Diffraction Xcalibur diffractometer

;
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.1204
_diffrn_reflns_number            109454
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_theta_min         2.5
_diffrn_reflns_theta_max         37.08
_diffrn_reflns_theta_full        36.85
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.983
_reflns_number_total             23678
_reflns_number_gt                14720
_reflns_threshold_expression     I>2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'



#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.  

The atoms of one C4 chain were modelled as being disordered over two sets of 
 sites with occupancies refined to 0.708(3) and its complement. The
solvent was modelled as two MeOH molecules, both disordered over two
  sets of sites with occupancies constrained, after trial refinement, to be 
the same as those of the disordered C4 chain. Geometries of disordered 
 atoms were restrained to ideal values. Hydroxyl H atoms were not
included.
The atoms of the minor component of the disordered C4 alkyl chain did 
not support anisotropic refinement even with appropriate restraints and
 were therefore refined with isotropic displacement parameters 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0228P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         23678
_refine_ls_number_parameters     653
_refine_ls_number_restraints     122
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0576
_refine_ls_wR_factor_gt          0.0524
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_restrained_S_all      0.845
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.043(4)
_refine_diff_density_max         2.859
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.172

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.598643(8) 0.034342(8) 0.575982(4) 0.01724(3) Uani 1 1 d . . .
Au2 Au 0.562331(8) 0.175363(8) 0.636918(4) 0.01844(3) Uani 1 1 d . A .
Br1 Br 0.5 0.21340(3) 0.75 0.03108(14) Uani 1 2 d S . .
Br2 Br 0.46429(3) 0.80310(2) 0.612662(12) 0.02973(10) Uani 1 1 d . . .
Br3 Br 0.99553(4) 0 0.5 0.04602(19) Uani 1 2 d S . .
C111 C 0.5266(3) 0.2240(3) 0.49563(15) 0.0159(10) Uani 0.708(3) 1 d PU A 1
H11A H 0.4696 0.241 0.4979 0.019 Uiso 0.708(3) 1 calc PR A 1
H11B H 0.5508 0.2508 0.4722 0.019 Uiso 0.708(3) 1 calc PR A 1
C112 C 0.5728(3) 0.2482(3) 0.53412(14) 0.0149(10) Uani 0.708(3) 1 d PDU A 1
H11C H 0.5868 0.2008 0.5492 0.018 Uiso 0.708(3) 1 calc PR A 1
H11D H 0.6242 0.2728 0.5259 0.018 Uiso 0.708(3) 1 calc PR A 1
C11 C 0.5285(5) 0.1378(5) 0.4882(2) 0.0175(15) Uani 0.708(3) 1 d PU A 1
H11E H 0.5118 0.127 0.4602 0.021 Uiso 0.708(3) 1 calc PR A 1
H11F H 0.5844 0.1184 0.4919 0.021 Uiso 0.708(3) 1 calc PR A 1
C113 C 0.5752(9) 0.1987(9) 0.5149(5) 0.045(4) Uani 0.292(3) 1 d PDU A 2
H11G H 0.6299 0.212 0.505 0.054 Uiso 0.292(3) 1 calc PR A 2
H11H H 0.5814 0.1825 0.5433 0.054 Uiso 0.292(3) 1 calc PR A 2
C114 C 0.5247(9) 0.2732(9) 0.5147(4) 0.034(3) Uiso 0.292(3) 1 d PDU A 2
H11I H 0.4706 0.2619 0.5033 0.04 Uiso 0.292(3) 1 calc PR A 2
H11J H 0.5513 0.3115 0.497 0.04 Uiso 0.292(3) 1 calc PR A 2
C11' C 0.5464(12) 0.1278(11) 0.4911(7) 0.015(4) Uiso 0.292(3) 1 d PDU A 2
H11K H 0.5896 0.0884 0.4893 0.018 Uiso 0.292(3) 1 calc PR A 2
H11L H 0.5292 0.1424 0.4636 0.018 Uiso 0.292(3) 1 calc PR A 2
C14' C 0.5138(12) 0.3089(15) 0.5572(7) 0.0189(13) Uani 0.292(3) 1 d PDU A 2
H14C H 0.5663 0.3085 0.5715 0.023 Uiso 0.292(3) 1 calc PR A 2
H14D H 0.4959 0.3632 0.5546 0.023 Uiso 0.292(3) 1 calc PR A 2
N121 N 0.47393(18) 0.09788(18) 0.51607(9) 0.0177(6) Uani 1 1 d . . .
C122 C 0.4907(2) 0.0647(2) 0.55171(10) 0.0155(7) Uani 1 1 d . A .
N123 N 0.41810(16) 0.04828(17) 0.56933(8) 0.0161(6) Uani 1 1 d . . .
C124 C 0.2702(2) 0.0661(2) 0.54708(11) 0.0197(8) Uani 1 1 d . . .
H124 H 0.2443 0.045 0.5701 0.024 Uiso 1 1 calc R A .
C125 C 0.2265(2) 0.0937(2) 0.51435(12) 0.0248(8) Uani 1 1 d . A .
H125 H 0.1691 0.0913 0.5152 0.03 Uiso 1 1 calc R . .
C126 C 0.2635(2) 0.1246(2) 0.48063(12) 0.0254(9) Uani 1 1 d . . .
H126 H 0.2311 0.1411 0.4587 0.03 Uiso 1 1 calc R A .
C127 C 0.3467(2) 0.1318(2) 0.47832(11) 0.0226(8) Uani 1 1 d . A .
H127 H 0.3724 0.1549 0.4558 0.027 Uiso 1 1 calc R . .
C128 C 0.3906(2) 0.1033(2) 0.51078(10) 0.0182(7) Uani 1 1 d . A .
C129 C 0.3540(2) 0.0712(2) 0.54413(11) 0.0165(7) Uani 1 1 d . A .
C12 C 0.4164(2) 0.0132(2) 0.60997(10) 0.0203(8) Uani 1 1 d . A .
H12A H 0.4571 0.0395 0.627 0.024 Uiso 1 1 calc R . .
H12B H 0.4323 -0.0417 0.6078 0.024 Uiso 1 1 calc R . .
C131 C 0.3080(2) 0.0830(2) 0.65092(10) 0.0186(7) Uani 1 1 d . A .
C132 C 0.3347(2) 0.0181(2) 0.63043(10) 0.0204(8) Uani 1 1 d . . .
C133 C 0.2867(2) -0.0473(2) 0.62835(11) 0.0253(9) Uani 1 1 d . A .
H133 H 0.3069 -0.0925 0.6157 0.03 Uiso 1 1 calc R . .
C134 C 0.2086(3) -0.0473(3) 0.64485(12) 0.0309(10) Uani 1 1 d . . .
H134 H 0.1748 -0.0914 0.6428 0.037 Uiso 1 1 calc R A .
C135 C 0.1823(3) 0.0186(3) 0.66417(12) 0.0322(11) Uani 1 1 d . A .
H135 H 0.1293 0.0198 0.6753 0.039 Uiso 1 1 calc R . .
C136 C 0.2313(2) 0.0827(3) 0.66771(11) 0.0282(9) Uani 1 1 d . . .
H136 H 0.2123 0.1269 0.6817 0.034 Uiso 1 1 calc R A .
C13 C 0.3608(2) 0.1543(2) 0.65792(10) 0.0202(8) Uani 1 1 d . . .
H13A H 0.3319 0.1891 0.6767 0.024 Uiso 1 1 calc R A .
H13B H 0.4112 0.1376 0.6714 0.024 Uiso 1 1 calc R . .
N141 N 0.38275(18) 0.19867(18) 0.62187(9) 0.0179(7) Uani 1 1 d . A .
C142 C 0.4596(2) 0.2166(2) 0.61124(11) 0.0183(7) Uani 1 1 d . . .
N143 N 0.45494(17) 0.26600(17) 0.58004(9) 0.0179(6) Uani 1 1 d D A .
C144 C 0.3395(2) 0.3325(2) 0.54392(11) 0.0220(8) Uani 1 1 d . . .
H144 H 0.3714 0.3625 0.526 0.026 Uiso 1 1 calc R . .
C145 C 0.2556(2) 0.3368(2) 0.54426(11) 0.0265(9) Uani 1 1 d . . .
H145 H 0.229 0.3695 0.5255 0.032 Uiso 1 1 calc R . .
C146 C 0.2096(2) 0.2945(2) 0.57135(12) 0.0258(9) Uani 1 1 d . . .
H146 H 0.1524 0.2997 0.5709 0.031 Uiso 1 1 calc R . .
C147 C 0.2441(2) 0.2451(2) 0.59890(11) 0.0212(8) Uani 1 1 d . A .
H147 H 0.2124 0.2164 0.6175 0.025 Uiso 1 1 calc R . .
C148 C 0.3280(2) 0.2396(2) 0.59796(10) 0.0177(7) Uani 1 1 d . . .
C149 C 0.3741(2) 0.2819(2) 0.57137(11) 0.0183(7) Uani 1 1 d . A .
C14 C 0.5298(4) 0.3023(6) 0.5624(3) 0.0189(13) Uani 0.708(3) 1 d PDU A 1
H14A H 0.5145 0.3498 0.5477 0.023 Uiso 0.708(3) 1 calc PR A 1
H14B H 0.567 0.317 0.5844 0.023 Uiso 0.708(3) 1 calc PR A 1
C211 C 0.7615(2) 0.1883(2) 0.58095(11) 0.0233(8) Uani 1 1 d . . .
H21A H 0.7641 0.2306 0.561 0.028 Uiso 1 1 calc R . .
H21B H 0.7106 0.1596 0.5762 0.028 Uiso 1 1 calc R . .
C212 C 0.8332(2) 0.1333(2) 0.57336(12) 0.0248(8) Uani 1 1 d . . .
H21C H 0.8696 0.1569 0.5532 0.03 Uiso 1 1 calc R . .
H21D H 0.8642 0.1274 0.5986 0.03 Uiso 1 1 calc R . .
C21 C 0.7578(2) 0.2238(2) 0.62301(11) 0.0244(9) Uani 1 1 d . . .
H21E H 0.8102 0.2492 0.6289 0.029 Uiso 1 1 calc R . .
H21F H 0.7152 0.264 0.6235 0.029 Uiso 1 1 calc R . .
N221 N 0.74067(18) 0.16625(19) 0.65455(9) 0.0189(6) Uani 1 1 d . A .
C222 C 0.6665(2) 0.1387(2) 0.66298(11) 0.0166(7) Uani 1 1 d . . .
N223 N 0.67546(18) 0.08501(18) 0.69207(9) 0.0181(6) Uani 1 1 d . A .
C224 C 0.7975(2) 0.0345(2) 0.73116(11) 0.0232(8) Uani 1 1 d . . .
H224 H 0.7695 -0.0006 0.7481 0.028 Uiso 1 1 calc R . .
C225 C 0.8818(2) 0.0427(3) 0.73265(11) 0.0287(9) Uani 1 1 d . . .
H225 H 0.912 0.0121 0.751 0.034 Uiso 1 1 calc R . .
C226 C 0.9224(2) 0.0947(2) 0.70788(11) 0.0229(8) Uani 1 1 d . . .
H226 H 0.9796 0.0987 0.71 0.027 Uiso 1 1 calc R . .
C227 C 0.8821(2) 0.1409(2) 0.68028(11) 0.0227(8) Uani 1 1 d . A .
H227 H 0.9097 0.1768 0.6636 0.027 Uiso 1 1 calc R . .
C228 C 0.7984(2) 0.1311(2) 0.67866(11) 0.0181(7) Uani 1 1 d . . .
C229 C 0.7569(2) 0.0808(2) 0.70330(11) 0.0206(8) Uani 1 1 d . A .
C22 C 0.6066(2) 0.0470(2) 0.71166(13) 0.0303(10) Uani 1 1 d . . .
H22A H 0.5599 0.0503 0.6931 0.036 Uiso 1 1 calc R A .
H22B H 0.5925 0.0776 0.7358 0.036 Uiso 1 1 calc R . .
C231 C 0.6239(2) -0.0966(2) 0.69673(11) 0.0197(7) Uani 1 1 d U . .
C232 C 0.6147(2) -0.0354(2) 0.72444(9) 0.0162(7) Uani 1 1 d U A .
C233 C 0.6076(3) -0.0537(3) 0.76484(11) 0.0328(10) Uani 1 1 d . . .
H233 H 0.6049 -0.0132 0.784 0.039 Uiso 1 1 calc R A .
C234 C 0.6045(3) -0.1288(3) 0.77794(13) 0.0441(13) Uani 1 1 d . A .
H234 H 0.5979 -0.1395 0.8057 0.053 Uiso 1 1 calc R . .
C235 C 0.6110(2) -0.1882(3) 0.75091(14) 0.0389(12) Uani 1 1 d . . .
H235 H 0.6088 -0.2402 0.7599 0.047 Uiso 1 1 calc R A .
C236 C 0.6208(2) -0.1722(3) 0.71074(13) 0.0308(9) Uani 1 1 d . A .
H236 H 0.6255 -0.2135 0.6922 0.037 Uiso 1 1 calc R . .
C23 C 0.6260(2) -0.0858(3) 0.65164(12) 0.0261(9) Uani 1 1 d . A .
H23A H 0.616 -0.1365 0.6389 0.031 Uiso 1 1 calc R . .
H23B H 0.5807 -0.0514 0.644 0.031 Uiso 1 1 calc R . .
N241 N 0.70115(17) -0.05368(17) 0.63475(9) 0.0170(6) Uani 1 1 d . . .
C242 C 0.7012(2) -0.0058(2) 0.60253(10) 0.0174(7) Uani 1 1 d . A .
N243 N 0.77966(18) 0.00519(18) 0.59213(9) 0.0181(6) Uani 1 1 d . . .
C244 C 0.9140(2) -0.0434(2) 0.61808(11) 0.0217(8) Uani 1 1 d . . .
H244 H 0.9479 -0.0156 0.6001 0.026 Uiso 1 1 calc R A .
C245 C 0.9454(3) -0.0929(2) 0.64653(11) 0.0254(8) Uani 1 1 d . A .
H245 H 1.0024 -0.0996 0.6479 0.03 Uiso 1 1 calc R . .
C246 C 0.8968(3) -0.1335(2) 0.67338(12) 0.0267(8) Uani 1 1 d . . .
H246 H 0.9212 -0.1669 0.6925 0.032 Uiso 1 1 calc R A .
C247 C 0.8131(2) -0.1260(2) 0.67259(11) 0.0227(8) Uani 1 1 d . A .
H247 H 0.7793 -0.1539 0.6906 0.027 Uiso 1 1 calc R . .
C248 C 0.7813(2) -0.0757(2) 0.64416(11) 0.0172(7) Uani 1 1 d . A .
C249 C 0.8298(2) -0.0360(2) 0.61704(10) 0.0180(7) Uani 1 1 d . A .
C24 C 0.8078(2) 0.0536(2) 0.55860(11) 0.0225(8) Uani 1 1 d . A .
H24A H 0.7638 0.059 0.5386 0.027 Uiso 1 1 calc R . .
H24B H 0.8542 0.0283 0.5452 0.027 Uiso 1 1 calc R . .
O101 O 0.5751(2) 0.6647(3) 0.63608(13) 0.0385(9) Uani 0.708(3) 1 d PDU A 1
C101 C 0.5668(5) 0.6225(4) 0.6003(2) 0.0381(15) Uani 0.708(3) 1 d PDU A 1
H10A H 0.611 0.6359 0.5819 0.057 Uiso 0.708(3) 1 calc PR A 1
H10B H 0.5148 0.6351 0.5877 0.057 Uiso 0.708(3) 1 calc PR A 1
H10C H 0.5687 0.5672 0.6063 0.057 Uiso 0.708(3) 1 calc PR A 1
O102 O 0.5824(6) 0.5203(6) 0.5780(3) 0.0385(9) Uani 0.292(3) 1 d PDU A 2
C102 C 0.5621(13) 0.5944(7) 0.5882(6) 0.0381(15) Uani 0.292(3) 1 d PDU A 2
H10D H 0.5325 0.5941 0.6138 0.057 Uiso 0.292(3) 1 calc PR A 2
H10E H 0.5278 0.6166 0.5672 0.057 Uiso 0.292(3) 1 calc PR A 2
H10F H 0.6114 0.6254 0.5911 0.057 Uiso 0.292(3) 1 calc PR A 2
O201 O 0.3872(2) 0.3225(3) 0.80665(11) 0.0316(10) Uani 0.708(3) 1 d PDU A 1
C201 C 0.3198(7) 0.3205(7) 0.7831(4) 0.0286(17) Uani 0.708(3) 1 d PDU A 1
H20A H 0.2715 0.3193 0.8001 0.043 Uiso 0.708(3) 1 calc PR A 1
H20B H 0.3211 0.2742 0.7662 0.043 Uiso 0.708(3) 1 calc PR A 1
H20C H 0.3184 0.3665 0.7659 0.043 Uiso 0.708(3) 1 calc PR A 1
O202 O 0.3183(6) 0.2484(6) 0.7529(3) 0.031(2) Uani 0.292(3) 1 d PDU A 2
C202 C 0.310(2) 0.3067(18) 0.7795(10) 0.0286(17) Uani 0.292(3) 1 d PDU A 2
H20D H 0.2855 0.2869 0.8044 0.043 Uiso 0.292(3) 1 calc PR A 2
H20E H 0.2744 0.3465 0.7681 0.043 Uiso 0.292(3) 1 calc PR A 2
H20F H 0.3628 0.3291 0.7855 0.043 Uiso 0.292(3) 1 calc PR A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
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
Au1 C122 2.028(3) . ?
Au1 C242 2.034(4) . ?
Au1 Au2 3.2318(2) . ?
Au2 C222 2.029(4) . ?
Au2 C142 2.030(4) . ?
C111 C11 1.515(9) . ?
C111 C112 1.548(7) . ?
C111 H11A 0.99 . ?
C111 H11B 0.99 . ?
C112 C14 1.506(10) . ?
C112 H11C 0.99 . ?
C112 H11D 0.99 . ?
C11 N121 1.467(8) . ?
C11 H11E 0.99 . ?
C11 H11F 0.99 . ?
C113 C11' 1.537(17) . ?
C113 C114 1.54(2) . ?
C113 H11G 0.99 . ?
C113 H11H 0.99 . ?
C114 C14' 1.55(3) . ?
C114 H11I 0.99 . ?
C114 H11J 0.99 . ?
C11' N121 1.55(2) . ?
C11' H11K 0.99 . ?
C11' H11L 0.99 . ?
C14' N143 1.44(2) . ?
C14' H14C 0.99 . ?
C14' H14D 0.99 . ?
N121 C122 1.346(5) . ?
N121 C128 1.390(4) . ?
C122 N123 1.365(4) . ?
N123 C129 1.408(4) . ?
N123 C12 1.482(4) . ?
C124 C129 1.390(5) . ?
C124 C125 1.392(5) . ?
C124 H124 0.95 . ?
C125 C126 1.385(6) . ?
C125 H125 0.95 . ?
C126 C127 1.381(6) . ?
C126 H126 0.95 . ?
C127 C128 1.392(5) . ?
C127 H127 0.95 . ?
C128 C129 1.381(5) . ?
C12 C132 1.514(5) . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
C131 C136 1.385(5) . ?
C131 C132 1.389(5) . ?
C131 C13 1.529(5) . ?
C132 C133 1.384(5) . ?
C133 C134 1.402(6) . ?
C133 H133 0.95 . ?
C134 C135 1.381(6) . ?
C134 H134 0.95 . ?
C135 C136 1.381(6) . ?
C135 H135 0.95 . ?
C136 H136 0.95 . ?
C13 N141 1.471(5) . ?
C13 H13A 0.99 . ?
C13 H13B 0.99 . ?
N141 C142 1.354(5) . ?
N141 C148 1.399(5) . ?
C142 N143 1.348(5) . ?
N143 C149 1.395(5) . ?
N143 C14 1.506(9) . ?
C144 C149 1.390(5) . ?
C144 C145 1.390(6) . ?
C144 H144 0.95 . ?
C145 C146 1.389(6) . ?
C145 H145 0.95 . ?
C146 C147 1.377(5) . ?
C146 H146 0.95 . ?
C147 C148 1.390(5) . ?
C147 H147 0.95 . ?
C148 C149 1.377(5) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C211 C21 1.530(5) . ?
C211 C212 1.540(5) . ?
C211 H21A 0.99 . ?
C211 H21B 0.99 . ?
C212 C24 1.525(6) . ?
C212 H21C 0.99 . ?
C212 H21D 0.99 . ?
C21 N221 1.476(5) . ?
C21 H21E 0.99 . ?
C21 H21F 0.99 . ?
N221 C222 1.345(5) . ?
N221 C228 1.387(4) . ?
C222 N223 1.351(5) . ?
N223 C229 1.398(5) . ?
N223 C22 1.467(5) . ?
C224 C229 1.397(5) . ?
C224 C225 1.401(5) . ?
C224 H224 0.95 . ?
C225 C226 1.394(6) . ?
C225 H225 0.95 . ?
C226 C227 1.389(5) . ?
C226 H226 0.95 . ?
C227 C228 1.394(5) . ?
C227 H227 0.95 . ?
C228 C229 1.380(5) . ?
C22 C232 1.496(5) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
C231 C236 1.392(6) . ?
C231 C232 1.414(5) . ?
C231 C23 1.512(5) . ?
C232 C233 1.386(5) . ?
C233 C234 1.372(7) . ?
C233 H233 0.95 . ?
C234 C235 1.372(7) . ?
C234 H234 0.95 . ?
C235 C236 1.374(6) . ?
C235 H235 0.95 . ?
C236 H236 0.95 . ?
C23 N241 1.472(4) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
N241 C242 1.355(5) . ?
N241 C248 1.414(5) . ?
C242 N243 1.355(5) . ?
N243 C249 1.372(5) . ?
N243 C24 1.471(5) . ?
C244 C245 1.380(5) . ?
C244 C249 1.398(5) . ?
C244 H244 0.95 . ?
C245 C246 1.392(6) . ?
C245 H245 0.95 . ?
C246 C247 1.389(6) . ?
C246 H246 0.95 . ?
C247 C248 1.390(5) . ?
C247 H247 0.95 . ?
C248 C249 1.389(5) . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
O101 C101 1.404(6) . ?
C101 H10A 0.98 . ?
C101 H10B 0.98 . ?
C101 H10C 0.98 . ?
O102 C102 1.370(9) . ?
C102 H10D 0.98 . ?
C102 H10E 0.98 . ?
C102 H10F 0.98 . ?
O201 C201 1.363(8) . ?
C201 H20A 0.98 . ?
C201 H20B 0.98 . ?
C201 H20C 0.98 . ?
O202 C202 1.351(10) . ?
C202 H20D 0.98 . ?
C202 H20E 0.98 . ?
C202 H20F 0.98 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C122 Au1 C242 174.19(15) . . ?
C122 Au1 Au2 83.68(10) . . ?
C242 Au1 Au2 98.11(10) . . ?
C222 Au2 C142 177.66(15) . . ?
C222 Au2 Au1 82.75(10) . . ?
C142 Au2 Au1 99.05(10) . . ?
C11 C111 C112 113.1(5) . . ?
C11 C111 H11A 109 . . ?
C112 C111 H11A 109 . . ?
C11 C111 H11B 109 . . ?
C112 C111 H11B 109 . . ?
H11A C111 H11B 107.8 . . ?
C14 C112 C111 116.9(4) . . ?
C14 C112 H11C 108.1 . . ?
C111 C112 H11C 108.1 . . ?
C14 C112 H11D 108.1 . . ?
C111 C112 H11D 108.1 . . ?
H11C C112 H11D 107.3 . . ?
N121 C11 C111 110.5(6) . . ?
N121 C11 H11E 109.6 . . ?
C111 C11 H11E 109.6 . . ?
N121 C11 H11F 109.5 . . ?
C111 C11 H11F 109.5 . . ?
H11E C11 H11F 108.1 . . ?
C11' C113 C114 120.1(14) . . ?
C11' C113 H11G 107.3 . . ?
C114 C113 H11G 107.3 . . ?
C11' C113 H11H 107.3 . . ?
C114 C113 H11H 107.3 . . ?
H11G C113 H11H 106.9 . . ?
C113 C114 C14' 113.2(14) . . ?
C113 C114 H11I 108.9 . . ?
C14' C114 H11I 108.9 . . ?
C113 C114 H11J 108.9 . . ?
C14' C114 H11J 108.9 . . ?
H11I C114 H11J 107.7 . . ?
C113 C11' N121 103.3(14) . . ?
C113 C11' H11K 111.1 . . ?
N121 C11' H11K 111.1 . . ?
C113 C11' H11L 111.1 . . ?
N121 C11' H11L 111.1 . . ?
H11K C11' H11L 109.1 . . ?
N143 C14' C114 110.6(18) . . ?
N143 C14' H14C 109.5 . . ?
C114 C14' H14C 109.5 . . ?
N143 C14' H14D 109.5 . . ?
C114 C14' H14D 109.5 . . ?
H14C C14' H14D 108.1 . . ?
C122 N121 C128 110.1(3) . . ?
C122 N121 C11 129.2(4) . . ?
C128 N121 C11 119.8(4) . . ?
C122 N121 C11' 117.2(8) . . ?
C128 N121 C11' 132.5(8) . . ?
N121 C122 N123 106.7(3) . . ?
N121 C122 Au1 130.0(3) . . ?
N123 C122 Au1 123.2(2) . . ?
C122 N123 C129 110.3(3) . . ?
C122 N123 C12 119.6(3) . . ?
C129 N123 C12 130.1(3) . . ?
C129 C124 C125 116.1(3) . . ?
C129 C124 H124 122 . . ?
C125 C124 H124 122 . . ?
C126 C125 C124 122.5(4) . . ?
C126 C125 H125 118.7 . . ?
C124 C125 H125 118.7 . . ?
C127 C126 C125 121.3(4) . . ?
C127 C126 H126 119.4 . . ?
C125 C126 H126 119.4 . . ?
C126 C127 C128 116.3(3) . . ?
C126 C127 H127 121.8 . . ?
C128 C127 H127 121.8 . . ?
C129 C128 N121 107.8(3) . . ?
C129 C128 C127 122.5(3) . . ?
N121 C128 C127 129.7(3) . . ?
C128 C129 C124 121.2(3) . . ?
C128 C129 N123 105.2(3) . . ?
C124 C129 N123 133.6(3) . . ?
N123 C12 C132 113.9(3) . . ?
N123 C12 H12A 108.8 . . ?
C132 C12 H12A 108.8 . . ?
N123 C12 H12B 108.8 . . ?
C132 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
C136 C131 C132 119.1(4) . . ?
C136 C131 C13 117.6(4) . . ?
C132 C131 C13 123.2(3) . . ?
C133 C132 C131 120.4(4) . . ?
C133 C132 C12 116.3(3) . . ?
C131 C132 C12 123.3(3) . . ?
C132 C133 C134 120.5(4) . . ?
C132 C133 H133 119.8 . . ?
C134 C133 H133 119.8 . . ?
C135 C134 C133 118.2(4) . . ?
C135 C134 H134 120.9 . . ?
C133 C134 H134 120.9 . . ?
C136 C135 C134 121.4(4) . . ?
C136 C135 H135 119.3 . . ?
C134 C135 H135 119.3 . . ?
C135 C136 C131 120.4(4) . . ?
C135 C136 H136 119.8 . . ?
C131 C136 H136 119.8 . . ?
N141 C13 C131 116.1(3) . . ?
N141 C13 H13A 108.3 . . ?
C131 C13 H13A 108.3 . . ?
N141 C13 H13B 108.3 . . ?
C131 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
C142 N141 C148 110.0(3) . . ?
C142 N141 C13 124.4(3) . . ?
C148 N141 C13 124.7(3) . . ?
N143 C142 N141 107.1(3) . . ?
N143 C142 Au2 126.5(3) . . ?
N141 C142 Au2 126.4(3) . . ?
C142 N143 C149 109.8(3) . . ?
C142 N143 C14' 134.1(8) . . ?
C149 N143 C14' 115.8(8) . . ?
C142 N143 C14 121.2(4) . . ?
C149 N143 C14 128.6(4) . . ?
C149 C144 C145 116.0(4) . . ?
C149 C144 H144 122 . . ?
C145 C144 H144 122 . . ?
C146 C145 C144 121.6(4) . . ?
C146 C145 H145 119.2 . . ?
C144 C145 H145 119.2 . . ?
C147 C146 C145 122.3(4) . . ?
C147 C146 H146 118.9 . . ?
C145 C146 H146 118.9 . . ?
C146 C147 C148 116.1(4) . . ?
C146 C147 H147 122 . . ?
C148 C147 H147 122 . . ?
C149 C148 C147 122.0(3) . . ?
C149 C148 N141 106.1(3) . . ?
C147 C148 N141 131.8(3) . . ?
C148 C149 C144 122.1(4) . . ?
C148 C149 N143 107.0(3) . . ?
C144 C149 N143 130.8(3) . . ?
C112 C14 N143 111.8(7) . . ?
C112 C14 H14A 109.3 . . ?
N143 C14 H14A 109.3 . . ?
C112 C14 H14B 109.3 . . ?
N143 C14 H14B 109.3 . . ?
H14A C14 H14B 107.9 . . ?
C21 C211 C212 115.5(3) . . ?
C21 C211 H21A 108.4 . . ?
C212 C211 H21A 108.4 . . ?
C21 C211 H21B 108.4 . . ?
C212 C211 H21B 108.4 . . ?
H21A C211 H21B 107.5 . . ?
C24 C212 C211 113.7(3) . . ?
C24 C212 H21C 108.8 . . ?
C211 C212 H21C 108.8 . . ?
C24 C212 H21D 108.8 . . ?
C211 C212 H21D 108.8 . . ?
H21C C212 H21D 107.7 . . ?
N221 C21 C211 112.7(3) . . ?
N221 C21 H21E 109.1 . . ?
C211 C21 H21E 109.1 . . ?
N221 C21 H21F 109.1 . . ?
C211 C21 H21F 109.1 . . ?
H21E C21 H21F 107.8 . . ?
C222 N221 C228 110.5(3) . . ?
C222 N221 C21 124.3(3) . . ?
C228 N221 C21 125.2(3) . . ?
N221 C222 N223 107.1(3) . . ?
N221 C222 Au2 124.9(3) . . ?
N223 C222 Au2 128.0(3) . . ?
C222 N223 C229 109.5(3) . . ?
C222 N223 C22 122.8(3) . . ?
C229 N223 C22 127.2(3) . . ?
C229 C224 C225 116.3(4) . . ?
C229 C224 H224 121.9 . . ?
C225 C224 H224 121.9 . . ?
C226 C225 C224 121.6(4) . . ?
C226 C225 H225 119.2 . . ?
C224 C225 H225 119.2 . . ?
C227 C226 C225 122.2(4) . . ?
C227 C226 H226 118.9 . . ?
C225 C226 H226 118.9 . . ?
C226 C227 C228 115.6(4) . . ?
C226 C227 H227 122.2 . . ?
C228 C227 H227 122.2 . . ?
C229 C228 N221 106.2(3) . . ?
C229 C228 C227 123.1(3) . . ?
N221 C228 C227 130.6(4) . . ?
C228 C229 C224 121.2(3) . . ?
C228 C229 N223 106.6(3) . . ?
C224 C229 N223 132.0(4) . . ?
N223 C22 C232 119.0(3) . . ?
N223 C22 H22A 107.6 . . ?
C232 C22 H22A 107.6 . . ?
N223 C22 H22B 107.6 . . ?
C232 C22 H22B 107.6 . . ?
H22A C22 H22B 107 . . ?
C236 C231 C232 118.9(4) . . ?
C236 C231 C23 116.7(4) . . ?
C232 C231 C23 123.8(3) . . ?
C233 C232 C231 118.0(4) . . ?
C233 C232 C22 119.2(4) . . ?
C231 C232 C22 122.7(3) . . ?
C234 C233 C232 121.9(4) . . ?
C234 C233 H233 119 . . ?
C232 C233 H233 119 . . ?
C235 C234 C233 120.0(4) . . ?
C235 C234 H234 120 . . ?
C233 C234 H234 120 . . ?
C234 C235 C236 119.6(4) . . ?
C234 C235 H235 120.2 . . ?
C236 C235 H235 120.2 . . ?
C235 C236 C231 121.4(4) . . ?
C235 C236 H236 119.3 . . ?
C231 C236 H236 119.3 . . ?
N241 C23 C231 116.4(3) . . ?
N241 C23 H23A 108.2 . . ?
C231 C23 H23A 108.2 . . ?
N241 C23 H23B 108.2 . . ?
C231 C23 H23B 108.2 . . ?
H23A C23 H23B 107.3 . . ?
C242 N241 C248 109.9(3) . . ?
C242 N241 C23 122.2(3) . . ?
C248 N241 C23 127.2(3) . . ?
N243 C242 N241 106.8(3) . . ?
N243 C242 Au1 129.6(3) . . ?
N241 C242 Au1 123.5(3) . . ?
C242 N243 C249 110.5(3) . . ?
C242 N243 C24 125.1(3) . . ?
C249 N243 C24 124.4(3) . . ?
C245 C244 C249 116.6(4) . . ?
C245 C244 H244 121.7 . . ?
C249 C244 H244 121.7 . . ?
C244 C245 C246 122.5(4) . . ?
C244 C245 H245 118.7 . . ?
C246 C245 H245 118.7 . . ?
C247 C246 C245 121.0(4) . . ?
C247 C246 H246 119.5 . . ?
C245 C246 H246 119.5 . . ?
C246 C247 C248 116.6(4) . . ?
C246 C247 H247 121.7 . . ?
C248 C247 H247 121.7 . . ?
C249 C248 C247 122.4(3) . . ?
C249 C248 N241 105.2(3) . . ?
C247 C248 N241 132.4(3) . . ?
N243 C249 C248 107.6(3) . . ?
N243 C249 C244 131.6(3) . . ?
C248 C249 C244 120.8(3) . . ?
N243 C24 C212 111.0(3) . . ?
N243 C24 H24A 109.4 . . ?
C212 C24 H24A 109.4 . . ?
N243 C24 H24B 109.4 . . ?
C212 C24 H24B 109.4 . . ?
H24A C24 H24B 108 . . ?
O101 C101 H10A 109.5 . . ?
O101 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
O101 C101 H10C 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
O102 C102 H10D 109.5 . . ?
O102 C102 H10E 109.5 . . ?
H10D C102 H10E 109.5 . . ?
O102 C102 H10F 109.5 . . ?
H10D C102 H10F 109.5 . . ?
H10E C102 H10F 109.5 . . ?
O201 C201 H20A 109.5 . . ?
O201 C201 H20B 109.5 . . ?
H20A C201 H20B 109.5 . . ?
O201 C201 H20C 109.5 . . ?
H20A C201 H20C 109.5 . . ?
H20B C201 H20C 109.5 . . ?
O202 C202 H20D 109.5 . . ?
O202 C202 H20E 109.5 . . ?
H20D C202 H20E 109.5 . . ?
O202 C202 H20F 109.5 . . ?
H20D C202 H20F 109.5 . . ?
H20E C202 H20F 109.5 . . ?


#===END
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lw1281


_database_code_depnum_ccdc_archive 'CCDC 834025'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_date             2010-05-11T14:41:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C55 H60 Au2 Br2 N8 O3'
_chemical_formula_moiety         'C52 H48 Au2 N8, 2(Br), 3(C H4 O)'
_chemical_formula_weight         1434.86

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  -P_2yn

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6255(3)
_cell_length_b                   27.8969(7)
_cell_length_c                   15.7022(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.297(3)
_cell_angle_gamma                90
_cell_volume                     5280.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9101
_cell_measurement_theta_min      2.5658
_cell_measurement_theta_max      29.899

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2792
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    7.115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_absorpt_correction_T_min  0.72108
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.0009
_diffrn_orient_matrix_ub_11      0.012951598
_diffrn_orient_matrix_ub_12      -0.0182963527
_diffrn_orient_matrix_ub_13      0.0325003291
_diffrn_orient_matrix_ub_21      -0.0569978247
_diffrn_orient_matrix_ub_22      -0.0055140411
_diffrn_orient_matrix_ub_23      -0.0094745147
_diffrn_orient_matrix_ub_31      0.0043577913
_diffrn_orient_matrix_ub_32      -0.0166025808
_diffrn_orient_matrix_ub_33      -0.0328601328
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0947
_diffrn_reflns_number            49310
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  
;
 Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       'ω scans'

_reflns_number_total             9275
_reflns_number_gt                5562
_reflns_threshold_expression     I>2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinement       
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction        
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'



#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

The Br ions were modelled as being disordered over 5 sites with  the sum
of their occupancy factors constrained to be 2. The other remaining peaks were
modelled as  three CH3OH solvent molecules. Methanol OH H atoms were 
refined as part of riding models with the position of one of them, H(201), 
restrained  for possible hydrogen bonds between H(201) and Br(3) 
and H(201) and Br(4). 

The central atoms of the C4 alkyl chains were modelled as being disordered
 over two sets of sites with occupancies set at 0.5 after trial
 refinement. Geometries were restrained to ideal values. Some C-C and 
C-N bond lengths were also restrained.

Displacement parameters for the disordered alkyl chains, each 
 Phenimidazole ring and the solvent were restrained to reasonable values.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0292P)²+163.8824P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9275
_refine_ls_number_parameters     703
_refine_ls_number_restraints     537
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.0954
_refine_ls_wR_factor_ref         0.2095
_refine_ls_wR_factor_gt          0.1958
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_restrained_S_all      1.2
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.623
_refine_diff_density_min         -1.672
_refine_diff_density_rms         0.19

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.21358(7) 0.06659(3) 0.22538(5) 0.0381(2) Uani 1 1 d . E .
Au2 Au 0.20672(9) 0.17870(3) 0.21770(6) 0.0561(3) Uani 1 1 d . . .
Br1 Br 0.7076(4) 0.29633(17) 0.2131(3) 0.0871(19) Uani 0.686(9) 1 d P A 1
Br2 Br 0.9982(5) 0.4775(3) 0.3832(4) 0.093(3) Uani 0.482(9) 1 d P B 2
Br3 Br 0.592(2) 0.4801(14) 0.157(2) 0.34(3) Uani 0.27(2) 1 d PD C 3
Br4 Br 0.5624(10) 0.5055(4) 0.0769(13) 0.096(7) Uani 0.246(13) 1 d PD . 4
Br5 Br 0.733(2) 0.4485(14) 0.2589(18) 0.34(2) Uani 0.321(15) 1 d P D 5
C10 C 0.300(3) 0.1012(14) 0.038(2) 0.041(6) Uani 0.5 1 d PDU E 1
H10A H 0.3791 0.0938 0.0458 0.049 Uiso 0.5 1 calc PR E 1
H10B H 0.2939 0.1139 0.095 0.049 Uiso 0.5 1 calc PR E 1
C10' C 0.265(4) 0.1021(11) -0.028(3) 0.056(7) Uani 0.5 1 d PDU E 2
H10C H 0.3266 0.0949 -0.0532 0.068 Uiso 0.5 1 calc PR E 2
H10D H 0.2007 0.1134 -0.0769 0.068 Uiso 0.5 1 calc PR E 2
C11 C 0.2335(16) 0.0562(7) 0.0151(14) 0.046(4) Uani 1 1 d DU . .
H11A H 0.2251 0.0479 -0.0479 0.056 Uiso 0.5 1 calc PR E 1
H11B H 0.2748 0.0299 0.0528 0.056 Uiso 0.5 1 calc PR E 1
H11C H 0.2346 0.0285 -0.0239 0.056 Uiso 0.5 1 d PR E 2
H11D H 0.2887 0.0502 0.0737 0.056 Uiso 0.5 1 d PR E 2
N121 N 0.1237(11) 0.0596(5) 0.0272(9) 0.030(3) Uani 1 1 d U E .
C122 C 0.0978(14) 0.0651(6) 0.1047(11) 0.029(3) Uani 1 1 d U . .
N123 N -0.0114(11) 0.0680(5) 0.0865(9) 0.029(3) Uani 1 1 d U E .
C124 C -0.1704(14) 0.0617(7) -0.0582(11) 0.035(3) Uani 1 1 d U . .
H124 H -0.2299 0.0638 -0.033 0.042 Uiso 1 1 calc R . .
C125 C -0.1909(15) 0.0574(7) -0.1506(12) 0.039(3) Uani 1 1 d U . .
H125 H -0.265 0.0582 -0.1889 0.046 Uiso 1 1 calc R . .
C126 C -0.1025(14) 0.0520(6) -0.1866(11) 0.033(3) Uani 1 1 d U . .
H126 H -0.119 0.0469 -0.249 0.04 Uiso 1 1 calc R . .
C127 C 0.0086(14) 0.0537(6) -0.1354(11) 0.031(3) Uani 1 1 d U E .
H127 H 0.0685 0.0524 -0.1604 0.037 Uiso 1 1 calc R . .
C128 C 0.0231(13) 0.0575(6) -0.0460(11) 0.027(3) Uani 1 1 d U . .
C129 C -0.0609(14) 0.0627(7) -0.0045(11) 0.030(3) Uani 1 1 d U E .
C12 C -0.0641(16) 0.0715(7) 0.1556(11) 0.038(5) Uani 1 1 d . . .
H12A H -0.0108 0.0857 0.2091 0.045 Uiso 1 1 calc R E .
H12B H -0.0813 0.0386 0.1716 0.045 Uiso 1 1 calc R . .
C131 C -0.1774(17) 0.1502(8) 0.1253(11) 0.044(5) Uani 1 1 d . . .
C132 C -0.1678(16) 0.1002(8) 0.1327(12) 0.041(5) Uani 1 1 d . E .
C133 C -0.2654(18) 0.0753(10) 0.1213(13) 0.059(7) Uani 1 1 d . . .
H133 H -0.261 0.0414 0.1262 0.071 Uiso 1 1 calc R E .
C134 C -0.369(2) 0.0959(12) 0.1033(15) 0.072(7) Uani 1 1 d U E .
H134 H -0.4335 0.0771 0.097 0.086 Uiso 1 1 calc R . .
C135 C -0.3744(19) 0.1436(12) 0.0950(14) 0.073(7) Uani 1 1 d U . .
H135 H -0.4456 0.1583 0.0792 0.088 Uiso 1 1 calc R E .
C136 C -0.2813(19) 0.1733(11) 0.1083(13) 0.067(7) Uani 1 1 d U E .
H136 H -0.2877 0.2072 0.1061 0.081 Uiso 1 1 calc R . .
C13 C -0.0723(17) 0.1807(7) 0.1435(12) 0.041(5) Uani 1 1 d . E .
H13A H -0.0917 0.2142 0.1538 0.05 Uiso 1 1 calc R . .
H13B H -0.0187 0.1692 0.1995 0.05 Uiso 1 1 calc R . .
N141 N -0.0172(16) 0.1811(6) 0.0746(10) 0.050(4) Uani 1 1 d DU . .
C142 C 0.0972(18) 0.1798(7) 0.0987(14) 0.055(5) Uani 1 1 d DU E .
N143 N 0.1172(15) 0.1838(6) 0.0171(11) 0.049(4) Uani 1 1 d U . .
C144 C 0.001(2) 0.1931(7) -0.1480(12) 0.049(4) Uani 1 1 d U . .
H144 H 0.0622 0.1937 -0.1716 0.059 Uiso 1 1 calc R E .
C145 C -0.106(2) 0.1974(7) -0.2037(14) 0.058(5) Uani 1 1 d DU E .
H145 H -0.1212 0.2004 -0.2665 0.069 Uiso 1 1 calc R . .
C146 C -0.1870(19) 0.1971(7) -0.1644(12) 0.052(4) Uani 1 1 d DU . .
H146 H -0.2603 0.2022 -0.2022 0.063 Uiso 1 1 calc R E .
C147 C -0.1750(18) 0.1899(7) -0.0726(13) 0.049(4) Uani 1 1 d DU E .
H147 H -0.238 0.1892 -0.0513 0.059 Uiso 1 1 calc R . .
C148 C -0.0694(17) 0.1840(7) -0.0147(11) 0.040(4) Uani 1 1 d DU E .
C149 C 0.0191(18) 0.1879(7) -0.0543(12) 0.041(4) Uani 1 1 d U E .
C14 C 0.2330(17) 0.1871(8) 0.0059(16) 0.057(5) Uani 1 1 d DU E .
H14A H 0.2884 0.1925 0.0646 0.068 Uiso 0.5 1 calc PR F 1
H14B H 0.2362 0.2144 -0.0334 0.068 Uiso 0.5 1 calc PR F 1
H14C H 0.2737 0.2147 0.0398 0.068 Uiso 0.5 1 d PR F 2
H14D H 0.2266 0.1919 -0.0579 0.068 Uiso 0.5 1 d PR F 2
C15 C 0.261(3) 0.1399(10) -0.036(2) 0.043(6) Uani 0.5 1 d PDU E 1
H15A H 0.1938 0.1284 -0.082 0.052 Uiso 0.5 1 calc PR E 1
H15B H 0.3195 0.146 -0.064 0.052 Uiso 0.5 1 calc PR E 1
C15' C 0.301(4) 0.1408(16) 0.044(3) 0.057(7) Uani 0.5 1 d PDU E 2
H15C H 0.3816 0.1472 0.0584 0.068 Uiso 0.5 1 calc PR E 2
H15D H 0.2852 0.1304 0.0996 0.068 Uiso 0.5 1 calc PR E 2
C20 C 0.124(4) 0.1026(16) 0.408(3) 0.055(7) Uani 0.5 1 d PU E 1
H20A H 0.1309 0.1131 0.349 0.066 Uiso 0.5 1 calc PR E 1
H20B H 0.0452 0.0959 0.4003 0.066 Uiso 0.5 1 calc PR E 1
C20' C 0.159(3) 0.1048(10) 0.475(2) 0.041(6) Uani 0.5 1 d PDU E 2
H20C H 0.1006 0.0975 0.5034 0.05 Uiso 0.5 1 calc PR E 2
H20D H 0.2242 0.1171 0.5215 0.05 Uiso 0.5 1 calc PR E 2
C21 C 0.1919(16) 0.0573(7) 0.4369(15) 0.051(5) Uani 1 1 d DU . .
H21A H 0.1966 0.0503 0.4997 0.061 Uiso 0.5 1 calc PR E 1
H21B H 0.1535 0.0301 0.3999 0.061 Uiso 0.5 1 calc PR E 1
H21C H 0.1875 0.0297 0.4754 0.061 Uiso 0.5 1 d PR E 2
H21D H 0.1389 0.0517 0.3771 0.061 Uiso 0.5 1 d PR E 2
N221 N 0.3050(12) 0.0616(5) 0.4288(9) 0.036(3) Uani 1 1 d U E .
C222 C 0.3229(15) 0.0666(7) 0.3502(11) 0.034(3) Uani 1 1 d U . .
N223 N 0.4323(12) 0.0659(5) 0.3638(9) 0.030(3) Uani 1 1 d DU E .
C224 C 0.5986(16) 0.0622(7) 0.5129(12) 0.039(3) Uani 1 1 d U . .
H224 H 0.6579 0.0637 0.4874 0.046 Uiso 1 1 calc R . .
C225 C 0.6140(18) 0.0577(7) 0.6031(12) 0.044(3) Uani 1 1 d U . .
H225 H 0.688 0.0549 0.6411 0.053 Uiso 1 1 calc R . .
C226 C 0.5283(16) 0.0570(7) 0.6427(13) 0.049(3) Uani 1 1 d DU . .
H226 H 0.5451 0.0561 0.7058 0.058 Uiso 1 1 calc R . .
C227 C 0.4196(16) 0.0574(7) 0.5900(12) 0.045(3) Uani 1 1 d DU E .
H227 H 0.3602 0.0552 0.6154 0.053 Uiso 1 1 calc R . .
C228 C 0.3992(16) 0.0613(7) 0.4971(12) 0.038(3) Uani 1 1 d U . .
C229 C 0.4898(15) 0.0642(7) 0.4639(11) 0.034(3) Uani 1 1 d U E .
C22 C 0.4907(15) 0.0699(7) 0.3010(10) 0.048(6) Uani 1 1 d D . .
H22A H 0.4379 0.0827 0.2458 0.058 Uiso 1 1 calc R E .
H22B H 0.5093 0.0369 0.2873 0.058 Uiso 1 1 calc R . .
C231 C 0.5909(14) 0.1492(7) 0.3104(12) 0.041(4) Uani 1 1 d DU . .
C232 C 0.5990(16) 0.1000(8) 0.3180(12) 0.049(6) Uani 1 1 d D E .
C233 C 0.703(2) 0.0776(13) 0.3362(14) 0.086(10) Uani 1 1 d . . .
H233 H 0.711 0.0437 0.3402 0.103 Uiso 1 1 calc R E .
C234 C 0.799(2) 0.1093(10) 0.3486(16) 0.077(7) Uani 1 1 d DU E .
H234 H 0.8713 0.096 0.3638 0.092 Uiso 1 1 calc R . .
C235 C 0.786(2) 0.1568(10) 0.3390(15) 0.077(6) Uani 1 1 d DU . .
H235 H 0.8483 0.177 0.3445 0.092 Uiso 1 1 calc R E .
C236 C 0.6823(19) 0.1760(10) 0.3214(16) 0.076(8) Uani 1 1 d DU E .
H236 H 0.6745 0.2099 0.3167 0.091 Uiso 1 1 calc R . .
C23 C 0.4815(14) 0.1776(7) 0.2884(11) 0.044(3) Uani 1 1 d DU E .
H23A H 0.4957 0.2109 0.2728 0.053 Uiso 1 1 calc R . .
H23B H 0.4278 0.1631 0.2354 0.053 Uiso 1 1 calc R . .
N241 N 0.4347(12) 0.1789(5) 0.3568(9) 0.031(2) Uani 1 1 d DU . .
C242 C 0.3210(15) 0.1824(6) 0.3438(12) 0.033(3) Uani 1 1 d U E .
N243 N 0.2963(13) 0.1855(6) 0.4196(10) 0.041(3) Uani 1 1 d U . .
C244 C 0.4167(16) 0.1943(7) 0.5762(13) 0.043(3) Uani 1 1 d U . .
H244 H 0.3578 0.1966 0.6022 0.052 Uiso 1 1 calc R E .
C245 C 0.5249(15) 0.1979(7) 0.6283(13) 0.040(3) Uani 1 1 d U E .
H245 H 0.5407 0.2022 0.6908 0.048 Uiso 1 1 calc R . .
C246 C 0.6172(16) 0.1953(7) 0.5889(12) 0.038(3) Uani 1 1 d U . .
H246 H 0.6921 0.1978 0.6252 0.046 Uiso 1 1 calc R E .
C247 C 0.5925(16) 0.1892(7) 0.5006(12) 0.038(3) Uani 1 1 d U E .
H247 H 0.6493 0.1866 0.4724 0.046 Uiso 1 1 calc R . .
C248 C 0.4772(16) 0.1867(7) 0.4496(13) 0.038(3) Uani 1 1 d U E .
C249 C 0.3951(17) 0.1874(7) 0.4882(13) 0.043(3) Uani 1 1 d U E .
C24 C 0.1861(18) 0.1886(8) 0.4303(16) 0.061(5) Uani 1 1 d DU E .
H24A H 0.1302 0.1938 0.3717 0.073 Uiso 0.5 1 calc PR G 1
H24B H 0.1824 0.2159 0.4697 0.073 Uiso 0.5 1 calc PR G 1
H24C H 0.1472 0.2159 0.3939 0.073 Uiso 0.5 1 d PR G 2
H24D H 0.1935 0.196 0.4935 0.073 Uiso 0.5 1 d PR G 2
C25 C 0.162(4) 0.1408(12) 0.472(3) 0.062(7) Uani 0.5 1 d PDU E 1
H25A H 0.2309 0.1303 0.5178 0.074 Uiso 0.5 1 calc PR E 1
H25B H 0.1053 0.1467 0.5028 0.074 Uiso 0.5 1 calc PR E 1
C25' C 0.115(3) 0.1447(13) 0.404(2) 0.042(7) Uani 0.5 1 d PDU E 2
H25C H 0.1173 0.1334 0.3451 0.051 Uiso 0.5 1 calc PR E 2
H25D H 0.0375 0.1525 0.4003 0.051 Uiso 0.5 1 calc PR E 2
O101 O 0.945(2) 0.2683(14) 0.3218(16) 0.189(14) Uani 1 1 d U . .
H101 H 0.8788 0.276 0.2952 0.284 Uiso 1 1 calc R . .
C101 C 1.012(3) 0.313(2) 0.356(2) 0.199(17) Uani 1 1 d U . .
H10E H 1.0183 0.3172 0.4194 0.299 Uiso 1 1 calc R . .
H10F H 0.9741 0.3408 0.3224 0.299 Uiso 1 1 calc R . .
H10G H 1.0856 0.3097 0.3486 0.299 Uiso 1 1 calc R . .
O201 O 0.3732(16) 0.4442(7) 0.0874(13) 0.122(7) Uani 1 1 d U . .
H201 H 0.43 0.4592 0.085 0.183 Uiso 1 1 calc RD . .
C201 C 0.396(3) 0.3908(11) 0.0909(19) 0.113(10) Uani 1 1 d U . .
H20E H 0.4492 0.3837 0.0581 0.17 Uiso 1 1 calc R . .
H20F H 0.3268 0.3735 0.0638 0.17 Uiso 1 1 calc R . .
H20G H 0.4271 0.3808 0.1532 0.17 Uiso 1 1 calc R . .
O301 O 0.4687(15) 0.2556(7) 0.1135(10) 0.093(6) Uani 1 1 d DU . .
H301 H 0.5339 0.2626 0.1433 0.139 Uiso 1 1 calc R . .
C301 C 0.445(3) 0.2760(14) 0.0342(18) 0.156(14) Uani 1 1 d DU . .
H30A H 0.38 0.2966 0.0251 0.234 Uiso 1 1 calc R . .
H30B H 0.43 0.2511 -0.012 0.234 Uiso 1 1 calc R . .
H30C H 0.5087 0.2953 0.0307 0.234 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
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
Au1 C122 2.021(16) . ?
Au1 C222 2.035(17) . ?
Au1 Au2 3.1301(11) . ?
Au2 C142 1.97(2) . ?
Au2 C242 2.077(18) . ?
C10 C11 1.49(4) . ?
C10 C15 1.549(19) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
C10' C15' 1.537(19) . ?
C10' C11 1.553(19) . ?
C10' H10C 0.99 . ?
C10' H10D 0.99 . ?
C11 N121 1.46(2) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C11 H11C 0.99 . ?
C11 H11D 0.99 . ?
N121 C122 1.36(2) . ?
N121 C128 1.44(2) . ?
C122 N123 1.32(2) . ?
N123 C129 1.39(2) . ?
N123 C12 1.44(2) . ?
C124 C129 1.39(2) . ?
C124 C125 1.40(2) . ?
C124 H124 0.95 . ?
C125 C126 1.40(2) . ?
C125 H125 0.95 . ?
C126 C127 1.39(2) . ?
C126 H126 0.95 . ?
C127 C128 1.37(2) . ?
C127 H127 0.95 . ?
C128 C129 1.41(2) . ?
C12 C132 1.48(3) . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
C131 C132 1.40(3) . ?
C131 C136 1.41(3) . ?
C131 C13 1.53(3) . ?
C132 C133 1.38(3) . ?
C133 C134 1.38(3) . ?
C133 H133 0.95 . ?
C134 C135 1.34(3) . ?
C134 H134 0.95 . ?
C135 C136 1.40(4) . ?
C135 H135 0.95 . ?
C136 H136 0.95 . ?
C13 N141 1.45(2) . ?
C13 H13A 0.99 . ?
C13 H13B 0.99 . ?
N141 C148 1.36(2) . ?
N141 C142 1.380(17) . ?
C142 N143 1.38(3) . ?
N143 C149 1.41(2) . ?
N143 C14 1.53(3) . ?
C144 C145 1.38(3) . ?
C144 C149 1.43(2) . ?
C144 H144 0.95 . ?
C145 C146 1.35(2) . ?
C145 H145 0.95 . ?
C146 C147 1.42(3) . ?
C146 H146 0.95 . ?
C147 C148 1.38(2) . ?
C147 H147 0.95 . ?
C148 C149 1.43(3) . ?
C14 C15 1.551(19) . ?
C14 C15' 1.57(5) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C14 H14C 0.99 . ?
C14 H14D 0.99 . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C15' H15C 0.99 . ?
C15' H15D 0.99 . ?
C20 C25 1.45(6) . ?
C20 C21 1.52(5) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C20' C25' 1.551(19) . ?
C20' C21 1.558(18) . ?
C20' H20C 0.99 . ?
C20' H20D 0.99 . ?
C21 N221 1.48(2) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C21 H21C 0.99 . ?
C21 H21D 0.99 . ?
N221 C222 1.33(2) . ?
N221 C228 1.34(2) . ?
C222 N223 1.33(2) . ?
N223 C22 1.401(15) . ?
N223 C229 1.52(2) . ?
C224 C229 1.36(2) . ?
C224 C225 1.38(2) . ?
C224 H224 0.95 . ?
C225 C226 1.40(3) . ?
C225 H225 0.95 . ?
C226 C227 1.38(2) . ?
C226 H226 0.95 . ?
C227 C228 1.41(2) . ?
C227 H227 0.95 . ?
C228 C229 1.39(3) . ?
C22 C232 1.556(16) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
C231 C236 1.34(3) . ?
C231 C232 1.38(3) . ?
C231 C23 1.540(16) . ?
C232 C233 1.41(3) . ?
C233 C234 1.46(4) . ?
C233 H233 0.95 . ?
C234 C235 1.34(2) . ?
C234 H234 0.95 . ?
C235 C236 1.36(2) . ?
C235 H235 0.95 . ?
C236 H236 0.95 . ?
C23 N241 1.372(15) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
N241 C242 1.39(2) . ?
N241 C248 1.41(2) . ?
C242 N243 1.32(2) . ?
N243 C249 1.39(2) . ?
N243 C24 1.45(3) . ?
C244 C249 1.34(3) . ?
C244 C245 1.37(3) . ?
C244 H244 0.95 . ?
C245 C246 1.47(2) . ?
C245 H245 0.95 . ?
C246 C247 1.34(2) . ?
C246 H246 0.95 . ?
C247 C248 1.44(2) . ?
C247 H247 0.95 . ?
C248 C249 1.35(3) . ?
C24 C25' 1.50(4) . ?
C24 C25 1.556(19) . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
C24 H24C 0.99 . ?
C24 H24D 0.99 . ?
C25 H25A 0.99 . ?
C25 H25B 0.99 . ?
C25' H25C 0.99 . ?
C25' H25D 0.99 . ?
O101 C101 1.51(5) . ?
O101 H101 0.84 . ?
C101 H10E 0.98 . ?
C101 H10F 0.98 . ?
C101 H10G 0.98 . ?
O201 C201 1.52(3) . ?
O201 H201 0.84 . ?
C201 H20E 0.98 . ?
C201 H20F 0.98 . ?
C201 H20G 0.98 . ?
O301 C301 1.320(17) . ?
O301 H301 0.84 . ?
C301 H30A 0.98 . ?
C301 H30B 0.98 . ?
C301 H30C 0.98 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C122 Au1 C222 176.5(8) . . ?
C122 Au1 Au2 88.8(5) . . ?
C222 Au1 Au2 92.3(5) . . ?
C142 Au2 C242 176.3(7) . . ?
C142 Au2 Au1 93.2(6) . . ?
C242 Au2 Au1 90.5(5) . . ?
C11 C10 C15 112(3) . . ?
C11 C10 H10A 109.2 . . ?
C15 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C15 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C15' C10' C11 108(3) . . ?
C15' C10' H10C 110 . . ?
C11 C10' H10C 110 . . ?
C15' C10' H10D 110 . . ?
C11 C10' H10D 110 . . ?
H10C C10' H10D 108.4 . . ?
N121 C11 C10 114(2) . . ?
N121 C11 C10' 112(2) . . ?
N121 C11 H11A 108.8 . . ?
C10 C11 H11A 108.8 . . ?
N121 C11 H11B 108.8 . . ?
C10 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
N121 C11 H11C 108.6 . . ?
C10' C11 H11C 108.8 . . ?
N121 C11 H11D 108.9 . . ?
C10' C11 H11D 110.1 . . ?
H11C C11 H11D 107.8 . . ?
C122 N121 C128 109.2(13) . . ?
C122 N121 C11 128.0(15) . . ?
C128 N121 C11 122.8(14) . . ?
N123 C122 N121 109.0(14) . . ?
N123 C122 Au1 128.1(12) . . ?
N121 C122 Au1 122.8(12) . . ?
C122 N123 C129 109.7(14) . . ?
C122 N123 C12 121.9(14) . . ?
C129 N123 C12 128.2(14) . . ?
C129 C124 C125 118.4(17) . . ?
C129 C124 H124 120.8 . . ?
C125 C124 H124 120.8 . . ?
C124 C125 C126 120.2(16) . . ?
C124 C125 H125 119.9 . . ?
C126 C125 H125 119.9 . . ?
C127 C126 C125 123.3(16) . . ?
C127 C126 H126 118.3 . . ?
C125 C126 H126 118.3 . . ?
C128 C127 C126 113.6(17) . . ?
C128 C127 H127 123.2 . . ?
C126 C127 H127 123.2 . . ?
C127 C128 C129 126.5(16) . . ?
C127 C128 N121 129.9(16) . . ?
C129 C128 N121 103.5(13) . . ?
N123 C129 C124 133.7(16) . . ?
N123 C129 C128 108.5(14) . . ?
C124 C129 C128 117.8(15) . . ?
N123 C12 C132 115.3(14) . . ?
N123 C12 H12A 108.5 . . ?
C132 C12 H12A 108.5 . . ?
N123 C12 H12B 108.5 . . ?
C132 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C132 C131 C136 121(2) . . ?
C132 C131 C13 119.3(19) . . ?
C136 C131 C13 119(2) . . ?
C133 C132 C131 116(2) . . ?
C133 C132 C12 117(2) . . ?
C131 C132 C12 127.3(18) . . ?
C134 C133 C132 125(3) . . ?
C134 C133 H133 117.5 . . ?
C132 C133 H133 117.5 . . ?
C135 C134 C133 117(3) . . ?
C135 C134 H134 121.5 . . ?
C133 C134 H134 121.5 . . ?
C134 C135 C136 124(2) . . ?
C134 C135 H135 118.1 . . ?
C136 C135 H135 118.1 . . ?
C135 C136 C131 117(3) . . ?
C135 C136 H136 121.6 . . ?
C131 C136 H136 121.6 . . ?
N141 C13 C131 116.5(16) . . ?
N141 C13 H13A 108.2 . . ?
C131 C13 H13A 108.2 . . ?
N141 C13 H13B 108.2 . . ?
C131 C13 H13B 108.2 . . ?
H13A C13 H13B 107.3 . . ?
C148 N141 C142 115.5(18) . . ?
C148 N141 C13 125.2(18) . . ?
C142 N141 C13 119.3(17) . . ?
N141 C142 N143 102.0(17) . . ?
N141 C142 Au2 130.1(16) . . ?
N143 C142 Au2 127.6(16) . . ?
C142 N143 C149 112.7(17) . . ?
C142 N143 C14 123.9(18) . . ?
C149 N143 C14 123.3(16) . . ?
C145 C144 C149 119(2) . . ?
C145 C144 H144 120.4 . . ?
C149 C144 H144 120.4 . . ?
C146 C145 C144 116.4(19) . . ?
C146 C145 H145 121.8 . . ?
C144 C145 H145 121.8 . . ?
C145 C146 C147 127(2) . . ?
C145 C146 H146 116.5 . . ?
C147 C146 H146 116.5 . . ?
C148 C147 C146 118(2) . . ?
C148 C147 H147 120.8 . . ?
C146 C147 H147 120.8 . . ?
N141 C148 C147 139.5(19) . . ?
N141 C148 C149 104.5(17) . . ?
C147 C148 C149 115.4(17) . . ?
N143 C149 C144 131(2) . . ?
N143 C149 C148 105.2(15) . . ?
C144 C149 C148 123(2) . . ?
N143 C14 C15 110(2) . . ?
N143 C14 C15' 110(2) . . ?
N143 C14 H14A 109.7 . . ?
C15 C14 H14A 109.7 . . ?
N143 C14 H14B 109.7 . . ?
C15 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N143 C14 H14C 110.2 . . ?
C15' C14 H14C 107.2 . . ?
N143 C14 H14D 109.5 . . ?
C15' C14 H14D 111.8 . . ?
H14C C14 H14D 108.2 . . ?
C10 C15 C14 110(3) . . ?
C10 C15 H15A 109.7 . . ?
C14 C15 H15A 109.7 . . ?
C10 C15 H15B 109.7 . . ?
C14 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C10' C15' C14 107(3) . . ?
C10' C15' H15C 110.4 . . ?
C14 C15' H15C 110.4 . . ?
C10' C15' H15D 110.4 . . ?
C14 C15' H15D 110.4 . . ?
H15C C15' H15D 108.6 . . ?
C25 C20 C21 111(4) . . ?
C25 C20 H20A 109.4 . . ?
C21 C20 H20A 109.4 . . ?
C25 C20 H20B 109.4 . . ?
C21 C20 H20B 109.4 . . ?
H20A C20 H20B 108 . . ?
C25' C20' C21 115(3) . . ?
C25' C20' H20C 108.6 . . ?
C21 C20' H20C 108.6 . . ?
C25' C20' H20D 108.6 . . ?
C21 C20' H20D 108.6 . . ?
H20C C20' H20D 107.6 . . ?
N221 C21 C20 112(2) . . ?
N221 C21 C20' 110(2) . . ?
N221 C21 H21A 109.2 . . ?
C20 C21 H21A 109.2 . . ?
N221 C21 H21B 109.2 . . ?
C20 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
N221 C21 H21C 110.2 . . ?
C20' C21 H21C 110.9 . . ?
N221 C21 H21D 109.2 . . ?
C20' C21 H21D 108.3 . . ?
H21C C21 H21D 108.2 . . ?
C222 N221 C228 112.8(16) . . ?
C222 N221 C21 121.7(16) . . ?
C228 N221 C21 125.5(15) . . ?
N221 C222 N223 107.8(15) . . ?
N221 C222 Au1 129.9(14) . . ?
N223 C222 Au1 121.9(12) . . ?
C222 N223 C22 128.6(15) . . ?
C222 N223 C229 108.6(14) . . ?
C22 N223 C229 122.6(14) . . ?
C229 C224 C225 113.3(19) . . ?
C229 C224 H224 123.3 . . ?
C225 C224 H224 123.3 . . ?
C224 C225 C226 124.5(19) . . ?
C224 C225 H225 117.7 . . ?
C226 C225 H225 117.7 . . ?
C227 C226 C225 119.8(18) . . ?
C227 C226 H226 120.1 . . ?
C225 C226 H226 120.1 . . ?
C226 C227 C228 117.8(19) . . ?
C226 C227 H227 121.1 . . ?
C228 C227 H227 121.1 . . ?
N221 C228 C229 109.3(15) . . ?
N221 C228 C227 132.2(19) . . ?
C229 C228 C227 118.4(17) . . ?
C224 C229 C228 126.0(17) . . ?
C224 C229 N223 132.5(16) . . ?
C228 C229 N223 101.3(14) . . ?
N223 C22 C232 122.8(14) . . ?
N223 C22 H22A 106.6 . . ?
C232 C22 H22A 106.6 . . ?
N223 C22 H22B 106.6 . . ?
C232 C22 H22B 106.6 . . ?
H22A C22 H22B 106.6 . . ?
C236 C231 C232 120(2) . . ?
C236 C231 C23 115(2) . . ?
C232 C231 C23 124.7(18) . . ?
C231 C232 C233 120(2) . . ?
C231 C232 C22 118.9(19) . . ?
C233 C232 C22 121(2) . . ?
C232 C233 C234 116(3) . . ?
C232 C233 H233 121.8 . . ?
C234 C233 H233 121.8 . . ?
C235 C234 C233 121(3) . . ?
C235 C234 H234 119.5 . . ?
C233 C234 H234 119.5 . . ?
C234 C235 C236 119(3) . . ?
C234 C235 H235 120.3 . . ?
C236 C235 H235 120.3 . . ?
C231 C236 C235 123(3) . . ?
C231 C236 H236 118.6 . . ?
C235 C236 H236 118.6 . . ?
N241 C23 C231 113.8(14) . . ?
N241 C23 H23A 108.8 . . ?
C231 C23 H23A 108.8 . . ?
N241 C23 H23B 108.8 . . ?
C231 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C23 N241 C242 123.5(15) . . ?
C23 N241 C248 133.8(16) . . ?
C242 N241 C248 101.5(15) . . ?
N243 C242 N241 112.5(16) . . ?
N243 C242 Au2 125.5(13) . . ?
N241 C242 Au2 122.0(13) . . ?
C242 N243 C249 107.7(16) . . ?
C242 N243 C24 126.8(17) . . ?
C249 N243 C24 125.4(17) . . ?
C249 C244 C245 119(2) . . ?
C249 C244 H244 120.5 . . ?
C245 C244 H244 120.5 . . ?
C244 C245 C246 121.2(18) . . ?
C244 C245 H245 119.4 . . ?
C246 C245 H245 119.4 . . ?
C247 C246 C245 118.1(18) . . ?
C247 C246 H246 121 . . ?
C245 C246 H246 121 . . ?
C246 C247 C248 117.9(19) . . ?
C246 C247 H247 121 . . ?
C248 C247 H247 121 . . ?
C249 C248 N241 111.0(17) . . ?
C249 C248 C247 122.4(18) . . ?
N241 C248 C247 126.3(18) . . ?
C244 C249 C248 121(2) . . ?
C244 C249 N243 132(2) . . ?
C248 C249 N243 106.6(17) . . ?
N243 C24 C25' 116(2) . . ?
N243 C24 C25 108(2) . . ?
N243 C24 H24A 110.1 . . ?
C25 C24 H24A 110.1 . . ?
N243 C24 H24B 110.1 . . ?
C25 C24 H24B 110.1 . . ?
H24A C24 H24B 108.4 . . ?
N243 C24 H24C 107.9 . . ?
C25' C24 H24C 108.5 . . ?
N243 C24 H24D 108.7 . . ?
C25' C24 H24D 108.2 . . ?
H24C C24 H24D 107.6 . . ?
C20 C25 C24 113(4) . . ?
C20 C25 H25A 108.9 . . ?
C24 C25 H25A 108.9 . . ?
C20 C25 H25B 108.9 . . ?
C24 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
C24 C25' C20' 110(3) . . ?
C24 C25' H25C 109.7 . . ?
C20' C25' H25C 109.7 . . ?
C24 C25' H25D 109.7 . . ?
C20' C25' H25D 109.7 . . ?
H25C C25' H25D 108.2 . . ?
C101 O101 H101 109.5 . . ?
O101 C101 H10E 109.5 . . ?
O101 C101 H10F 109.5 . . ?
H10E C101 H10F 109.5 . . ?
O101 C101 H10G 109.5 . . ?
H10E C101 H10G 109.5 . . ?
H10F C101 H10G 109.5 . . ?
C201 O201 H201 109.5 . . ?
O201 C201 H20E 109.5 . . ?
O201 C201 H20F 109.5 . . ?
H20E C201 H20F 109.5 . . ?
O201 C201 H20G 109.5 . . ?
H20E C201 H20G 109.5 . . ?
H20F C201 H20G 109.5 . . ?
C301 O301 H301 109.5 . . ?
O301 C301 H30A 109.5 . . ?
O301 C301 H30B 109.5 . . ?
H30A C301 H30B 109.5 . . ?
O301 C301 H30C 109.5 . . ?
H30A C301 H30C 109.5 . . ?
H30B C301 H30C 109.5 . . ?

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
O101 H101 Br1 0.84 2.24 3.07(3) 174.8 .
O201 H201 Br4 0.84 2.15 2.982(16) 172.7 .
O201 H201 Br3 0.84 2.1 2.831(18) 144.9 .
O301 H301 Br1 0.84 2.34 3.167(17) 169 .

#===END
