# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

####################################################################### 
# 
# 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_structure4
_database_code_depnum_ccdc_archive 'CCDC 1589788'
_audit_update_record             
;
2017-12-07 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;
_audit_creation_date             2017-09-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '(C24 H36 Br2 Cu N12 O8), 2(H2O)'
_chemical_formula_sum            'C24 H40 Br2 Cu N12 O10'
_chemical_formula_weight         880.04
_chemical_melting_point          ?
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.5931(19)
_cell_length_b                   9.5094(19)
_cell_length_c                   13.177(3)
_cell_angle_alpha                103.046(8)
_cell_angle_beta                 106.647(9)
_cell_angle_gamma                94.822(8)
_cell_volume                     876.7(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    997
_cell_measurement_temperature    200
_cell_measurement_theta_max      20.83
_cell_measurement_theta_min      2.80
_shelx_estimated_absorpt_T_max   0.985
_shelx_estimated_absorpt_T_min   0.756
_exptl_absorpt_coefficient_mu    2.970
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0696 before and 0.0588 after correction. The Ratio of minimum to maximum transmission is 0.8571. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'greenish yellow'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             447
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_unetI/netI     0.1200
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8450
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.227
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1918
_reflns_number_total             3083
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3083
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0480
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0238P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0885
_refine_special_details          
;
Hydrogen atoms of water molecules were not localized.
;
# start Validation Reply Form
_vrf_PLAT306_ab11                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1 Check
RESPONSE: O-atom of water molecule with non-localized H-atoms
;
# end Validation Reply Form
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 N12(H12), C11(H11), N22(H22), C21(H21)
2.c X=CH2 refined with riding coordinates:
 N13(H13A,H13B), N23(H23A,H23B)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Br1 Br 0.17123(8) 0.33578(6) 1.02405(5) 0.02962(19) Uani 1 1 d . . . . .
Cu1 Cu 0.5000 0.5000 1.0000 0.0237(3) Uani 1 2 d S T P . .
O11 O 0.0427(6) 0.6853(4) 0.5581(3) 0.0461(12) Uani 1 1 d . . . . .
O12 O 0.3431(5) 0.6553(4) 0.5788(3) 0.0354(10) Uani 1 1 d . . . . .
N11 N 0.3326(6) 0.5315(4) 0.8606(4) 0.0218(11) Uani 1 1 d . . . . .
N12 N 0.1512(6) 0.5518(4) 0.8487(4) 0.0275(12) Uani 1 1 d . . . . .
H12 H 0.0935 0.5400 0.8960 0.033 Uiso 1 1 calc R . . . .
N13 N -0.1048(6) 0.6160(5) 0.7247(4) 0.0420(14) Uani 1 1 d . . . . .
H13A H -0.1767 0.6058 0.7652 0.050 Uiso 1 1 calc R . . . .
H13B H -0.1487 0.6419 0.6633 0.050 Uiso 1 1 calc R . . . .
C11 C 0.3640(7) 0.5587(5) 0.7727(4) 0.0234(13) Uani 1 1 d . . . . .
H11 H 0.4791 0.5533 0.7581 0.028 Uiso 1 1 calc R . . . .
C12 C 0.2081(7) 0.5964(5) 0.7037(4) 0.0218(13) Uani 1 1 d . . . . .
C13 C 0.0722(8) 0.5918(5) 0.7564(5) 0.0250(13) Uani 1 1 d . . . . .
C14 C 0.1831(9) 0.6476(6) 0.6057(5) 0.0309(15) Uani 1 1 d . . . . .
C15 C 0.3343(9) 0.7178(7) 0.4866(5) 0.0477(18) Uani 1 1 d . . . . .
H15A H 0.2289 0.6629 0.4217 0.057 Uiso 1 1 calc R . . . .
H15B H 0.3155 0.8211 0.5054 0.057 Uiso 1 1 calc R . . . .
C16 C 0.5084(9) 0.7087(8) 0.4625(5) 0.067(2) Uani 1 1 d . . . . .
H16A H 0.5057 0.7503 0.4005 0.101 Uiso 1 1 calc GR . . . .
H16B H 0.5253 0.6061 0.4436 0.101 Uiso 1 1 calc GR . . . .
H16C H 0.6117 0.7637 0.5270 0.101 Uiso 1 1 calc GR . . . .
O21 O 0.7513(6) -0.0886(4) 0.7441(4) 0.0542(14) Uani 1 1 d . . . . .
O22 O 0.8740(5) 0.1232(3) 0.7260(3) 0.0320(10) Uani 1 1 d . . . . .
N21 N 0.5524(6) 0.3118(4) 0.9140(4) 0.0235(11) Uani 1 1 d . . . . .
N22 N 0.4645(6) 0.1801(4) 0.9146(4) 0.0245(11) Uani 1 1 d . . . . .
H22 H 0.3793 0.1702 0.9469 0.029 Uiso 1 1 calc R . . . .
N23 N 0.4586(6) -0.0718(4) 0.8473(4) 0.0441(15) Uani 1 1 d . . . . .
H23A H 0.3717 -0.0929 0.8760 0.053 Uiso 1 1 calc R . . . .
H23B H 0.5017 -0.1426 0.8106 0.053 Uiso 1 1 calc R . . . .
C21 C 0.6678(7) 0.2794(5) 0.8575(4) 0.0237(13) Uani 1 1 d . . . . .
H21 H 0.7487 0.3498 0.8441 0.028 Uiso 1 1 calc R . . . .
C22 C 0.6561(7) 0.1274(5) 0.8197(4) 0.0200(13) Uani 1 1 d . . . . .
C23 C 0.5254(7) 0.0680(5) 0.8594(4) 0.0225(13) Uani 1 1 d . . . . .
C24 C 0.7616(8) 0.0423(6) 0.7591(5) 0.0276(14) Uani 1 1 d . . . . .
C25 C 0.9959(8) 0.0454(6) 0.6742(5) 0.0427(17) Uani 1 1 d . . . . .
H25A H 0.9217 -0.0213 0.6023 0.051 Uiso 1 1 calc R . . . .
H25B H 1.0632 -0.0134 0.7211 0.051 Uiso 1 1 calc R . . . .
C26 C 1.1319(8) 0.1562(6) 0.6587(5) 0.0424(17) Uani 1 1 d . . . . .
H26A H 1.0646 0.2093 0.6082 0.064 Uiso 1 1 calc GR . . . .
H26B H 1.2204 0.1063 0.6282 0.064 Uiso 1 1 calc GR . . . .
H26C H 1.1995 0.2252 0.7297 0.064 Uiso 1 1 calc GR . . . .
O1 O 0.1318(6) -0.0754(5) 0.9262(4) 0.0591(13) Uani 1 1 d . . . . .


_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
Cu1 N11 2.014(4) . ?
Cu1 N11 2.014(4) 2_667 ?
Cu1 N21 2.027(4) . ?
Cu1 N21 2.027(4) 2_667 ?
O11 C14 1.200(6) . ?
O12 C14 1.360(6) . ?
O12 C15 1.457(6) . ?
N11 N12 1.376(5) . ?
N11 C11 1.322(6) . ?
N12 H12 0.8800 . ?
N12 C13 1.346(6) . ?
N13 H13A 0.8800 . ?
N13 H13B 0.8800 . ?
N13 C13 1.344(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.399(7) . ?
C12 C13 1.403(7) . ?
C12 C14 1.448(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.450(8) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O21 C24 1.207(5) . ?
O22 C24 1.329(6) . ?
O22 C25 1.455(6) . ?
N21 N22 1.372(5) . ?
N21 C21 1.316(6) . ?
N22 H22 0.8800 . ?
N22 C23 1.343(6) . ?
N23 H23A 0.8800 . ?
N23 H23B 0.8800 . ?
N23 C23 1.340(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.405(6) . ?
C22 C23 1.384(6) . ?
C22 C24 1.456(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.501(7) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?

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
N11 Cu1 N11 180.0(2) . 2_667 ?
N11 Cu1 N21 89.58(16) 2_667 . ?
N11 Cu1 N21 90.42(16) 2_667 2_667 ?
N11 Cu1 N21 90.42(17) . . ?
N11 Cu1 N21 89.58(16) . 2_667 ?
N21 Cu1 N21 180.0 . 2_667 ?
C14 O12 C15 114.4(4) . . ?
N12 N11 Cu1 121.8(3) . . ?
C11 N11 Cu1 132.9(4) . . ?
C11 N11 N12 104.6(4) . . ?
N11 N12 H12 123.8 . . ?
C13 N12 N11 112.3(4) . . ?
C13 N12 H12 123.8 . . ?
H13A N13 H13B 120.0 . . ?
C13 N13 H13A 120.0 . . ?
C13 N13 H13B 120.0 . . ?
N11 C11 H11 123.9 . . ?
N11 C11 C12 112.2(4) . . ?
C12 C11 H11 123.9 . . ?
C11 C12 C13 104.8(5) . . ?
C11 C12 C14 131.6(5) . . ?
C13 C12 C14 123.2(5) . . ?
N12 C13 C12 106.1(5) . . ?
N13 C13 N12 124.2(5) . . ?
N13 C13 C12 129.7(5) . . ?
O11 C14 O12 124.6(5) . . ?
O11 C14 C12 124.4(5) . . ?
O12 C14 C12 110.9(5) . . ?
O12 C15 H15A 110.1 . . ?
O12 C15 H15B 110.1 . . ?
H15A C15 H15B 108.4 . . ?
C16 C15 O12 108.0(5) . . ?
C16 C15 H15A 110.1 . . ?
C16 C15 H15B 110.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C24 O22 C25 115.8(4) . . ?
N22 N21 Cu1 119.6(3) . . ?
C21 N21 Cu1 134.7(3) . . ?
C21 N21 N22 105.6(4) . . ?
N21 N22 H22 124.4 . . ?
C23 N22 N21 111.2(4) . . ?
C23 N22 H22 124.4 . . ?
H23A N23 H23B 120.0 . . ?
C23 N23 H23A 120.0 . . ?
C23 N23 H23B 120.0 . . ?
N21 C21 H21 124.4 . . ?
N21 C21 C22 111.3(4) . . ?
C22 C21 H21 124.4 . . ?
C21 C22 C24 130.6(4) . . ?
C23 C22 C21 104.9(4) . . ?
C23 C22 C24 124.4(4) . . ?
N22 C23 C22 107.1(4) . . ?
N23 C23 N22 122.4(4) . . ?
N23 C23 C22 130.4(4) . . ?
O21 C24 O22 123.8(5) . . ?
O21 C24 C22 122.7(5) . . ?
O22 C24 C22 113.4(4) . . ?
O22 C25 H25A 110.1 . . ?
O22 C25 H25B 110.1 . . ?
O22 C25 C26 108.2(4) . . ?
H25A C25 H25B 108.4 . . ?
C26 C25 H25A 110.1 . . ?
C26 C25 H25B 110.1 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_structure3
_database_code_depnum_ccdc_archive 'CCDC 1589790'
_audit_update_record             
;
2017-12-07 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;
_audit_creation_date             2017-09-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H36 Br2 Cu N12 O8, 2(H2 O)'
_chemical_formula_sum            'C24 H40 Br2 Cu N12 O10'
_chemical_formula_weight         880.04
_chemical_melting_point          ?
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_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                   11.262(3)
_cell_length_b                   7.5904(17)
_cell_length_c                   21.555(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.803(7)
_cell_angle_gamma                90
_cell_volume                     1836.0(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.85
_shelx_estimated_absorpt_T_max   0.609
_shelx_estimated_absorpt_T_min   0.507
_exptl_absorpt_coefficient_mu    2.837
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0602 before and 0.0460 after correction. The Ratio of minimum to maximum transmission is 0.8833. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'orangish green'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.253
_exptl_crystal_size_min          0.194
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32014
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.676
_diffrn_reflns_theta_min         1.896
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4878
_reflns_number_total             5628
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         5628
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0248
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0256P)²+1.0326P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0602
_refine_special_details          
;
 Positions of H-atoms of water molecule were refined in unrestricted way.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 N12(H12), C11(H11), N22(H22), C21(H21)
2.c X=CH2 refined with riding coordinates:
 N13(H13A,H13B), N23(H23A,H23B)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Br1 Br 0.11181(2) 0.83157(2) 0.46538(2) 0.01734(4) Uani 1 1 d . . . . .
Cu1 Cu 0.0000 0.5000 0.5000 0.01383(6) Uani 1 2 d S T P . .
O11 O 0.55011(10) 0.26891(16) 0.58481(6) 0.0245(2) Uani 1 1 d . . . . .
O12 O 0.50174(9) 0.55773(14) 0.58781(5) 0.0199(2) Uani 1 1 d . . . . .
N11 N 0.15778(11) 0.40025(16) 0.53201(6) 0.0170(2) Uani 1 1 d . . . . .
N12 N 0.18477(11) 0.22429(17) 0.52890(6) 0.0200(3) Uani 1 1 d . . . . .
H12 H 0.1331 0.1420 0.5164 0.024 Uiso 1 1 calc R . . . .
N13 N 0.34851(14) 0.03133(19) 0.55018(8) 0.0339(4) Uani 1 1 d . . . . .
H13A H 0.3044 -0.0614 0.5398 0.041 Uiso 1 1 calc R . . . .
H13B H 0.4245 0.0182 0.5625 0.041 Uiso 1 1 calc R . . . .
C11 C 0.25819(13) 0.47896(19) 0.55233(7) 0.0170(3) Uani 1 1 d . . . . .
H11 H 0.2663 0.6022 0.5591 0.020 Uiso 1 1 calc R . . . .
C12 C 0.35114(13) 0.35735(19) 0.56264(7) 0.0171(3) Uani 1 1 d . . . . .
C13 C 0.29979(13) 0.1934(2) 0.54724(7) 0.0200(3) Uani 1 1 d . . . . .
C14 C 0.47629(13) 0.3868(2) 0.57975(7) 0.0181(3) Uani 1 1 d . . . . .
C15 C 0.62542(13) 0.5995(2) 0.60625(8) 0.0213(3) Uani 1 1 d . . . . .
H15A H 0.6773 0.5562 0.5746 0.026 Uiso 1 1 calc R . . . .
H15B H 0.6508 0.5433 0.6466 0.026 Uiso 1 1 calc R . . . .
C16 C 0.63422(16) 0.7965(2) 0.61179(10) 0.0314(4) Uani 1 1 d . . . . .
H16A H 0.6059 0.8506 0.5720 0.047 Uiso 1 1 calc GR . . . .
H16B H 0.7174 0.8301 0.6226 0.047 Uiso 1 1 calc GR . . . .
H16C H 0.5851 0.8372 0.6444 0.047 Uiso 1 1 calc GR . . . .
O21 O 0.04894(13) 0.11554(17) 0.22764(6) 0.0335(3) Uani 1 1 d . . . . .
O22 O -0.06388(11) -0.01851(15) 0.29544(5) 0.0252(2) Uani 1 1 d . . . . .
N21 N 0.01951(11) 0.39780(16) 0.41487(6) 0.0161(2) Uani 1 1 d . . . . .
N22 N 0.08197(11) 0.49105(16) 0.37348(6) 0.0165(2) Uani 1 1 d . . . . .
H22 H 0.1150 0.5944 0.3817 0.020 Uiso 1 1 calc R . . . .
N23 N 0.14145(13) 0.47318(19) 0.27100(6) 0.0250(3) Uani 1 1 d . . . . .
H23A H 0.1759 0.5771 0.2748 0.030 Uiso 1 1 calc R . . . .
H23B H 0.1428 0.4137 0.2360 0.030 Uiso 1 1 calc R . . . .
C21 C -0.01481(13) 0.2512(2) 0.38534(7) 0.0169(3) Uani 1 1 d . . . . .
H21 H -0.0598 0.1604 0.4026 0.020 Uiso 1 1 calc R . . . .
C22 C 0.02418(13) 0.24736(19) 0.32492(7) 0.0164(3) Uani 1 1 d . . . . .
C23 C 0.08654(13) 0.40501(19) 0.31881(7) 0.0164(3) Uani 1 1 d . . . . .
C24 C 0.00634(14) 0.1121(2) 0.27736(7) 0.0198(3) Uani 1 1 d . . . . .
C25 C -0.08716(19) -0.1607(2) 0.25140(10) 0.0356(4) Uani 1 1 d . . . . .
H25A H -0.0123 -0.2232 0.2444 0.043 Uiso 1 1 calc R . . . .
H25B H -0.1223 -0.1143 0.2110 0.043 Uiso 1 1 calc R . . . .
C26 C -0.1729(2) -0.2836(3) 0.27924(12) 0.0480(6) Uani 1 1 d . . . . .
H26A H -0.1920 -0.3816 0.2505 0.072 Uiso 1 1 calc GR . . . .
H26B H -0.2461 -0.2196 0.2865 0.072 Uiso 1 1 calc GR . . . .
H26C H -0.1366 -0.3295 0.3189 0.072 Uiso 1 1 calc GR . . . .
O1 O 0.24628(11) -0.20280(16) 0.33344(5) 0.0208(2) Uani 1 1 d . . . . .
H1A H 0.304(2) -0.234(3) 0.3558(10) 0.031 Uiso 1 1 d R . . . .
H1B H 0.211(2) -0.151(3) 0.3539(11) 0.031 Uiso 1 1 d R . . . .


_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
Cu1 N11 2.0003(13) . ?
Cu1 N11 2.0003(13) 3_566 ?
Cu1 N21 2.0211(12) . ?
Cu1 N21 2.0212(12) 3_566 ?
O11 C14 1.2198(19) . ?
O12 C14 1.3372(19) . ?
O12 C15 1.4512(17) . ?
N11 N12 1.3726(18) . ?
N11 C11 1.3208(18) . ?
N12 H12 0.8800 . ?
N12 C13 1.3428(19) . ?
N13 H13A 0.8800 . ?
N13 H13B 0.8800 . ?
N13 C13 1.346(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.399(2) . ?
C12 C13 1.400(2) . ?
C12 C14 1.444(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.502(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O21 C24 1.211(2) . ?
O22 C24 1.3461(19) . ?
O22 C25 1.447(2) . ?
N21 N22 1.3772(17) . ?
N21 C21 1.3235(19) . ?
N22 H22 0.8800 . ?
N22 C23 1.3520(18) . ?
N23 H23A 0.8800 . ?
N23 H23B 0.8800 . ?
N23 C23 1.3486(19) . ?
C21 H21 0.9500 . ?
C21 C22 1.409(2) . ?
C22 C23 1.399(2) . ?
C22 C24 1.453(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.503(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
O1 H1A 0.81(2) . ?
O1 H1B 0.74(2) . ?

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
N11 Cu1 N11 180.0 . 3_566 ?
N11 Cu1 N21 89.61(5) 3_566 . ?
N11 Cu1 N21 89.60(5) . 3_566 ?
N11 Cu1 N21 90.40(5) . . ?
N11 Cu1 N21 90.40(5) 3_566 3_566 ?
N21 Cu1 N21 180.00(3) . 3_566 ?
C14 O12 C15 115.99(12) . . ?
N12 N11 Cu1 123.05(9) . . ?
C11 N11 Cu1 130.86(10) . . ?
C11 N11 N12 105.63(12) . . ?
N11 N12 H12 124.2 . . ?
C13 N12 N11 111.57(12) . . ?
C13 N12 H12 124.2 . . ?
H13A N13 H13B 120.0 . . ?
C13 N13 H13A 120.0 . . ?
C13 N13 H13B 120.0 . . ?
N11 C11 H11 124.4 . . ?
N11 C11 C12 111.25(13) . . ?
C12 C11 H11 124.4 . . ?
C11 C12 C13 105.07(12) . . ?
C11 C12 C14 129.77(14) . . ?
C13 C12 C14 124.94(13) . . ?
N12 C13 N13 123.55(14) . . ?
N12 C13 C12 106.48(13) . . ?
N13 C13 C12 129.96(14) . . ?
O11 C14 O12 124.26(14) . . ?
O11 C14 C12 123.56(14) . . ?
O12 C14 C12 112.16(13) . . ?
O12 C15 H15A 110.3 . . ?
O12 C15 H15B 110.3 . . ?
O12 C15 C16 107.15(13) . . ?
H15A C15 H15B 108.5 . . ?
C16 C15 H15A 110.3 . . ?
C16 C15 H15B 110.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C24 O22 C25 116.00(13) . . ?
N22 N21 Cu1 119.41(9) . . ?
C21 N21 Cu1 135.22(10) . . ?
C21 N21 N22 105.37(11) . . ?
N21 N22 H22 124.0 . . ?
C23 N22 N21 112.03(12) . . ?
C23 N22 H22 124.0 . . ?
H23A N23 H23B 120.0 . . ?
C23 N23 H23A 120.0 . . ?
C23 N23 H23B 120.0 . . ?
N21 C21 H21 124.4 . . ?
N21 C21 C22 111.15(13) . . ?
C22 C21 H21 124.4 . . ?
C21 C22 C24 129.15(14) . . ?
C23 C22 C21 105.49(12) . . ?
C23 C22 C24 125.35(14) . . ?
N22 C23 C22 105.96(13) . . ?
N23 C23 N22 122.28(14) . . ?
N23 C23 C22 131.75(14) . . ?
O21 C24 O22 123.91(14) . . ?
O21 C24 C22 124.61(15) . . ?
O22 C24 C22 111.48(13) . . ?
O22 C25 H25A 110.4 . . ?
O22 C25 H25B 110.4 . . ?
O22 C25 C26 106.74(16) . . ?
H25A C25 H25B 108.6 . . ?
C26 C25 H25A 110.4 . . ?
C26 C25 H25B 110.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
H1A O1 H1B 104(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_structure2
_database_code_depnum_ccdc_archive 'CCDC 1589789'
_audit_update_record             
;
2017-12-07 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;
_audit_creation_date             2017-09-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H36 Br Cu N12 O8 1+, Br 1-, H2O'
_chemical_formula_sum            'C24 H38 Br2 Cu N12 O9'
_chemical_formula_weight         862.02
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   30.7828(17)
_cell_length_b                   5.6317(3)
_cell_length_c                   20.8991(12)
_cell_angle_alpha                90
_cell_angle_beta                 100.075(2)
_cell_angle_gamma                90
_cell_volume                     3567.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7875
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.19
_shelx_estimated_absorpt_T_max   0.931
_shelx_estimated_absorpt_T_min   0.297
_exptl_absorpt_coefficient_mu    2.916
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0709 before and 0.0515 after correction. The Ratio of minimum to maximum transmission is 0.7786. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27621
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.874
_diffrn_reflns_theta_min         2.189
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6714
_reflns_number_total             8500
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.376(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         8500
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0331
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0405P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0816
_refine_special_details          
;
Hydrogen atoms of the water molecule were not localized. 
The largest residual electron density peak located near 
water O1 is probably due to imperfect twin correction.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.624(10)
 0.376(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C25(H25A,H25B), C35(H35A,H35B), C45(H45A,H45B)
3.b Aromatic/amide H refined with riding coordinates:
 N12(H12), N22(H22), N32(H32), N42(H42), C11(H11), C21(H21), C31(H31), C41(H41)
3.c X=CH2 refined with riding coordinates:
 N13(H13A,H13B), N23(H23A,H23B), N33(H33A,H33B), N43(H43A,H43B)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C26(H26A,H26B,H26C), C36(H36A,H36B,H36C), C46(H46A,H46B,
 H46C)
;
# start Validation Reply Form
_vrf_PLAT111_mo_culbr_0m         
;
PROBLEM: ADDSYM Detects New (Pseudo) Centre of Symmetry . 100 %Fit
RESPONSE: -1 symmetry is violated through ordering of Br- and H2O positions.
;
_vrf_PLAT113_mo_culbr_0m         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New Space Group C2/c Check
RESPONSE: The crystal structure is pseudo-centrosymmetric.
;
_vrf_PLAT306_mo_culbr_0m         
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1 Check
RESPONSE: O-atom of water molecule with non-localized H-atoms.
;
# end Validation Reply Form

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Br1 Br 0.49936(2) -0.25737(6) 0.50032(2) 0.01931(11) Uani 1 1 d . . . . .
Cu1 Cu 0.49919(2) 0.23632(8) 0.50078(2) 0.01258(12) Uani 1 1 d . . . . .
O11 O 0.66600(15) 0.3850(9) 0.3463(2) 0.0315(11) Uani 1 1 d . . . . .
O12 O 0.65859(14) 0.6247(7) 0.4306(2) 0.0295(10) Uani 1 1 d . . . . .
O21 O 0.33226(15) 0.1369(9) 0.2580(2) 0.0349(11) Uani 1 1 d . . . . .
O22 O 0.33432(15) -0.1096(8) 0.3441(2) 0.0361(12) Uani 1 1 d . . . . .
O31 O 0.33140(14) 0.3930(8) 0.6531(2) 0.0309(10) Uani 1 1 d . . . . .
O32 O 0.34047(14) 0.6362(8) 0.5704(2) 0.0298(11) Uani 1 1 d . . . . .
O41 O 0.66767(13) 0.1089(8) 0.74057(19) 0.0310(11) Uani 1 1 d . . . . .
O42 O 0.66358(16) -0.1336(9) 0.6544(2) 0.0376(12) Uani 1 1 d . . . . .
N11 N 0.54576(14) 0.2483(8) 0.44474(19) 0.0171(9) Uani 1 1 d . . . . .
N12 N 0.55059(16) 0.0851(8) 0.3971(2) 0.0183(10) Uani 1 1 d . . . . .
H12 H 0.5325 -0.0344 0.3856 0.022 Uiso 1 1 calc R . . . .
N13 N 0.5983(2) -0.0022(10) 0.3232(3) 0.0369(17) Uani 1 1 d . . . . .
H13A H 0.5824 -0.1265 0.3082 0.044 Uiso 1 1 calc R . . . .
H13B H 0.6220 0.0349 0.3073 0.044 Uiso 1 1 calc R . . . .
N21 N 0.45100(15) 0.2364(8) 0.42162(19) 0.0166(9) Uani 1 1 d . . . . .
N22 N 0.44709(16) 0.4064(8) 0.3735(2) 0.0180(10) Uani 1 1 d . . . . .
H22 H 0.4658 0.5239 0.3726 0.022 Uiso 1 1 calc R . . . .
N23 N 0.3993(2) 0.5143(10) 0.2768(3) 0.0441(18) Uani 1 1 d . . . . .
H23A H 0.4156 0.6390 0.2717 0.053 Uiso 1 1 calc R . . . .
H23B H 0.3754 0.4839 0.2482 0.053 Uiso 1 1 calc R . . . .
N31 N 0.45264(14) 0.2546(7) 0.5574(2) 0.0176(9) Uani 1 1 d . . . . .
N32 N 0.44899(15) 0.0988(8) 0.6068(2) 0.0175(10) Uani 1 1 d . . . . .
H32 H 0.4679 -0.0161 0.6197 0.021 Uiso 1 1 calc R . . . .
N33 N 0.4018(2) 0.0240(9) 0.6834(3) 0.0293(15) Uani 1 1 d . . . . .
H33A H 0.4187 -0.0927 0.7013 0.035 Uiso 1 1 calc R . . . .
H33B H 0.3778 0.0618 0.6985 0.035 Uiso 1 1 calc R . . . .
N41 N 0.54745(15) 0.2283(7) 0.5798(2) 0.0168(9) Uani 1 1 d . . . . .
N42 N 0.55061(15) 0.3840(8) 0.6311(2) 0.0165(10) Uani 1 1 d . . . . .
H42 H 0.5312 0.4963 0.6344 0.020 Uiso 1 1 calc R . . . .
N43 N 0.5977(2) 0.4672(9) 0.7312(3) 0.0296(14) Uani 1 1 d . . . . .
H43A H 0.5804 0.5825 0.7402 0.035 Uiso 1 1 calc R . . . .
H43B H 0.6219 0.4327 0.7586 0.035 Uiso 1 1 calc R . . . .
C11 C 0.57934(19) 0.3930(10) 0.4471(3) 0.0193(12) Uani 1 1 d . . . . .
H11 H 0.5848 0.5238 0.4761 0.023 Uiso 1 1 calc R . . . .
C12 C 0.6063(2) 0.3322(10) 0.4018(3) 0.0214(13) Uani 1 1 d . . . . .
C13 C 0.58621(19) 0.1318(10) 0.3709(3) 0.0186(13) Uani 1 1 d . . . . .
C14 C 0.6462(2) 0.4431(12) 0.3889(3) 0.0233(14) Uani 1 1 d . . . . .
C15 C 0.6966(2) 0.7613(13) 0.4190(3) 0.0361(16) Uani 1 1 d . . . . .
H15A H 0.6905 0.8371 0.3756 0.043 Uiso 1 1 calc R . . . .
H15B H 0.7228 0.6579 0.4214 0.043 Uiso 1 1 calc R . . . .
C16 C 0.7039(3) 0.9468(13) 0.4718(4) 0.044(2) Uani 1 1 d . . . . .
H16A H 0.6776 1.0466 0.4688 0.065 Uiso 1 1 calc GR . . . .
H16B H 0.7293 1.0457 0.4667 0.065 Uiso 1 1 calc GR . . . .
H16C H 0.7097 0.8685 0.5144 0.065 Uiso 1 1 calc GR . . . .
C21 C 0.4161(2) 0.0980(10) 0.4057(3) 0.0188(12) Uani 1 1 d . . . . .
H21 H 0.4096 -0.0338 0.4308 0.023 Uiso 1 1 calc R . . . .
C22 C 0.38984(19) 0.1695(10) 0.3474(3) 0.0206(13) Uani 1 1 d . . . . .
C23 C 0.4111(2) 0.3699(11) 0.3284(3) 0.0215(13) Uani 1 1 d . . . . .
C24 C 0.3499(2) 0.0698(12) 0.3123(3) 0.0254(14) Uani 1 1 d . . . . .
C25 C 0.2944(2) -0.2299(16) 0.3084(4) 0.054(2) Uani 1 1 d . . . . .
H25A H 0.2695 -0.1169 0.2993 0.065 Uiso 1 1 calc R . . . .
H25B H 0.3003 -0.2936 0.2665 0.065 Uiso 1 1 calc R . . . .
C26 C 0.2839(3) -0.4247(16) 0.3503(4) 0.060(3) Uani 1 1 d . . . . .
H26A H 0.3102 -0.5223 0.3639 0.090 Uiso 1 1 calc GR . . . .
H26B H 0.2603 -0.5230 0.3260 0.090 Uiso 1 1 calc GR . . . .
H26C H 0.2741 -0.3582 0.3887 0.090 Uiso 1 1 calc GR . . . .
C31 C 0.4187(2) 0.3971(10) 0.5530(3) 0.0192(13) Uani 1 1 d . . . . .
H31 H 0.4128 0.5233 0.5225 0.023 Uiso 1 1 calc R . . . .
C32 C 0.39202(19) 0.3405(10) 0.5988(3) 0.0175(12) Uani 1 1 d . . . . .
C33 C 0.4127(2) 0.1441(10) 0.6332(3) 0.0189(12) Uani 1 1 d . . . . .
C34 C 0.3526(2) 0.4562(11) 0.6107(3) 0.0229(15) Uani 1 1 d . . . . .
C35 C 0.3024(2) 0.7713(12) 0.5803(3) 0.0373(16) Uani 1 1 d . . . . .
H35A H 0.3076 0.8455 0.6239 0.045 Uiso 1 1 calc R . . . .
H35B H 0.2761 0.6676 0.5765 0.045 Uiso 1 1 calc R . . . .
C36 C 0.2957(3) 0.9604(13) 0.5277(4) 0.043(2) Uani 1 1 d . . . . .
H36A H 0.3228 1.0540 0.5301 0.065 Uiso 1 1 calc GR . . . .
H36B H 0.2714 1.0649 0.5340 0.065 Uiso 1 1 calc GR . . . .
H36C H 0.2887 0.8843 0.4849 0.065 Uiso 1 1 calc GR . . . .
C41 C 0.5819(2) 0.0881(11) 0.5931(3) 0.0196(13) Uani 1 1 d . . . . .
H41 H 0.5880 -0.0393 0.5663 0.024 Uiso 1 1 calc R . . . .
C42 C 0.6086(2) 0.1506(10) 0.6522(3) 0.0198(12) Uani 1 1 d . . . . .
C43 C 0.5869(2) 0.3435(10) 0.6755(3) 0.0200(12) Uani 1 1 d . . . . .
C44 C 0.6486(3) 0.0435(12) 0.6872(3) 0.0259(15) Uani 1 1 d . . . . .
C45 C 0.7029(2) -0.2501(14) 0.6878(4) 0.051(2) Uani 1 1 d . . . . .
H45A H 0.6982 -0.3090 0.7307 0.062 Uiso 1 1 calc R . . . .
H45B H 0.7280 -0.1378 0.6946 0.062 Uiso 1 1 calc R . . . .
C46 C 0.7123(3) -0.4545(15) 0.6455(5) 0.064(3) Uani 1 1 d . . . . .
H46A H 0.6881 -0.5698 0.6417 0.096 Uiso 1 1 calc GR . . . .
H46B H 0.7400 -0.5313 0.6652 0.096 Uiso 1 1 calc GR . . . .
H46C H 0.7148 -0.3950 0.6023 0.096 Uiso 1 1 calc GR . . . .
Br2 Br 0.49898(2) -0.26192(10) 0.71996(3) 0.03095(14) Uani 1 1 d . . . . .
O1 O 0.49785(15) -0.2441(6) 0.3040(2) 0.0353(10) Uani 1 1 d . . . . .


_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
Br1 Cu1 2.7804(6) . ?
Br1 Cu1 2.8514(6) 1_545 ?
Cu1 Br1 2.8514(6) 1_565 ?
Cu1 N11 2.005(4) . ?
Cu1 N21 2.020(4) . ?
Cu1 N31 2.014(4) . ?
Cu1 N41 2.019(4) . ?
O11 C14 1.208(8) . ?
O12 C14 1.354(8) . ?
O12 C15 1.455(7) . ?
O21 C24 1.228(8) . ?
O22 C24 1.343(8) . ?
O22 C25 1.484(8) . ?
O31 C34 1.239(8) . ?
O32 C34 1.329(8) . ?
O32 C35 1.441(7) . ?
O41 C44 1.223(8) . ?
O42 C44 1.337(8) . ?
O42 C45 1.445(8) . ?
N11 N12 1.382(6) . ?
N11 C11 1.310(7) . ?
N12 H12 0.8800 . ?
N12 C13 1.335(7) . ?
N13 H13A 0.8800 . ?
N13 H13B 0.8800 . ?
N13 C13 1.353(7) . ?
N21 N22 1.378(6) . ?
N21 C21 1.323(7) . ?
N22 H22 0.8800 . ?
N22 C23 1.341(7) . ?
N23 H23A 0.8800 . ?
N23 H23B 0.8800 . ?
N23 C23 1.348(8) . ?
N31 N32 1.375(6) . ?
N31 C31 1.308(7) . ?
N32 H32 0.8800 . ?
N32 C33 1.352(7) . ?
N33 H33A 0.8800 . ?
N33 H33B 0.8800 . ?
N33 C33 1.341(7) . ?
N41 N42 1.375(6) . ?
N41 C41 1.312(7) . ?
N42 H42 0.8800 . ?
N42 C43 1.342(7) . ?
N43 H43A 0.8800 . ?
N43 H43B 0.8800 . ?
N43 C43 1.347(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.406(8) . ?
C12 C13 1.390(8) . ?
C12 C14 1.446(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.509(11) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C21 H21 0.9500 . ?
C21 C22 1.398(8) . ?
C22 C23 1.396(8) . ?
C22 C24 1.432(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.474(11) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C31 H31 0.9500 . ?
C31 C32 1.402(8) . ?
C32 C33 1.410(8) . ?
C32 C34 1.438(9) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.518(10) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C41 H41 0.9500 . ?
C41 C42 1.404(8) . ?
C42 C43 1.406(8) . ?
C42 C44 1.449(9) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.509(11) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?

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
Cu1 Br1 Cu1 179.52(3) . 1_545 ?
Br1 Cu1 Br1 179.52(3) . 1_565 ?
N11 Cu1 Br1 87.84(12) . 1_565 ?
N11 Cu1 Br1 91.70(12) . . ?
N11 Cu1 N21 91.10(17) . . ?
N11 Cu1 N31 175.13(12) . . ?
N11 Cu1 N41 88.83(18) . . ?
N21 Cu1 Br1 89.93(12) . . ?
N21 Cu1 Br1 89.92(13) . 1_565 ?
N31 Cu1 Br1 87.30(12) . 1_565 ?
N31 Cu1 Br1 93.16(12) . . ?
N31 Cu1 N21 89.13(18) . . ?
N31 Cu1 N41 91.05(17) . . ?
N41 Cu1 Br1 88.79(12) . . ?
N41 Cu1 Br1 91.36(12) . 1_565 ?
N41 Cu1 N21 178.71(12) . . ?
C14 O12 C15 115.8(5) . . ?
C24 O22 C25 115.4(6) . . ?
C34 O32 C35 117.2(5) . . ?
C44 O42 C45 115.2(6) . . ?
N12 N11 Cu1 125.2(3) . . ?
C11 N11 Cu1 129.7(4) . . ?
C11 N11 N12 104.9(4) . . ?
N11 N12 H12 124.3 . . ?
C13 N12 N11 111.3(4) . . ?
C13 N12 H12 124.3 . . ?
H13A N13 H13B 120.0 . . ?
C13 N13 H13A 120.0 . . ?
C13 N13 H13B 120.0 . . ?
N22 N21 Cu1 123.7(3) . . ?
C21 N21 Cu1 130.9(4) . . ?
C21 N21 N22 105.2(4) . . ?
N21 N22 H22 124.4 . . ?
C23 N22 N21 111.3(4) . . ?
C23 N22 H22 124.4 . . ?
H23A N23 H23B 120.0 . . ?
C23 N23 H23A 120.0 . . ?
C23 N23 H23B 120.0 . . ?
N32 N31 Cu1 124.7(3) . . ?
C31 N31 Cu1 129.2(3) . . ?
C31 N31 N32 106.0(4) . . ?
N31 N32 H32 124.2 . . ?
C33 N32 N31 111.5(4) . . ?
C33 N32 H32 124.2 . . ?
H33A N33 H33B 120.0 . . ?
C33 N33 H33A 120.0 . . ?
C33 N33 H33B 120.0 . . ?
N42 N41 Cu1 124.4(3) . . ?
C41 N41 Cu1 129.7(4) . . ?
C41 N41 N42 105.9(4) . . ?
N41 N42 H42 124.2 . . ?
C43 N42 N41 111.6(4) . . ?
C43 N42 H42 124.2 . . ?
H43A N43 H43B 120.0 . . ?
C43 N43 H43A 120.0 . . ?
C43 N43 H43B 120.0 . . ?
N11 C11 H11 123.9 . . ?
N11 C11 C12 112.2(5) . . ?
C12 C11 H11 123.9 . . ?
C11 C12 C14 129.9(6) . . ?
C13 C12 C11 104.1(5) . . ?
C13 C12 C14 126.0(5) . . ?
N12 C13 N13 122.9(6) . . ?
N12 C13 C12 107.4(5) . . ?
N13 C13 C12 129.6(6) . . ?
O11 C14 O12 123.9(6) . . ?
O11 C14 C12 125.1(6) . . ?
O12 C14 C12 111.0(6) . . ?
O12 C15 H15A 110.7 . . ?
O12 C15 H15B 110.7 . . ?
O12 C15 C16 105.4(5) . . ?
H15A C15 H15B 108.8 . . ?
C16 C15 H15A 110.7 . . ?
C16 C15 H15B 110.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N21 C21 H21 124.2 . . ?
N21 C21 C22 111.7(5) . . ?
C22 C21 H21 124.2 . . ?
C21 C22 C24 130.3(6) . . ?
C23 C22 C21 104.7(5) . . ?
C23 C22 C24 125.0(6) . . ?
N22 C23 N23 122.9(6) . . ?
N22 C23 C22 107.1(5) . . ?
N23 C23 C22 130.0(6) . . ?
O21 C24 O22 123.4(6) . . ?
O21 C24 C22 123.6(6) . . ?
O22 C24 C22 112.9(6) . . ?
O22 C25 H25A 110.4 . . ?
O22 C25 H25B 110.4 . . ?
H25A C25 H25B 108.6 . . ?
C26 C25 O22 106.8(7) . . ?
C26 C25 H25A 110.4 . . ?
C26 C25 H25B 110.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N31 C31 H31 124.2 . . ?
N31 C31 C32 111.6(5) . . ?
C32 C31 H31 124.2 . . ?
C31 C32 C33 105.0(5) . . ?
C31 C32 C34 129.0(6) . . ?
C33 C32 C34 126.0(5) . . ?
N32 C33 C32 105.8(5) . . ?
N33 C33 N32 124.2(6) . . ?
N33 C33 C32 130.0(5) . . ?
O31 C34 O32 123.2(6) . . ?
O31 C34 C32 124.0(6) . . ?
O32 C34 C32 112.7(6) . . ?
O32 C35 H35A 110.5 . . ?
O32 C35 H35B 110.5 . . ?
O32 C35 C36 106.2(6) . . ?
H35A C35 H35B 108.7 . . ?
C36 C35 H35A 110.5 . . ?
C36 C35 H35B 110.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N41 C41 H41 124.3 . . ?
N41 C41 C42 111.3(5) . . ?
C42 C41 H41 124.3 . . ?
C41 C42 C43 105.0(5) . . ?
C41 C42 C44 130.9(6) . . ?
C43 C42 C44 124.1(6) . . ?
N42 C43 N43 124.0(6) . . ?
N42 C43 C42 106.2(5) . . ?
N43 C43 C42 129.7(6) . . ?
O41 C44 O42 122.7(6) . . ?
O41 C44 C42 124.3(6) . . ?
O42 C44 C42 113.0(6) . . ?
O42 C45 H45A 110.3 . . ?
O42 C45 H45B 110.3 . . ?
O42 C45 C46 107.1(6) . . ?
H45A C45 H45B 108.6 . . ?
C46 C45 H45A 110.3 . . ?
C46 C45 H45B 110.3 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 N11 N12 C13 -176.0(4) . . . . ?
Cu1 N11 C11 C12 175.8(4) . . . . ?
Cu1 N21 N22 C23 -177.1(4) . . . . ?
Cu1 N21 C21 C22 176.8(4) . . . . ?
Cu1 N31 N32 C33 -175.4(4) . . . . ?
Cu1 N31 C31 C32 175.2(4) . . . . ?
Cu1 N41 N42 C43 -177.4(4) . . . . ?
Cu1 N41 C41 C42 177.0(4) . . . . ?
N11 N12 C13 N13 179.9(5) . . . . ?
N11 N12 C13 C12 0.3(6) . . . . ?
N11 C11 C12 C13 -0.5(6) . . . . ?
N11 C11 C12 C14 -179.6(6) . . . . ?
N12 N11 C11 C12 0.6(6) . . . . ?
N21 N22 C23 N23 178.8(6) . . . . ?
N21 N22 C23 C22 0.7(6) . . . . ?
N21 C21 C22 C23 -1.1(6) . . . . ?
N21 C21 C22 C24 179.0(6) . . . . ?
N22 N21 C21 C22 1.5(6) . . . . ?
N31 N32 C33 N33 -178.0(5) . . . . ?
N31 N32 C33 C32 -0.1(6) . . . . ?
N31 C31 C32 C33 -0.1(7) . . . . ?
N31 C31 C32 C34 178.5(6) . . . . ?
N32 N31 C31 C32 0.0(6) . . . . ?
N41 N42 C43 N43 -178.7(5) . . . . ?
N41 N42 C43 C42 -0.2(6) . . . . ?
N41 C41 C42 C43 1.0(7) . . . . ?
N41 C41 C42 C44 177.8(6) . . . . ?
N42 N41 C41 C42 -1.1(6) . . . . ?
C11 N11 N12 C13 -0.6(6) . . . . ?
C11 C12 C13 N12 0.1(6) . . . . ?
C11 C12 C13 N13 -179.5(6) . . . . ?
C11 C12 C14 O11 -175.9(6) . . . . ?
C11 C12 C14 O12 3.2(9) . . . . ?
C13 C12 C14 O11 5.2(10) . . . . ?
C13 C12 C14 O12 -175.7(5) . . . . ?
C14 O12 C15 C16 -178.9(5) . . . . ?
C14 C12 C13 N12 179.2(6) . . . . ?
C14 C12 C13 N13 -0.4(10) . . . . ?
C15 O12 C14 O11 3.7(9) . . . . ?
C15 O12 C14 C12 -175.4(5) . . . . ?
C21 N21 N22 C23 -1.4(6) . . . . ?
C21 C22 C23 N22 0.2(6) . . . . ?
C21 C22 C23 N23 -177.6(6) . . . . ?
C21 C22 C24 O21 -172.7(6) . . . . ?
C21 C22 C24 O22 5.5(9) . . . . ?
C23 C22 C24 O21 7.5(10) . . . . ?
C23 C22 C24 O22 -174.3(6) . . . . ?
C24 O22 C25 C26 177.9(7) . . . . ?
C24 C22 C23 N22 -179.9(6) . . . . ?
C24 C22 C23 N23 2.2(10) . . . . ?
C25 O22 C24 O21 1.8(10) . . . . ?
C25 O22 C24 C22 -176.4(6) . . . . ?
C31 N31 N32 C33 0.1(6) . . . . ?
C31 C32 C33 N32 0.1(6) . . . . ?
C31 C32 C33 N33 177.8(6) . . . . ?
C31 C32 C34 O31 -179.4(6) . . . . ?
C31 C32 C34 O32 2.0(9) . . . . ?
C33 C32 C34 O31 -1.1(10) . . . . ?
C33 C32 C34 O32 -179.7(5) . . . . ?
C34 O32 C35 C36 -179.2(6) . . . . ?
C34 C32 C33 N32 -178.5(6) . . . . ?
C34 C32 C33 N33 -0.8(10) . . . . ?
C35 O32 C34 O31 4.2(9) . . . . ?
C35 O32 C34 C32 -177.2(5) . . . . ?
C41 N41 N42 C43 0.8(6) . . . . ?
C41 C42 C43 N42 -0.4(6) . . . . ?
C41 C42 C43 N43 177.9(6) . . . . ?
C41 C42 C44 O41 -176.0(6) . . . . ?
C41 C42 C44 O42 5.3(10) . . . . ?
C43 C42 C44 O41 0.3(10) . . . . ?
C43 C42 C44 O42 -178.4(6) . . . . ?
C44 O42 C45 C46 175.6(6) . . . . ?
C44 C42 C43 N42 -177.5(5) . . . . ?
C44 C42 C43 N43 0.9(10) . . . . ?
C45 O42 C44 O41 2.7(9) . . . . ?
C45 O42 C44 C42 -178.6(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.624(10)
2 0.376(10)

