# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_25d
_audit_block_doi                 10.5517/cc1j5plz
_database_code_depnum_ccdc_archive 'CCDC 1405651'
_audit_update_record             
;
2015-09-08 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'[1, 5-bis(1-methylimidazolium)pentane]- [PbBr3]2'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6.50 H11 Br3 N2 Pb'
_chemical_formula_weight         564.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+3/4, -y+5/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+5/4, -y+3/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+5/4, -y+5/4, z+1/4'

_cell_length_a                   29.498(4)
_cell_length_b                   22.319(3)
_cell_length_c                   7.7732(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5117.6(11)
_cell_formula_units_Z            16
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4510
_cell_measurement_theta_min      2.2885
_cell_measurement_theta_max      27.2647

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.929
_exptl_crystal_F_000             4016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    22.517
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.045
_exptl_absorpt_correction_T_max  0.099
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9313
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.289
_diffrn_reflns_theta_max         25.494
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_point_group_measured_fraction_full 0.953
_reflns_number_total             2275
_reflns_number_gt                1741
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_max     0.896
_reflns_Friedel_fraction_full    0.900

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0340P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00069(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 617 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2275
_refine_ls_number_parameters     126
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0778
_refine_ls_wR_factor_gt          0.0728
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb -0.00031(2) -0.25021(2) 0.2358(4) 0.0401(2) Uani 1 1 d . . . . .
Br1 Br 0.07426(5) -0.21053(6) 0.45759(14) 0.0496(4) Uani 1 1 d . . . . .
Br2 Br 0.05921(5) -0.31867(7) 0.00581(17) 0.0627(5) Uani 1 1 d . . . . .
Br3 Br 0.01184(5) -0.14819(6) -0.0144(2) 0.0600(4) Uani 1 1 d . . . . .
N1 N 0.0831(5) -0.4986(5) 0.797(2) 0.065(4) Uani 1 1 d . . . . .
N2 N 0.1013(4) -0.4238(5) 0.6346(14) 0.054(3) Uani 1 1 d . . . . .
C1 C 0.0000 -0.5000 1.026(8) 0.18(2) Uani 1 2 d S T P . .
H1A H -0.0052 -0.5337 0.9497 0.221 Uiso 0.5 1 calc R U P A 1
H1B H 0.0052 -0.4663 0.9497 0.221 Uiso 0.5 1 calc R U P A 1
C2 C 0.0418(12) -0.5113(15) 1.082(4) 0.076(12) Uani 0.66(5) 1 d . . P B 1
H2A H 0.0395 -0.5400 1.1757 0.091 Uiso 0.66(5) 1 calc R U P B 1
H2B H 0.0539 -0.4745 1.1304 0.091 Uiso 0.66(5) 1 calc R U P B 1
C2' C 0.025(2) -0.544(2) 0.972(8) 0.07(2) Uani 0.34(5) 1 d . . P B 2
H2'1 H 0.0130 -0.5562 0.8611 0.082 Uiso 0.34(5) 1 calc R U P B 2
H2'2 H 0.0204 -0.5771 1.0501 0.082 Uiso 0.34(5) 1 calc R U P B 2
C3 C 0.0772(6) -0.5361(7) 0.949(3) 0.096(7) Uani 1 1 d . . . . .
H3A H 0.1063 -0.5403 1.0064 0.115 Uiso 1 1 calc R U . B 1
H3B H 0.0677 -0.5758 0.9129 0.115 Uiso 1 1 calc R U . B 1
C4 C 0.1041(5) -0.4465(6) 0.7942(18) 0.049(3) Uani 1 1 d . . . . .
H4 H 0.1184 -0.4285 0.8873 0.058 Uiso 1 1 calc R U . . .
C5 C 0.0774(6) -0.4632(8) 0.537(2) 0.079(5) Uani 1 1 d . . . . .
H5 H 0.0700 -0.4586 0.4212 0.094 Uiso 1 1 calc R U . . .
C6 C 0.0670(7) -0.5083(7) 0.633(3) 0.071(6) Uani 1 1 d . . . . .
H6 H 0.0510 -0.5421 0.5978 0.085 Uiso 1 1 calc R U . . .
C7 C 0.1196(5) -0.3664(6) 0.581(2) 0.072(5) Uani 1 1 d . . . . .
H7A H 0.1435 -0.3727 0.4990 0.107 Uiso 1 1 calc R U . . .
H7B H 0.1313 -0.3454 0.6790 0.107 Uiso 1 1 calc R U . . .
H7C H 0.0960 -0.3430 0.5285 0.107 Uiso 1 1 calc R U . . .


_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
Pb1 Br1 2.932(2) . ?
Pb1 Br2 2.935(3) . ?
Pb1 Br3 3.005(3) 6_545 ?
Pb1 Br3 3.016(3) . ?
Pb1 Br2 3.128(3) 6_545 ?
Pb1 Br1 3.194(3) 6_544 ?
Br1 Pb1 3.194(3) 6_545 ?
Br2 Pb1 3.128(3) 6_544 ?
Br3 Pb1 3.005(3) 6_544 ?
N1 C4 1.317(17) . ?
N1 C6 1.38(2) . ?
N1 C3 1.46(2) . ?
N2 C4 1.342(17) . ?
N2 C5 1.360(19) . ?
N2 C7 1.453(18) . ?
C1 C2' 1.30(5) . ?
C1 C2' 1.30(5) 2_545 ?
C1 C2 1.33(4) . ?
C1 C2 1.33(4) 2_545 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.57(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2' C3 1.56(6) . ?
C2' H2'1 0.9700 . ?
C2' H2'2 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4 0.9300 . ?
C5 C6 1.29(2) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?

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
Br1 Pb1 Br2 93.82(4) . . ?
Br1 Pb1 Br3 86.15(9) . 6_545 ?
Br2 Pb1 Br3 93.93(4) . 6_545 ?
Br1 Pb1 Br3 93.55(4) . . ?
Br2 Pb1 Br3 85.93(9) . . ?
Br3 Pb1 Br3 179.66(5) 6_545 . ?
Br1 Pb1 Br2 82.75(8) . 6_545 ?
Br2 Pb1 Br2 175.38(11) . 6_545 ?
Br3 Pb1 Br2 82.79(9) 6_545 6_545 ?
Br3 Pb1 Br2 97.33(4) . 6_545 ?
Br1 Pb1 Br1 173.40(10) . 6_544 ?
Br2 Pb1 Br1 81.56(8) . 6_544 ?
Br3 Pb1 Br1 98.82(4) 6_545 6_544 ?
Br3 Pb1 Br1 81.47(8) . 6_544 ?
Br2 Pb1 Br1 102.11(4) 6_545 6_544 ?
Pb1 Br1 Pb1 78.63(3) . 6_545 ?
Pb1 Br2 Pb1 79.66(4) . 6_544 ?
Pb1 Br3 Pb1 80.42(4) 6_544 . ?
C4 N1 C6 106.6(13) . . ?
C4 N1 C3 125.2(15) . . ?
C6 N1 C3 128.2(14) . . ?
C4 N2 C5 107.8(13) . . ?
C4 N2 C7 125.2(12) . . ?
C5 N2 C7 127.0(13) . . ?
C2' C1 C2' 142(7) . 2_545 ?
C2 C1 C2 142(6) . 2_545 ?
C2 C1 H1A 101.6 . . ?
C2 C1 H1A 101.6 2_545 . ?
C2 C1 H1B 101.6 . . ?
C2 C1 H1B 101.6 2_545 . ?
H1A C1 H1B 104.6 . . ?
C1 C2 C3 118(4) . . ?
C1 C2 H2A 107.9 . . ?
C3 C2 H2A 107.9 . . ?
C1 C2 H2B 107.9 . . ?
C3 C2 H2B 107.9 . . ?
H2A C2 H2B 107.2 . . ?
C1 C2' C3 121(5) . . ?
C1 C2' H2'1 107.1 . . ?
C3 C2' H2'1 107.1 . . ?
C1 C2' H2'2 107.1 . . ?
C3 C2' H2'2 107.1 . . ?
H2'1 C2' H2'2 106.8 . . ?
N1 C3 C2' 106(2) . . ?
N1 C3 C2 114.2(16) . . ?
N1 C3 H3A 108.7 . . ?
C2 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
C2 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
N1 C4 N2 108.7(13) . . ?
N1 C4 H4 125.7 . . ?
N2 C4 H4 125.7 . . ?
C6 C5 N2 107.5(17) . . ?
C6 C5 H5 126.2 . . ?
N2 C5 H5 126.2 . . ?
C5 C6 N1 109.4(15) . . ?
C5 C6 H6 125.3 . . ?
N1 C6 H6 125.3 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_refine_diff_density_max         1.000
_refine_diff_density_min         -1.750
_refine_diff_density_rms         0.231

####################################################################### 
# 
# 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_100d
_audit_block_doi                 10.5517/cc1jd839
_database_code_depnum_ccdc_archive 'CCDC 1411960'
_audit_update_record             
;
2015-09-08 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'[1, 5-bis(1-methylimidazolium)pentane]- [PbBr3]2'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6.50 H11 Br3 N2 Pb'
_chemical_formula_weight         564.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+3/4, -y+5/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+5/4, -y+3/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+5/4, -y+5/4, z+1/4'

_cell_length_a                   29.787(5)
_cell_length_b                   22.327(4)
_cell_length_c                   7.8007(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5187.9(16)
_cell_formula_units_Z            16
_cell_measurement_temperature    373(2)
_cell_measurement_reflns_used    3397
_cell_measurement_theta_min      2.2825
_cell_measurement_theta_max      24.1241

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.889
_exptl_crystal_F_000             4016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    22.212
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.047
_exptl_absorpt_correction_T_max  0.101
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      373(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9463
_diffrn_reflns_av_unetI/netI     0.0868
_diffrn_reflns_av_R_equivalents  0.1070
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.280
_diffrn_reflns_theta_max         25.486
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             2375
_reflns_number_gt                1521
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_max     0.957
_reflns_Friedel_fraction_full    0.958

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0830P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00079(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 527 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2375
_refine_ls_number_parameters     116
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1579
_refine_ls_wR_factor_gt          0.1355
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.25008(3) 0.50037(4) 0.7623(7) 0.0559(4) Uani 1 1 d . . . . .
Br1 Br 0.17643(8) 0.46072(13) 0.5421(3) 0.0681(9) Uani 1 1 d . . . . .
Br2 Br 0.19082(9) 0.56827(14) 0.9948(4) 0.0836(10) Uani 1 1 d . . . . .
Br3 Br 0.23832(11) 0.39772(13) 1.0154(4) 0.0827(9) Uani 1 1 d . . . . .
N1 N 0.1668(8) 0.7496(9) 0.204(4) 0.082(8) Uani 1 1 d . . . . .
N2 N 0.1482(7) 0.6735(10) 0.366(3) 0.066(6) Uani 1 1 d . . . . .
C1 C 0.2500 0.7500 -0.003(14) 0.21(4) Uani 1 2 d S T P . .
H1A H 0.2618 0.7804 0.0735 0.250 Uiso 0.5 1 calc R U P . .
H1B H 0.2382 0.7196 0.0736 0.250 Uiso 0.5 1 calc R U P . .
C2 C 0.214(2) 0.775(3) -0.049(10) 0.37(7) Uani 1 1 d . . . . .
H2A H 0.2040 0.7518 -0.1471 0.447 Uiso 1 1 calc R U . . .
H2B H 0.2233 0.8134 -0.0946 0.447 Uiso 1 1 calc R U . . .
C3 C 0.1725(12) 0.7880(15) 0.049(6) 0.116(13) Uani 1 1 d . . . . .
H3A H 0.1468 0.7824 -0.0260 0.139 Uiso 1 1 calc R U . . .
H3B H 0.1729 0.8297 0.0840 0.139 Uiso 1 1 calc R U . . .
C4 C 0.1464(9) 0.6981(11) 0.208(4) 0.067(7) Uani 1 1 d . . . . .
H4 H 0.1322 0.6805 0.1147 0.081 Uiso 1 1 calc R U . . .
C5 C 0.1719(11) 0.7135(19) 0.462(5) 0.102(11) Uani 1 1 d . . . . .
H5 H 0.1792 0.7094 0.5779 0.122 Uiso 1 1 calc R U . . .
C6 C 0.1828(11) 0.7591(15) 0.363(5) 0.088(11) Uani 1 1 d . . . . .
H6 H 0.1990 0.7926 0.3974 0.105 Uiso 1 1 calc R U . . .
C7 C 0.1294(10) 0.6164(13) 0.420(4) 0.101(11) Uani 1 1 d . . . . .
H7A H 0.1024 0.6232 0.4842 0.151 Uiso 1 1 calc R U . . .
H7B H 0.1508 0.5957 0.4907 0.151 Uiso 1 1 calc R U . . .
H7C H 0.1227 0.5926 0.3210 0.151 Uiso 1 1 calc R U . . .


_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
Pb1 Br1 2.924(4) . ?
Pb1 Br2 2.950(4) . ?
Pb1 Br3 3.001(5) 10_564 ?
Pb1 Br3 3.045(5) . ?
Pb1 Br2 3.131(5) 10_564 ?
Pb1 Br1 3.211(4) 10_565 ?
Br1 Pb1 3.211(4) 10_564 ?
Br2 Pb1 3.131(5) 10_565 ?
Br3 Pb1 3.001(5) 10_565 ?
N1 C4 1.30(3) . ?
N1 C6 1.35(4) . ?
N1 C3 1.49(4) . ?
N2 C4 1.35(3) . ?
N2 C5 1.37(4) . ?
N2 C7 1.45(4) . ?
C1 C2 1.26(7) 14_565 ?
C1 C2 1.26(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.48(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4 0.9300 . ?
C5 C6 1.32(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?

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
Br1 Pb1 Br2 93.89(7) . . ?
Br1 Pb1 Br3 86.49(14) . 10_564 ?
Br2 Pb1 Br3 94.24(9) . 10_564 ?
Br1 Pb1 Br3 93.82(8) . . ?
Br2 Pb1 Br3 85.38(15) . . ?
Br3 Pb1 Br3 179.52(19) 10_564 . ?
Br1 Pb1 Br2 83.23(14) . 10_564 ?
Br2 Pb1 Br2 176.12(18) . 10_564 ?
Br3 Pb1 Br2 83.02(14) 10_564 10_564 ?
Br3 Pb1 Br2 97.38(9) . 10_564 ?
Br1 Pb1 Br1 173.17(17) . 10_565 ?
Br2 Pb1 Br1 81.44(13) . 10_565 ?
Br3 Pb1 Br1 98.78(8) 10_564 10_565 ?
Br3 Pb1 Br1 80.88(14) . 10_565 ?
Br2 Pb1 Br1 101.66(7) 10_564 10_565 ?
Pb1 Br1 Pb1 78.81(6) . 10_564 ?
Pb1 Br2 Pb1 79.73(7) . 10_565 ?
Pb1 Br3 Pb1 80.34(7) 10_565 . ?
C4 N1 C6 106(3) . . ?
C4 N1 C3 126(3) . . ?
C6 N1 C3 128(3) . . ?
C4 N2 C5 105(3) . . ?
C4 N2 C7 127(2) . . ?
C5 N2 C7 128(3) . . ?
C2 C1 C2 147(10) 14_565 . ?
C2 C1 H1A 100.1 14_565 . ?
C2 C1 H1A 100.1 . . ?
C2 C1 H1B 100.1 14_565 . ?
C2 C1 H1B 100.1 . . ?
H1A C1 H1B 104.2 . . ?
C1 C2 C3 131(8) . . ?
C1 C2 H2A 104.6 . . ?
C3 C2 H2A 104.6 . . ?
C1 C2 H2B 104.6 . . ?
C3 C2 H2B 104.6 . . ?
H2A C2 H2B 105.7 . . ?
C2 C3 N1 113(3) . . ?
C2 C3 H3A 108.9 . . ?
N1 C3 H3A 108.9 . . ?
C2 C3 H3B 108.9 . . ?
N1 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
N1 C4 N2 112(3) . . ?
N1 C4 H4 124.2 . . ?
N2 C4 H4 124.2 . . ?
C6 C5 N2 108(3) . . ?
C6 C5 H5 126.0 . . ?
N2 C5 H5 126.0 . . ?
C5 C6 N1 109(3) . . ?
C5 C6 H6 125.3 . . ?
N1 C6 H6 125.3 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_refine_diff_density_max         1.732
_refine_diff_density_min         -1.940
_refine_diff_density_rms         0.277

####################################################################### 
# 
# 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_140d
_audit_block_doi                 10.5517/cc1jd88g
_database_code_depnum_ccdc_archive 'CCDC 1411965'
_audit_update_record             
;
2015-09-08 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'[1, 5-bis(1-methylimidazolium)pentane]- [PbBr3]2'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6.50 H11 Br3 N2 Pb'
_chemical_formula_weight         564.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+3/4, -y+5/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+5/4, -y+3/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+5/4, -y+5/4, z+1/4'

_cell_length_a                   29.942(5)
_cell_length_b                   22.309(4)
_cell_length_c                   7.8155(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5220.6(14)
_cell_formula_units_Z            16
_cell_measurement_temperature    413(2)
_cell_measurement_reflns_used    3630
_cell_measurement_theta_min      2.2793
_cell_measurement_theta_max      24.4849

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.871
_exptl_crystal_F_000             4016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    22.073
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.047
_exptl_absorpt_correction_T_max  0.102
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      413(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9453
_diffrn_reflns_av_unetI/netI     0.0847
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.277
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             2390
_reflns_number_gt                1501
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_max     0.949
_reflns_Friedel_fraction_full    0.951

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0919P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00091(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 524 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2390
_refine_ls_number_parameters     116
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1681
_refine_ls_wR_factor_gt          0.1436
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.24994(3) 0.50046(4) 0.7635(10) 0.0629(5) Uani 1 1 d . . . . .
Br1 Br 0.17675(8) 0.46089(13) 0.5418(3) 0.0776(9) Uani 1 1 d . . . . .
Br2 Br 0.19100(9) 0.56804(14) 0.9952(4) 0.0935(11) Uani 1 1 d . . . . .
Br3 Br 0.23836(11) 0.39757(14) 1.0159(4) 0.0931(10) Uani 1 1 d . . . . .
N1 N 0.1677(9) 0.7498(9) 0.198(4) 0.092(9) Uani 1 1 d . . . . .
N2 N 0.1478(7) 0.6746(11) 0.360(3) 0.077(6) Uani 1 1 d . . . . .
C1 C 0.2500 0.7500 -0.012(18) 0.27(7) Uani 1 2 d S T P . .
H1A H 0.2618 0.7804 0.0646 0.325 Uiso 0.5 1 calc R U P . .
H1B H 0.2382 0.7196 0.0646 0.325 Uiso 0.5 1 calc R U P . .
C2 C 0.215(3) 0.774(3) -0.054(10) 0.31(6) Uani 1 1 d . . . . .
H2A H 0.2051 0.7515 -0.1527 0.366 Uiso 1 1 calc R U . . .
H2B H 0.2244 0.8129 -0.0991 0.366 Uiso 1 1 calc R U . . .
C3 C 0.1729(13) 0.7873(14) 0.048(6) 0.137(16) Uani 1 1 d . . . . .
H3A H 0.1733 0.8290 0.0836 0.164 Uiso 1 1 calc R U . . .
H3B H 0.1472 0.7817 -0.0258 0.164 Uiso 1 1 calc R U . . .
C4 C 0.1470(9) 0.6993(13) 0.206(4) 0.078(7) Uani 1 1 d . . . . .
H4 H 0.1329 0.6818 0.1130 0.094 Uiso 1 1 calc R U . . .
C5 C 0.1715(12) 0.715(2) 0.456(5) 0.126(15) Uani 1 1 d . . . . .
H5 H 0.1784 0.7099 0.5707 0.151 Uiso 1 1 calc R U . . .
C6 C 0.1828(13) 0.7596(16) 0.364(6) 0.106(12) Uani 1 1 d . . . . .
H6 H 0.1984 0.7931 0.4015 0.127 Uiso 1 1 calc R U . . .
C7 C 0.1299(11) 0.6179(14) 0.419(5) 0.122(13) Uani 1 1 d . . . . .
H7A H 0.1075 0.6250 0.5041 0.183 Uiso 1 1 calc R U . . .
H7B H 0.1535 0.5941 0.4668 0.183 Uiso 1 1 calc R U . . .
H7C H 0.1168 0.5969 0.3238 0.183 Uiso 1 1 calc R U . . .


_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
Pb1 Br1 2.930(5) . ?
Pb1 Br2 2.944(6) . ?
Pb1 Br3 3.007(6) 10_564 ?
Pb1 Br3 3.046(6) . ?
Pb1 Br2 3.140(6) 10_564 ?
Pb1 Br1 3.208(6) 10_565 ?
Br1 Pb1 3.208(6) 10_564 ?
Br2 Pb1 3.140(6) 10_565 ?
Br3 Pb1 3.007(6) 10_565 ?
N1 C4 1.29(3) . ?
N1 C6 1.39(5) . ?
N1 C3 1.45(5) . ?
N2 C4 1.32(3) . ?
N2 C5 1.36(4) . ?
N2 C7 1.45(4) . ?
C1 C2 1.22(8) 14_565 ?
C1 C2 1.22(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.53(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4 0.9300 . ?
C5 C6 1.28(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?

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
Br1 Pb1 Br2 93.99(8) . . ?
Br1 Pb1 Br3 86.2(2) . 10_564 ?
Br2 Pb1 Br3 94.49(9) . 10_564 ?
Br1 Pb1 Br3 94.06(8) . . ?
Br2 Pb1 Br3 85.4(2) . . ?
Br3 Pb1 Br3 179.7(2) 10_564 . ?
Br1 Pb1 Br2 83.09(19) . 10_564 ?
Br2 Pb1 Br2 176.0(2) . 10_564 ?
Br3 Pb1 Br2 82.69(19) 10_564 10_564 ?
Br3 Pb1 Br2 97.46(9) . 10_564 ?
Br1 Pb1 Br1 173.6(2) . 10_565 ?
Br2 Pb1 Br1 81.69(18) . 10_565 ?
Br3 Pb1 Br1 98.81(8) 10_564 10_565 ?
Br3 Pb1 Br1 80.88(19) . 10_565 ?
Br2 Pb1 Br1 101.44(7) 10_564 10_565 ?
Pb1 Br1 Pb1 78.94(6) . 10_564 ?
Pb1 Br2 Pb1 79.86(7) . 10_565 ?
Pb1 Br3 Pb1 80.41(7) 10_565 . ?
C4 N1 C6 104(3) . . ?
C4 N1 C3 127(3) . . ?
C6 N1 C3 129(3) . . ?
C4 N2 C5 104(3) . . ?
C4 N2 C7 130(3) . . ?
C5 N2 C7 126(3) . . ?
C2 C1 C2 148(10) 14_565 . ?
C2 C1 H1A 99.7 14_565 . ?
C2 C1 H1A 99.7 . . ?
C2 C1 H1B 99.7 14_565 . ?
C2 C1 H1B 99.7 . . ?
H1A C1 H1B 104.1 . . ?
C1 C2 C3 130(9) . . ?
C1 C2 H2A 104.6 . . ?
C3 C2 H2A 104.6 . . ?
C1 C2 H2B 104.6 . . ?
C3 C2 H2B 104.6 . . ?
H2A C2 H2B 105.7 . . ?
N1 C3 C2 114(3) . . ?
N1 C3 H3A 108.8 . . ?
C2 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
N1 C4 N2 114(3) . . ?
N1 C4 H4 123.2 . . ?
N2 C4 H4 123.2 . . ?
C6 C5 N2 110(4) . . ?
C6 C5 H5 124.9 . . ?
N2 C5 H5 124.9 . . ?
C5 C6 N1 108(3) . . ?
C5 C6 H6 125.9 . . ?
N1 C6 H6 125.9 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_refine_diff_density_max         1.733
_refine_diff_density_min         -1.880
_refine_diff_density_rms         0.303

