# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_hi_rl1_sq
_database_code_depnum_ccdc_archive 'CCDC 1845737'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
#==============================================================================
_audit_creation_date             2016-03-31

_audit_block_code                hi_rl1
_audit_block_refno               2687
_audit_block_usercomment         'gu07KS2, irregular, black'


_audit_creation_method           
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
# start Validation Reply Form
_vrf_PLAT910_hi_rl1_sq           
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         17 Note
RESPONSE: limited by diffractometer
;
_vrf_CHEMW03_hi_rl1_sq           
;
PROBLEM: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.99 <> 1.01
RESPONSE: see _platon_squeeze
;
# end Validation Reply Form

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C35.50 H59 Cl11 Cu2 N14'
_chemical_formula_weight         1198.99
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            black
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C36 H54 Cl10 Cu2 N14'
_chemical_oxdiff_usercomment     'gu07KS2, irregular, black'
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'
Cl Cl 0.1484 0.1585 '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'

_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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
_chemical_absolute_configuration .
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   32.8999(4)
_cell_length_b                   14.17669(13)
_cell_length_c                   24.7543(3)
_cell_angle_alpha                90
_cell_angle_beta                 112.0818(14)
_cell_angle_gamma                90
_cell_volume                     10698.8(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    29937
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      31.4750
_cell_measurement_theta_min      3.2990
_shelx_estimated_absorpt_T_max   0.874
_shelx_estimated_absorpt_T_min   0.874
_exptl_absorpt_coefficient_mu    1.386
_exptl_absorpt_correction_T_max  0.87620
_exptl_absorpt_correction_T_min  0.87620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41p (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             4920
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-38 9 1 0.0719
-10 8 -26 0.0991
39 -4 -27 0.0667
13 19 3 0.0135
-14 -19 -3 0.0411
38 -9 -1 0.0719
-1 -2 5 0.0800
5 4 0 0.0111
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.055
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-37.9864 8.9974 1.0042 -0.0370 0.2922 -0.9370
-9.9912 7.9986 -25.9909 0.0416 -0.5439 -0.8387
38.9912 -3.9978 -26.9964 0.0743 -0.9152 0.3842
12.9982 18.9919 2.9999 0.9958 0.0752 -0.1612
-13.9978 -18.9919 -2.9998 -1.0072 -0.0691 0.1418
37.9864 -8.9974 -1.0042 0.0370 -0.2922 0.9370
-1.0000 -2.0000 5.0000 -0.0615 0.1203 0.1161
5.0000 4.0000 0.0000 0.2310 -0.0134 -0.0011

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            133467
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.008
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -43.00  57.00   0.50   17.50    --   26.87 -77.00  30.00  200
  2  ω      6.00  96.00   0.50   17.50    --   26.87  57.00 150.00  180
  3  ω    -20.00  69.00   0.50   17.50    --   26.87 -99.00-120.00  178
  4  ω     52.00  96.00   0.50   17.50    --   26.87  57.00 -90.00   88
  5  ω    -42.00  41.00   0.50   17.50    --   26.87 -57.00 120.00  166
  6  ω    -46.00  34.00   0.50   17.50    --   26.87 -38.00-120.00  160
  7  ω     -2.00  84.00   0.50   17.50    --   26.87  77.00  30.00  172
  8  ω     35.00  61.00   0.50   17.50    --   26.87  57.00-150.00   52
  9  ω    -20.00  69.00   0.50   17.50    --   26.87 -99.00   0.00  178
 10  ω      4.00  33.00   0.50   17.50    --   26.87  77.00 -60.00   58
 11  ω    -17.00  15.00   0.50   17.50    --   26.87 -99.00  90.00   64
 12  ω     31.00  69.00   0.50   17.50    --   26.87 -99.00  90.00   76
 13  ω      2.00  91.00   0.50   17.50    --   26.87  38.00  30.00  178
 14  ω      3.00  29.00   0.50   17.50    --   26.87  77.00 120.00   52
 15  ω      0.00  97.00   0.50   17.50    --   26.87  77.00-150.00  194
 16  ω     11.00  54.00   0.50   17.50    --   26.87  45.00-132.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0114555000
_diffrn_orient_matrix_UB_12      0.0434286000
_diffrn_orient_matrix_UB_13      0.0073613000
_diffrn_orient_matrix_UB_21      -0.0060450000
_diffrn_orient_matrix_UB_22      0.0042186000
_diffrn_orient_matrix_UB_23      0.0245470000
_diffrn_orient_matrix_UB_31      0.0193330000
_diffrn_orient_matrix_UB_32      -0.0244523000
_diffrn_orient_matrix_UB_33      0.0173115000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13017
_reflns_number_total             16336
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file,
 see _platon_squeeze_.
 
 _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       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2018/3
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         16336
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0409
_refine_ls_restrained_S_all      7.745
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0489P)²+17.9394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1068
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C51-Cl1 \\sim C51-Cl52 \\sim C61-Cl61 \\sim C61-Cl62 \\sim C71_$1-Cl71_$1
\\sim C71_$1-Cl72_$1 ~
 C71_$1-Cl73_$1 \\sim C71_$1-Cl74_$1
 with sigma of 0.02
 Cl51-Cl52 \\sim Cl61-Cl62 \\sim Cl71_$1-Cl72_$1 \\sim Cl73_$1-Cl74_$1
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl71, C71, Cl72, Cl73, Cl74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H71A)=Sof(H71B)=Sof(Cl73)=Sof(Cl74)=1-FVAR(1)
 Sof(Cl71)=Sof(H71C)=Sof(H71D)=Sof(Cl72)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C71(H71C,H71D), C71(H71A,H71B), C51(H51A,H51B), C61(H61A,H61B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C19(H19), C22(H22)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
Cu1 Cu 0.48069(2) 0.24614(2) 0.45468(2) 0.01641(6) Uani 1 1 d . . . . .
Cl1 Cl 0.50146(2) 0.16409(4) 0.53748(2) 0.02465(10) Uani 1 1 d D . . . .
N1 N 0.53852(5) 0.25459(11) 0.44858(7) 0.0171(3) Uani 1 1 d . . . . .
C1 C 0.54539(6) 0.33749(13) 0.42246(8) 0.0162(3) Uani 1 1 d . . . . .
Cu2 Cu 0.68912(2) 0.81351(2) 0.25840(2) 0.01727(6) Uani 1 1 d . . . . .
Cl2 Cl 0.41122(2) 0.19676(3) 0.41607(2) 0.02363(10) Uani 1 1 d . . . . .
N2 N 0.56569(6) 0.10370(11) 0.47159(7) 0.0203(3) Uani 1 1 d . . . . .
C2 C 0.50752(6) 0.39974(13) 0.40193(8) 0.0159(3) Uani 1 1 d . . . . .
Cl3 Cl 0.75701(2) 0.87214(4) 0.29985(3) 0.03022(12) Uani 1 1 d . . . . .
N3 N 0.61140(6) 0.22826(12) 0.51531(8) 0.0215(3) Uani 1 1 d . . . . .
C3 C 0.50988(6) 0.48317(13) 0.37509(9) 0.0181(4) Uani 1 1 d . . . . .
H3 H 0.485287 0.524334 0.362657 0.022 Uiso 1 1 calc R . . . .
Cl4 Cl 0.66739(2) 0.88014(4) 0.17012(2) 0.03062(12) Uani 1 1 d . . . . .
N4 N 0.47219(5) 0.36988(11) 0.41561(7) 0.0173(3) Uani 1 1 d . . . . .
C4 C 0.54831(6) 0.50919(13) 0.36553(8) 0.0164(3) Uani 1 1 d . . . . .
N5 N 0.40873(5) 0.42784(12) 0.42245(7) 0.0197(3) Uani 1 1 d . . . . .
C5 C 0.58527(6) 0.44606(13) 0.38384(8) 0.0157(3) Uani 1 1 d . . . . .
N6 N 0.41283(6) 0.42074(13) 0.33128(8) 0.0235(4) Uani 1 1 d . . . . .
C6 C 0.58245(6) 0.36046(13) 0.41214(8) 0.0177(4) Uani 1 1 d . . . . .
H6 H 0.606655 0.318251 0.424161 0.021 Uiso 1 1 calc R . . . .
N9 N 0.63123(5) 0.80332(11) 0.26442(7) 0.0174(3) Uani 1 1 d . . . . .
C7 C 0.57211(6) 0.19658(13) 0.47818(8) 0.0171(3) Uani 1 1 d . . . . .
N10 N 0.59881(5) 0.94772(11) 0.23107(7) 0.0202(3) Uani 1 1 d . . . . .
C8 C 0.52828(7) 0.06576(15) 0.42307(10) 0.0275(5) Uani 1 1 d . . . . .
H8A H 0.503298 0.058263 0.435128 0.041 Uiso 1 1 calc GR . . . .
H8B H 0.536106 0.004316 0.411616 0.041 Uiso 1 1 calc GR . . . .
H8C H 0.520352 0.109263 0.389934 0.041 Uiso 1 1 calc GR . . . .
N11 N 0.55886(5) 0.81252(11) 0.19460(7) 0.0181(3) Uani 1 1 d . . . . .
C9 C 0.58700(7) 0.03649(15) 0.51915(10) 0.0271(5) Uani 1 1 d . . . . .
H9A H 0.608384 -0.001371 0.509744 0.041 Uiso 1 1 calc GR . . . .
H9B H 0.564789 -0.005104 0.523911 0.041 Uiso 1 1 calc GR . . . .
H9C H 0.602023 0.071185 0.555469 0.041 Uiso 1 1 calc GR . . . .
N12 N 0.69871(5) 0.69180(11) 0.29920(7) 0.0165(3) Uani 1 1 d . . . . .
C10 C 0.61523(8) 0.31609(15) 0.54716(10) 0.0282(5) Uani 1 1 d . . . . .
H10A H 0.628741 0.364212 0.530875 0.042 Uiso 1 1 calc GR . . . .
H10B H 0.633513 0.306002 0.588338 0.042 Uiso 1 1 calc GR . . . .
H10C H 0.586002 0.337260 0.543737 0.042 Uiso 1 1 calc GR . . . .
N13 N 0.76234(5) 0.63766(12) 0.29128(8) 0.0208(3) Uani 1 1 d . . . . .
C11 C 0.65273(7) 0.18273(18) 0.52161(11) 0.0317(5) Uani 1 1 d . . . . .
H11A H 0.666782 0.158189 0.561347 0.048 Uiso 1 1 calc GR . . . .
H11B H 0.672156 0.228786 0.514022 0.048 Uiso 1 1 calc GR . . . .
H11C H 0.647000 0.130638 0.493697 0.048 Uiso 1 1 calc GR . . . .
N14 N 0.75824(5) 0.64115(12) 0.38272(8) 0.0214(3) Uani 1 1 d . . . . .
C12 C 0.43160(6) 0.40651(13) 0.38939(8) 0.0177(4) Uani 1 1 d . . . . .
N7 N 0.54945(5) 0.59224(11) 0.33978(7) 0.0171(3) Uani 1 1 d . . . . .
C13 C 0.43105(7) 0.43577(16) 0.48563(9) 0.0254(4) Uani 1 1 d . . . . .
H13A H 0.433346 0.373216 0.503379 0.038 Uiso 1 1 calc GR . . . .
H13B H 0.414292 0.477651 0.501039 0.038 Uiso 1 1 calc GR . . . .
H13C H 0.460503 0.461772 0.494839 0.038 Uiso 1 1 calc GR . . . .
N8 N 0.62242(5) 0.46692(11) 0.37573(7) 0.0158(3) Uani 1 1 d . . . . .
C14 C 0.36109(7) 0.41309(16) 0.40189(11) 0.0282(5) Uani 1 1 d . . . . .
H14A H 0.346340 0.474111 0.398508 0.042 Uiso 1 1 calc GR . . . .
H14B H 0.354318 0.373192 0.429744 0.042 Uiso 1 1 calc GR . . . .
H14C H 0.350840 0.382116 0.363702 0.042 Uiso 1 1 calc GR . . . .
C15 C 0.42650(9) 0.3670(2) 0.29094(10) 0.0362(5) Uani 1 1 d . . . . .
H15A H 0.446370 0.405341 0.278823 0.054 Uiso 1 1 calc GR . . . .
H15B H 0.400653 0.349877 0.256617 0.054 Uiso 1 1 calc GR . . . .
H15C H 0.441669 0.309566 0.310200 0.054 Uiso 1 1 calc GR . . . .
C16 C 0.38075(8) 0.49452(18) 0.30491(11) 0.0355(6) Uani 1 1 d . . . . .
H16A H 0.351952 0.465929 0.284121 0.053 Uiso 1 1 calc GR . . . .
H16B H 0.389611 0.530744 0.277434 0.053 Uiso 1 1 calc GR . . . .
H16C H 0.379085 0.536605 0.335421 0.053 Uiso 1 1 calc GR . . . .
C17 C 0.62566(6) 0.72139(13) 0.29243(8) 0.0163(3) Uani 1 1 d . . . . .
C18 C 0.66397(6) 0.66047(13) 0.31350(8) 0.0148(3) Uani 1 1 d . . . . .
C19 C 0.66212(6) 0.57672(13) 0.34075(8) 0.0161(3) Uani 1 1 d . . . . .
H19 H 0.687009 0.536403 0.353722 0.019 Uiso 1 1 calc R . . . .
C20 C 0.62355(6) 0.54980(12) 0.34974(8) 0.0148(3) Uani 1 1 d . . . . .
C21 C 0.58636(6) 0.61231(13) 0.33121(8) 0.0158(3) Uani 1 1 d . . . . .
C22 C 0.58895(6) 0.69774(13) 0.30282(8) 0.0170(3) Uani 1 1 d . . . . .
H22 H 0.564586 0.739531 0.290721 0.020 Uiso 1 1 calc R . . . .
C23 C 0.59618(6) 0.85327(13) 0.23047(8) 0.0164(3) Uani 1 1 d . . . . .
C24 C 0.63295(8) 0.99681(16) 0.27828(10) 0.0304(5) Uani 1 1 d . . . . .
H24A H 0.640831 0.959804 0.314216 0.046 Uiso 1 1 calc GR . . . .
H24B H 0.622106 1.058851 0.284123 0.046 Uiso 1 1 calc GR . . . .
H24C H 0.658853 1.004789 0.268238 0.046 Uiso 1 1 calc GR . . . .
C25 C 0.57697(7) 1.00411(15) 0.17843(10) 0.0282(5) Uani 1 1 d . . . . .
H25A H 0.563050 0.962036 0.145149 0.042 Uiso 1 1 calc GR . . . .
H25B H 0.598664 1.043792 0.170909 0.042 Uiso 1 1 calc GR . . . .
H25C H 0.554601 1.044184 0.184030 0.042 Uiso 1 1 calc GR . . . .
C26 C 0.55863(8) 0.71900(15) 0.17047(10) 0.0268(4) Uani 1 1 d . . . . .
H26A H 0.588692 0.700701 0.176167 0.040 Uiso 1 1 calc GR . . . .
H26B H 0.540559 0.719592 0.128700 0.040 Uiso 1 1 calc GR . . . .
H26C H 0.546487 0.673637 0.190258 0.040 Uiso 1 1 calc GR . . . .
C27 C 0.51563(6) 0.85245(16) 0.18422(9) 0.0236(4) Uani 1 1 d . . . . .
H27A H 0.518880 0.909051 0.208214 0.035 Uiso 1 1 calc GR . . . .
H27B H 0.497742 0.805867 0.194531 0.035 Uiso 1 1 calc GR . . . .
H27C H 0.501264 0.869201 0.142951 0.035 Uiso 1 1 calc GR . . . .
C28 C 0.73962(6) 0.65577(13) 0.32481(9) 0.0173(4) Uani 1 1 d . . . . .
C29 C 0.74043(8) 0.62679(17) 0.22831(10) 0.0292(5) Uani 1 1 d . . . . .
H29A H 0.709896 0.607755 0.218905 0.044 Uiso 1 1 calc GR . . . .
H29B H 0.755543 0.578394 0.214578 0.044 Uiso 1 1 calc GR . . . .
H29C H 0.741142 0.686904 0.209139 0.044 Uiso 1 1 calc GR . . . .
C30 C 0.81000(7) 0.65056(17) 0.31221(12) 0.0324(5) Uani 1 1 d . . . . .
H30A H 0.820306 0.681740 0.350331 0.049 Uiso 1 1 calc GR . . . .
H30B H 0.817271 0.689625 0.284433 0.049 Uiso 1 1 calc GR . . . .
H30C H 0.824278 0.588925 0.315846 0.049 Uiso 1 1 calc GR . . . .
C31 C 0.74424(7) 0.69346(17) 0.42334(9) 0.0271(4) Uani 1 1 d . . . . .
H31A H 0.727841 0.749589 0.403915 0.041 Uiso 1 1 calc GR . . . .
H31B H 0.770044 0.712690 0.457117 0.041 Uiso 1 1 calc GR . . . .
H31C H 0.725418 0.653304 0.436319 0.041 Uiso 1 1 calc GR . . . .
C32 C 0.79044(8) 0.56662(18) 0.40877(11) 0.0344(5) Uani 1 1 d . . . . .
H32A H 0.792794 0.526361 0.377898 0.052 Uiso 1 1 calc GR . . . .
H32B H 0.781036 0.528537 0.435017 0.052 Uiso 1 1 calc GR . . . .
H32C H 0.819051 0.595049 0.430846 0.052 Uiso 1 1 calc GR . . . .
Cl71 Cl 0.67708(15) 0.20345(14) 0.37973(17) 0.1311(14) Uani 0.655(3) 1 d D U P
A -1
C71 C 0.70133(12) 0.3146(2) 0.38672(17) 0.0671(10) Uani 1 1 d D U . . .
H71C H 0.679740 0.362554 0.387654 0.080 Uiso 0.655(3) 1 calc R . P A -1
H71D H 0.726428 0.317358 0.424593 0.080 Uiso 0.655(3) 1 calc R . P A -1
H71A H 0.717719 0.346941 0.365778 0.080 Uiso 0.345(3) 1 calc R . P A -2
H71B H 0.683098 0.362152 0.396394 0.080 Uiso 0.345(3) 1 calc R . P A -2
Cl72 Cl 0.71950(6) 0.34374(9) 0.33304(9) 0.0829(7) Uani 0.655(3) 1 d D U P A -1
Cl73 Cl 0.73656(9) 0.2673(3) 0.44786(17) 0.0974(14) Uani 0.345(3) 1 d D U P A
-2
Cl74 Cl 0.66587(16) 0.2241(3) 0.3396(3) 0.117(2) Uani 0.345(3) 1 d D U P A -2
Cl51 Cl 0.69876(2) 0.48397(5) 0.50454(3) 0.04235(15) Uani 1 1 d D . . . .
C51 C 0.74167(9) 0.4941(3) 0.57357(12) 0.0466(7) Uani 1 1 d D . . . .
H51A H 0.748165 0.431289 0.592324 0.056 Uiso 1 1 calc R . . . .
H51B H 0.732347 0.536156 0.598716 0.056 Uiso 1 1 calc R . . . .
Cl52 Cl 0.78974(2) 0.54044(6) 0.56683(3) 0.04740(17) Uani 1 1 d D . . . .
Cl61 Cl 0.64398(2) 0.71966(5) 0.46238(3) 0.03778(14) Uani 1 1 d D . . . .
C61 C 0.59610(8) 0.78940(16) 0.43752(11) 0.0295(5) Uani 1 1 d D . . . .
H61A H 0.589009 0.809767 0.471230 0.035 Uiso 1 1 calc R . . . .
H61B H 0.571238 0.751270 0.411492 0.035 Uiso 1 1 calc R . . . .
Cl62 Cl 0.60294(2) 0.89022(4) 0.39929(3) 0.03993(14) Uani 1 1 d 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 Cl1 2.2287(5) . ?
Cu1 N1 1.9679(17) . ?
Cu1 Cl2 2.2327(5) . ?
Cu1 N4 1.9718(16) . ?
N1 C1 1.400(2) . ?
N1 C7 1.351(2) . ?
C1 C2 1.454(3) . ?
C1 C6 1.376(3) . ?
Cu2 Cl3 2.2382(5) . ?
Cu2 Cl4 2.2369(6) . ?
Cu2 N9 1.9707(16) . ?
Cu2 N12 1.9640(16) . ?
N2 C7 1.334(2) . ?
N2 C8 1.461(3) . ?
N2 C9 1.471(3) . ?
C2 C3 1.373(3) . ?
C2 N4 1.393(2) . ?
N3 C7 1.350(2) . ?
N3 C10 1.454(3) . ?
N3 C11 1.460(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.420(3) . ?
N4 C12 1.350(2) . ?
C4 C5 1.439(2) . ?
C4 N7 1.346(2) . ?
N5 C12 1.338(3) . ?
N5 C13 1.461(3) . ?
N5 C14 1.470(3) . ?
C5 C6 1.422(2) . ?
C5 N8 1.344(2) . ?
N6 C12 1.350(3) . ?
N6 C15 1.455(3) . ?
N6 C16 1.455(3) . ?
C6 H6 0.9500 . ?
N9 C17 1.400(2) . ?
N9 C23 1.345(2) . ?
N10 C23 1.342(2) . ?
N10 C24 1.458(3) . ?
N10 C25 1.466(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
N11 C23 1.345(2) . ?
N11 C26 1.453(3) . ?
N11 C27 1.461(2) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
N12 C18 1.390(2) . ?
N12 C28 1.354(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N13 C28 1.334(3) . ?
N13 C29 1.459(3) . ?
N13 C30 1.466(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
N14 C28 1.347(3) . ?
N14 C31 1.456(3) . ?
N14 C32 1.463(3) . ?
N7 C21 1.340(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
N8 C20 1.347(2) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.453(2) . ?
C17 C22 1.368(3) . ?
C18 C19 1.378(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.420(3) . ?
C20 C21 1.439(2) . ?
C21 C22 1.419(2) . ?
C22 H22 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
Cl71 C71 1.745(4) . ?
C71 H71C 0.9900 . ?
C71 H71D 0.9900 . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C71 Cl72 1.700(4) . ?
C71 Cl73 1.663(5) . ?
C71 Cl74 1.829(5) . ?
Cl51 C51 1.766(3) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 Cl52 1.777(3) . ?
Cl61 C61 1.763(2) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 Cl62 1.775(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
Cl1 Cu1 Cl2 98.09(2) . . ?
N1 Cu1 Cl1 97.54(5) . . ?
N1 Cu1 Cl2 148.19(5) . . ?
N1 Cu1 N4 82.60(6) . . ?
N4 Cu1 Cl1 148.58(5) . . ?
N4 Cu1 Cl2 97.78(5) . . ?
C1 N1 Cu1 114.53(12) . . ?
C7 N1 Cu1 122.59(13) . . ?
C7 N1 C1 121.34(16) . . ?
N1 C1 C2 113.90(16) . . ?
C6 C1 N1 126.35(17) . . ?
C6 C1 C2 119.62(16) . . ?
Cl4 Cu2 Cl3 100.85(2) . . ?
N9 Cu2 Cl3 144.96(5) . . ?
N9 Cu2 Cl4 98.16(5) . . ?
N12 Cu2 Cl3 98.67(5) . . ?
N12 Cu2 Cl4 143.51(5) . . ?
N12 Cu2 N9 82.51(6) . . ?
C7 N2 C8 120.64(16) . . ?
C7 N2 C9 122.38(17) . . ?
C8 N2 C9 114.84(17) . . ?
C3 C2 C1 119.69(17) . . ?
C3 C2 N4 125.69(17) . . ?
N4 C2 C1 114.47(16) . . ?
C7 N3 C10 121.30(18) . . ?
C7 N3 C11 122.72(19) . . ?
C10 N3 C11 115.69(18) . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.35(17) . . ?
C4 C3 H3 119.3 . . ?
C2 N4 Cu1 114.34(12) . . ?
C12 N4 Cu1 120.68(13) . . ?
C12 N4 C2 122.09(16) . . ?
C3 C4 C5 119.09(16) . . ?
N7 C4 C3 119.43(16) . . ?
N7 C4 C5 121.48(17) . . ?
C12 N5 C13 120.01(16) . . ?
C12 N5 C14 121.85(18) . . ?
C13 N5 C14 115.05(18) . . ?
C6 C5 C4 118.82(17) . . ?
N8 C5 C4 121.64(16) . . ?
N8 C5 C6 119.53(16) . . ?
C12 N6 C15 121.15(18) . . ?
C12 N6 C16 123.3(2) . . ?
C16 N6 C15 115.33(19) . . ?
C1 C6 C5 121.34(17) . . ?
C1 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C17 N9 Cu2 114.12(12) . . ?
C23 N9 Cu2 122.68(13) . . ?
C23 N9 C17 120.35(16) . . ?
N2 C7 N1 118.35(17) . . ?
N2 C7 N3 118.59(17) . . ?
N3 C7 N1 123.03(17) . . ?
C23 N10 C24 120.83(17) . . ?
C23 N10 C25 121.76(18) . . ?
C24 N10 C25 115.13(17) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C23 N11 C26 121.71(17) . . ?
C23 N11 C27 122.44(17) . . ?
C26 N11 C27 115.27(17) . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C18 N12 Cu2 115.03(12) . . ?
C28 N12 Cu2 120.76(13) . . ?
C28 N12 C18 121.87(16) . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C28 N13 C29 121.19(17) . . ?
C28 N13 C30 122.07(19) . . ?
C29 N13 C30 115.07(18) . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C28 N14 C31 121.42(17) . . ?
C28 N14 C32 122.99(18) . . ?
C31 N14 C32 115.34(18) . . ?
N4 C12 N6 122.90(18) . . ?
N5 C12 N4 118.35(17) . . ?
N5 C12 N6 118.74(17) . . ?
C21 N7 C4 116.69(16) . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C5 N8 C20 116.95(15) . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
N6 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N9 C17 C18 114.42(16) . . ?
C22 C17 N9 125.87(17) . . ?
C22 C17 C18 119.67(17) . . ?
N12 C18 C17 113.82(16) . . ?
C19 C18 N12 126.27(17) . . ?
C19 C18 C17 119.71(17) . . ?
C18 C19 H19 119.5 . . ?
C18 C19 C20 120.97(17) . . ?
C20 C19 H19 119.5 . . ?
N8 C20 C19 119.73(16) . . ?
N8 C20 C21 121.11(17) . . ?
C19 C20 C21 119.16(16) . . ?
N7 C21 C20 122.11(16) . . ?
N7 C21 C22 119.11(16) . . ?
C22 C21 C20 118.78(17) . . ?
C17 C22 C21 121.60(17) . . ?
C17 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
N9 C23 N11 122.80(17) . . ?
N10 C23 N9 118.83(17) . . ?
N10 C23 N11 118.35(16) . . ?
N10 C24 H24A 109.5 . . ?
N10 C24 H24B 109.5 . . ?
N10 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N10 C25 H25A 109.5 . . ?
N10 C25 H25B 109.5 . . ?
N10 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N11 C26 H26A 109.5 . . ?
N11 C26 H26B 109.5 . . ?
N11 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N11 C27 H27A 109.5 . . ?
N11 C27 H27B 109.5 . . ?
N11 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N13 C28 N12 118.17(18) . . ?
N13 C28 N14 119.73(17) . . ?
N14 C28 N12 122.06(18) . . ?
N13 C29 H29A 109.5 . . ?
N13 C29 H29B 109.5 . . ?
N13 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N13 C30 H30A 109.5 . . ?
N13 C30 H30B 109.5 . . ?
N13 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N14 C31 H31A 109.5 . . ?
N14 C31 H31B 109.5 . . ?
N14 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N14 C32 H32A 109.5 . . ?
N14 C32 H32B 109.5 . . ?
N14 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Cl71 C71 H71C 108.5 . . ?
Cl71 C71 H71D 108.5 . . ?
H71C C71 H71D 107.5 . . ?
H71A C71 H71B 108.0 . . ?
Cl72 C71 Cl71 115.1(2) . . ?
Cl72 C71 H71C 108.5 . . ?
Cl72 C71 H71D 108.5 . . ?
Cl73 C71 H71A 109.5 . . ?
Cl73 C71 H71B 109.5 . . ?
Cl73 C71 Cl74 110.9(3) . . ?
Cl74 C71 H71A 109.5 . . ?
Cl74 C71 H71B 109.5 . . ?
Cl51 C51 H51A 109.5 . . ?
Cl51 C51 H51B 109.5 . . ?
Cl51 C51 Cl52 110.79(15) . . ?
H51A C51 H51B 108.1 . . ?
Cl52 C51 H51A 109.5 . . ?
Cl52 C51 H51B 109.5 . . ?
Cl61 C61 H61A 109.4 . . ?
Cl61 C61 H61B 109.4 . . ?
Cl61 C61 Cl62 111.21(13) . . ?
H61A C61 H61B 108.0 . . ?
Cl62 C61 H61A 109.4 . . ?
Cl62 C61 H61B 109.4 . . ?

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 N1 C1 C2 -3.1(2) . . . . ?
Cu1 N1 C1 C6 -178.99(16) . . . . ?
Cu1 N1 C7 N2 55.5(2) . . . . ?
Cu1 N1 C7 N3 -122.53(18) . . . . ?
Cu1 N4 C12 N5 63.9(2) . . . . ?
Cu1 N4 C12 N6 -114.73(18) . . . . ?
N1 C1 C2 C3 -179.55(17) . . . . ?
N1 C1 C2 N4 4.6(2) . . . . ?
N1 C1 C6 C5 178.39(18) . . . . ?
C1 N1 C7 N2 -139.42(19) . . . . ?
C1 N1 C7 N3 42.5(3) . . . . ?
C1 C2 C3 C4 1.6(3) . . . . ?
C1 C2 N4 Cu1 -4.0(2) . . . . ?
C1 C2 N4 C12 -164.86(17) . . . . ?
Cu2 N9 C17 C18 1.8(2) . . . . ?
Cu2 N9 C17 C22 179.24(16) . . . . ?
Cu2 N9 C23 N10 -57.8(2) . . . . ?
Cu2 N9 C23 N11 120.32(18) . . . . ?
Cu2 N12 C18 C17 3.4(2) . . . . ?
Cu2 N12 C18 C19 178.30(15) . . . . ?
Cu2 N12 C28 N13 -60.5(2) . . . . ?
Cu2 N12 C28 N14 117.13(18) . . . . ?
C2 C1 C6 C5 2.7(3) . . . . ?
C2 C3 C4 C5 0.7(3) . . . . ?
C2 C3 C4 N7 -179.08(18) . . . . ?
C2 N4 C12 N5 -136.42(19) . . . . ?
C2 N4 C12 N6 44.9(3) . . . . ?
C3 C2 N4 Cu1 -179.57(16) . . . . ?
C3 C2 N4 C12 19.6(3) . . . . ?
C3 C4 C5 C6 -1.4(3) . . . . ?
C3 C4 C5 N8 179.79(18) . . . . ?
C3 C4 N7 C21 -179.12(18) . . . . ?
N4 C2 C3 C4 176.94(18) . . . . ?
C4 C5 C6 C1 -0.3(3) . . . . ?
C4 C5 N8 C20 0.1(3) . . . . ?
C4 N7 C21 C20 -1.5(3) . . . . ?
C4 N7 C21 C22 178.30(17) . . . . ?
C5 C4 N7 C21 1.1(3) . . . . ?
C5 N8 C20 C19 178.98(17) . . . . ?
C5 N8 C20 C21 -0.5(3) . . . . ?
C6 C1 C2 C3 -3.3(3) . . . . ?
C6 C1 C2 N4 -179.16(17) . . . . ?
C6 C5 N8 C20 -178.70(17) . . . . ?
N9 C17 C18 N12 -3.4(2) . . . . ?
N9 C17 C18 C19 -178.66(17) . . . . ?
N9 C17 C22 C21 179.44(18) . . . . ?
C7 N1 C1 C2 -169.24(17) . . . . ?
C7 N1 C1 C6 14.8(3) . . . . ?
C8 N2 C7 N1 15.9(3) . . . . ?
C8 N2 C7 N3 -165.93(19) . . . . ?
C9 N2 C7 N1 -146.6(2) . . . . ?
C9 N2 C7 N3 31.6(3) . . . . ?
N12 C18 C19 C20 -175.95(18) . . . . ?
C10 N3 C7 N1 29.4(3) . . . . ?
C10 N3 C7 N2 -148.6(2) . . . . ?
C11 N3 C7 N1 -144.2(2) . . . . ?
C11 N3 C7 N2 37.8(3) . . . . ?
N7 C4 C5 C6 178.41(18) . . . . ?
N7 C4 C5 N8 -0.4(3) . . . . ?
N7 C21 C22 C17 -179.36(18) . . . . ?
C13 N5 C12 N4 16.4(3) . . . . ?
C13 N5 C12 N6 -164.86(18) . . . . ?
N8 C5 C6 C1 178.51(18) . . . . ?
N8 C20 C21 N7 1.3(3) . . . . ?
N8 C20 C21 C22 -178.53(17) . . . . ?
C14 N5 C12 N4 -142.70(19) . . . . ?
C14 N5 C12 N6 36.0(3) . . . . ?
C15 N6 C12 N4 23.8(3) . . . . ?
C15 N6 C12 N5 -154.8(2) . . . . ?
C16 N6 C12 N4 -151.0(2) . . . . ?
C16 N6 C12 N5 30.4(3) . . . . ?
C17 N9 C23 N10 142.41(19) . . . . ?
C17 N9 C23 N11 -39.4(3) . . . . ?
C17 C18 C19 C20 -1.4(3) . . . . ?
C18 N12 C28 N13 137.73(19) . . . . ?
C18 N12 C28 N14 -44.6(3) . . . . ?
C18 C17 C22 C21 -3.3(3) . . . . ?
C18 C19 C20 N8 179.03(17) . . . . ?
C18 C19 C20 C21 -1.5(3) . . . . ?
C19 C20 C21 N7 -178.23(18) . . . . ?
C19 C20 C21 C22 2.0(3) . . . . ?
C20 C21 C22 C17 0.4(3) . . . . ?
C22 C17 C18 N12 179.00(17) . . . . ?
C22 C17 C18 C19 3.8(3) . . . . ?
C23 N9 C17 C18 163.24(17) . . . . ?
C23 N9 C17 C22 -19.4(3) . . . . ?
C24 N10 C23 N9 -17.4(3) . . . . ?
C24 N10 C23 N11 164.38(19) . . . . ?
C25 N10 C23 N9 144.6(2) . . . . ?
C25 N10 C23 N11 -33.6(3) . . . . ?
C26 N11 C23 N9 -27.0(3) . . . . ?
C26 N11 C23 N10 151.20(19) . . . . ?
C27 N11 C23 N9 143.82(19) . . . . ?
C27 N11 C23 N10 -38.0(3) . . . . ?
C28 N12 C18 C17 166.18(17) . . . . ?
C28 N12 C18 C19 -19.0(3) . . . . ?
C29 N13 C28 N12 -19.7(3) . . . . ?
C29 N13 C28 N14 162.58(19) . . . . ?
C30 N13 C28 N12 144.83(19) . . . . ?
C30 N13 C28 N14 -32.8(3) . . . . ?
C31 N14 C28 N12 -23.7(3) . . . . ?
C31 N14 C28 N13 153.91(19) . . . . ?
C32 N14 C28 N12 150.3(2) . . . . ?
C32 N14 C28 N13 -32.1(3) . . . . ?
_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.163 0.250 135 42 ' '
2 -0.000 0.336 0.750 135 42 ' '
3 0.000 0.663 0.250 135 42 ' '
4 0.500 0.836 0.750 135 42 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.159
_oxdiff_exptl_absorpt_empirical_full_min 0.860
_cell_oxdiff_length_a            32.8944(4)
_cell_oxdiff_length_b            14.18103(17)
_cell_oxdiff_length_c            24.7519(3)
_cell_oxdiff_angle_alpha         90.0123(10)
_cell_oxdiff_angle_beta          112.0884(11)
_cell_oxdiff_angle_gamma         89.9616(10)
_cell_oxdiff_volume              10698.8(2)
_cell_oxdiff_measurement_reflns_used 29937
_diffrn_measurement_specimen_support 'polyimid foil'


####################################################################### 
# 
# 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_rl48n
_database_code_depnum_ccdc_archive 'CCDC 1845743'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
#============================================================================== 
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H58 Cl4 N16 Ni2'
_chemical_formula_weight         974.20

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.613(2)
_cell_length_b                   10.551(2)
_cell_length_c                   20.871(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.99(3)
_cell_angle_gamma                90
_cell_volume                     2286.1(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    1274
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      26.0

_exptl_crystal_description       'box shaped'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_F_000             1020
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    1.104
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'O-Scan    '
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12756
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.995
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6655
_reflns_number_gt                5079
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'COLLECT (Bruker AXS, 1997-2009)'
_computing_cell_refinement       'DENZO/SCALEPACK (Bruker AXS, 1997-2009)'
_computing_data_reduction        'DENZO/SCALEPACK (Bruker AXS, 1997-2009)'
_computing_structure_solution    'SHELXS-2016 (Sheldrick 2016)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'XPMA (Zsolnai, Huttner, 1994)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_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)+(0.0488P)²+0.5659P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6655
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0948
_refine_ls_wR_factor_gt          0.0860
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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
Ni1 Ni 0.84704(2) 0.59417(2) 0.16603(2) 0.01884(7) Uani 1 1 d . . . . .
Cl2 Cl 0.70276(4) 0.56029(4) 0.22976(2) 0.02615(10) Uani 1 1 d . . . . .
Cl3 Cl 1.04403(4) 0.51875(4) 0.16460(2) 0.02928(11) Uani 1 1 d . . . . .
N1 N 0.74771(14) 0.60173(12) 0.07396(7) 0.0186(3) Uani 1 1 d . . . . .
N2 N 0.73570(14) 0.54640(13) -0.03720(7) 0.0217(3) Uani 1 1 d . . . . .
N3 N 0.75583(15) 0.39215(13) 0.04284(8) 0.0230(3) Uani 1 1 d . . . . .
N4 N 0.86032(13) 0.77976(13) 0.15355(7) 0.0183(3) Uani 1 1 d . . . . .
N5 N 1.03109(14) 0.82442(13) 0.23932(7) 0.0205(3) Uani 1 1 d . . . . .
N6 N 1.00523(14) 0.94730(13) 0.14595(7) 0.0209(3) Uani 1 1 d . . . . .
N7 N 0.43531(14) 0.90264(12) -0.04102(7) 0.0187(3) Uani 1 1 d . . . . .
N21 N 0.3251(2) 0.9594(2) 0.11098(11) 0.0528(5) Uani 1 1 d . . . . .
C1 C 0.69224(16) 0.72352(15) 0.06176(8) 0.0180(3) Uani 1 1 d . . . . .
C2 C 0.75739(16) 0.82247(15) 0.10515(8) 0.0178(3) Uani 1 1 d . . . . .
C3 C 0.71207(16) 0.94407(15) 0.09795(8) 0.0189(3) Uani 1 1 d . . . . .
H3 H 0.752344 1.006721 0.126314 0.023 Uiso 1 1 calc R U . . .
C4 C 0.60458(16) 0.97609(15) 0.04789(8) 0.0181(3) Uani 1 1 d . . . . .
C5 C 0.53835(16) 0.87791(15) 0.00633(8) 0.0177(3) Uani 1 1 d . . . . .
C6 C 0.58444(16) 0.75134(15) 0.01575(8) 0.0190(3) Uani 1 1 d . . . . .
H6 H 0.540488 0.686620 -0.009800 0.023 Uiso 1 1 calc R U . . .
C7 C 0.74520(16) 0.51657(16) 0.02686(9) 0.0199(3) Uani 1 1 d . . . . .
C8 C 0.66040(19) 0.46905(18) -0.08979(9) 0.0272(4) Uani 1 1 d . . . . .
H8A H 0.621374 0.399963 -0.071129 0.041 Uiso 1 1 calc R U . . .
H8B H 0.716020 0.436248 -0.116710 0.041 Uiso 1 1 calc R U . . .
H8C H 0.594457 0.520222 -0.116004 0.041 Uiso 1 1 calc R U . . .
C9 C 0.78901(18) 0.66357(17) -0.05791(9) 0.0251(4) Uani 1 1 d . . . . .
H9A H 0.720136 0.720988 -0.075164 0.038 Uiso 1 1 calc R U . . .
H9B H 0.836636 0.644796 -0.091145 0.038 Uiso 1 1 calc R U . . .
H9C H 0.845262 0.701874 -0.021018 0.038 Uiso 1 1 calc R U . . .
C10 C 0.73196(19) 0.34740(17) 0.10514(9) 0.0266(4) Uani 1 1 d . . . . .
H10A H 0.811090 0.348058 0.137303 0.040 Uiso 1 1 calc R U . . .
H10B H 0.698512 0.262634 0.100085 0.040 Uiso 1 1 calc R U . . .
H10C H 0.670536 0.401985 0.119162 0.040 Uiso 1 1 calc R U . . .
C11 C 0.82836(19) 0.30380(17) 0.01017(11) 0.0307(4) Uani 1 1 d . . . . .
H11A H 0.860310 0.347686 -0.023484 0.046 Uiso 1 1 calc R U . . .
H11B H 0.772926 0.235930 -0.009036 0.046 Uiso 1 1 calc R U . . .
H11C H 0.899407 0.269865 0.041605 0.046 Uiso 1 1 calc R U . . .
C12 C 0.96183(16) 0.85127(15) 0.17897(8) 0.0192(3) Uani 1 1 d . . . . .
C13 C 0.97476(18) 0.75419(17) 0.28654(9) 0.0241(4) Uani 1 1 d . . . . .
H13A H 0.883092 0.766169 0.277004 0.036 Uiso 1 1 calc R U . . .
H13B H 1.010199 0.784453 0.329920 0.036 Uiso 1 1 calc R U . . .
H13C H 0.993869 0.665659 0.283817 0.036 Uiso 1 1 calc R U . . .
C14 C 1.17163(17) 0.82839(19) 0.25320(10) 0.0293(4) Uani 1 1 d . . . . .
H14A H 1.200603 0.852459 0.214308 0.044 Uiso 1 1 calc R U . . .
H14B H 1.205168 0.746174 0.267228 0.044 Uiso 1 1 calc R U . . .
H14C H 1.201557 0.889155 0.287193 0.044 Uiso 1 1 calc R U . . .
C15 C 1.06122(19) 1.06214(17) 0.17914(10) 0.0283(4) Uani 1 1 d . . . . .
H15A H 1.054935 1.059005 0.224343 0.042 Uiso 1 1 calc R U . . .
H15B H 1.015406 1.134847 0.158641 0.042 Uiso 1 1 calc R U . . .
H15C H 1.150142 1.068093 0.176280 0.042 Uiso 1 1 calc R U . . .
C16 C 0.99052(18) 0.94745(18) 0.07553(9) 0.0261(4) Uani 1 1 d . . . . .
H16A H 0.972231 0.862997 0.059102 0.039 Uiso 1 1 calc R U . . .
H16B H 1.068717 0.976858 0.064260 0.039 Uiso 1 1 calc R U . . .
H16C H 0.920828 1.002595 0.056469 0.039 Uiso 1 1 calc R U . . .
C21 C 0.4027(2) 0.9064(2) 0.14669(11) 0.0361(5) Uani 1 1 d . . . . .
C22 C 0.5013(2) 0.8386(2) 0.19296(11) 0.0396(5) Uani 1 1 d . . . . .
H22A H 0.471166 0.822928 0.232548 0.059 Uiso 1 1 calc R U . . .
H22B H 0.578381 0.888693 0.202735 0.059 Uiso 1 1 calc R U . . .
H22C H 0.519295 0.759322 0.174112 0.059 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
Ni1 N4 1.9843(14) . ?
Ni1 N1 1.9920(16) . ?
Ni1 Cl3 2.2430(6) . ?
Ni1 Cl2 2.2557(7) . ?
N1 C7 1.328(2) . ?
N1 C1 1.414(2) . ?
N2 C7 1.357(2) . ?
N2 C9 1.462(2) . ?
N2 C8 1.465(2) . ?
N3 C7 1.353(2) . ?
N3 C10 1.454(2) . ?
N3 C11 1.464(2) . ?
N4 C12 1.332(2) . ?
N4 C2 1.399(2) . ?
N5 C12 1.350(2) . ?
N5 C13 1.457(2) . ?
N5 C14 1.460(2) . ?
N6 C12 1.359(2) . ?
N6 C16 1.445(2) . ?
N6 C15 1.459(2) . ?
N7 C5 1.339(2) . ?
N7 C4 1.346(2) 3_675 ?
N21 C21 1.136(3) . ?
C1 C6 1.364(2) . ?
C1 C2 1.459(2) . ?
C2 C3 1.367(2) . ?
C3 C4 1.418(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.437(2) . ?
C5 C6 1.422(2) . ?
C6 H6 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C21 C22 1.456(3) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 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
N4 Ni1 N1 82.63(6) . . ?
N4 Ni1 Cl3 104.86(4) . . ?
N1 Ni1 Cl3 108.01(5) . . ?
N4 Ni1 Cl2 108.01(4) . . ?
N1 Ni1 Cl2 106.69(5) . . ?
Cl3 Ni1 Cl2 134.46(2) . . ?
C7 N1 C1 122.53(15) . . ?
C7 N1 Ni1 127.75(12) . . ?
C1 N1 Ni1 109.09(11) . . ?
C7 N2 C9 122.24(15) . . ?
C7 N2 C8 121.77(15) . . ?
C9 N2 C8 115.73(15) . . ?
C7 N3 C10 120.94(14) . . ?
C7 N3 C11 121.85(15) . . ?
C10 N3 C11 114.57(14) . . ?
C12 N4 C2 123.41(14) . . ?
C12 N4 Ni1 125.48(12) . . ?
C2 N4 Ni1 110.27(10) . . ?
C12 N5 C13 121.16(14) . . ?
C12 N5 C14 121.00(15) . . ?
C13 N5 C14 115.24(15) . . ?
C12 N6 C16 122.70(15) . . ?
C12 N6 C15 121.73(15) . . ?
C16 N6 C15 115.41(14) . . ?
C5 N7 C4 117.04(14) . 3_675 ?
C6 C1 N1 125.39(15) . . ?
C6 C1 C2 120.21(15) . . ?
N1 C1 C2 114.37(14) . . ?
C3 C2 N4 125.83(15) . . ?
C3 C2 C1 119.52(15) . . ?
N4 C2 C1 114.58(14) . . ?
C2 C3 C4 121.00(15) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
N7 C4 C3 119.47(15) 3_675 . ?
N7 C4 C5 121.15(15) 3_675 . ?
C3 C4 C5 119.37(15) . . ?
N7 C5 C6 119.35(15) . . ?
N7 C5 C4 121.81(15) . . ?
C6 C5 C4 118.84(15) . . ?
C1 C6 C5 120.91(15) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
N1 C7 N3 119.08(16) . . ?
N1 C7 N2 123.96(15) . . ?
N3 C7 N2 116.94(15) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 N5 119.43(15) . . ?
N4 C12 N6 123.50(16) . . ?
N5 C12 N6 116.97(15) . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N6 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N21 C21 C22 179.4(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 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
C7 N1 C1 C6 33.7(2) . . . . ?
Ni1 N1 C1 C6 -154.71(14) . . . . ?
C7 N1 C1 C2 -148.66(16) . . . . ?
Ni1 N1 C1 C2 22.94(16) . . . . ?
C12 N4 C2 C3 -32.1(3) . . . . ?
Ni1 N4 C2 C3 157.88(14) . . . . ?
C12 N4 C2 C1 150.93(15) . . . . ?
Ni1 N4 C2 C1 -19.06(17) . . . . ?
C6 C1 C2 C3 -2.1(2) . . . . ?
N1 C1 C2 C3 -179.91(14) . . . . ?
C6 C1 C2 N4 175.03(15) . . . . ?
N1 C1 C2 N4 -2.8(2) . . . . ?
N4 C2 C3 C4 -178.37(15) . . . . ?
C1 C2 C3 C4 -1.6(2) . . . . ?
C2 C3 C4 N7 -178.15(15) . . . 3_675 ?
C2 C3 C4 C5 3.3(2) . . . . ?
C4 N7 C5 C6 179.93(15) 3_675 . . . ?
C4 N7 C5 C4 -0.4(3) 3_675 . . . ?
N7 C4 C5 N7 0.5(3) 3_675 . . . ?
C3 C4 C5 N7 179.03(15) . . . . ?
N7 C4 C5 C6 -179.91(15) 3_675 . . . ?
C3 C4 C5 C6 -1.3(2) . . . . ?
N1 C1 C6 C5 -178.42(15) . . . . ?
C2 C1 C6 C5 4.0(2) . . . . ?
N7 C5 C6 C1 177.32(15) . . . . ?
C4 C5 C6 C1 -2.3(2) . . . . ?
C1 N1 C7 N3 -156.28(15) . . . . ?
Ni1 N1 C7 N3 33.8(2) . . . . ?
C1 N1 C7 N2 25.4(3) . . . . ?
Ni1 N1 C7 N2 -144.50(14) . . . . ?
C10 N3 C7 N1 18.3(2) . . . . ?
C11 N3 C7 N1 -142.28(18) . . . . ?
C10 N3 C7 N2 -163.32(16) . . . . ?
C11 N3 C7 N2 36.1(2) . . . . ?
C9 N2 C7 N1 31.1(3) . . . . ?
C8 N2 C7 N1 -142.79(17) . . . . ?
C9 N2 C7 N3 -147.21(16) . . . . ?
C8 N2 C7 N3 38.9(2) . . . . ?
C2 N4 C12 N5 155.70(15) . . . . ?
Ni1 N4 C12 N5 -35.8(2) . . . . ?
C2 N4 C12 N6 -28.1(2) . . . . ?
Ni1 N4 C12 N6 140.38(14) . . . . ?
C13 N5 C12 N4 -23.3(2) . . . . ?
C14 N5 C12 N4 137.56(17) . . . . ?
C13 N5 C12 N6 160.26(15) . . . . ?
C14 N5 C12 N6 -38.9(2) . . . . ?
C16 N6 C12 N4 -29.6(2) . . . . ?
C15 N6 C12 N4 145.56(17) . . . . ?
C16 N6 C12 N5 146.70(16) . . . . ?
C15 N6 C12 N5 -38.1(2) . . . . ?

_refine_diff_density_max         0.373
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.072

####################################################################### 
# 
# 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_rl160
_database_code_depnum_ccdc_archive 'CCDC 1845742'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
#==============================================================================

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H72 Cl6 Cu4 N18'
_chemical_formula_weight         1416.13

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.421(2)
_cell_length_b                   12.244(2)
_cell_length_c                   13.040(3)
_cell_angle_alpha                111.35(3)
_cell_angle_beta                 90.14(3)
_cell_angle_gamma                91.30(3)
_cell_volume                     1549.2(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    120
_cell_measurement_reflns_used    9086
_cell_measurement_theta_min      1.95
_cell_measurement_theta_max      30.11

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_F_000             728
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.664
_shelx_estimated_absorpt_T_min   0.732
_shelx_estimated_absorpt_T_max   0.851
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'O-Scan    '
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26330
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.955
_diffrn_reflns_theta_max         30.112
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9086
_reflns_number_gt                6272
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'COLLECT (Bruker AXS, 1997-2009)'
_computing_cell_refinement       'DENZO/SKALEPACK (Bruker AXS, 1997-2009)'
_computing_data_reduction        'DENZO/SKALEPACK (Bruker AXS, 1997-2009)'
_computing_structure_solution    'SHELXS-2016 (sheldrick 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'XPMA (Zsolnai, Huttner, 1994)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0676P)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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9086
_refine_ls_number_parameters     369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.1269
_refine_ls_wR_factor_gt          0.1130
_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
Cu1 Cu 0.69392(3) 0.45570(3) 0.27031(2) 0.02718(9) Uani 1 1 d . . . . .
Cu2 Cu 1.01921(3) 0.07477(3) -0.22585(2) 0.03338(10) Uani 1 1 d . . . . .
Cl1 Cl 0.69871(6) 0.57300(6) 0.44778(5) 0.03872(16) Uani 1 1 d . . . . .
Cl2 Cl 0.53943(6) 0.54271(6) 0.21107(5) 0.03606(15) Uani 1 1 d . . . . .
Cl3 Cl 0.86524(7) 0.10105(7) -0.32990(6) 0.04378(18) Uani 1 1 d . . . . .
N1 N 0.76815(18) 0.31844(17) 0.28977(15) 0.0271(4) Uani 1 1 d . . . . .
N2 N 0.7060(2) 0.3017(2) 0.45454(17) 0.0351(5) Uani 1 1 d . . . . .
N3 N 0.9222(2) 0.32287(19) 0.42343(16) 0.0319(5) Uani 1 1 d . . . . .
N4 N 0.78550(18) 0.39205(18) 0.12706(16) 0.0271(4) Uani 1 1 d . . . . .
N5 N 0.8063(2) 0.55913(19) 0.08488(17) 0.0324(5) Uani 1 1 d . . . . .
N6 N 0.74443(19) 0.38456(18) -0.05389(16) 0.0293(4) Uani 1 1 d . . . . .
N7 N 1.00968(18) 0.03648(17) -0.09118(15) 0.0258(4) Uani 1 1 d . . . . .
N8 N 1.1992(2) 0.07720(19) -0.28803(17) 0.0353(5) Uani 1 1 d . . . . .
N9 N 0.4037(3) 0.1418(3) 0.0505(2) 0.0570(7) Uani 1 1 d . . . . .
C1 C 0.8323(2) 0.2447(2) 0.19847(18) 0.0260(5) Uani 1 1 d . . . . .
C2 C 0.8385(2) 0.2828(2) 0.10483(18) 0.0258(5) Uani 1 1 d . . . . .
C3 C 0.9006(2) 0.2134(2) 0.01139(18) 0.0266(5) Uani 1 1 d . . . . .
H3 H 0.907712 0.238159 -0.047891 0.032 Uiso 1 1 calc R U . . .
C4 C 0.9537(2) 0.1055(2) 0.00358(18) 0.0248(5) Uani 1 1 d . . . . .
C5 C 1.0557(2) -0.0672(2) -0.09497(18) 0.0254(5) Uani 1 1 d . . . . .
C6 C 1.1162(2) -0.1408(2) -0.19147(19) 0.0269(5) Uani 1 1 d . . . . .
H6 H 1.120951 -0.117796 -0.251925 0.032 Uiso 1 1 calc R U . . .
C7 C 0.7993(2) 0.3130(2) 0.38971(19) 0.0294(5) Uani 1 1 d . . . . .
C8 C 0.5772(3) 0.2630(3) 0.4104(2) 0.0469(7) Uani 1 1 d . . . . .
H8A H 0.523388 0.329816 0.427420 0.070 Uiso 1 1 calc R U . . .
H8B H 0.542285 0.209979 0.442721 0.070 Uiso 1 1 calc R U . . .
H8C H 0.581136 0.223877 0.331961 0.070 Uiso 1 1 calc R U . . .
C9 C 0.7169(3) 0.3475(3) 0.5745(2) 0.0480(8) Uani 1 1 d . . . . .
H9A H 0.725328 0.283582 0.599904 0.072 Uiso 1 1 calc R U . . .
H9B H 0.641482 0.390261 0.605496 0.072 Uiso 1 1 calc R U . . .
H9C H 0.791145 0.398811 0.596997 0.072 Uiso 1 1 calc R U . . .
C10 C 0.9750(3) 0.2556(3) 0.4857(2) 0.0447(7) Uani 1 1 d . . . . .
H10A H 0.906949 0.212303 0.504436 0.067 Uiso 1 1 calc R U . . .
H10B H 1.015859 0.308249 0.551824 0.067 Uiso 1 1 calc R U . . .
H10C H 1.036853 0.202056 0.441619 0.067 Uiso 1 1 calc R U . . .
C11 C 1.0190(2) 0.3780(3) 0.3749(2) 0.0393(6) Uani 1 1 d . . . . .
H11A H 1.049094 0.320985 0.307588 0.059 Uiso 1 1 calc R U . . .
H11B H 1.089690 0.407459 0.425575 0.059 Uiso 1 1 calc R U . . .
H11C H 0.981419 0.441531 0.359887 0.059 Uiso 1 1 calc R U . . .
C12 C 0.7785(2) 0.4438(2) 0.05163(19) 0.0277(5) Uani 1 1 d . . . . .
C13 C 0.8717(3) 0.6215(3) 0.1890(2) 0.0386(6) Uani 1 1 d . . . . .
H13A H 0.809431 0.652703 0.245704 0.058 Uiso 1 1 calc R U . . .
H13B H 0.923580 0.684497 0.182724 0.058 Uiso 1 1 calc R U . . .
H13C H 0.925388 0.568467 0.207463 0.058 Uiso 1 1 calc R U . . .
C14 C 0.7356(3) 0.6356(2) 0.0415(2) 0.0415(7) Uani 1 1 d . . . . .
H14A H 0.673281 0.589548 -0.012013 0.062 Uiso 1 1 calc R U . . .
H14B H 0.794497 0.673118 0.007518 0.062 Uiso 1 1 calc R U . . .
H14C H 0.692794 0.694098 0.100718 0.062 Uiso 1 1 calc R U . . .
C15 C 0.6566(2) 0.2831(2) -0.0855(2) 0.0353(6) Uani 1 1 d . . . . .
H15A H 0.699887 0.215065 -0.132620 0.053 Uiso 1 1 calc R U . . .
H15B H 0.583884 0.297154 -0.123988 0.053 Uiso 1 1 calc R U . . .
H15C H 0.628021 0.270383 -0.020719 0.053 Uiso 1 1 calc R U . . .
C16 C 0.7906(3) 0.4178(3) -0.1446(2) 0.0372(6) Uani 1 1 d . . . . .
H16A H 0.721498 0.450196 -0.172298 0.056 Uiso 1 1 calc R U . . .
H16B H 0.821449 0.349846 -0.202368 0.056 Uiso 1 1 calc R U . . .
H16C H 0.858985 0.475354 -0.118498 0.056 Uiso 1 1 calc R U . . .
C17 C 1.2149(3) 0.0902(3) -0.3847(2) 0.0437(7) Uani 1 1 d . . . . .
H17 H 1.142446 0.091355 -0.426080 0.052 Uiso 1 1 calc R U . . .
C18 C 1.3336(3) 0.1020(4) -0.4255(3) 0.0668(10) Uani 1 1 d . . . . .
H18 H 1.340979 0.111865 -0.492706 0.080 Uiso 1 1 calc R U . . .
C19 C 1.4416(3) 0.0991(4) -0.3657(3) 0.0696(11) Uani 1 1 d . . . . .
H19 H 1.522754 0.109398 -0.390787 0.084 Uiso 1 1 calc R U . . .
C20 C 1.4281(3) 0.0808(3) -0.2685(3) 0.0532(8) Uani 1 1 d . . . . .
H20 H 1.499694 0.074469 -0.228534 0.064 Uiso 1 1 calc R U . . .
C21 C 1.3053(3) 0.0720(3) -0.2312(2) 0.0423(6) Uani 1 1 d . . . . .
H21 H 1.295921 0.062049 -0.164232 0.051 Uiso 1 1 calc R U . . .
C31 C 0.4025(3) 0.2469(3) 0.1292(3) 0.0494(8) Uani 1 1 d . . . . .
H31 H 0.441233 0.309197 0.115419 0.059 Uiso 1 1 calc R U . . .
C32 C 0.3478(3) 0.2693(3) 0.2297(3) 0.0528(8) Uani 1 1 d . . . . .
H32 H 0.347949 0.345064 0.281957 0.063 Uiso 1 1 calc R U . . .
C33 C 0.2925(3) 0.1777(3) 0.2518(3) 0.0528(8) Uani 1 1 d . . . . .
H33 H 0.255431 0.190006 0.319771 0.063 Uiso 1 1 calc R U . . .
C34 C 0.2929(3) 0.0679(3) 0.1723(3) 0.0512(8) Uani 1 1 d . . . . .
H34 H 0.256082 0.004039 0.184758 0.061 Uiso 1 1 calc R U . . .
C35 C 0.3490(3) 0.0546(3) 0.0734(3) 0.0539(8) Uani 1 1 d . . . . .
H35 H 0.348671 -0.020102 0.019271 0.065 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
Cu1 N1 1.9637(19) . ?
Cu1 N4 1.998(2) . ?
Cu1 Cl2 2.2349(9) . ?
Cu1 Cl1 2.2354(11) . ?
Cu2 N7 1.9779(19) . ?
Cu2 N8 2.049(2) . ?
Cu2 Cl3 2.2022(9) . ?
N1 C7 1.368(3) . ?
N1 C1 1.388(3) . ?
N2 C7 1.328(3) . ?
N2 C8 1.458(3) . ?
N2 C9 1.460(3) . ?
N3 C7 1.342(3) . ?
N3 C10 1.465(3) . ?
N3 C11 1.468(3) . ?
N4 C12 1.352(3) . ?
N4 C2 1.390(3) . ?
N5 C12 1.342(3) . ?
N5 C13 1.452(3) . ?
N5 C14 1.467(3) . ?
N6 C12 1.343(3) . ?
N6 C15 1.458(3) . ?
N6 C16 1.463(3) . ?
N7 C5 1.351(3) . ?
N7 C4 1.359(3) . ?
N8 C17 1.338(3) . ?
N8 C21 1.345(3) . ?
N9 C31 1.323(4) . ?
N9 C35 1.326(4) . ?
C1 C6 1.365(3) 2_755 ?
C1 C2 1.458(3) . ?
C2 C3 1.379(3) . ?
C3 C4 1.414(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.433(3) 2_755 ?
C5 C6 1.413(3) . ?
C6 H6 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.373(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.377(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.372(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.385(4) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C31 C32 1.366(4) . ?
C31 H31 0.9300 . ?
C32 C33 1.371(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.366(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.373(5) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?

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
N1 Cu1 N4 81.85(8) . . ?
N1 Cu1 Cl2 152.16(7) . . ?
N4 Cu1 Cl2 96.11(6) . . ?
N1 Cu1 Cl1 96.97(6) . . ?
N4 Cu1 Cl1 148.24(6) . . ?
Cl2 Cu1 Cl1 98.88(4) . . ?
N7 Cu2 N8 115.90(8) . . ?
N7 Cu2 Cl3 130.37(6) . . ?
N8 Cu2 Cl3 113.50(7) . . ?
C7 N1 C1 117.21(19) . . ?
C7 N1 Cu1 124.18(16) . . ?
C1 N1 Cu1 114.49(15) . . ?
C7 N2 C8 120.7(2) . . ?
C7 N2 C9 123.0(2) . . ?
C8 N2 C9 115.3(2) . . ?
C7 N3 C10 123.2(2) . . ?
C7 N3 C11 120.3(2) . . ?
C10 N3 C11 114.6(2) . . ?
C12 N4 C2 122.99(19) . . ?
C12 N4 Cu1 121.54(15) . . ?
C2 N4 Cu1 114.73(15) . . ?
C12 N5 C13 121.5(2) . . ?
C12 N5 C14 121.4(2) . . ?
C13 N5 C14 113.8(2) . . ?
C12 N6 C15 121.9(2) . . ?
C12 N6 C16 122.8(2) . . ?
C15 N6 C16 115.3(2) . . ?
C5 N7 C4 117.72(19) . . ?
C5 N7 Cu2 118.23(15) . . ?
C4 N7 Cu2 123.96(16) . . ?
C17 N8 C21 117.7(2) . . ?
C17 N8 Cu2 120.59(19) . . ?
C21 N8 Cu2 121.64(19) . . ?
C31 N9 C35 116.5(3) . . ?
C6 C1 N1 124.3(2) 2_755 . ?
C6 C1 C2 120.1(2) 2_755 . ?
N1 C1 C2 115.6(2) . . ?
C3 C2 N4 128.7(2) . . ?
C3 C2 C1 118.5(2) . . ?
N4 C2 C1 112.7(2) . . ?
C2 C3 C4 121.5(2) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
N7 C4 C3 120.3(2) . . ?
N7 C4 C5 120.1(2) . 2_755 ?
C3 C4 C5 119.6(2) . 2_755 ?
N7 C5 C6 119.5(2) . . ?
N7 C5 C4 122.2(2) . 2_755 ?
C6 C5 C4 118.3(2) . 2_755 ?
C1 C6 C5 121.9(2) 2_755 . ?
C1 C6 H6 119.1 2_755 . ?
C5 C6 H6 119.1 . . ?
N2 C7 N3 120.4(2) . . ?
N2 C7 N1 119.1(2) . . ?
N3 C7 N1 120.5(2) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 N6 119.4(2) . . ?
N5 C12 N4 118.0(2) . . ?
N6 C12 N4 122.7(2) . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N6 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N8 C17 C18 122.7(3) . . ?
N8 C17 H17 118.6 . . ?
C18 C17 H17 118.6 . . ?
C17 C18 C19 119.2(3) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C20 C19 C18 119.2(3) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C19 C20 C21 118.5(3) . . ?
C19 C20 H20 120.7 . . ?
C21 C20 H20 120.7 . . ?
N8 C21 C20 122.7(3) . . ?
N8 C21 H21 118.7 . . ?
C20 C21 H21 118.7 . . ?
N9 C31 C32 123.9(3) . . ?
N9 C31 H31 118.0 . . ?
C32 C31 H31 118.0 . . ?
C31 C32 C33 118.6(3) . . ?
C31 C32 H32 120.7 . . ?
C33 C32 H32 120.7 . . ?
C34 C33 C32 118.9(3) . . ?
C34 C33 H33 120.6 . . ?
C32 C33 H33 120.6 . . ?
C33 C34 C35 118.2(3) . . ?
C33 C34 H34 120.9 . . ?
C35 C34 H34 120.9 . . ?
N9 C35 C34 124.0(3) . . ?
N9 C35 H35 118.0 . . ?
C34 C35 H35 118.0 . . ?

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
C7 N1 C1 C6 26.2(4) . . . 2_755 ?
Cu1 N1 C1 C6 -175.66(19) . . . 2_755 ?
C7 N1 C1 C2 -156.0(2) . . . . ?
Cu1 N1 C1 C2 2.2(3) . . . . ?
C12 N4 C2 C3 5.8(4) . . . . ?
Cu1 N4 C2 C3 176.0(2) . . . . ?
C12 N4 C2 C1 -178.7(2) . . . . ?
Cu1 N4 C2 C1 -8.4(2) . . . . ?
C6 C1 C2 C3 -1.9(3) 2_755 . . . ?
N1 C1 C2 C3 -179.8(2) . . . . ?
C6 C1 C2 N4 -177.9(2) 2_755 . . . ?
N1 C1 C2 N4 4.1(3) . . . . ?
N4 C2 C3 C4 177.5(2) . . . . ?
C1 C2 C3 C4 2.2(3) . . . . ?
C5 N7 C4 C3 -178.2(2) . . . . ?
Cu2 N7 C4 C3 -1.7(3) . . . . ?
C5 N7 C4 C5 -0.4(4) . . . 2_755 ?
Cu2 N7 C4 C5 176.17(16) . . . 2_755 ?
C2 C3 C4 N7 177.2(2) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . 2_755 ?
C4 N7 C5 C6 -179.1(2) . . . . ?
Cu2 N7 C5 C6 4.1(3) . . . . ?
C4 N7 C5 C4 0.4(4) . . . 2_755 ?
Cu2 N7 C5 C4 -176.36(17) . . . 2_755 ?
N7 C5 C6 C1 178.0(2) . . . 2_755 ?
C4 C5 C6 C1 -1.6(3) 2_755 . . 2_755 ?
C8 N2 C7 N3 -165.2(2) . . . . ?
C9 N2 C7 N3 27.2(4) . . . . ?
C8 N2 C7 N1 17.0(4) . . . . ?
C9 N2 C7 N1 -150.6(2) . . . . ?
C10 N3 C7 N2 39.5(4) . . . . ?
C11 N3 C7 N2 -157.0(2) . . . . ?
C10 N3 C7 N1 -142.8(2) . . . . ?
C11 N3 C7 N1 20.7(4) . . . . ?
C1 N1 C7 N2 -130.3(2) . . . . ?
Cu1 N1 C7 N2 73.9(3) . . . . ?
C1 N1 C7 N3 52.0(3) . . . . ?
Cu1 N1 C7 N3 -103.9(2) . . . . ?
C13 N5 C12 N6 -165.4(2) . . . . ?
C14 N5 C12 N6 36.7(3) . . . . ?
C13 N5 C12 N4 15.1(3) . . . . ?
C14 N5 C12 N4 -142.9(2) . . . . ?
C15 N6 C12 N5 -149.2(2) . . . . ?
C16 N6 C12 N5 29.7(3) . . . . ?
C15 N6 C12 N4 30.3(3) . . . . ?
C16 N6 C12 N4 -150.7(2) . . . . ?
C2 N4 C12 N5 -138.1(2) . . . . ?
Cu1 N4 C12 N5 52.3(3) . . . . ?
C2 N4 C12 N6 42.3(3) . . . . ?
Cu1 N4 C12 N6 -127.3(2) . . . . ?
C21 N8 C17 C18 -2.1(5) . . . . ?
Cu2 N8 C17 C18 174.5(3) . . . . ?
N8 C17 C18 C19 0.8(6) . . . . ?
C17 C18 C19 C20 2.0(6) . . . . ?
C18 C19 C20 C21 -3.3(6) . . . . ?
C17 N8 C21 C20 0.7(4) . . . . ?
Cu2 N8 C21 C20 -175.9(2) . . . . ?
C19 C20 C21 N8 2.0(5) . . . . ?
C35 N9 C31 C32 -0.8(5) . . . . ?
N9 C31 C32 C33 1.2(5) . . . . ?
C31 C32 C33 C34 -0.8(4) . . . . ?
C32 C33 C34 C35 0.1(4) . . . . ?
C31 N9 C35 C34 0.0(5) . . . . ?
C33 C34 C35 N9 0.4(5) . . . . ?

_refine_diff_density_max         0.610
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.114

####################################################################### 
# 
# 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_rlgu11k3_sq
_database_code_depnum_ccdc_archive 'CCDC 1845740'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33.80 H55.60 Cl8.60 Cu3 N14'
_chemical_formula_weight         1153.61

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.862(4)
_cell_length_b                   24.311(5)
_cell_length_c                   14.152(3)
_cell_angle_alpha                90
_cell_angle_beta                 117.18(3)
_cell_angle_gamma                90
_cell_volume                     6691(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    15915
_cell_measurement_theta_min      1
_cell_measurement_theta_max      26

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_F_000             2358
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.319
_shelx_estimated_absorpt_T_min   0.558
_shelx_estimated_absorpt_T_max   0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.558
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'O-Scan    '
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48995
_diffrn_reflns_av_unetI/netI     0.1071
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.094
_diffrn_reflns_theta_max         27.500
_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 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7694
_reflns_number_gt                4019
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'COLLECT (Bruker AXS, 1997-2009)'
_computing_cell_refinement       'DENZO/SKALEPACK (Bruker AXS, 1997-2009)'
_computing_data_reduction        'DENZO/SKALEPACK (Bruker AXS, 1997-2009)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'XPMA (Zsolnai, Huttner, 1994)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_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)+(0.1557P)²+3.4672P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7694
_refine_ls_number_parameters     288
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1632
_refine_ls_R_factor_gt           0.0842
_refine_ls_wR_factor_ref         0.2789
_refine_ls_wR_factor_gt          0.2351
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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
Cu1 Cu 0.32928(4) 0.10105(3) 0.20620(6) 0.0414(3) Uani 1 1 d . . . . .
Cu2 Cu 0.41255(8) 0.23577(6) 0.69839(11) 0.0425(5) Uani 0.5 1 d . . P . .
Cl1 Cl 0.31262(10) 0.11667(8) 0.03977(13) 0.0518(5) Uani 1 1 d . . . . .
Cl2 Cl 0.38999(10) 0.02357(7) 0.24016(12) 0.0481(5) Uani 1 1 d . . . . .
Cl3 Cl 0.48650(15) 0.22788(14) 0.8579(2) 0.0398(8) Uani 0.5 1 d . . P . .
N1 N 0.2477(3) 0.1430(2) 0.1943(4) 0.0416(13) Uani 1 1 d . . . . .
N2 N 0.1868(3) 0.2132(2) 0.0724(4) 0.0450(14) Uani 1 1 d . . . . .
N3 N 0.1595(3) 0.1218(3) 0.0293(4) 0.0519(15) Uani 1 1 d . . . . .
N4 N 0.3680(3) 0.1254(2) 0.3546(4) 0.0419(13) Uani 1 1 d . . . . .
N5 N 0.4133(3) 0.0720(2) 0.5098(4) 0.0448(14) Uani 1 1 d . . . . .
N6 N 0.4849(3) 0.1089(2) 0.4435(4) 0.0433(14) Uani 1 1 d . . . . .
N7 N 0.3163(3) 0.2419(2) 0.5856(4) 0.0462(14) Uani 1 1 d . . . . .
C1 C 0.2589(4) 0.1696(3) 0.2879(5) 0.0421(16) Uani 1 1 d . . . . .
C2 C 0.3251(4) 0.1588(3) 0.3763(5) 0.0426(16) Uani 1 1 d . . . . .
C3 C 0.3428(4) 0.1828(3) 0.4724(5) 0.0459(17) Uani 1 1 d . . . . .
H3 H 0.386167 0.176406 0.528420 0.055 Uiso 1 1 calc R U . . .
C4 C 0.2958(4) 0.2177(3) 0.4883(5) 0.0458(17) Uani 1 1 d . . . . .
C5 C 0.2295(4) 0.2264(3) 0.4032(5) 0.0476(17) Uani 1 1 d . . . . .
C6 C 0.2126(4) 0.2014(3) 0.3027(5) 0.0491(18) Uani 1 1 d . . . . .
H6 H 0.169136 0.206995 0.246258 0.059 Uiso 1 1 calc R U . . .
C7 C 0.1986(4) 0.1597(3) 0.0998(5) 0.0419(16) Uani 1 1 d . . . . .
C8 C 0.2427(4) 0.2536(3) 0.1236(5) 0.0526(19) Uani 1 1 d . . . . .
H8A H 0.239198 0.270512 0.182232 0.079 Uiso 1 1 calc R U . . .
H8B H 0.239023 0.281329 0.072904 0.079 Uiso 1 1 calc R U . . .
H8C H 0.286257 0.235332 0.148830 0.079 Uiso 1 1 calc R U . . .
C9 C 0.1182(5) 0.2355(4) 0.0048(6) 0.065(2) Uani 1 1 d . . . . .
H9A H 0.116140 0.248294 -0.060728 0.098 Uiso 1 1 calc R U . . .
H9B H 0.109114 0.265554 0.040609 0.098 Uiso 1 1 calc R U . . .
H9C H 0.084379 0.207239 -0.009711 0.098 Uiso 1 1 calc R U . . .
C10 C 0.1333(4) 0.1295(4) -0.0850(5) 0.061(2) Uani 1 1 d . . . . .
H10A H 0.144858 0.165745 -0.098599 0.092 Uiso 1 1 calc R U . . .
H10B H 0.084235 0.125150 -0.119759 0.092 Uiso 1 1 calc R U . . .
H10C H 0.153614 0.102651 -0.111876 0.092 Uiso 1 1 calc R U . . .
C11 C 0.1610(5) 0.0636(4) 0.0633(7) 0.073(2) Uani 1 1 d . . . . .
H11A H 0.120195 0.044979 0.013518 0.110 Uiso 1 1 calc R U . . .
H11B H 0.162947 0.062745 0.132501 0.110 Uiso 1 1 calc R U . . .
H11C H 0.200738 0.045473 0.065931 0.110 Uiso 1 1 calc R U . . .
C12 C 0.4213(4) 0.1021(3) 0.4351(5) 0.0438(17) Uani 1 1 d . . . . .
C13 C 0.4615(4) 0.0737(3) 0.6230(5) 0.0544(19) Uani 1 1 d . . . . .
H13A H 0.476918 0.037044 0.647880 0.082 Uiso 1 1 calc R U . . .
H13B H 0.438972 0.088856 0.661472 0.082 Uiso 1 1 calc R U . . .
H13C H 0.500273 0.096160 0.633901 0.082 Uiso 1 1 calc R U . . .
C14 C 0.3465(4) 0.0474(3) 0.4840(6) 0.0546(19) Uani 1 1 d . . . . .
H14A H 0.320202 0.072147 0.504018 0.082 Uiso 1 1 calc R U . . .
H14B H 0.353163 0.013378 0.522064 0.082 Uiso 1 1 calc R U . . .
H14C H 0.322144 0.040363 0.409043 0.082 Uiso 1 1 calc R U . . .
C15 C 0.5418(4) 0.0703(3) 0.4990(6) 0.058(2) Uani 1 1 d . . . . .
H15A H 0.576073 0.087336 0.562336 0.087 Uiso 1 1 calc R U . . .
H15B H 0.561789 0.060534 0.453435 0.087 Uiso 1 1 calc R U . . .
H15C H 0.524786 0.037832 0.517679 0.087 Uiso 1 1 calc R U . . .
C16 C 0.4946(4) 0.1482(3) 0.3756(6) 0.062(2) Uani 1 1 d . . . . .
H16A H 0.468168 0.180672 0.370048 0.093 Uiso 1 1 calc R U . . .
H16B H 0.479702 0.132483 0.306306 0.093 Uiso 1 1 calc R U . . .
H16C H 0.542419 0.157712 0.405012 0.093 Uiso 1 1 calc R U . . .
C21 C 0.7211(5) 0.0785(4) 0.7289(6) 0.059(2) Uani 0.9 1 d . . P . .
H21A H 0.707605 0.088524 0.655660 0.071 Uiso 0.9 1 calc R U P . .
H21B H 0.693683 0.047043 0.728380 0.071 Uiso 0.9 1 calc R U P . .
Cl4 Cl 0.70337(18) 0.13295(10) 0.7914(2) 0.0879(9) Uani 0.9 1 d . . P . .
Cl5 Cl 0.80849(15) 0.05939(12) 0.7900(2) 0.0924(9) Uani 0.9 1 d . . P . .


_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 N4 1.964(5) . ?
Cu1 N1 1.994(5) . ?
Cu1 Cl2 2.2266(18) . ?
Cu1 Cl1 2.2451(18) . ?
Cu2 N7 1.982(6) . ?
Cu2 Cl3 2.100(3) . ?
Cu2 Cl3 2.673(3) 2_656 ?
N1 C7 1.340(8) . ?
N1 C1 1.392(8) . ?
N2 C7 1.348(8) . ?
N2 C9 1.465(9) . ?
N2 C8 1.475(9) . ?
N3 C7 1.340(8) . ?
N3 C10 1.461(8) . ?
N3 C11 1.491(10) . ?
N4 C12 1.329(8) . ?
N4 C2 1.375(8) . ?
N5 C12 1.360(8) . ?
N5 C13 1.462(9) . ?
N5 C14 1.464(9) . ?
N6 C12 1.350(9) . ?
N6 C16 1.438(9) . ?
N6 C15 1.467(9) . ?
N7 C5 1.329(9) 7_556 ?
N7 C4 1.370(8) . ?
C1 C6 1.362(9) . ?
C1 C2 1.441(9) . ?
C2 C3 1.365(9) . ?
C3 C4 1.427(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.415(10) . ?
C5 C6 1.432(9) . ?
C6 H6 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C21 Cl4 1.732(9) . ?
C21 Cl5 1.761(9) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?

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
N4 Cu1 N1 82.4(2) . . ?
N4 Cu1 Cl2 95.83(16) . . ?
N1 Cu1 Cl2 150.82(17) . . ?
N4 Cu1 Cl1 148.79(18) . . ?
N1 Cu1 Cl1 96.60(15) . . ?
Cl2 Cu1 Cl1 99.47(7) . . ?
N7 Cu2 Cl3 152.3(2) . . ?
N7 Cu2 Cl3 118.87(18) . 2_656 ?
Cl3 Cu2 Cl3 88.76(11) . 2_656 ?
Cu2 Cl3 Cu2 90.49(11) . 2_656 ?
C7 N1 C1 121.4(5) . . ?
C7 N1 Cu1 121.1(4) . . ?
C1 N1 Cu1 113.4(4) . . ?
C7 N2 C9 123.3(6) . . ?
C7 N2 C8 119.6(6) . . ?
C9 N2 C8 116.5(6) . . ?
C7 N3 C10 122.0(6) . . ?
C7 N3 C11 120.0(6) . . ?
C10 N3 C11 114.8(6) . . ?
C12 N4 C2 118.8(5) . . ?
C12 N4 Cu1 124.6(4) . . ?
C2 N4 Cu1 114.3(4) . . ?
C12 N5 C13 123.6(6) . . ?
C12 N5 C14 119.7(6) . . ?
C13 N5 C14 114.9(5) . . ?
C12 N6 C16 118.9(6) . . ?
C12 N6 C15 123.7(6) . . ?
C16 N6 C15 115.8(6) . . ?
C5 N7 C4 116.7(6) 7_556 . ?
C5 N7 Cu2 121.9(5) 7_556 . ?
C4 N7 Cu2 121.1(5) . . ?
C6 C1 N1 126.1(6) . . ?
C6 C1 C2 119.6(6) . . ?
N1 C1 C2 114.2(5) . . ?
C3 C2 N4 124.3(6) . . ?
C3 C2 C1 120.1(6) . . ?
N4 C2 C1 115.6(5) . . ?
C2 C3 C4 121.0(6) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
N7 C4 C5 122.0(6) . . ?
N7 C4 C3 119.0(6) . . ?
C5 C4 C3 119.0(6) . . ?
N7 C5 C4 121.3(6) 7_556 . ?
N7 C5 C6 119.8(7) 7_556 . ?
C4 C5 C6 118.8(6) . . ?
C1 C6 C5 121.3(7) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
N3 C7 N1 118.9(6) . . ?
N3 C7 N2 118.4(6) . . ?
N1 C7 N2 122.7(6) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 N6 119.2(6) . . ?
N4 C12 N5 121.4(7) . . ?
N6 C12 N5 119.3(6) . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N6 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Cl4 C21 Cl5 113.4(5) . . ?
Cl4 C21 H21A 108.9 . . ?
Cl5 C21 H21A 108.9 . . ?
Cl4 C21 H21B 108.9 . . ?
Cl5 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?

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
C7 N1 C1 C6 22.0(11) . . . . ?
Cu1 N1 C1 C6 179.6(6) . . . . ?
C7 N1 C1 C2 -161.4(6) . . . . ?
Cu1 N1 C1 C2 -3.9(7) . . . . ?
C12 N4 C2 C3 20.1(10) . . . . ?
Cu1 N4 C2 C3 -176.2(5) . . . . ?
C12 N4 C2 C1 -162.7(6) . . . . ?
Cu1 N4 C2 C1 1.0(7) . . . . ?
C6 C1 C2 C3 -3.9(10) . . . . ?
N1 C1 C2 C3 179.3(6) . . . . ?
C6 C1 C2 N4 178.8(6) . . . . ?
N1 C1 C2 N4 2.0(9) . . . . ?
N4 C2 C3 C4 178.9(6) . . . . ?
C1 C2 C3 C4 1.8(10) . . . . ?
C5 N7 C4 C5 0.7(11) 7_556 . . . ?
Cu2 N7 C4 C5 -173.2(5) . . . . ?
C5 N7 C4 C3 -179.4(6) 7_556 . . . ?
Cu2 N7 C4 C3 6.8(9) . . . . ?
C2 C3 C4 N7 -178.7(6) . . . . ?
C2 C3 C4 C5 1.2(11) . . . . ?
N7 C4 C5 N7 -0.7(12) . . . 7_556 ?
C3 C4 C5 N7 179.4(6) . . . 7_556 ?
N7 C4 C5 C6 177.7(6) . . . . ?
C3 C4 C5 C6 -2.2(10) . . . . ?
N1 C1 C6 C5 179.3(6) . . . . ?
C2 C1 C6 C5 2.9(11) . . . . ?
N7 C5 C6 C1 178.6(7) 7_556 . . . ?
C4 C5 C6 C1 0.2(11) . . . . ?
C10 N3 C7 N1 -146.4(7) . . . . ?
C11 N3 C7 N1 12.3(10) . . . . ?
C10 N3 C7 N2 33.6(10) . . . . ?
C11 N3 C7 N2 -167.7(7) . . . . ?
C1 N1 C7 N3 -137.5(7) . . . . ?
Cu1 N1 C7 N3 66.6(8) . . . . ?
C1 N1 C7 N2 42.5(10) . . . . ?
Cu1 N1 C7 N2 -113.4(6) . . . . ?
C9 N2 C7 N3 34.1(9) . . . . ?
C8 N2 C7 N3 -154.8(6) . . . . ?
C9 N2 C7 N1 -145.8(6) . . . . ?
C8 N2 C7 N1 25.2(9) . . . . ?
C2 N4 C12 N6 -126.2(6) . . . . ?
Cu1 N4 C12 N6 72.0(8) . . . . ?
C2 N4 C12 N5 53.0(9) . . . . ?
Cu1 N4 C12 N5 -108.9(6) . . . . ?
C16 N6 C12 N4 9.8(9) . . . . ?
C15 N6 C12 N4 -155.2(6) . . . . ?
C16 N6 C12 N5 -169.4(6) . . . . ?
C15 N6 C12 N5 25.7(9) . . . . ?
C13 N5 C12 N4 -140.7(7) . . . . ?
C14 N5 C12 N4 23.1(9) . . . . ?
C13 N5 C12 N6 38.5(9) . . . . ?
C14 N5 C12 N6 -157.7(6) . . . . ?

_refine_diff_density_max         1.551
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.127



####################################################################### 
# 
# 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_rl142b_sq
_database_code_depnum_ccdc_archive 'CCDC 1845745'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
#==============================================================================

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33.50 H55 Cl9 Cu4 N14'
_chemical_formula_weight         1227.12

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.981(2)
_cell_length_b                   11.378(2)
_cell_length_c                   13.973(3)
_cell_angle_alpha                81.33(3)
_cell_angle_beta                 89.49(3)
_cell_angle_gamma                73.31(3)
_cell_volume                     1652.1(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100
_cell_measurement_reflns_used    8741
_cell_measurement_theta_min      1.89
_cell_measurement_theta_max      29.00

_exptl_crystal_description       'box shaped'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_F_000             623
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    1.666
_shelx_estimated_absorpt_T_min   0.435
_shelx_estimated_absorpt_T_max   0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.442
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'O-Scan    '
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25225
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.891
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             8738
_reflns_number_gt                4345
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'COLLECT (Bruker AXS, 1997-2009)'
_computing_cell_refinement       'DENZO/SKALEPACK (Bruker AXS, 1997-2009)'
_computing_data_reduction        'DENZO/SKALEPACK (Bruker AXS, 1997-2009)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'XPMA (Zsolnai, Huttner, 1994)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_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)+(0.1875P)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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8738
_refine_ls_number_parameters     364
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1294
_refine_ls_R_factor_gt           0.0915
_refine_ls_wR_factor_ref         0.3056
_refine_ls_wR_factor_gt          0.2791
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.012
_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
Cu1 Cu 0.36360(7) 0.32381(6) 0.87586(5) 0.0733(3) Uani 1 1 d . . . . .
Cu2 Cu 0.12562(6) 0.23079(6) 0.42604(5) 0.0664(3) Uani 1 1 d . . . . .
Cl1 Cl 0.56843(15) 0.21272(16) 0.88504(14) 0.0899(5) Uani 1 1 d . . . . .
Cl2 Cl 0.33621(18) 0.35664(15) 1.02783(13) 0.0955(6) Uani 1 1 d . . . . .
Cl3 Cl 0.21456(14) 0.06832(16) 0.36977(13) 0.0851(5) Uani 1 1 d . . . . .
N4 N 0.3135(4) 0.2531(4) 0.7681(3) 0.0601(11) Uani 1 1 d . . . . .
N5 N 0.3883(4) 0.0416(4) 0.8216(3) 0.0640(11) Uani 1 1 d . . . . .
N6 N 0.4304(4) 0.1132(5) 0.6661(4) 0.0720(13) Uani 1 1 d . . . . .
N7 N 0.0461(3) 0.3825(4) 0.4734(3) 0.0545(10) Uani 1 1 d . . . . .
C1 C 0.1795(5) 0.4589(5) 0.7280(4) 0.0645(14) Uani 1 1 d . . . . .
C2 C 0.2283(4) 0.3371(5) 0.7001(4) 0.0564(12) Uani 1 1 d . . . . .
C3 C 0.1827(4) 0.3135(5) 0.6167(4) 0.0541(11) Uani 1 1 d . . . . .
H3 H 0.212445 0.234642 0.599496 0.065 Uiso 1 1 calc R U . . .
C4 C 0.0910(4) 0.4075(5) 0.5559(3) 0.0494(11) Uani 1 1 d . . . . .
C5 C 0.0430(5) 0.5260(5) 0.5821(4) 0.0565(12) Uani 1 1 d . . . . .
C6 C 0.0883(5) 0.5500(5) 0.6696(4) 0.0636(14) Uani 1 1 d . . . . .
H6 H 0.056282 0.627982 0.687921 0.076 Uiso 1 1 calc R U . . .
C12 C 0.3752(5) 0.1366(5) 0.7512(4) 0.0587(12) Uani 1 1 d . . . . .
C13 C 0.4980(6) -0.0663(5) 0.8332(5) 0.0736(16) Uani 1 1 d . . . . .
H13A H 0.474805 -0.135581 0.815439 0.110 Uiso 1 1 calc R U . . .
H13B H 0.528435 -0.085538 0.899513 0.110 Uiso 1 1 calc R U . . .
H13C H 0.563705 -0.049772 0.792268 0.110 Uiso 1 1 calc R U . . .
C14 C 0.3035(7) 0.0528(6) 0.9031(4) 0.0801(17) Uani 1 1 d . . . . .
H14A H 0.343777 0.074079 0.956034 0.120 Uiso 1 1 calc R U . . .
H14B H 0.285658 -0.024844 0.923229 0.120 Uiso 1 1 calc R U . . .
H14C H 0.225506 0.116541 0.883688 0.120 Uiso 1 1 calc R U . . .
C15 C 0.4766(6) 0.2043(7) 0.6030(6) 0.087(2) Uani 1 1 d . . . . .
H15A H 0.414434 0.245839 0.551834 0.131 Uiso 1 1 calc R U . . .
H15B H 0.554873 0.162952 0.575665 0.131 Uiso 1 1 calc R U . . .
H15C H 0.490929 0.264035 0.639898 0.131 Uiso 1 1 calc R U . . .
C16 C 0.4334(6) -0.0024(6) 0.6284(5) 0.0743(16) Uani 1 1 d . . . . .
H16A H 0.519521 -0.054774 0.630421 0.111 Uiso 1 1 calc R U . . .
H16B H 0.400265 0.017775 0.562686 0.111 Uiso 1 1 calc R U . . .
H16C H 0.382382 -0.045236 0.667523 0.111 Uiso 1 1 calc R U . . .
N1 N 0.2329(5) 0.4746(4) 0.8131(4) 0.0735(14) Uani 0.5 1 d D . P A 1
N2 N 0.0278(12) 0.5888(11) 0.8801(11) 0.048(3) Uani 0.5 1 d D . P A 1
N3 N 0.2180(10) 0.6290(9) 0.9118(8) 0.064(3) Uani 0.5 1 d D . P A 1
C7 C 0.1597(12) 0.5566(11) 0.8671(11) 0.067(5) Uani 0.5 1 d D . P A 1
C8 C -0.037(2) 0.4946(16) 0.8780(14) 0.063(5) Uani 0.5 1 d D . P A 1
H8A H -0.090300 0.493192 0.932945 0.095 Uiso 0.5 1 calc R U P A 1
H8B H 0.024314 0.414795 0.880292 0.095 Uiso 0.5 1 calc R U P A 1
H8C H -0.088909 0.513493 0.819499 0.095 Uiso 0.5 1 calc R U P A 1
C9 C -0.0517(14) 0.7203(10) 0.8786(13) 0.067(4) Uani 0.5 1 d D . P A 1
H9A H -0.095846 0.727447 0.938024 0.100 Uiso 0.5 1 calc R U P A 1
H9B H -0.112416 0.743720 0.825035 0.100 Uiso 0.5 1 calc R U P A 1
H9C H 0.002046 0.774126 0.871732 0.100 Uiso 0.5 1 calc R U P A 1
C10 C 0.3490(13) 0.625(2) 0.8956(14) 0.089(6) Uani 0.5 1 d D . P A 1
H10A H 0.399320 0.587186 0.954005 0.133 Uiso 0.5 1 calc R U P A 1
H10B H 0.354703 0.708220 0.877482 0.133 Uiso 0.5 1 calc R U P A 1
H10C H 0.380164 0.577713 0.844684 0.133 Uiso 0.5 1 calc R U P A 1
C11 C 0.1787(18) 0.6847(14) 1.0007(11) 0.107(7) Uani 0.5 1 d D . P A 1
H11A H 0.158169 0.773465 0.985540 0.160 Uiso 0.5 1 calc R U P A 1
H11B H 0.247125 0.654580 1.048618 0.160 Uiso 0.5 1 calc R U P A 1
H11C H 0.105410 0.662047 1.025536 0.160 Uiso 0.5 1 calc R U P A 1
N21 N 0.2329(5) 0.4746(4) 0.8131(4) 0.0735(14) Uani 0.5 1 d D . P A 2
N22 N 0.0730(18) 0.6156(11) 0.8630(9) 0.067(5) Uani 0.5 1 d D . P A 2
N23 N 0.289(2) 0.6326(13) 0.8735(10) 0.089(5) Uani 0.5 1 d D U P A 2
C27 C 0.2003(16) 0.5806(12) 0.8464(12) 0.084(6) Uani 0.5 1 d D . P A 2
C28 C -0.0076(16) 0.5334(17) 0.8702(13) 0.060(6) Uani 0.5 1 d D . P A 2
H28A H -0.047256 0.539307 0.807997 0.089 Uiso 0.5 1 calc R U P A 2
H28B H -0.071894 0.557090 0.916294 0.089 Uiso 0.5 1 calc R U P A 2
H28C H 0.043216 0.449378 0.890993 0.089 Uiso 0.5 1 calc R U P A 2
C29 C 0.014(2) 0.7483(13) 0.8672(14) 0.088(5) Uani 0.5 1 d D . P A 2
H29A H -0.012792 0.758578 0.931787 0.132 Uiso 0.5 1 calc R U P A 2
H29B H -0.058544 0.779549 0.822945 0.132 Uiso 0.5 1 calc R U P A 2
H29C H 0.074538 0.793350 0.849561 0.132 Uiso 0.5 1 calc R U P A 2
C30 C 0.4100(19) 0.6071(15) 0.8286(17) 0.122(8) Uani 0.5 1 d D U P A 2
H30A H 0.450724 0.519190 0.839231 0.183 Uiso 0.5 1 calc R U P A 2
H30B H 0.462658 0.648617 0.856117 0.183 Uiso 0.5 1 calc R U P A 2
H30C H 0.397466 0.636355 0.760234 0.183 Uiso 0.5 1 calc R U P A 2
C31 C 0.278(2) 0.6812(17) 0.9633(16) 0.131(8) Uani 0.5 1 d D . P A 2
H31A H 0.355530 0.697659 0.979002 0.197 Uiso 0.5 1 calc R U P A 2
H31B H 0.260507 0.621630 1.013942 0.197 Uiso 0.5 1 calc R U P A 2
H31C H 0.209092 0.756856 0.957091 0.197 Uiso 0.5 1 calc R U P A 2
C21 C 0.1349(11) -0.1274(12) 0.2168(11) 0.119(4) Uani 0.75 1 d . . P . .
H21A H 0.218267 -0.184634 0.211146 0.143 Uiso 0.45 1 calc R U P B 1
H21B H 0.141922 -0.067291 0.257292 0.143 Uiso 0.45 1 calc R U P B 1
H21C H 0.226125 -0.142365 0.212468 0.143 Uiso 0.3 1 calc R U P C 2
H21D H 0.106091 -0.069882 0.262607 0.143 Uiso 0.3 1 calc R U P C 2
Cl21 Cl 0.0576(3) -0.0484(3) 0.0929(3) 0.1376(13) Uani 0.75 1 d . . P D .
Cl22 Cl 0.0317(5) -0.2008(6) 0.2583(4) 0.0980(14) Uani 0.45 1 d . . P D 1
Cl23 Cl 0.1038(11) -0.2776(10) 0.2676(9) 0.131(3) Uani 0.3 1 d . . P D 2


_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 N4 1.963(5) . ?
Cu1 N21 1.981(4) . ?
Cu1 N1 1.981(4) . ?
Cu1 Cl2 2.214(2) . ?
Cu1 Cl1 2.2353(18) . ?
Cu2 N7 1.910(5) . ?
Cu2 Cl3 2.0921(18) . ?
N4 C12 1.359(7) . ?
N4 C2 1.385(6) . ?
N5 C12 1.323(7) . ?
N5 C13 1.442(7) . ?
N5 C14 1.462(8) . ?
N6 C12 1.358(7) . ?
N6 C15 1.459(8) . ?
N6 C16 1.481(9) . ?
N7 C5 1.352(6) 2_566 ?
N7 C4 1.358(6) . ?
C1 C6 1.380(6) . ?
C1 N21 1.387(7) . ?
C1 N1 1.387(7) . ?
C1 C2 1.447(8) . ?
C2 C3 1.365(7) . ?
C3 C4 1.415(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.402(7) . ?
C5 C6 1.416(8) . ?
C6 H6 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
N1 C7 1.363(14) . ?
N2 C7 1.405(14) . ?
N2 C8 1.453(13) . ?
N2 C9 1.498(12) . ?
N3 C7 1.394(13) . ?
N3 C10 1.444(13) . ?
N3 C11 1.484(14) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
N21 C27 1.311(14) . ?
N22 C27 1.367(15) . ?
N22 C28 1.454(15) . ?
N22 C29 1.473(13) . ?
N23 C27 1.363(14) . ?
N23 C30 1.432(17) . ?
N23 C31 1.437(15) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C21 Cl22 1.644(11) . ?
C21 Cl23 1.872(15) . ?
C21 Cl21 1.910(17) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C21 H21D 0.9700 . ?

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
N4 Cu1 N21 82.15(19) . . ?
N4 Cu1 N1 82.15(19) . . ?
N4 Cu1 Cl2 147.65(16) . . ?
N21 Cu1 Cl2 98.08(17) . . ?
N1 Cu1 Cl2 98.08(17) . . ?
N4 Cu1 Cl1 96.44(14) . . ?
N21 Cu1 Cl1 146.64(19) . . ?
N1 Cu1 Cl1 146.64(19) . . ?
Cl2 Cu1 Cl1 100.26(7) . . ?
N7 Cu2 Cl3 177.93(13) . . ?
C12 N4 C2 121.5(4) . . ?
C12 N4 Cu1 122.3(3) . . ?
C2 N4 Cu1 115.2(4) . . ?
C12 N5 C13 123.0(5) . . ?
C12 N5 C14 120.1(5) . . ?
C13 N5 C14 115.8(5) . . ?
C12 N6 C15 122.4(6) . . ?
C12 N6 C16 120.5(5) . . ?
C15 N6 C16 116.8(6) . . ?
C5 N7 C4 118.6(5) 2_566 . ?
C5 N7 Cu2 120.1(4) 2_566 . ?
C4 N7 Cu2 120.6(3) . . ?
C6 C1 N21 125.1(5) . . ?
C6 C1 N1 125.1(5) . . ?
C6 C1 C2 119.6(5) . . ?
N21 C1 C2 115.3(4) . . ?
N1 C1 C2 115.3(4) . . ?
C3 C2 N4 127.0(5) . . ?
C3 C2 C1 119.5(4) . . ?
N4 C2 C1 113.4(5) . . ?
C2 C3 C4 120.9(5) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
N7 C4 C5 119.6(4) . . ?
N7 C4 C3 120.2(5) . . ?
C5 C4 C3 120.1(5) . . ?
N7 C5 C4 121.8(5) 2_566 . ?
N7 C5 C6 119.2(5) 2_566 . ?
C4 C5 C6 119.1(4) . . ?
C1 C6 C5 120.8(5) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
N5 C12 N6 117.7(5) . . ?
N5 C12 N4 119.4(5) . . ?
N6 C12 N4 122.8(5) . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N6 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C7 N1 C1 118.1(7) . . ?
C7 N1 Cu1 120.8(7) . . ?
C1 N1 Cu1 113.6(4) . . ?
C7 N2 C8 118.6(14) . . ?
C7 N2 C9 122.6(12) . . ?
C8 N2 C9 117.9(14) . . ?
C7 N3 C10 121.5(13) . . ?
C7 N3 C11 127.4(13) . . ?
C10 N3 C11 108.4(14) . . ?
N1 C7 N3 117.9(10) . . ?
N1 C7 N2 129.8(11) . . ?
N3 C7 N2 112.1(11) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C27 N21 C1 122.2(8) . . ?
C27 N21 Cu1 124.2(7) . . ?
C1 N21 Cu1 113.6(4) . . ?
C27 N22 C28 124.7(11) . . ?
C27 N22 C29 116.4(15) . . ?
C28 N22 C29 118.7(16) . . ?
C27 N23 C30 119.4(14) . . ?
C27 N23 C31 119.4(18) . . ?
C30 N23 C31 118.8(19) . . ?
N21 C27 N23 121.4(15) . . ?
N21 C27 N22 110.5(10) . . ?
N23 C27 N22 127.4(15) . . ?
N22 C28 H28A 109.5 . . ?
N22 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N22 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N22 C29 H29A 109.5 . . ?
N22 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N22 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N23 C30 H30A 109.5 . . ?
N23 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N23 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N23 C31 H31A 109.5 . . ?
N23 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N23 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Cl22 C21 Cl21 100.5(6) . . ?
Cl23 C21 Cl21 116.7(7) . . ?
Cl22 C21 H21A 111.7 . . ?
Cl21 C21 H21A 111.7 . . ?
Cl22 C21 H21B 111.7 . . ?
Cl21 C21 H21B 111.7 . . ?
H21A C21 H21B 109.4 . . ?
Cl23 C21 H21C 108.1 . . ?
Cl21 C21 H21C 108.1 . . ?
Cl23 C21 H21D 108.1 . . ?
Cl21 C21 H21D 108.1 . . ?
H21C C21 H21D 107.3 . . ?

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
C12 N4 C2 C3 8.8(8) . . . . ?
Cu1 N4 C2 C3 176.9(4) . . . . ?
C12 N4 C2 C1 -175.6(5) . . . . ?
Cu1 N4 C2 C1 -7.5(6) . . . . ?
C6 C1 C2 C3 -0.5(8) . . . . ?
N21 C1 C2 C3 -179.1(5) . . . . ?
N1 C1 C2 C3 -179.1(5) . . . . ?
C6 C1 C2 N4 -176.4(5) . . . . ?
N21 C1 C2 N4 5.0(7) . . . . ?
N1 C1 C2 N4 5.0(7) . . . . ?
N4 C2 C3 C4 177.0(5) . . . . ?
C1 C2 C3 C4 1.6(8) . . . . ?
C5 N7 C4 C5 0.9(8) 2_566 . . . ?
Cu2 N7 C4 C5 171.1(3) . . . . ?
C5 N7 C4 C3 179.0(4) 2_566 . . . ?
Cu2 N7 C4 C3 -10.8(6) . . . . ?
C2 C3 C4 N7 -179.7(5) . . . . ?
C2 C3 C4 C5 -1.6(7) . . . . ?
N7 C4 C5 N7 -0.9(8) . . . 2_566 ?
C3 C4 C5 N7 -179.0(4) . . . 2_566 ?
N7 C4 C5 C6 178.5(5) . . . . ?
C3 C4 C5 C6 0.4(7) . . . . ?
N21 C1 C6 C5 177.7(6) . . . . ?
N1 C1 C6 C5 177.7(6) . . . . ?
C2 C1 C6 C5 -0.7(9) . . . . ?
N7 C5 C6 C1 -179.9(5) 2_566 . . . ?
C4 C5 C6 C1 0.8(8) . . . . ?
C13 N5 C12 N6 30.3(8) . . . . ?
C14 N5 C12 N6 -162.5(5) . . . . ?
C13 N5 C12 N4 -146.5(5) . . . . ?
C14 N5 C12 N4 20.7(7) . . . . ?
C15 N6 C12 N5 -150.0(5) . . . . ?
C16 N6 C12 N5 36.7(7) . . . . ?
C15 N6 C12 N4 26.7(8) . . . . ?
C16 N6 C12 N4 -146.6(5) . . . . ?
C2 N4 C12 N5 -138.2(5) . . . . ?
Cu1 N4 C12 N5 54.5(6) . . . . ?
C2 N4 C12 N6 45.2(7) . . . . ?
Cu1 N4 C12 N6 -122.1(5) . . . . ?
C6 C1 N1 C7 31.3(11) . . . . ?
C2 C1 N1 C7 -150.2(8) . . . . ?
C6 C1 N1 Cu1 -178.7(5) . . . . ?
C2 C1 N1 Cu1 -0.2(7) . . . . ?
C1 N1 C7 N3 -141.7(9) . . . . ?
Cu1 N1 C7 N3 70.5(13) . . . . ?
C1 N1 C7 N2 32.7(17) . . . . ?
Cu1 N1 C7 N2 -115.1(13) . . . . ?
C10 N3 C7 N1 5.0(17) . . . . ?
C11 N3 C7 N1 -153.8(11) . . . . ?
C10 N3 C7 N2 -170.4(13) . . . . ?
C11 N3 C7 N2 30.8(17) . . . . ?
C8 N2 C7 N1 32(2) . . . . ?
C9 N2 C7 N1 -136.7(15) . . . . ?
C8 N2 C7 N3 -153.0(14) . . . . ?
C9 N2 C7 N3 38.0(19) . . . . ?
C6 C1 N21 C27 0.0(13) . . . . ?
C2 C1 N21 C27 178.5(10) . . . . ?
C6 C1 N21 Cu1 -178.7(5) . . . . ?
C2 C1 N21 Cu1 -0.2(7) . . . . ?
C1 N21 C27 N23 -130.2(13) . . . . ?
Cu1 N21 C27 N23 48.4(18) . . . . ?
C1 N21 C27 N22 59.3(15) . . . . ?
Cu1 N21 C27 N22 -122.1(10) . . . . ?
C30 N23 C27 N21 28(2) . . . . ?
C31 N23 C27 N21 -134.3(18) . . . . ?
C30 N23 C27 N22 -163.3(16) . . . . ?
C31 N23 C27 N22 35(2) . . . . ?
C28 N22 C27 N21 16(2) . . . . ?
C29 N22 C27 N21 -159.2(13) . . . . ?
C28 N22 C27 N23 -153.3(16) . . . . ?
C29 N22 C27 N23 31(2) . . . . ?

_refine_diff_density_max         2.061
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.138



####################################################################### 
# 
# 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_rl49b
_database_code_depnum_ccdc_archive 'CCDC 1845744'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
#==============================================================================

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H33 Cl2 N9 Ni'
_chemical_formula_weight         577.20

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   10.592(2)
_cell_length_b                   22.989(5)
_cell_length_c                   22.638(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.46(3)
_cell_angle_gamma                90
_cell_volume                     5512.2(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    100
_cell_measurement_reflns_used    1862
_cell_measurement_theta_min      1
_cell_measurement_theta_max      26

_exptl_crystal_description       'box shaped'
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_F_000             2416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.350
_exptl_absorpt_coefficient_mu    0.929
_shelx_estimated_absorpt_T_min   0.654
_shelx_estimated_absorpt_T_max   0.737
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'O-Scan    '
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24293
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_av_R_equivalents  0.0610
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              31
_reflns_limit_k_min              -30
_reflns_limit_l_max              30
_reflns_limit_l_min              -30
_diffrn_reflns_theta_min         1.772
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             24293
_reflns_number_gt                17623
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_max     0.991
_reflns_Friedel_fraction_full    0.992

_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       'COLLECT (Bruker AXS, 1997-2009)'
_computing_cell_refinement       'DENZO/SCALEPACK (Bruker AXS, 1997-2009)'
_computing_data_reduction        'DENZO/SCALEPACK (Bruker AXS, 1997-2009)'
_computing_structure_solution    'SHELXS-2016 (Sheldrick 2016)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'XPMA (Zsolnai, Huttner, 1994)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0733P)²+5.7719P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.148(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         24293
_refine_ls_number_parameters     1334
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0597
_refine_ls_wR_factor_ref         0.1597
_refine_ls_wR_factor_gt          0.1392
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
Ni1 Ni 0.75182(9) 0.56781(5) 0.40992(4) 0.0270(2) Uani 1 1 d . . . . .
Ni2 Ni 0.26422(8) 0.55817(5) 0.11658(4) 0.0258(2) Uani 1 1 d . . . . .
Ni3 Ni 0.73372(9) 0.80859(5) 1.15839(4) 0.0258(2) Uani 1 1 d . . . . .
Ni4 Ni 0.24795(9) 0.79615(5) 0.86455(4) 0.0292(3) Uani 1 1 d . . . . .
Cl1 Cl 0.6999(2) 0.63118(12) 0.33912(11) 0.0471(6) Uani 1 1 d . . . . .
Cl2 Cl 0.94248(19) 0.52874(12) 0.39785(10) 0.0373(5) Uani 1 1 d . . . . .
Cl3 Cl 0.4363(2) 0.50213(11) 0.11865(9) 0.0366(5) Uani 1 1 d . . . . .
Cl4 Cl 0.23875(19) 0.60847(10) 0.20038(8) 0.0308(4) Uani 1 1 d . . . . .
Cl5 Cl 0.5617(2) 0.86445(12) 1.15565(10) 0.0385(6) Uani 1 1 d . . . . .
Cl6 Cl 0.7513(2) 0.75849(9) 1.07338(9) 0.0327(5) Uani 1 1 d . . . . .
Cl7 Cl 0.0507(2) 0.83081(13) 0.87015(10) 0.0452(6) Uani 1 1 d . . . . .
Cl8 Cl 0.2918(2) 0.73649(12) 0.93930(11) 0.0498(6) Uani 1 1 d . . . . .
N1 N 0.7458(6) 0.5844(3) 0.4962(3) 0.0232(14) Uani 1 1 d . . . . .
N2 N 0.9075(7) 0.6509(3) 0.5069(3) 0.0337(17) Uani 1 1 d . . . . .
N3 N 0.9141(6) 0.5662(3) 0.5631(3) 0.0279(15) Uani 1 1 d . . . . .
N4 N 0.5857(6) 0.5313(3) 0.4259(3) 0.0238(14) Uani 1 1 d . . . . .
N5 N 0.5272(6) 0.5009(3) 0.3327(3) 0.0247(14) Uani 1 1 d . . . . .
N6 N 0.3902(6) 0.5603(3) 0.3853(3) 0.0272(15) Uani 1 1 d . . . . .
N7 N 0.3107(6) 0.4912(3) 0.5911(3) 0.0258(15) Uani 1 1 d . . . . .
N8 N 0.4935(6) 0.5423(3) 0.6677(3) 0.0277(16) Uani 1 1 d . . . . .
N31 N 0.2588(6) 0.5811(3) 0.0315(3) 0.0235(14) Uani 1 1 d . . . . .
N32 N 0.4080(6) 0.5665(3) -0.0450(3) 0.0264(15) Uani 1 1 d . . . . .
N33 N 0.4400(6) 0.6355(3) 0.0275(3) 0.0278(15) Uani 1 1 d . . . . .
N34 N 0.0918(6) 0.5295(3) 0.0988(3) 0.0264(15) Uani 1 1 d . . . . .
N35 N 0.0284(6) 0.4939(3) 0.1893(3) 0.0245(14) Uani 1 1 d . . . . .
N36 N -0.1022(6) 0.5583(3) 0.1394(3) 0.0287(15) Uani 1 1 d . . . . .
N37 N -0.1820(6) 0.4915(3) -0.0687(3) 0.0260(15) Uani 1 1 d . . . . .
N38 N -0.0063(6) 0.5512(3) -0.1420(3) 0.0253(15) Uani 1 1 d . . . . .
N61 N 0.9071(5) 0.8357(3) 1.1762(3) 0.0236(14) Uani 1 1 d . . . . .
N62 N 0.9735(5) 0.8674(3) 1.0841(3) 0.0226(14) Uani 1 1 d . . . . .
N63 N 1.1032(5) 0.8055(3) 1.1379(3) 0.0235(14) Uani 1 1 d . . . . .
N64 N 0.7402(5) 0.7873(3) 1.2435(3) 0.0235(15) Uani 1 1 d . . . . .
N65 N 0.5847(6) 0.8014(3) 1.3179(3) 0.0256(15) Uani 1 1 d . . . . .
N66 N 0.5610(6) 0.7303(3) 1.2466(3) 0.0252(15) Uani 1 1 d . . . . .
N67 N 1.0034(6) 0.8174(3) 1.4174(3) 0.0263(15) Uani 1 1 d . . . . .
N68 N 1.1821(6) 0.8735(3) 1.3440(3) 0.0273(15) Uani 1 1 d . . . . .
N91 N 0.2643(6) 0.7780(3) 0.7797(3) 0.0253(15) Uani 1 1 d . . . . .
N92 N 0.1093(7) 0.7092(3) 0.7659(3) 0.0341(17) Uani 1 1 d . . . . .
N93 N 0.1037(6) 0.7922(3) 0.7078(3) 0.0289(16) Uani 1 1 d . . . . .
N94 N 0.4097(6) 0.8382(3) 0.8509(3) 0.0270(15) Uani 1 1 d . . . . .
N95 N 0.4477(6) 0.8732(3) 0.9443(3) 0.0283(15) Uani 1 1 d . . . . .
N96 N 0.6077(6) 0.8236(4) 0.8968(3) 0.0344(17) Uani 1 1 d . . . . .
N97 N 0.6944(6) 0.8842(3) 0.6897(3) 0.0267(15) Uani 1 1 d . . . . .
N98 N 0.5301(6) 0.8219(3) 0.6119(3) 0.0276(15) Uani 1 1 d . . . . .
C1 C 0.6467(6) 0.5590(4) 0.5253(3) 0.0219(16) Uani 1 1 d . . . . .
C2 C 0.5523(7) 0.5319(4) 0.4856(3) 0.0228(16) Uani 1 1 d . . . . .
C3 C 0.4442(7) 0.5087(4) 0.5087(3) 0.0230(16) Uani 1 1 d . . . . .
H3 H 0.386332 0.490855 0.483516 0.028 Uiso 1 1 calc R U . . .
C4 C 0.4177(7) 0.5112(4) 0.5706(3) 0.0205(17) Uani 1 1 d . . . . .
C5 C 0.2900(7) 0.4951(4) 0.6504(3) 0.0252(17) Uani 1 1 d . . . . .
C6 C 0.1789(7) 0.4729(4) 0.6758(4) 0.0276(18) Uani 1 1 d . . . . .
H6 H 0.118710 0.454915 0.651877 0.033 Uiso 1 1 calc R U . . .
C7 C 0.1587(8) 0.4777(4) 0.7347(4) 0.0317(19) Uani 1 1 d . . . . .
H7 H 0.084336 0.463433 0.750748 0.038 Uiso 1 1 calc R U . . .
C8 C 0.2510(8) 0.5045(4) 0.7722(4) 0.032(2) Uani 1 1 d . . . . .
H8 H 0.235513 0.508191 0.812400 0.039 Uiso 1 1 calc R U . . .
C9 C 0.3601(8) 0.5244(4) 0.7497(3) 0.0316(19) Uani 1 1 d . . . . .
H9 H 0.420508 0.540446 0.774904 0.038 Uiso 1 1 calc R U . . .
C10 C 0.3844(7) 0.5212(4) 0.6885(3) 0.0277(18) Uani 1 1 d . . . . .
C11 C 0.5113(7) 0.5373(4) 0.6089(3) 0.0239(17) Uani 1 1 d . . . . .
C12 C 0.6239(7) 0.5607(4) 0.5845(3) 0.0258(16) Uani 1 1 d . . . . .
H12 H 0.683425 0.577511 0.609605 0.031 Uiso 1 1 calc R U . . .
C13 C 0.8534(7) 0.6001(4) 0.5228(3) 0.0253(17) Uani 1 1 d . . . . .
C14 C 1.0454(8) 0.6581(5) 0.5021(4) 0.042(2) Uani 1 1 d . . . . .
H14A H 1.078032 0.674896 0.537942 0.062 Uiso 1 1 calc R U . . .
H14B H 1.063952 0.683299 0.469484 0.062 Uiso 1 1 calc R U . . .
H14C H 1.083969 0.620870 0.495800 0.062 Uiso 1 1 calc R U . . .
C15 C 0.8319(9) 0.6976(4) 0.4818(4) 0.044(2) Uani 1 1 d . . . . .
H15A H 0.827894 0.693342 0.439637 0.066 Uiso 1 1 calc R U . . .
H15B H 0.869804 0.734371 0.491514 0.066 Uiso 1 1 calc R U . . .
H15C H 0.748209 0.696032 0.497634 0.066 Uiso 1 1 calc R U . . .
C16 C 0.9914(8) 0.5896(4) 0.6101(4) 0.037(2) Uani 1 1 d . . . . .
H16A H 1.078436 0.580637 0.602872 0.056 Uiso 1 1 calc R U . . .
H16B H 0.966477 0.572720 0.647031 0.056 Uiso 1 1 calc R U . . .
H16C H 0.980768 0.631045 0.611833 0.056 Uiso 1 1 calc R U . . .
C17 C 0.8972(8) 0.5036(4) 0.5632(4) 0.033(2) Uani 1 1 d . . . . .
H17A H 0.848278 0.492484 0.596827 0.050 Uiso 1 1 calc R U . . .
H17B H 0.978228 0.484960 0.565054 0.050 Uiso 1 1 calc R U . . .
H17C H 0.853968 0.491989 0.527652 0.050 Uiso 1 1 calc R U . . .
C18 C 0.5002(7) 0.5305(4) 0.3823(3) 0.0240(17) Uani 1 1 d . . . . .
C19 C 0.4894(7) 0.5204(4) 0.2741(3) 0.0306(19) Uani 1 1 d . . . . .
H19A H 0.430696 0.493112 0.257251 0.046 Uiso 1 1 calc R U . . .
H19B H 0.562436 0.523083 0.249370 0.046 Uiso 1 1 calc R U . . .
H19C H 0.450036 0.557931 0.276839 0.046 Uiso 1 1 calc R U . . .
C20 C 0.6328(7) 0.4596(4) 0.3335(4) 0.0310(19) Uani 1 1 d . . . . .
H20A H 0.708122 0.478784 0.320516 0.047 Uiso 1 1 calc R U . . .
H20B H 0.613952 0.427678 0.307485 0.047 Uiso 1 1 calc R U . . .
H20C H 0.645271 0.445211 0.372899 0.047 Uiso 1 1 calc R U . . .
C21 C 0.2756(7) 0.5431(4) 0.3537(4) 0.035(2) Uani 1 1 d . . . . .
H21A H 0.286171 0.504653 0.337842 0.053 Uiso 1 1 calc R U . . .
H21B H 0.259492 0.569920 0.322033 0.053 Uiso 1 1 calc R U . . .
H21C H 0.205628 0.543290 0.380392 0.053 Uiso 1 1 calc R U . . .
C22 C 0.3794(8) 0.6114(4) 0.4222(4) 0.034(2) Uani 1 1 d . . . . .
H22A H 0.334520 0.601624 0.457549 0.051 Uiso 1 1 calc R U . . .
H22B H 0.334265 0.641201 0.401155 0.051 Uiso 1 1 calc R U . . .
H22C H 0.462172 0.625274 0.432495 0.051 Uiso 1 1 calc R U . . .
C31 C 0.1523(6) 0.5604(4) 0.0014(3) 0.0245(16) Uani 1 1 d . . . . .
C32 C 0.0580(7) 0.5337(4) 0.0389(3) 0.0235(17) Uani 1 1 d . . . . .
C33 C -0.0507(7) 0.5117(4) 0.0151(3) 0.0259(18) Uani 1 1 d . . . . .
H33 H -0.108704 0.493559 0.039628 0.031 Uiso 1 1 calc R U . . .
C34 C -0.0774(6) 0.5159(3) -0.0465(3) 0.0210(16) Uani 1 1 d . . . . .
C35 C -0.1993(7) 0.4967(4) -0.1279(3) 0.0278(18) Uani 1 1 d . . . . .
C36 C -0.3067(7) 0.4704(4) -0.1553(3) 0.0281(18) Uani 1 1 d . . . . .
H36 H -0.364667 0.450647 -0.132015 0.034 Uiso 1 1 calc R U . . .
C37 C -0.3263(8) 0.4734(4) -0.2147(4) 0.033(2) Uani 1 1 d . . . . .
H37 H -0.394702 0.454450 -0.232051 0.040 Uiso 1 1 calc R U . . .
C38 C -0.2405(8) 0.5062(4) -0.2503(3) 0.0324(19) Uani 1 1 d . . . . .
H38 H -0.255392 0.509716 -0.290671 0.039 Uiso 1 1 calc R U . . .
C39 C -0.1386(7) 0.5318(4) -0.2258(3) 0.0283(18) Uani 1 1 d . . . . .
H39 H -0.084239 0.552912 -0.249754 0.034 Uiso 1 1 calc R U . . .
C40 C -0.1119(7) 0.5274(4) -0.1643(3) 0.0244(17) Uani 1 1 d . . . . .
C41 C 0.0135(7) 0.5451(3) -0.0842(3) 0.0224(17) Uani 1 1 d . . . . .
C42 C 0.1257(6) 0.5675(4) -0.0579(3) 0.0237(16) Uani 1 1 d . . . . .
H42 H 0.182766 0.587632 -0.081357 0.028 Uiso 1 1 calc R U . . .
C43 C 0.3670(7) 0.5940(4) 0.0038(3) 0.0231(17) Uani 1 1 d . . . . .
C44 C 0.3848(8) 0.5044(4) -0.0540(4) 0.034(2) Uani 1 1 d . . . . .
H44A H 0.356389 0.487305 -0.017780 0.050 Uiso 1 1 calc R U . . .
H44B H 0.461537 0.485783 -0.066102 0.050 Uiso 1 1 calc R U . . .
H44C H 0.321355 0.499332 -0.084074 0.050 Uiso 1 1 calc R U . . .
C45 C 0.4757(8) 0.5969(4) -0.0915(4) 0.036(2) Uani 1 1 d . . . . .
H45A H 0.476711 0.637843 -0.083200 0.054 Uiso 1 1 calc R U . . .
H45B H 0.434198 0.590183 -0.128717 0.054 Uiso 1 1 calc R U . . .
H45C H 0.560795 0.582649 -0.093195 0.054 Uiso 1 1 calc R U . . .
C46 C 0.3900(8) 0.6793(4) 0.0678(4) 0.0314(19) Uani 1 1 d . . . . .
H46A H 0.303147 0.686845 0.058153 0.047 Uiso 1 1 calc R U . . .
H46B H 0.437872 0.714559 0.064151 0.047 Uiso 1 1 calc R U . . .
H46C H 0.396204 0.665256 0.107685 0.047 Uiso 1 1 calc R U . . .
C47 C 0.5766(8) 0.6341(5) 0.0246(4) 0.040(2) Uani 1 1 d . . . . .
H47A H 0.603555 0.596355 0.011740 0.059 Uiso 1 1 calc R U . . .
H47B H 0.611697 0.642134 0.062954 0.059 Uiso 1 1 calc R U . . .
H47C H 0.605093 0.662995 -0.002928 0.059 Uiso 1 1 calc R U . . .
C48 C 0.0048(7) 0.5267(4) 0.1414(3) 0.0237(17) Uani 1 1 d . . . . .
C49 C -0.0146(8) 0.5100(4) 0.2479(3) 0.0306(19) Uani 1 1 d . . . . .
H49A H -0.056463 0.546984 0.246113 0.046 Uiso 1 1 calc R U . . .
H49B H 0.056649 0.512536 0.274302 0.046 Uiso 1 1 calc R U . . .
H49C H -0.072212 0.481043 0.262087 0.046 Uiso 1 1 calc R U . . .
C50 C 0.1282(8) 0.4499(4) 0.1884(4) 0.033(2) Uani 1 1 d . . . . .
H50A H 0.141914 0.437471 0.148486 0.049 Uiso 1 1 calc R U . . .
H50B H 0.103473 0.417215 0.211974 0.049 Uiso 1 1 calc R U . . .
H50C H 0.204828 0.466253 0.204170 0.049 Uiso 1 1 calc R U . . .
C51 C -0.2224(8) 0.5372(4) 0.1633(4) 0.039(2) Uani 1 1 d . . . . .
H51A H -0.214662 0.496719 0.173264 0.058 Uiso 1 1 calc R U . . .
H51B H -0.288110 0.542021 0.134285 0.058 Uiso 1 1 calc R U . . .
H51C H -0.243022 0.558968 0.198126 0.058 Uiso 1 1 calc R U . . .
C52 C -0.1088(8) 0.6128(4) 0.1068(4) 0.035(2) Uani 1 1 d . . . . .
H52A H -0.025088 0.627546 0.100937 0.052 Uiso 1 1 calc R U . . .
H52B H -0.157127 0.640559 0.128809 0.052 Uiso 1 1 calc R U . . .
H52C H -0.148694 0.606215 0.069145 0.052 Uiso 1 1 calc R U . . .
C61 C 0.9405(7) 0.8331(3) 1.2361(3) 0.0224(16) Uani 1 1 d . . . . .
C62 C 0.8458(7) 0.8078(4) 1.2743(3) 0.0229(16) Uani 1 1 d . . . . .
C63 C 0.8694(7) 0.8030(4) 1.3337(3) 0.0256(17) Uani 1 1 d . . . . .
H63 H 0.809801 0.785159 1.357659 0.031 Uiso 1 1 calc R U . . .
C64 C 0.9805(7) 0.8241(4) 1.3590(3) 0.0241(17) Uani 1 1 d . . . . .
C65 C 1.1117(7) 0.8376(4) 1.4397(3) 0.0271(18) Uani 1 1 d . . . . .
C66 C 1.1394(7) 0.8299(4) 1.5007(3) 0.0314(19) Uani 1 1 d . . . . .
H66 H 1.082886 0.810160 1.524694 0.038 Uiso 1 1 calc R U . . .
C67 C 1.2488(8) 0.8514(4) 1.5239(4) 0.034(2) Uani 1 1 d . . . . .
H67 H 1.266700 0.845986 1.563819 0.041 Uiso 1 1 calc R U . . .
C68 C 1.3355(8) 0.8818(4) 1.4883(3) 0.0304(19) Uani 1 1 d . . . . .
H68 H 1.408923 0.896623 1.505338 0.037 Uiso 1 1 calc R U . . .
C69 C 1.3138(7) 0.8898(4) 1.4296(4) 0.0296(19) Uani 1 1 d . . . . .
H69 H 1.371689 0.910153 1.406927 0.035 Uiso 1 1 calc R U . . .
C70 C 1.2016(7) 0.8668(4) 1.4028(3) 0.0232(17) Uani 1 1 d . . . . .
C71 C 1.0735(7) 0.8519(4) 1.3220(3) 0.0251(19) Uani 1 1 d . . . . .
C72 C 1.0501(7) 0.8556(4) 1.2604(3) 0.0230(17) Uani 1 1 d . . . . .
H72 H 1.109155 0.873280 1.236149 0.028 Uiso 1 1 calc R U . . .
C73 C 0.9960(7) 0.8368(4) 1.1337(3) 0.0231(17) Uani 1 1 d . . . . .
C74 C 1.0199(8) 0.8503(4) 1.0259(3) 0.0315(19) Uani 1 1 d . . . . .
H74A H 1.064957 0.814185 1.029191 0.047 Uiso 1 1 calc R U . . .
H74B H 1.075489 0.879846 1.011199 0.047 Uiso 1 1 calc R U . . .
H74C H 0.949836 0.845644 0.999202 0.047 Uiso 1 1 calc R U . . .
C75 C 0.8697(7) 0.9096(4) 1.0826(4) 0.0284(19) Uani 1 1 d . . . . .
H75A H 0.791947 0.889813 1.073817 0.043 Uiso 1 1 calc R U . . .
H75B H 0.885592 0.938187 1.052654 0.043 Uiso 1 1 calc R U . . .
H75C H 0.863478 0.928423 1.120322 0.043 Uiso 1 1 calc R U . . .
C76 C 1.2249(7) 0.8259(4) 1.1140(4) 0.0316(19) Uani 1 1 d . . . . .
H76A H 1.212920 0.862709 1.094804 0.047 Uiso 1 1 calc R U . . .
H76B H 1.255872 0.798040 1.086083 0.047 Uiso 1 1 calc R U . . .
H76C H 1.284899 0.830154 1.145751 0.047 Uiso 1 1 calc R U . . .
C77 C 1.1116(8) 0.7522(4) 1.1726(4) 0.0301(19) Uani 1 1 d . . . . .
H77A H 1.141312 0.761165 1.211673 0.045 Uiso 1 1 calc R U . . .
H77B H 1.169366 0.725782 1.154053 0.045 Uiso 1 1 calc R U . . .
H77C H 1.029727 0.734442 1.174741 0.045 Uiso 1 1 calc R U . . .
C78 C 0.6312(7) 0.7727(4) 1.2700(3) 0.0264(18) Uani 1 1 d . . . . .
C79 C 0.6073(8) 0.8629(4) 1.3263(4) 0.0305(19) Uani 1 1 d . . . . .
H79A H 0.668826 0.868261 1.357187 0.046 Uiso 1 1 calc R U . . .
H79B H 0.529861 0.881652 1.337093 0.046 Uiso 1 1 calc R U . . .
H79C H 0.638063 0.879460 1.290297 0.046 Uiso 1 1 calc R U . . .
C80 C 0.5132(8) 0.7724(4) 1.3636(4) 0.036(2) Uani 1 1 d . . . . .
H80A H 0.425679 0.782826 1.359918 0.054 Uiso 1 1 calc R U . . .
H80B H 0.544412 0.784123 1.401685 0.054 Uiso 1 1 calc R U . . .
H80C H 0.521972 0.731045 1.359411 0.054 Uiso 1 1 calc R U . . .
C81 C 0.6145(7) 0.6866(4) 1.2079(3) 0.0297(19) Uani 1 1 d . . . . .
H81A H 0.611869 0.700362 1.167888 0.045 Uiso 1 1 calc R U . . .
H81B H 0.566448 0.651290 1.210853 0.045 Uiso 1 1 calc R U . . .
H81C H 0.700424 0.679178 1.219364 0.045 Uiso 1 1 calc R U . . .
C82 C 0.4225(7) 0.7315(5) 1.2482(4) 0.039(2) Uani 1 1 d . . . . .
H82A H 0.392868 0.701685 1.274400 0.058 Uiso 1 1 calc R U . . .
H82B H 0.389292 0.724779 1.209251 0.058 Uiso 1 1 calc R U . . .
H82C H 0.394784 0.768787 1.262108 0.058 Uiso 1 1 calc R U . . .
C91 C 0.3662(7) 0.8049(4) 0.7521(3) 0.0265(17) Uani 1 1 d . . . . .
C92 C 0.4506(7) 0.8362(4) 0.7911(3) 0.0244(17) Uani 1 1 d . . . . .
C93 C 0.5569(7) 0.8630(4) 0.7707(3) 0.0255(18) Uani 1 1 d . . . . .
H93 H 0.608504 0.884056 0.796392 0.031 Uiso 1 1 calc R U . . .
C94 C 0.5879(7) 0.8584(4) 0.7093(3) 0.0241(17) Uani 1 1 d . . . . .
C95 C 0.7178(7) 0.8786(4) 0.6315(3) 0.0263(17) Uani 1 1 d . . . . .
C96 C 0.8284(7) 0.9057(4) 0.6081(4) 0.0310(19) Uani 1 1 d . . . . .
H96 H 0.882759 0.926029 0.633093 0.037 Uiso 1 1 calc R U . . .
C97 C 0.8549(8) 0.9018(4) 0.5486(4) 0.032(2) Uani 1 1 d . . . . .
H97 H 0.926478 0.919674 0.533449 0.038 Uiso 1 1 calc R U . . .
C98 C 0.7726(8) 0.8706(4) 0.5107(4) 0.035(2) Uani 1 1 d . . . . .
H98 H 0.791272 0.867956 0.470753 0.041 Uiso 1 1 calc R U . . .
C99 C 0.6668(7) 0.8444(4) 0.5314(3) 0.0309(19) Uani 1 1 d . . . . .
H99 H 0.613746 0.824230 0.505696 0.037 Uiso 1 1 calc R U . . .
C100 C 0.6372(7) 0.8479(4) 0.5930(3) 0.0264(17) Uani 1 1 d . . . . .
C101 C 0.5067(7) 0.8266(4) 0.6695(3) 0.0284(18) Uani 1 1 d . . . . .
C102 C 0.3942(7) 0.8007(4) 0.6929(3) 0.0272(17) Uani 1 1 d . . . . .
H102 H 0.339377 0.780888 0.667678 0.033 Uiso 1 1 calc R U . . .
C103 C 0.1597(7) 0.7601(4) 0.7493(3) 0.0275(18) Uani 1 1 d . . . . .
C104 C 0.1872(9) 0.6633(4) 0.7936(5) 0.048(3) Uani 1 1 d . . . . .
H10A H 0.272779 0.666783 0.780411 0.072 Uiso 1 1 calc R U . . .
H10B H 0.154629 0.625795 0.782651 0.072 Uiso 1 1 calc R U . . .
H10C H 0.184857 0.667385 0.835788 0.072 Uiso 1 1 calc R U . . .
C105 C -0.0260(8) 0.6992(5) 0.7654(4) 0.045(2) Uani 1 1 d . . . . .
H10D H -0.069303 0.735801 0.763306 0.068 Uiso 1 1 calc R U . . .
H10E H -0.049601 0.679182 0.800858 0.068 Uiso 1 1 calc R U . . .
H10F H -0.048453 0.675934 0.731694 0.068 Uiso 1 1 calc R U . . .
C106 C 0.1175(8) 0.8554(4) 0.7070(4) 0.032(2) Uani 1 1 d . . . . .
H10G H 0.150792 0.868320 0.744293 0.048 Uiso 1 1 calc R U . . .
H10H H 0.036551 0.873054 0.700102 0.048 Uiso 1 1 calc R U . . .
H10I H 0.174156 0.866370 0.676027 0.048 Uiso 1 1 calc R U . . .
C107 C 0.0341(9) 0.7676(5) 0.6586(4) 0.040(2) Uani 1 1 d . . . . .
H10J H 0.050832 0.726662 0.656212 0.061 Uiso 1 1 calc R U . . .
H10K H 0.059801 0.786129 0.622614 0.061 Uiso 1 1 calc R U . . .
H10L H -0.054655 0.773769 0.664263 0.061 Uiso 1 1 calc R U . . .
C108 C 0.4896(7) 0.8459(4) 0.8957(3) 0.0268(18) Uani 1 1 d . . . . .
C109 C 0.3385(8) 0.9109(5) 0.9407(4) 0.039(2) Uani 1 1 d . . . . .
H10M H 0.331178 0.926467 0.901481 0.058 Uiso 1 1 calc R U . . .
H10N H 0.347942 0.942256 0.968453 0.058 Uiso 1 1 calc R U . . .
H10O H 0.263886 0.889095 0.949851 0.058 Uiso 1 1 calc R U . . .
C110 C 0.4863(8) 0.8561(5) 1.0042(4) 0.038(2) Uani 1 1 d . . . . .
H11A H 0.533992 0.820641 1.002500 0.057 Uiso 1 1 calc R U . . .
H11B H 0.412637 0.850210 1.027934 0.057 Uiso 1 1 calc R U . . .
H11C H 0.537427 0.886227 1.021405 0.057 Uiso 1 1 calc R U . . .
C111 C 0.6390(9) 0.7707(5) 0.8648(4) 0.046(2) Uani 1 1 d . . . . .
H11D H 0.562735 0.751696 0.852284 0.070 Uiso 1 1 calc R U . . .
H11E H 0.686442 0.745241 0.890194 0.070 Uiso 1 1 calc R U . . .
H11F H 0.688592 0.780395 0.830873 0.070 Uiso 1 1 calc R U . . .
C112 C 0.7116(7) 0.8518(5) 0.9298(4) 0.042(2) Uani 1 1 d . . . . .
H11G H 0.696523 0.892879 0.931959 0.063 Uiso 1 1 calc R U . . .
H11H H 0.789914 0.844733 0.910040 0.063 Uiso 1 1 calc R U . . .
H11I H 0.715876 0.835949 0.969061 0.063 Uiso 1 1 calc R U . . .
N201 N 1.1960(9) 0.7202(4) 1.3576(4) 0.052(2) Uani 1 1 d . . . . .
N301 N 0.2754(10) 0.6608(5) 0.6329(5) 0.068(3) Uani 1 1 d . . . . .
N401 N -0.2103(10) 0.6466(4) -0.0970(6) 0.074(3) Uani 1 1 d . . . . .
N501 N -0.2634(10) 0.6972(5) 0.6477(6) 0.074(3) Uani 1 1 d . . . . .
C201 C 1.1161(9) 0.6965(4) 1.3342(4) 0.037(2) Uani 1 1 d . . . . .
C202 C 1.0151(9) 0.6639(4) 1.3055(5) 0.045(2) Uani 1 1 d . . . . .
H20D H 1.043627 0.649801 1.268025 0.067 Uiso 1 1 calc R U . . .
H20E H 0.943319 0.688794 1.299667 0.067 Uiso 1 1 calc R U . . .
H20F H 0.991704 0.631590 1.329988 0.067 Uiso 1 1 calc R U . . .
C301 C 0.3457(11) 0.6753(5) 0.5976(6) 0.057(3) Uani 1 1 d . . . . .
C302 C 0.4346(11) 0.6946(5) 0.5535(5) 0.065(3) Uani 1 1 d . . . . .
H30A H 0.481434 0.727268 0.568534 0.097 Uiso 1 1 calc R U . . .
H30B H 0.389624 0.705961 0.518372 0.097 Uiso 1 1 calc R U . . .
H30C H 0.491713 0.663538 0.544406 0.097 Uiso 1 1 calc R U . . .
C401 C -0.1348(11) 0.6703(5) -0.0704(6) 0.057(3) Uani 1 1 d . . . . .
C402 C -0.0388(12) 0.6997(5) -0.0388(5) 0.065(3) Uani 1 1 d . . . . .
H40A H 0.032281 0.674227 -0.033481 0.098 Uiso 1 1 calc R U . . .
H40B H -0.070077 0.711305 -0.000933 0.098 Uiso 1 1 calc R U . . .
H40C H -0.013120 0.733486 -0.060538 0.098 Uiso 1 1 calc R U . . .
C501 C -0.3252(11) 0.6835(6) 0.6884(7) 0.065(4) Uani 1 1 d . . . . .
C502 C -0.4001(12) 0.6651(6) 0.7377(6) 0.070(4) Uani 1 1 d . . . . .
H50D H -0.439864 0.628617 0.728625 0.104 Uiso 1 1 calc R U . . .
H50E H -0.463621 0.693791 0.745614 0.104 Uiso 1 1 calc R U . . .
H50F H -0.346782 0.660580 0.771928 0.104 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
Ni1 N4 1.985(6) . ?
Ni1 N1 1.991(6) . ?
Ni1 Cl2 2.229(2) . ?
Ni1 Cl1 2.231(2) . ?
Ni2 N34 1.980(6) . ?
Ni2 N31 1.998(6) . ?
Ni2 Cl3 2.232(2) . ?
Ni2 Cl4 2.240(2) . ?
Ni3 N61 1.978(6) . ?
Ni3 N64 1.988(6) . ?
Ni3 Cl5 2.230(2) . ?
Ni3 Cl6 2.252(2) . ?
Ni4 N91 1.974(6) . ?
Ni4 N94 1.994(7) . ?
Ni4 Cl8 2.224(3) . ?
Ni4 Cl7 2.240(2) . ?
N1 C13 1.336(9) . ?
N1 C1 1.374(9) . ?
N2 C13 1.351(11) . ?
N2 C15 1.453(12) . ?
N2 C14 1.475(10) . ?
N3 C13 1.356(10) . ?
N3 C16 1.443(10) . ?
N3 C17 1.450(12) . ?
N4 C18 1.334(9) . ?
N4 C2 1.399(9) . ?
N5 C18 1.345(10) . ?
N5 C19 1.454(9) . ?
N5 C20 1.468(10) . ?
N6 C18 1.354(10) . ?
N6 C22 1.448(11) . ?
N6 C21 1.459(9) . ?
N7 C4 1.312(10) . ?
N7 C5 1.365(10) . ?
N8 C10 1.343(10) . ?
N8 C11 1.351(10) . ?
N31 C43 1.344(9) . ?
N31 C31 1.396(9) . ?
N32 C43 1.347(9) . ?
N32 C45 1.457(10) . ?
N32 C44 1.464(11) . ?
N33 C43 1.338(10) . ?
N33 C47 1.450(10) . ?
N33 C46 1.460(10) . ?
N34 C48 1.340(9) . ?
N34 C32 1.402(9) . ?
N35 C48 1.342(10) . ?
N35 C49 1.455(9) . ?
N35 C50 1.464(11) . ?
N36 C48 1.347(10) . ?
N36 C52 1.455(12) . ?
N36 C51 1.471(10) . ?
N37 C34 1.336(9) . ?
N37 C35 1.357(10) . ?
N38 C41 1.330(9) . ?
N38 C40 1.340(10) . ?
N61 C73 1.353(9) . ?
N61 C61 1.399(9) . ?
N62 C73 1.344(10) . ?
N62 C74 1.464(9) . ?
N62 C75 1.466(10) . ?
N63 C73 1.347(10) . ?
N63 C77 1.457(11) . ?
N63 C76 1.478(9) . ?
N64 C78 1.348(10) . ?
N64 C62 1.396(9) . ?
N65 C78 1.364(10) . ?
N65 C79 1.445(11) . ?
N65 C80 1.450(10) . ?
N66 C78 1.334(10) . ?
N66 C81 1.452(10) . ?
N66 C82 1.468(10) . ?
N67 C65 1.332(10) . ?
N67 C64 1.351(9) . ?
N68 C71 1.345(10) . ?
N68 C70 1.353(9) . ?
N91 C103 1.363(10) . ?
N91 C91 1.397(10) . ?
N92 C103 1.341(11) . ?
N92 C105 1.451(10) . ?
N92 C104 1.476(12) . ?
N93 C103 1.332(10) . ?
N93 C107 1.446(10) . ?
N93 C106 1.460(11) . ?
N94 C108 1.327(9) . ?
N94 C92 1.426(9) . ?
N95 C108 1.346(10) . ?
N95 C109 1.448(11) . ?
N95 C110 1.467(10) . ?
N96 C108 1.351(10) . ?
N96 C111 1.455(12) . ?
N96 C112 1.475(11) . ?
N97 C95 1.349(10) . ?
N97 C94 1.352(10) . ?
N98 C101 1.334(10) . ?
N98 C100 1.355(10) . ?
C1 C12 1.366(10) . ?
C1 C2 1.475(10) . ?
C2 C3 1.371(10) . ?
C3 C4 1.431(10) . ?
C3 H3 0.9300 . ?
C4 C11 1.442(10) . ?
C5 C6 1.408(11) . ?
C5 C10 1.446(10) . ?
C6 C7 1.357(11) . ?
C6 H6 0.9300 . ?
C7 C8 1.429(12) . ?
C7 H7 0.9300 . ?
C8 C9 1.347(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.413(11) . ?
C9 H9 0.9300 . ?
C11 C12 1.422(11) . ?
C12 H12 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C31 C42 1.379(10) . ?
C31 C32 1.453(10) . ?
C32 C33 1.365(10) . ?
C33 C34 1.424(10) . ?
C33 H33 0.9300 . ?
C34 C41 1.455(10) . ?
C35 C36 1.426(11) . ?
C35 C40 1.430(11) . ?
C36 C37 1.361(11) . ?
C36 H36 0.9300 . ?
C37 C38 1.433(12) . ?
C37 H37 0.9300 . ?
C38 C39 1.345(11) . ?
C38 H38 0.9300 . ?
C39 C40 1.423(10) . ?
C39 H39 0.9300 . ?
C41 C42 1.423(10) . ?
C42 H42 0.9300 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C61 C72 1.382(10) . ?
C61 C62 1.451(11) . ?
C62 C63 1.370(10) . ?
C63 C64 1.392(10) . ?
C63 H63 0.9300 . ?
C64 C71 1.448(11) . ?
C65 C66 1.419(10) . ?
C65 C70 1.439(11) . ?
C66 C67 1.362(11) . ?
C66 H66 0.9300 . ?
C67 C68 1.411(12) . ?
C67 H67 0.9300 . ?
C68 C69 1.359(11) . ?
C68 H68 0.9300 . ?
C69 C70 1.431(10) . ?
C69 H69 0.9300 . ?
C71 C72 1.415(10) . ?
C72 H72 0.9300 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
C75 H75A 0.9600 . ?
C75 H75B 0.9600 . ?
C75 H75C 0.9600 . ?
C76 H76A 0.9600 . ?
C76 H76B 0.9600 . ?
C76 H76C 0.9600 . ?
C77 H77A 0.9600 . ?
C77 H77B 0.9600 . ?
C77 H77C 0.9600 . ?
C79 H79A 0.9600 . ?
C79 H79B 0.9600 . ?
C79 H79C 0.9600 . ?
C80 H80A 0.9600 . ?
C80 H80B 0.9600 . ?
C80 H80C 0.9600 . ?
C81 H81A 0.9600 . ?
C81 H81B 0.9600 . ?
C81 H81C 0.9600 . ?
C82 H82A 0.9600 . ?
C82 H82B 0.9600 . ?
C82 H82C 0.9600 . ?
C91 C102 1.378(10) . ?
C91 C92 1.443(11) . ?
C92 C93 1.367(11) . ?
C93 C94 1.436(10) . ?
C93 H93 0.9300 . ?
C94 C101 1.439(11) . ?
C95 C100 1.405(11) . ?
C95 C96 1.433(11) . ?
C96 C97 1.381(11) . ?
C96 H96 0.9300 . ?
C97 C98 1.412(12) . ?
C97 H97 0.9300 . ?
C98 C99 1.359(12) . ?
C98 H98 0.9300 . ?
C99 C100 1.433(11) . ?
C99 H99 0.9300 . ?
C101 C102 1.436(11) . ?
C102 H102 0.9300 . ?
C104 H10A 0.9600 . ?
C104 H10B 0.9600 . ?
C104 H10C 0.9600 . ?
C105 H10D 0.9600 . ?
C105 H10E 0.9600 . ?
C105 H10F 0.9600 . ?
C106 H10G 0.9600 . ?
C106 H10H 0.9600 . ?
C106 H10I 0.9600 . ?
C107 H10J 0.9600 . ?
C107 H10K 0.9600 . ?
C107 H10L 0.9600 . ?
C109 H10M 0.9600 . ?
C109 H10N 0.9600 . ?
C109 H10O 0.9600 . ?
C110 H11A 0.9600 . ?
C110 H11B 0.9600 . ?
C110 H11C 0.9600 . ?
C111 H11D 0.9600 . ?
C111 H11E 0.9600 . ?
C111 H11F 0.9600 . ?
C112 H11G 0.9600 . ?
C112 H11H 0.9600 . ?
C112 H11I 0.9600 . ?
N201 C201 1.133(12) . ?
N301 C301 1.146(16) . ?
N401 C401 1.136(16) . ?
N501 C501 1.176(17) . ?
C201 C202 1.456(14) . ?
C202 H20D 0.9600 . ?
C202 H20E 0.9600 . ?
C202 H20F 0.9600 . ?
C301 C302 1.447(18) . ?
C302 H30A 0.9600 . ?
C302 H30B 0.9600 . ?
C302 H30C 0.9600 . ?
C401 C402 1.412(18) . ?
C402 H40A 0.9600 . ?
C402 H40B 0.9600 . ?
C402 H40C 0.9600 . ?
C501 C502 1.440(19) . ?
C502 H50D 0.9600 . ?
C502 H50E 0.9600 . ?
C502 H50F 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
N4 Ni1 N1 82.3(2) . . ?
N4 Ni1 Cl2 131.1(2) . . ?
N1 Ni1 Cl2 103.51(19) . . ?
N4 Ni1 Cl1 101.15(19) . . ?
N1 Ni1 Cl1 124.7(2) . . ?
Cl2 Ni1 Cl1 113.16(10) . . ?
N34 Ni2 N31 82.6(3) . . ?
N34 Ni2 Cl3 124.3(2) . . ?
N31 Ni2 Cl3 100.93(19) . . ?
N34 Ni2 Cl4 103.12(19) . . ?
N31 Ni2 Cl4 132.7(2) . . ?
Cl3 Ni2 Cl4 112.58(9) . . ?
N61 Ni3 N64 81.6(2) . . ?
N61 Ni3 Cl5 125.6(2) . . ?
N64 Ni3 Cl5 101.0(2) . . ?
N61 Ni3 Cl6 104.65(19) . . ?
N64 Ni3 Cl6 134.4(2) . . ?
Cl5 Ni3 Cl6 110.11(9) . . ?
N91 Ni4 N94 82.5(3) . . ?
N91 Ni4 Cl8 126.2(2) . . ?
N94 Ni4 Cl8 104.0(2) . . ?
N91 Ni4 Cl7 102.67(19) . . ?
N94 Ni4 Cl7 129.7(2) . . ?
Cl8 Ni4 Cl7 111.44(11) . . ?
C13 N1 C1 123.4(6) . . ?
C13 N1 Ni1 117.5(5) . . ?
C1 N1 Ni1 114.8(5) . . ?
C13 N2 C15 120.7(7) . . ?
C13 N2 C14 122.6(8) . . ?
C15 N2 C14 115.5(7) . . ?
C13 N3 C16 123.0(8) . . ?
C13 N3 C17 120.9(7) . . ?
C16 N3 C17 116.0(7) . . ?
C18 N4 C2 122.6(6) . . ?
C18 N4 Ni1 117.9(5) . . ?
C2 N4 Ni1 113.7(5) . . ?
C18 N5 C19 123.2(7) . . ?
C18 N5 C20 119.0(6) . . ?
C19 N5 C20 114.5(6) . . ?
C18 N6 C22 120.7(6) . . ?
C18 N6 C21 123.5(7) . . ?
C22 N6 C21 115.7(7) . . ?
C4 N7 C5 118.1(7) . . ?
C10 N8 C11 116.3(6) . . ?
C43 N31 C31 122.5(6) . . ?
C43 N31 Ni2 119.3(5) . . ?
C31 N31 Ni2 113.4(5) . . ?
C43 N32 C45 122.1(7) . . ?
C43 N32 C44 121.2(7) . . ?
C45 N32 C44 116.7(7) . . ?
C43 N33 C47 122.6(7) . . ?
C43 N33 C46 122.1(6) . . ?
C47 N33 C46 114.3(7) . . ?
C48 N34 C32 121.8(6) . . ?
C48 N34 Ni2 120.5(5) . . ?
C32 N34 Ni2 113.7(5) . . ?
C48 N35 C49 122.5(7) . . ?
C48 N35 C50 120.5(7) . . ?
C49 N35 C50 114.8(6) . . ?
C48 N36 C52 121.3(7) . . ?
C48 N36 C51 122.7(8) . . ?
C52 N36 C51 115.7(7) . . ?
C34 N37 C35 116.1(7) . . ?
C41 N38 C40 116.9(7) . . ?
C73 N61 C61 121.2(6) . . ?
C73 N61 Ni3 120.8(5) . . ?
C61 N61 Ni3 114.3(5) . . ?
C73 N62 C74 123.5(7) . . ?
C73 N62 C75 119.6(6) . . ?
C74 N62 C75 114.4(6) . . ?
C73 N63 C77 122.4(6) . . ?
C73 N63 C76 122.8(7) . . ?
C77 N63 C76 114.4(6) . . ?
C78 N64 C62 123.1(6) . . ?
C78 N64 Ni3 118.0(5) . . ?
C62 N64 Ni3 115.0(5) . . ?
C78 N65 C79 121.2(7) . . ?
C78 N65 C80 122.6(7) . . ?
C79 N65 C80 116.2(7) . . ?
C78 N66 C81 121.8(7) . . ?
C78 N66 C82 122.1(7) . . ?
C81 N66 C82 115.0(7) . . ?
C65 N67 C64 118.6(7) . . ?
C71 N68 C70 116.5(7) . . ?
C103 N91 C91 122.4(6) . . ?
C103 N91 Ni4 118.5(5) . . ?
C91 N91 Ni4 114.6(5) . . ?
C103 N92 C105 122.1(8) . . ?
C103 N92 C104 121.4(7) . . ?
C105 N92 C104 116.0(8) . . ?
C103 N93 C107 123.3(8) . . ?
C103 N93 C106 121.1(7) . . ?
C107 N93 C106 115.5(7) . . ?
C108 N94 C92 122.2(7) . . ?
C108 N94 Ni4 119.3(5) . . ?
C92 N94 Ni4 113.5(5) . . ?
C108 N95 C109 120.1(7) . . ?
C108 N95 C110 122.7(7) . . ?
C109 N95 C110 115.4(7) . . ?
C108 N96 C111 121.5(7) . . ?
C108 N96 C112 122.0(8) . . ?
C111 N96 C112 116.5(7) . . ?
C95 N97 C94 116.0(7) . . ?
C101 N98 C100 115.8(7) . . ?
C12 C1 N1 126.9(7) . . ?
C12 C1 C2 119.1(7) . . ?
N1 C1 C2 113.8(6) . . ?
C3 C2 N4 125.7(7) . . ?
C3 C2 C1 119.7(6) . . ?
N4 C2 C1 114.6(6) . . ?
C2 C3 C4 121.9(7) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
N7 C4 C3 120.6(7) . . ?
N7 C4 C11 121.7(7) . . ?
C3 C4 C11 117.7(7) . . ?
N7 C5 C6 121.2(7) . . ?
N7 C5 C10 119.9(7) . . ?
C6 C5 C10 118.9(7) . . ?
C7 C6 C5 120.7(8) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C8 120.4(8) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 120.5(7) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 121.1(7) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
N8 C10 C9 119.3(7) . . ?
N8 C10 C5 122.2(7) . . ?
C9 C10 C5 118.4(7) . . ?
N8 C11 C12 118.3(7) . . ?
N8 C11 C4 121.8(7) . . ?
C12 C11 C4 119.9(7) . . ?
C1 C12 C11 121.7(7) . . ?
C1 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
N1 C13 N2 118.4(7) . . ?
N1 C13 N3 123.1(7) . . ?
N2 C13 N3 118.4(7) . . ?
N2 C14 H14A 109.5 . . ?
N2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 H15A 109.5 . . ?
N2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N3 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 H17A 109.5 . . ?
N3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 C18 N5 118.5(7) . . ?
N4 C18 N6 122.4(7) . . ?
N5 C18 N6 119.0(7) . . ?
N5 C19 H19A 109.5 . . ?
N5 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N5 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N5 C20 H20A 109.5 . . ?
N5 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N5 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N6 C21 H21A 109.5 . . ?
N6 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N6 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N6 C22 H22A 109.5 . . ?
N6 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N6 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C42 C31 N31 126.3(7) . . ?
C42 C31 C32 118.9(6) . . ?
N31 C31 C32 114.5(6) . . ?
C33 C32 N34 124.4(7) . . ?
C33 C32 C31 120.5(7) . . ?
N34 C32 C31 115.0(6) . . ?
C32 C33 C34 121.5(7) . . ?
C32 C33 H33 119.3 . . ?
C34 C33 H33 119.3 . . ?
N37 C34 C33 119.8(7) . . ?
N37 C34 C41 121.6(7) . . ?
C33 C34 C41 118.6(6) . . ?
N37 C35 C36 119.5(7) . . ?
N37 C35 C40 122.0(7) . . ?
C36 C35 C40 118.5(7) . . ?
C37 C36 C35 121.5(8) . . ?
C37 C36 H36 119.3 . . ?
C35 C36 H36 119.3 . . ?
C36 C37 C38 119.4(8) . . ?
C36 C37 H37 120.3 . . ?
C38 C37 H37 120.3 . . ?
C39 C38 C37 120.6(8) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C38 C39 C40 121.6(8) . . ?
C38 C39 H39 119.2 . . ?
C40 C39 H39 119.2 . . ?
N38 C40 C39 120.0(7) . . ?
N38 C40 C35 121.8(7) . . ?
C39 C40 C35 118.3(7) . . ?
N38 C41 C42 119.8(7) . . ?
N38 C41 C34 121.7(6) . . ?
C42 C41 C34 118.4(6) . . ?
C31 C42 C41 121.8(7) . . ?
C31 C42 H42 119.1 . . ?
C41 C42 H42 119.1 . . ?
N33 C43 N31 117.6(7) . . ?
N33 C43 N32 118.3(7) . . ?
N31 C43 N32 124.1(7) . . ?
N32 C44 H44A 109.5 . . ?
N32 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N32 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N32 C45 H45A 109.5 . . ?
N32 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N32 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N33 C46 H46A 109.5 . . ?
N33 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N33 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N33 C47 H47A 109.5 . . ?
N33 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N33 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N35 C48 N34 118.9(7) . . ?
N35 C48 N36 118.8(7) . . ?
N34 C48 N36 122.2(7) . . ?
N35 C49 H49A 109.5 . . ?
N35 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
N35 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N35 C50 H50A 109.5 . . ?
N35 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
N35 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N36 C51 H51A 109.5 . . ?
N36 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
N36 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N36 C52 H52A 109.5 . . ?
N36 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
N36 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C72 C61 N61 125.2(7) . . ?
C72 C61 C62 119.6(6) . . ?
N61 C61 C62 115.1(6) . . ?
C63 C62 N64 127.0(7) . . ?
C63 C62 C61 119.8(7) . . ?
N64 C62 C61 113.1(6) . . ?
C62 C63 C64 121.5(7) . . ?
C62 C63 H63 119.3 . . ?
C64 C63 H63 119.3 . . ?
N67 C64 C63 120.5(7) . . ?
N67 C64 C71 119.9(6) . . ?
C63 C64 C71 119.5(7) . . ?
N67 C65 C66 119.7(7) . . ?
N67 C65 C70 120.9(7) . . ?
C66 C65 C70 119.4(7) . . ?
C67 C66 C65 119.9(8) . . ?
C67 C66 H66 120.0 . . ?
C65 C66 H66 120.0 . . ?
C66 C67 C68 121.0(8) . . ?
C66 C67 H67 119.5 . . ?
C68 C67 H67 119.5 . . ?
C69 C68 C67 121.3(7) . . ?
C69 C68 H68 119.4 . . ?
C67 C68 H68 119.4 . . ?
C68 C69 C70 119.9(8) . . ?
C68 C69 H69 120.0 . . ?
C70 C69 H69 120.0 . . ?
N68 C70 C69 119.7(7) . . ?
N68 C70 C65 121.8(7) . . ?
C69 C70 C65 118.5(7) . . ?
N68 C71 C72 119.1(7) . . ?
N68 C71 C64 122.1(7) . . ?
C72 C71 C64 118.8(7) . . ?
C61 C72 C71 120.7(7) . . ?
C61 C72 H72 119.6 . . ?
C71 C72 H72 119.6 . . ?
N62 C73 N63 118.9(7) . . ?
N62 C73 N61 118.9(7) . . ?
N63 C73 N61 122.1(7) . . ?
N62 C74 H74A 109.5 . . ?
N62 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
N62 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
N62 C75 H75A 109.5 . . ?
N62 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
N62 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
N63 C76 H76A 109.5 . . ?
N63 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
N63 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
N63 C77 H77A 109.5 . . ?
N63 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
N63 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
N66 C78 N64 118.8(7) . . ?
N66 C78 N65 117.7(7) . . ?
N64 C78 N65 123.3(7) . . ?
N65 C79 H79A 109.5 . . ?
N65 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
N65 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
N65 C80 H80A 109.5 . . ?
N65 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
N65 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
N66 C81 H81A 109.5 . . ?
N66 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
N66 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
N66 C82 H82A 109.5 . . ?
N66 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
N66 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C102 C91 N91 125.3(7) . . ?
C102 C91 C92 119.5(7) . . ?
N91 C91 C92 115.1(6) . . ?
C93 C92 N94 124.2(7) . . ?
C93 C92 C91 121.8(7) . . ?
N94 C92 C91 113.9(7) . . ?
C92 C93 C94 119.2(7) . . ?
C92 C93 H93 120.4 . . ?
C94 C93 H93 120.4 . . ?
N97 C94 C93 118.8(7) . . ?
N97 C94 C101 120.9(7) . . ?
C93 C94 C101 120.2(7) . . ?
N97 C95 C100 122.6(7) . . ?
N97 C95 C96 118.5(7) . . ?
C100 C95 C96 118.9(7) . . ?
C97 C96 C95 120.4(8) . . ?
C97 C96 H96 119.8 . . ?
C95 C96 H96 119.8 . . ?
C96 C97 C98 119.7(8) . . ?
C96 C97 H97 120.2 . . ?
C98 C97 H97 120.2 . . ?
C99 C98 C97 121.5(8) . . ?
C99 C98 H98 119.2 . . ?
C97 C98 H98 119.2 . . ?
C98 C99 C100 119.8(8) . . ?
C98 C99 H99 120.1 . . ?
C100 C99 H99 120.1 . . ?
N98 C100 C95 122.1(7) . . ?
N98 C100 C99 118.2(7) . . ?
C95 C100 C99 119.7(7) . . ?
N98 C101 C102 119.2(7) . . ?
N98 C101 C94 122.5(7) . . ?
C102 C101 C94 118.3(7) . . ?
C91 C102 C101 121.0(7) . . ?
C91 C102 H102 119.5 . . ?
C101 C102 H102 119.5 . . ?
N93 C103 N92 120.4(7) . . ?
N93 C103 N91 123.0(8) . . ?
N92 C103 N91 116.5(7) . . ?
N92 C104 H10A 109.5 . . ?
N92 C104 H10B 109.5 . . ?
H10A C104 H10B 109.5 . . ?
N92 C104 H10C 109.5 . . ?
H10A C104 H10C 109.5 . . ?
H10B C104 H10C 109.5 . . ?
N92 C105 H10D 109.5 . . ?
N92 C105 H10E 109.5 . . ?
H10D C105 H10E 109.5 . . ?
N92 C105 H10F 109.5 . . ?
H10D C105 H10F 109.5 . . ?
H10E C105 H10F 109.5 . . ?
N93 C106 H10G 109.5 . . ?
N93 C106 H10H 109.5 . . ?
H10G C106 H10H 109.5 . . ?
N93 C106 H10I 109.5 . . ?
H10G C106 H10I 109.5 . . ?
H10H C106 H10I 109.5 . . ?
N93 C107 H10J 109.5 . . ?
N93 C107 H10K 109.5 . . ?
H10J C107 H10K 109.5 . . ?
N93 C107 H10L 109.5 . . ?
H10J C107 H10L 109.5 . . ?
H10K C107 H10L 109.5 . . ?
N94 C108 N95 118.3(7) . . ?
N94 C108 N96 123.3(7) . . ?
N95 C108 N96 118.2(7) . . ?
N95 C109 H10M 109.5 . . ?
N95 C109 H10N 109.5 . . ?
H10M C109 H10N 109.5 . . ?
N95 C109 H10O 109.5 . . ?
H10M C109 H10O 109.5 . . ?
H10N C109 H10O 109.5 . . ?
N95 C110 H11A 109.5 . . ?
N95 C110 H11B 109.5 . . ?
H11A C110 H11B 109.5 . . ?
N95 C110 H11C 109.5 . . ?
H11A C110 H11C 109.5 . . ?
H11B C110 H11C 109.5 . . ?
N96 C111 H11D 109.5 . . ?
N96 C111 H11E 109.5 . . ?
H11D C111 H11E 109.5 . . ?
N96 C111 H11F 109.5 . . ?
H11D C111 H11F 109.5 . . ?
H11E C111 H11F 109.5 . . ?
N96 C112 H11G 109.5 . . ?
N96 C112 H11H 109.5 . . ?
H11G C112 H11H 109.5 . . ?
N96 C112 H11I 109.5 . . ?
H11G C112 H11I 109.5 . . ?
H11H C112 H11I 109.5 . . ?
N201 C201 C202 177.7(11) . . ?
C201 C202 H20D 109.5 . . ?
C201 C202 H20E 109.5 . . ?
H20D C202 H20E 109.5 . . ?
C201 C202 H20F 109.5 . . ?
H20D C202 H20F 109.5 . . ?
H20E C202 H20F 109.5 . . ?
N301 C301 C302 178.9(13) . . ?
C301 C302 H30A 109.5 . . ?
C301 C302 H30B 109.5 . . ?
H30A C302 H30B 109.5 . . ?
C301 C302 H30C 109.5 . . ?
H30A C302 H30C 109.5 . . ?
H30B C302 H30C 109.5 . . ?
N401 C401 C402 178.3(13) . . ?
C401 C402 H40A 109.5 . . ?
C401 C402 H40B 109.5 . . ?
H40A C402 H40B 109.5 . . ?
C401 C402 H40C 109.5 . . ?
H40A C402 H40C 109.5 . . ?
H40B C402 H40C 109.5 . . ?
N501 C501 C502 178.4(14) . . ?
C501 C502 H50D 109.5 . . ?
C501 C502 H50E 109.5 . . ?
H50D C502 H50E 109.5 . . ?
C501 C502 H50F 109.5 . . ?
H50D C502 H50F 109.5 . . ?
H50E C502 H50F 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
C13 N1 C1 C12 20.4(13) . . . . ?
Ni1 N1 C1 C12 176.3(7) . . . . ?
C13 N1 C1 C2 -165.2(7) . . . . ?
Ni1 N1 C1 C2 -9.2(8) . . . . ?
C18 N4 C2 C3 28.5(13) . . . . ?
Ni1 N4 C2 C3 -178.7(7) . . . . ?
C18 N4 C2 C1 -153.3(8) . . . . ?
Ni1 N4 C2 C1 -0.5(9) . . . . ?
C12 C1 C2 C3 -0.4(12) . . . . ?
N1 C1 C2 C3 -175.3(7) . . . . ?
C12 C1 C2 N4 -178.7(7) . . . . ?
N1 C1 C2 N4 6.3(10) . . . . ?
N4 C2 C3 C4 179.9(8) . . . . ?
C1 C2 C3 C4 1.7(12) . . . . ?
C5 N7 C4 C3 -179.5(7) . . . . ?
C5 N7 C4 C11 -0.6(12) . . . . ?
C2 C3 C4 N7 176.7(8) . . . . ?
C2 C3 C4 C11 -2.2(12) . . . . ?
C4 N7 C5 C6 -178.2(8) . . . . ?
C4 N7 C5 C10 0.5(12) . . . . ?
N7 C5 C6 C7 -179.2(8) . . . . ?
C10 C5 C6 C7 2.1(12) . . . . ?
C5 C6 C7 C8 -1.0(13) . . . . ?
C6 C7 C8 C9 -1.2(13) . . . . ?
C7 C8 C9 C10 2.2(14) . . . . ?
C11 N8 C10 C9 179.3(8) . . . . ?
C11 N8 C10 C5 -0.7(12) . . . . ?
C8 C9 C10 N8 178.9(8) . . . . ?
C8 C9 C10 C5 -1.0(13) . . . . ?
N7 C5 C10 N8 0.2(13) . . . . ?
C6 C5 C10 N8 178.9(8) . . . . ?
N7 C5 C10 C9 -179.8(8) . . . . ?
C6 C5 C10 C9 -1.1(12) . . . . ?
C10 N8 C11 C12 178.1(7) . . . . ?
C10 N8 C11 C4 0.6(12) . . . . ?
N7 C4 C11 N8 0.1(13) . . . . ?
C3 C4 C11 N8 179.0(8) . . . . ?
N7 C4 C11 C12 -177.4(8) . . . . ?
C3 C4 C11 C12 1.5(11) . . . . ?
N1 C1 C12 C11 173.9(8) . . . . ?
C2 C1 C12 C11 -0.3(12) . . . . ?
N8 C11 C12 C1 -177.8(8) . . . . ?
C4 C11 C12 C1 -0.3(12) . . . . ?
C1 N1 C13 N2 -139.8(8) . . . . ?
Ni1 N1 C13 N2 64.8(9) . . . . ?
C1 N1 C13 N3 43.5(12) . . . . ?
Ni1 N1 C13 N3 -111.9(7) . . . . ?
C15 N2 C13 N1 25.1(12) . . . . ?
C14 N2 C13 N1 -141.9(8) . . . . ?
C15 N2 C13 N3 -158.0(8) . . . . ?
C14 N2 C13 N3 34.9(11) . . . . ?
C16 N3 C13 N1 -151.0(8) . . . . ?
C17 N3 C13 N1 24.7(11) . . . . ?
C16 N3 C13 N2 32.3(11) . . . . ?
C17 N3 C13 N2 -152.0(8) . . . . ?
C2 N4 C18 N5 -145.7(8) . . . . ?
Ni1 N4 C18 N5 62.6(9) . . . . ?
C2 N4 C18 N6 37.3(12) . . . . ?
Ni1 N4 C18 N6 -114.4(7) . . . . ?
C19 N5 C18 N4 -143.4(7) . . . . ?
C20 N5 C18 N4 14.9(11) . . . . ?
C19 N5 C18 N6 33.8(11) . . . . ?
C20 N5 C18 N6 -167.9(7) . . . . ?
C22 N6 C18 N4 25.2(12) . . . . ?
C21 N6 C18 N4 -153.1(8) . . . . ?
C22 N6 C18 N5 -151.8(8) . . . . ?
C21 N6 C18 N5 29.9(11) . . . . ?
C43 N31 C31 C42 -22.2(13) . . . . ?
Ni2 N31 C31 C42 -177.5(7) . . . . ?
C43 N31 C31 C32 163.6(7) . . . . ?
Ni2 N31 C31 C32 8.4(9) . . . . ?
C48 N34 C32 C33 -29.0(13) . . . . ?
Ni2 N34 C32 C33 173.4(7) . . . . ?
C48 N34 C32 C31 155.0(8) . . . . ?
Ni2 N34 C32 C31 -2.6(9) . . . . ?
C42 C31 C32 C33 5.4(12) . . . . ?
N31 C31 C32 C33 180.0(7) . . . . ?
C42 C31 C32 N34 -178.5(7) . . . . ?
N31 C31 C32 N34 -3.9(10) . . . . ?
N34 C32 C33 C34 -178.0(8) . . . . ?
C31 C32 C33 C34 -2.2(12) . . . . ?
C35 N37 C34 C33 -179.1(8) . . . . ?
C35 N37 C34 C41 -1.4(11) . . . . ?
C32 C33 C34 N37 176.9(8) . . . . ?
C32 C33 C34 C41 -0.8(12) . . . . ?
C34 N37 C35 C36 178.1(7) . . . . ?
C34 N37 C35 C40 -1.1(12) . . . . ?
N37 C35 C36 C37 -178.5(8) . . . . ?
C40 C35 C36 C37 0.7(13) . . . . ?
C35 C36 C37 C38 -3.0(13) . . . . ?
C36 C37 C38 C39 2.6(13) . . . . ?
C37 C38 C39 C40 0.1(13) . . . . ?
C41 N38 C40 C39 -179.4(7) . . . . ?
C41 N38 C40 C35 -0.2(12) . . . . ?
C38 C39 C40 N38 176.8(8) . . . . ?
C38 C39 C40 C35 -2.4(12) . . . . ?
N37 C35 C40 N38 2.0(13) . . . . ?
C36 C35 C40 N38 -177.2(7) . . . . ?
N37 C35 C40 C39 -178.8(8) . . . . ?
C36 C35 C40 C39 2.0(12) . . . . ?
C40 N38 C41 C42 178.0(7) . . . . ?
C40 N38 C41 C34 -2.2(11) . . . . ?
N37 C34 C41 N38 3.2(12) . . . . ?
C33 C34 C41 N38 -179.1(7) . . . . ?
N37 C34 C41 C42 -177.0(7) . . . . ?
C33 C34 C41 C42 0.7(11) . . . . ?
N31 C31 C42 C41 -179.4(8) . . . . ?
C32 C31 C42 C41 -5.5(12) . . . . ?
N38 C41 C42 C31 -177.6(8) . . . . ?
C34 C41 C42 C31 2.5(12) . . . . ?
C47 N33 C43 N31 146.5(8) . . . . ?
C46 N33 C43 N31 -21.4(11) . . . . ?
C47 N33 C43 N32 -31.4(12) . . . . ?
C46 N33 C43 N32 160.8(7) . . . . ?
C31 N31 C43 N33 150.7(7) . . . . ?
Ni2 N31 C43 N33 -55.5(9) . . . . ?
C31 N31 C43 N32 -31.6(12) . . . . ?
Ni2 N31 C43 N32 122.2(7) . . . . ?
C45 N32 C43 N33 -37.7(11) . . . . ?
C44 N32 C43 N33 143.1(8) . . . . ?
C45 N32 C43 N31 144.6(8) . . . . ?
C44 N32 C43 N31 -34.6(11) . . . . ?
C49 N35 C48 N34 145.2(7) . . . . ?
C50 N35 C48 N34 -16.8(11) . . . . ?
C49 N35 C48 N36 -31.0(11) . . . . ?
C50 N35 C48 N36 167.0(7) . . . . ?
C32 N34 C48 N35 145.0(8) . . . . ?
Ni2 N34 C48 N35 -59.0(9) . . . . ?
C32 N34 C48 N36 -39.0(12) . . . . ?
Ni2 N34 C48 N36 117.1(7) . . . . ?
C52 N36 C48 N35 150.3(8) . . . . ?
C51 N36 C48 N35 -37.2(11) . . . . ?
C52 N36 C48 N34 -25.8(11) . . . . ?
C51 N36 C48 N34 146.8(8) . . . . ?
C73 N61 C61 C72 29.5(12) . . . . ?
Ni3 N61 C61 C72 -172.2(6) . . . . ?
C73 N61 C61 C62 -154.8(7) . . . . ?
Ni3 N61 C61 C62 3.5(9) . . . . ?
C78 N64 C62 C63 17.6(13) . . . . ?
Ni3 N64 C62 C63 175.1(7) . . . . ?
C78 N64 C62 C61 -166.7(7) . . . . ?
Ni3 N64 C62 C61 -9.1(9) . . . . ?
C72 C61 C62 C63 -4.4(12) . . . . ?
N61 C61 C62 C63 179.7(7) . . . . ?
C72 C61 C62 N64 179.6(7) . . . . ?
N61 C61 C62 N64 3.7(10) . . . . ?
N64 C62 C63 C64 178.3(8) . . . . ?
C61 C62 C63 C64 2.8(12) . . . . ?
C65 N67 C64 C63 179.2(8) . . . . ?
C65 N67 C64 C71 0.9(12) . . . . ?
C62 C63 C64 N67 -178.1(8) . . . . ?
C62 C63 C64 C71 0.1(13) . . . . ?
C64 N67 C65 C66 -178.5(8) . . . . ?
C64 N67 C65 C70 1.0(12) . . . . ?
N67 C65 C66 C67 -178.8(8) . . . . ?
C70 C65 C66 C67 1.7(13) . . . . ?
C65 C66 C67 C68 0.4(14) . . . . ?
C66 C67 C68 C69 -1.1(14) . . . . ?
C67 C68 C69 C70 -0.5(13) . . . . ?
C71 N68 C70 C69 -178.6(8) . . . . ?
C71 N68 C70 C65 0.7(12) . . . . ?
C68 C69 C70 N68 -178.2(8) . . . . ?
C68 C69 C70 C65 2.5(12) . . . . ?
N67 C65 C70 N68 -1.9(12) . . . . ?
C66 C65 C70 N68 177.6(8) . . . . ?
N67 C65 C70 C69 177.3(8) . . . . ?
C66 C65 C70 C69 -3.1(12) . . . . ?
C70 N68 C71 C72 -177.5(8) . . . . ?
C70 N68 C71 C64 1.3(12) . . . . ?
N67 C64 C71 N68 -2.2(13) . . . . ?
C63 C64 C71 N68 179.5(8) . . . . ?
N67 C64 C71 C72 176.6(8) . . . . ?
C63 C64 C71 C72 -1.7(12) . . . . ?
N61 C61 C72 C71 178.3(8) . . . . ?
C62 C61 C72 C71 2.8(12) . . . . ?
N68 C71 C72 C61 179.0(8) . . . . ?
C64 C71 C72 C61 0.1(12) . . . . ?
C74 N62 C73 N63 29.5(11) . . . . ?
C75 N62 C73 N63 -169.3(7) . . . . ?
C74 N62 C73 N61 -146.6(8) . . . . ?
C75 N62 C73 N61 14.6(11) . . . . ?
C77 N63 C73 N62 -150.0(7) . . . . ?
C76 N63 C73 N62 37.6(11) . . . . ?
C77 N63 C73 N61 26.0(11) . . . . ?
C76 N63 C73 N61 -146.4(8) . . . . ?
C61 N61 C73 N62 -146.3(7) . . . . ?
Ni3 N61 C73 N62 56.8(10) . . . . ?
C61 N61 C73 N63 37.8(12) . . . . ?
Ni3 N61 C73 N63 -119.2(7) . . . . ?
C81 N66 C78 N64 22.0(11) . . . . ?
C82 N66 C78 N64 -145.2(8) . . . . ?
C81 N66 C78 N65 -161.8(7) . . . . ?
C82 N66 C78 N65 31.0(11) . . . . ?
C62 N64 C78 N66 -148.3(8) . . . . ?
Ni3 N64 C78 N66 54.8(10) . . . . ?
C62 N64 C78 N65 35.7(12) . . . . ?
Ni3 N64 C78 N65 -121.2(7) . . . . ?
C79 N65 C78 N66 -144.6(8) . . . . ?
C80 N65 C78 N66 36.8(11) . . . . ?
C79 N65 C78 N64 31.4(11) . . . . ?
C80 N65 C78 N64 -147.1(8) . . . . ?
C103 N91 C91 C102 -21.5(13) . . . . ?
Ni4 N91 C91 C102 -177.3(7) . . . . ?
C103 N91 C91 C92 162.4(8) . . . . ?
Ni4 N91 C91 C92 6.5(9) . . . . ?
C108 N94 C92 C93 -26.8(13) . . . . ?
Ni4 N94 C92 C93 178.3(7) . . . . ?
C108 N94 C92 C91 155.7(8) . . . . ?
Ni4 N94 C92 C91 0.8(9) . . . . ?
C102 C91 C92 C93 1.3(13) . . . . ?
N91 C91 C92 C93 177.7(8) . . . . ?
C102 C91 C92 N94 178.9(7) . . . . ?
N91 C91 C92 N94 -4.8(10) . . . . ?
N94 C92 C93 C94 -179.4(8) . . . . ?
C91 C92 C93 C94 -2.1(12) . . . . ?
C95 N97 C94 C93 -179.5(7) . . . . ?
C95 N97 C94 C101 0.7(11) . . . . ?
C92 C93 C94 N97 -178.8(8) . . . . ?
C92 C93 C94 C101 1.0(12) . . . . ?
C94 N97 C95 C100 -0.2(12) . . . . ?
C94 N97 C95 C96 179.2(7) . . . . ?
N97 C95 C96 C97 -179.0(8) . . . . ?
C100 C95 C96 C97 0.3(13) . . . . ?
C95 C96 C97 C98 -0.4(13) . . . . ?
C96 C97 C98 C99 0.4(14) . . . . ?
C97 C98 C99 C100 -0.3(14) . . . . ?
C101 N98 C100 C95 -0.9(12) . . . . ?
C101 N98 C100 C99 -179.8(8) . . . . ?
N97 C95 C100 N98 0.3(13) . . . . ?
C96 C95 C100 N98 -179.0(8) . . . . ?
N97 C95 C100 C99 179.1(8) . . . . ?
C96 C95 C100 C99 -0.2(12) . . . . ?
C98 C99 C100 N98 179.1(8) . . . . ?
C98 C99 C100 C95 0.2(13) . . . . ?
C100 N98 C101 C102 179.4(7) . . . . ?
C100 N98 C101 C94 1.5(12) . . . . ?
N97 C94 C101 N98 -1.5(12) . . . . ?
C93 C94 C101 N98 178.8(8) . . . . ?
N97 C94 C101 C102 -179.4(7) . . . . ?
C93 C94 C101 C102 0.9(12) . . . . ?
N91 C91 C102 C101 -175.3(8) . . . . ?
C92 C91 C102 C101 0.6(13) . . . . ?
N98 C101 C102 C91 -179.6(8) . . . . ?
C94 C101 C102 C91 -1.7(12) . . . . ?
C107 N93 C103 N92 -32.9(12) . . . . ?
C106 N93 C103 N92 151.7(8) . . . . ?
C107 N93 C103 N91 151.4(8) . . . . ?
C106 N93 C103 N91 -24.0(12) . . . . ?
C105 N92 C103 N93 -31.9(12) . . . . ?
C104 N92 C103 N93 156.9(8) . . . . ?
C105 N92 C103 N91 144.0(8) . . . . ?
C104 N92 C103 N91 -27.1(12) . . . . ?
C91 N91 C103 N93 -43.6(12) . . . . ?
Ni4 N91 C103 N93 111.3(8) . . . . ?
C91 N91 C103 N92 140.5(8) . . . . ?
Ni4 N91 C103 N92 -64.5(9) . . . . ?
C92 N94 C108 N95 149.8(8) . . . . ?
Ni4 N94 C108 N95 -56.7(10) . . . . ?
C92 N94 C108 N96 -35.6(13) . . . . ?
Ni4 N94 C108 N96 117.9(8) . . . . ?
C109 N95 C108 N94 -21.9(12) . . . . ?
C110 N95 C108 N94 142.2(8) . . . . ?
C109 N95 C108 N96 163.2(8) . . . . ?
C110 N95 C108 N96 -32.6(12) . . . . ?
C111 N96 C108 N94 -27.9(12) . . . . ?
C112 N96 C108 N94 151.6(8) . . . . ?
C111 N96 C108 N95 146.7(8) . . . . ?
C112 N96 C108 N95 -33.8(11) . . . . ?

_refine_diff_density_max         1.103
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.092

####################################################################### 
# 
# 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_hi_rl2
_database_code_depnum_ccdc_archive 'CCDC 1845738'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
#==============================================================================
_audit_creation_date             2016-04-01

_audit_block_code                hi_rl2
_audit_block_refno               2688
_audit_block_usercomment         'rl129, irregular, red'


_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:34:44 for OlexSys, GUI svn.r5337)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '2(Br), 2(C H2 Cl2), C46 H66 N14'
_chemical_formula_sum            'C48 H70 Br2 Cl4 N14'
_chemical_formula_weight         1144.80
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            red
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C48 H70 Br2 Cl4 N14'
_chemical_oxdiff_usercomment     'rl129, irregular, red'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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/c 1'
_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                   18.13680(10)
_cell_length_b                   13.78213(10)
_cell_length_c                   11.10358(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.7601(5)
_cell_angle_gamma                90
_cell_volume                     2706.95(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    70873
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.6450
_cell_measurement_theta_min      4.0560
_shelx_estimated_absorpt_T_max   0.685
_shelx_estimated_absorpt_T_min   0.685
_exptl_absorpt_coefficient_mu    4.089
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41p (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1188
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-9 -5 -2 0.0154
-5 0 -1 0.0111
5 0 1 0.0089
2 5 -2 0.0546
-2 -5 2 0.0546
-5 3 5 0.0501
5 -4 -5 0.0828
5 2 -5 0.0649
2 5 -1 0.0497
-5 0 -2 0.0122
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.020
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-8.9894 -5.0032 -2.0102 0.8938 0.0787 0.5490
-4.9938 -0.0027 -1.0057 0.4854 0.0374 -0.0056
4.9938 0.0027 1.0057 -0.4854 -0.0374 0.0056
2.0046 4.9992 -1.9968 -0.0584 0.3087 -0.5504
-2.0046 -4.9992 1.9968 0.0584 -0.3087 0.5504
-5.0080 2.9971 4.9924 0.1211 -0.7273 -0.3553
5.0078 -3.9968 -4.9924 -0.1195 0.7244 0.4670
5.0091 2.0013 -4.9923 -0.1291 0.7417 -0.2031
2.0021 4.9993 -0.9972 -0.1183 0.1799 -0.5528
-4.9913 -0.0028 -2.0053 0.5454 0.1663 -0.0031

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            160921
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.828
_diffrn_reflns_theta_min         4.066
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  21.00   1.00    2.00    --    0.00 -57.00 -90.00   90
  2  ω    -30.00  70.00   1.00    2.00    --    0.00  77.00-120.00  100
  3  ω    -30.00  70.00   1.00    2.00    --    0.00  77.00   0.00  100
  4  ω    -56.00  42.00   1.00    2.00    --   14.00 -74.00-132.08   98
  5  ω    -40.00   3.00   1.00    2.00    --   14.00 119.00  21.05   43
  6  ω    -31.00   4.00   1.00    2.00    --   22.00 118.00  99.05   35
  7  ω    -46.00 -14.00   1.00    2.00    --   26.00 148.00 -33.53   32
  8  ω    -17.00  12.00   1.00    4.00    --   30.00 108.00-172.83   29
  9  ω     -1.00  27.00   1.00    4.00    --   38.00  93.00  27.34   28
 10  ω      5.00  33.00   1.00    4.00    --   42.00  89.00 166.73   28
 11  ω      6.00  33.00   1.00    4.00    --   42.00  88.00  14.63   27
 12  ω      6.00  33.00   1.00    4.00    --   42.00  88.00 -34.04   27
 13  ω      7.00  35.00   1.00    4.00    --   42.00  86.00-131.63   28
 14  ω     12.00  38.00   1.00    4.00    --   46.00  84.00-106.24   26
 15  ω     13.00  40.00   1.00    4.00    --   46.00  83.00 121.82   27
 16  ω     13.00  45.00   1.00    4.00    --   46.00  82.00 102.96   32
 17  ω     14.00  46.00   1.00    4.00    --   46.00  81.00-178.50   32
 18  ω     23.00  49.00   1.00    4.00    --   54.00  78.00 -37.25   26
 19  ω     23.00 111.00   1.00    4.00    --   54.00-125.00 -90.00   88
 20  ω     23.00  49.00   1.00    4.00    --   54.00  78.00  17.09   26
 21  ω     23.00  49.00   1.00    4.00    --   54.00  78.00 -78.21   26
 22  ω     24.00 124.00   1.00    4.00    --   54.00  77.00  30.00  100
 23  ω     24.00 124.00   1.00    4.00    --   54.00  77.00-120.00  100
 24  ω    -18.00  80.00   1.00    4.00    --   54.00 -38.00  90.00   98
 25  ω     24.00 124.00   1.00    4.00    --   54.00  77.00  60.00  100
 26  ω     23.00  49.00   1.00    4.00    --   54.00  78.00  47.80   26
 27  ω     24.00 124.00   1.00    4.00    --   54.00  77.00-150.00  100
 28  ω     23.00  49.00   1.00    4.00    --   54.00  78.00-103.47   26
 29  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 -90.00  100
 30  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 -60.00  100
 31  ω     23.00  49.00   1.00    4.00    --   54.00  78.00 -14.31   26
 32  ω     23.00 111.00   1.00    4.00    --   54.00-125.00   0.00   88
 33  ω      1.00  96.00   1.00    4.00    --   54.00 -99.00  60.00   95
 34  ω     30.00 128.00   1.00    4.00    --   58.00  74.00  91.35   98
 35  ω     28.00 128.00   1.00    4.00    --   58.00  77.00-154.75  100
 36  ω     28.00 128.00   1.00    4.00    --   58.00  77.00 131.14  100
 37  ω     29.00 128.00   1.00    4.00    --   58.00  75.00 116.47   99
 38  ω     30.00 127.00   1.00    4.00    --   58.00  73.00  34.07   97
 39  ω     28.00 128.00   1.00    4.00    --   58.00  77.00-177.31  100
 40  ω     30.00 127.00   1.00    4.00    --   58.00  73.00-115.59   97
 41  ω     29.00 128.00   1.00    4.00    --   58.00  75.00-136.02   99
 42  ω     28.00 128.00   1.00    4.00    --   58.00  77.00 149.26  100
 43  ω     29.00 128.00   1.00    4.00    --   58.00  75.00 -22.90   99
 44  ω     29.00 128.00   1.00    4.00    --   58.00  75.00 103.68   99
 45  ω     32.00 132.00   1.00    4.00    --   62.00  77.00  33.98  100
 46  ω     33.00 132.00   1.00    4.00    --   62.00  76.00 145.57   99
 47  ω     41.00 131.00   1.00    4.00    --   62.00  57.00 -43.81   90
 48  ω     34.00 132.00   1.00    4.00    --   62.00  74.00 -17.62   98
 49  ω     38.00 135.00   1.00    4.00    --   66.00  73.00-161.26   97
 50  ω     44.00 136.00   1.00    4.00    --   66.00  50.00 133.93   92
 51  ω     44.00 134.00   1.00    4.00    --   66.00  62.00 -96.87   90
 52  ω     42.00 134.00   1.00    4.00    --   66.00  67.00 -18.77   92
 53  ω     37.00 136.00   1.00    4.00    --   66.00  76.00 160.06   99
 54  ω     45.00 135.00   1.00    4.00    --   66.00  56.00 -35.27   90
 55  ω     49.00 139.00   1.00    4.00    --   70.00  58.00 144.19   90
 56  ω     49.00 139.00   1.00    4.00    --   70.00  56.00 -98.04   90
 57  ω     40.00 140.00   1.00    4.00    --   70.00  77.00 -18.57  100
 58  ω     53.00 143.00   1.00    4.00    --   74.00  58.00  90.04   90
 59  ω     51.00 145.00   1.00    4.00    --   74.00  48.00 -12.22   94
 60  ω     51.00 142.00   1.00    4.00    --   74.00  66.00 137.21   91
 61  ω     50.00 142.00   1.00    4.00    --   74.00  67.00  26.95   92
 62  ω     57.00 147.00   1.00    4.00    --   78.00  55.00-123.70   90
 63  ω     55.00 145.00   1.00    4.00    --   78.00  64.00   3.81   90
 64  ω     55.00 145.00   1.00    4.00    --   78.00  64.00-114.43   90
 65  ω     57.00 148.00   1.00    4.00    --   78.00  52.00  59.88   91
 66  ω     57.00 148.00   1.00    4.00    --   78.00  53.00-160.93   91
 67  ω     54.00 152.00   1.00    8.00    --   82.00  74.00 -44.00   98
 68  ω     52.00 152.00   1.00    8.00    --   82.00  77.00-110.20  100
 69  ω     59.00 149.00   1.00    8.00    --   82.00  64.00 -79.41   90
 70  ω     55.00 151.00   1.00    8.00    --   82.00  72.00  60.68   96
 71  ω     63.00 157.00   1.00    8.00    --   86.00  48.00  97.55   94
 72  ω     64.00 154.00   1.00    8.00    --   86.00  63.00 158.19   90
 73  ω     64.00 156.00   1.00    8.00    --   86.00  50.00 -47.62   92
 74  ω     63.00 153.00   1.00    8.00    --   86.00  64.00-171.36   90
 75  ω     63.00 159.00   1.00    8.00    --   90.00  72.00-125.66   96
 76  ω     63.00 159.00   1.00    8.00    --   90.00  71.00 120.10   96
 77  ω     66.00 158.00   1.00    8.00    --   90.00  68.00 -10.49   92
 78  ω     61.00 160.00   1.00    8.00    --   90.00  75.00  52.58   99
 79  ω     69.00 166.00   1.00    8.00    --   94.00  41.00 -48.53   97
 80  ω     77.00 167.00   1.00    8.00    --   98.00  56.00  17.89   90
 81  ω     36.00 116.00   1.00    8.00    --  108.00-111.00-180.00   80
 82  ω     82.00 178.00   1.00    8.00    --  108.00  38.00  90.00   96
 83  ω     78.00 178.00   1.00    8.00    --  108.00  77.00  98.63  100
 84  ω     82.00 178.00   1.00    8.00    --  108.00  38.00-150.00   96
 85  ω     86.00 176.00   1.00    8.00    --  108.00  62.00 158.73   90
 86  ω     85.00 175.00   1.00    8.00    --  108.00  64.00 150.00   90
 87  ω     85.00 175.00   1.00    8.00    --  108.00  64.00  30.00   90
 88  ω     85.00 175.00   1.00    8.00    --  108.00  64.00   0.00   90
 89  ω     80.00 178.00   1.00    8.00    --  108.00  74.00  85.78   98
 90  ω     85.00 175.00   1.00    8.00    --  108.00  64.00 -90.00   90
 91  ω     85.00 175.00   1.00    8.00    --  108.00  64.00  60.00   90
 92  ω     85.00 175.00   1.00    8.00    --  108.00  64.00-120.00   90
 93  ω     36.00 116.00   1.00    8.00    --  108.00-111.00   0.00   80
 94  ω     85.00 175.00   1.00    8.00    --  108.00  64.00 -60.00   90
 95  ω     85.00 175.00   1.00    8.00    --  108.00  64.00-180.00   90
 96  ω     78.00 178.00   1.00    8.00    --  108.00  77.00 150.00  100
 97  ω     78.00 178.00   1.00    8.00    --  108.00  77.00-150.00  100
 98  ω     78.00 178.00   1.00    8.00    --  108.00  77.00 -30.00  100
 99  ω     78.00 178.00   1.00    8.00    --  108.00  77.00  30.00  100
100  ω     78.00 178.00   1.00    8.00    --  108.00  77.00 -90.00  100
101  ω     78.00 178.00   1.00    8.00    --  108.00  77.00  60.00  100
102  ω     82.00 178.00   1.00    8.00    --  108.00  38.00 120.00   96
103  ω     78.00 178.00   1.00    8.00    --  108.00  77.00-120.00  100
104  ω     37.00 125.00   1.00    8.00    --  108.00-132.00 -46.00   88
105  ω     87.00 178.00   1.00    8.00    --  108.00 137.00-160.00   91
106  ω     78.00 178.00   1.00    8.00    --  108.00  77.00 120.00  100
107  ω     78.00 178.00   1.00    8.00    --  108.00  77.00   0.00  100
108  ω     78.00 178.00   1.00    8.00    --  108.00  77.00-180.00  100
109  ω     82.00 178.00   1.00    8.00    --  108.00  38.00 -90.00   96
110  ω     82.00 178.00   1.00    8.00    --  108.00  38.00  60.00   96
111  ω     78.00 178.00   1.00    8.00    --  108.00  77.00 -60.00  100
112  ω     41.00 131.00   1.00    8.00    --  108.00 -64.00 -30.00   90
113  ω     85.00 175.00   1.00    8.00    --  108.00  64.00 -30.00   90
114  ω     85.00 175.00   1.00    8.00    --  108.00  64.00-150.00   90
115  ω    100.00 178.00   1.00    8.00    --  108.00 111.00-120.00   78
116  ω     78.00 178.00   1.00    8.00    --  108.00  77.00  90.00  100
117  ω     41.00 131.00   1.00    8.00    --  108.00 -64.00 150.00   90
118  ω     36.00 146.00   1.00    8.00    --  108.00 -92.00 -60.00  110
119  φ    120.00 240.00   1.00    2.00   0.00   0.00 -40.00    --   120
120  φ    120.00 240.00   1.00    2.00   0.00   0.00  40.00    --   120
121  φ      0.00 120.00   1.00    2.00   0.00   0.00 -60.00    --   120
122  φ      0.00 120.00   1.00    2.00   0.00   0.00  60.00    --   120
123  φ      0.00 120.00   1.00    2.00   0.00   0.00  40.00    --   120
124  φ    120.00 240.00   1.00    2.00   0.00   0.00  60.00    --   120
125  φ      0.00 120.00   1.00    2.00   0.00   0.00 -40.00    --   120
126  φ    120.00 240.00   1.00    2.00   0.00   0.00 -60.00    --   120
127  φ    120.00 240.00   1.00    4.00  54.00  54.00  40.00    --   120
128  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 -60.00  100
129  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 -90.00  100
130  φ    120.00 240.00   1.00    4.00  54.00  54.00 -40.00    --   120
131  ω     24.00 124.00   1.00    4.00    --   54.00  77.00  30.00  100
132  φ    120.00 240.00   1.00    4.00  54.00  54.00 -60.00    --   120
133  φ      0.00 120.00   1.00    4.00  54.00  54.00  60.00    --   120
134  φ      0.00 120.00   1.00    4.00  54.00  54.00 -60.00    --   120
135  ω    -16.00  84.00   1.00    4.00    --   54.00 -77.00  30.00  100
136  φ    240.00 360.00   1.00    4.00  54.00  54.00  60.00    --   120
137  φ      0.00 120.00   1.00    4.00  54.00  54.00  40.00    --   120
138  ω     24.00 124.00   1.00    4.00    --   54.00  77.00-180.00  100
139  ω     24.00 124.00   1.00    4.00    --   54.00  77.00-150.00  100
140  ω     24.00 124.00   1.00    4.00    --   54.00  77.00-120.00  100
141  φ    240.00 360.00   1.00    4.00  54.00  54.00 -60.00    --   120
142  φ    240.00 360.00   1.00    4.00  54.00  54.00  40.00    --   120
143  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 -30.00  100
144  ω     24.00 124.00   1.00    4.00    --   54.00  77.00   0.00  100
145  φ      0.00 120.00   1.00    4.00  54.00  54.00 -40.00    --   120
146  ω     24.00 124.00   1.00    4.00    --   54.00  77.00  60.00  100
147  ω     24.00 124.00   1.00    4.00    --   54.00  77.00  90.00  100
148  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 120.00  100
149  ω    -16.00  84.00   1.00    4.00    --   54.00 -77.00-120.00  100
150  ω    -16.00  84.00   1.00    4.00    --   54.00 -77.00-150.00  100
151  φ    240.00 360.00   1.00    4.00  54.00  54.00 -40.00    --   120
152  ω    -16.00  84.00   1.00    4.00    --   54.00 -77.00-180.00  100
153  ω    -16.00  84.00   1.00    4.00    --   54.00 -77.00 -90.00  100
154  ω    -16.00  84.00   1.00    4.00    --   54.00 -77.00 -60.00  100
155  ω    -16.00  84.00   1.00    4.00    --   54.00 -77.00 -30.00  100
156  ω    -16.00  84.00   1.00    4.00    --   54.00 -77.00   0.00  100
157  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 150.00  100
158  ω    -16.00  75.00   1.00    4.00    --   54.00 -77.00  60.00   91
159  φ    120.00 240.00   1.00    4.00  54.00  54.00  60.00    --   120
160  φ      0.00 270.00   1.00    0.50   0.00   0.00   0.00    --   270
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0850964000
_diffrn_orient_matrix_UB_12      -0.0015814000
_diffrn_orient_matrix_UB_13      -0.0601525000
_diffrn_orient_matrix_UB_21      0.0184627000
_diffrn_orient_matrix_UB_22      0.0028751000
_diffrn_orient_matrix_UB_23      -0.1288886000
_diffrn_orient_matrix_UB_31      0.0016625000
_diffrn_orient_matrix_UB_32      -0.1117310000
_diffrn_orient_matrix_UB_33      -0.0024336000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4965
_reflns_number_total             5194
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2017/1
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5194
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0417
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0519P)²+4.8954P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1107
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
Br Br 0.41823(2) 0.09099(2) 0.20718(3) 0.03203(11) Uani 1 1 d . . . . .
Cl1 Cl 0.04995(5) 0.24793(7) -0.09026(8) 0.0500(2) Uani 1 1 d . . . . .
Cl2 Cl 0.07181(7) 0.34944(10) -0.30565(9) 0.0727(3) Uani 1 1 d . . . . .
C51 C 0.00718(18) 0.2842(3) -0.2424(3) 0.0417(7) Uani 1 1 d . . . . .
H51A H -0.009934 0.226289 -0.293661 0.050 Uiso 1 1 calc R . . . .
H51B H -0.037550 0.325093 -0.241278 0.050 Uiso 1 1 calc R . . . .
N1 N 0.25441(11) 0.43990(15) 0.27392(18) 0.0181(4) Uani 1 1 d . . . . .
N2 N 0.31933(11) 0.34418(16) 0.15743(19) 0.0212(4) Uani 1 1 d . . . . .
N3 N 0.38633(11) 0.43004(16) 0.3252(2) 0.0225(4) Uani 1 1 d . . . . .
N4 N 0.28126(10) 0.55187(15) 0.08631(18) 0.0175(4) Uani 1 1 d . . . . .
N5 N 0.36860(11) 0.64459(16) 0.0162(2) 0.0227(5) Uani 1 1 d . . . . .
N6 N 0.28545(12) 0.55353(16) -0.12722(19) 0.0217(4) Uani 1 1 d . . . . .
N7 N -0.01244(11) 0.44086(16) 0.09963(18) 0.0190(4) Uani 1 1 d . . . . .
C1 C 0.19229(12) 0.46380(17) 0.1755(2) 0.0167(5) Uani 1 1 d . . . . .
C2 C 0.20696(12) 0.52352(17) 0.0758(2) 0.0165(5) Uani 1 1 d . . . . .
C3 C 0.14525(13) 0.55254(18) -0.0139(2) 0.0188(5) Uani 1 1 d . . . . .
H3 H 0.153431 0.590886 -0.080864 0.023 Uiso 1 1 calc R . . . .
C4 C 0.07039(13) 0.52709(18) -0.0094(2) 0.0176(5) Uani 1 1 d . . . . .
C5 C 0.05730(13) 0.46834(18) 0.0901(2) 0.0174(5) Uani 1 1 d . . . . .
C6 C 0.12076(13) 0.43774(18) 0.1816(2) 0.0189(5) Uani 1 1 d . . . . .
H6 H 0.113194 0.398429 0.248077 0.023 Uiso 1 1 calc R . . . .
C7 C 0.32071(13) 0.40506(18) 0.2509(2) 0.0193(5) Uani 1 1 d . . . . .
C8 C 0.38034(15) 0.3430(2) 0.0893(3) 0.0280(6) Uani 1 1 d . . . . .
H8A H 0.410903 0.401979 0.108358 0.042 Uiso 1 1 calc GR . . . .
H8B H 0.358350 0.340415 0.000380 0.042 Uiso 1 1 calc GR . . . .
H8C H 0.412362 0.285942 0.113660 0.042 Uiso 1 1 calc GR . . . .
C9 C 0.25838(15) 0.2741(2) 0.1177(3) 0.0265(6) Uani 1 1 d . . . . .
H9A H 0.226023 0.272858 0.177650 0.040 Uiso 1 1 calc GR . . . .
H9B H 0.279968 0.209507 0.112234 0.040 Uiso 1 1 calc GR . . . .
H9C H 0.228259 0.292982 0.036555 0.040 Uiso 1 1 calc GR . . . .
C10 C 0.45045(14) 0.3629(2) 0.3548(3) 0.0290(6) Uani 1 1 d . . . . .
H10A H 0.434928 0.299062 0.319212 0.043 Uiso 1 1 calc GR . . . .
H10B H 0.467217 0.356979 0.444698 0.043 Uiso 1 1 calc GR . . . .
H10C H 0.492071 0.387719 0.320439 0.043 Uiso 1 1 calc GR . . . .
C11 C 0.39850(14) 0.5245(2) 0.3857(3) 0.0277(6) Uani 1 1 d . . . . .
H11A H 0.359999 0.570164 0.343375 0.042 Uiso 1 1 calc GR . . . .
H11B H 0.448801 0.548662 0.382276 0.042 Uiso 1 1 calc GR . . . .
H11C H 0.394877 0.517977 0.472102 0.042 Uiso 1 1 calc GR . . . .
C12 C 0.30906(13) 0.58138(17) -0.0077(2) 0.0180(5) Uani 1 1 d . . . . .
C13 C 0.43428(15) 0.6329(2) -0.0390(3) 0.0297(6) Uani 1 1 d . . . . .
H13A H 0.479632 0.622501 0.026374 0.045 Uiso 1 1 calc GR . . . .
H13B H 0.440717 0.691446 -0.085676 0.045 Uiso 1 1 calc GR . . . .
H13C H 0.426462 0.576823 -0.094707 0.045 Uiso 1 1 calc GR . . . .
C14 C 0.38132(15) 0.7049(2) 0.1250(3) 0.0294(6) Uani 1 1 d . . . . .
H14A H 0.335068 0.707740 0.156801 0.044 Uiso 1 1 calc GR . . . .
H14B H 0.395154 0.770467 0.103992 0.044 Uiso 1 1 calc GR . . . .
H14C H 0.422396 0.677400 0.188284 0.044 Uiso 1 1 calc GR . . . .
C15 C 0.29359(17) 0.6152(2) -0.2303(3) 0.0311(6) Uani 1 1 d . . . . .
H15A H 0.309656 0.680261 -0.199540 0.047 Uiso 1 1 calc GR . . . .
H15B H 0.245005 0.619583 -0.289891 0.047 Uiso 1 1 calc GR . . . .
H15C H 0.331591 0.587347 -0.270690 0.047 Uiso 1 1 calc GR . . . .
C16 C 0.24770(14) 0.4617(2) -0.1638(2) 0.0260(6) Uani 1 1 d . . . . .
H16A H 0.247382 0.422665 -0.090163 0.039 Uiso 1 1 calc GR . . . .
H16B H 0.274681 0.426503 -0.217641 0.039 Uiso 1 1 calc GR . . . .
H16C H 0.195575 0.473927 -0.208415 0.039 Uiso 1 1 calc GR . . . .
C17 C 0.24133(14) 0.43556(19) 0.4003(2) 0.0205(5) Uani 1 1 d . . . . .
H17A H 0.290612 0.428599 0.459408 0.025 Uiso 1 1 calc R . . . .
H17B H 0.210845 0.377205 0.407806 0.025 Uiso 1 1 calc R . . . .
C18 C 0.20123(14) 0.5239(2) 0.4350(2) 0.0225(5) Uani 1 1 d . . . . .
C19 C 0.21920(17) 0.6171(2) 0.4048(3) 0.0380(7) Uani 1 1 d . . . . .
H19 H 0.256072 0.626617 0.356966 0.046 Uiso 1 1 calc R . . . .
C20 C 0.18406(18) 0.6964(2) 0.4434(4) 0.0436(8) Uani 1 1 d . . . . .
H20 H 0.198112 0.759975 0.424157 0.052 Uiso 1 1 calc R . . . .
C21 C 0.12869(17) 0.6842(2) 0.5097(3) 0.0388(7) Uani 1 1 d . . . . .
H21 H 0.104959 0.739060 0.536553 0.047 Uiso 1 1 calc R . . . .
C22 C 0.10814(18) 0.5919(2) 0.5366(3) 0.0386(7) Uani 1 1 d . . . . .
H22 H 0.069152 0.582575 0.580207 0.046 Uiso 1 1 calc R . . . .
C23 C 0.14483(16) 0.5125(2) 0.4994(3) 0.0298(6) Uani 1 1 d . . . . .
H23 H 0.130792 0.448967 0.518835 0.036 Uiso 1 1 calc 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
Cl1 C51 1.768(4) . ?
Cl2 C51 1.743(3) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
N1 C1 1.424(3) . ?
N1 C7 1.370(3) . ?
N1 C17 1.475(3) . ?
N2 C7 1.330(3) . ?
N2 C8 1.472(3) . ?
N2 C9 1.461(3) . ?
N3 C7 1.335(3) . ?
N3 C10 1.466(3) . ?
N3 C11 1.459(3) . ?
N4 C2 1.383(3) . ?
N4 C12 1.319(3) . ?
N5 C12 1.367(3) . ?
N5 C13 1.464(3) . ?
N5 C14 1.443(3) . ?
N6 C12 1.357(3) . ?
N6 C15 1.460(3) . ?
N6 C16 1.454(3) . ?
N7 C4 1.356(3) 3_565 ?
N7 C5 1.347(3) . ?
C1 C2 1.451(3) . ?
C1 C6 1.362(3) . ?
C2 C3 1.383(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.414(3) . ?
C4 C5 1.432(3) . ?
C5 C6 1.420(3) . ?
C6 H6 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.511(4) . ?
C18 C19 1.385(4) . ?
C18 C23 1.381(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.380(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.380(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.377(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.390(4) . ?
C23 H23 0.9500 . ?

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
Cl1 C51 H51A 109.7 . . ?
Cl1 C51 H51B 109.7 . . ?
Cl2 C51 Cl1 109.80(18) . . ?
Cl2 C51 H51A 109.7 . . ?
Cl2 C51 H51B 109.7 . . ?
H51A C51 H51B 108.2 . . ?
C1 N1 C17 118.23(19) . . ?
C7 N1 C1 121.1(2) . . ?
C7 N1 C17 119.71(19) . . ?
C7 N2 C8 121.4(2) . . ?
C7 N2 C9 122.4(2) . . ?
C9 N2 C8 116.2(2) . . ?
C7 N3 C10 122.0(2) . . ?
C7 N3 C11 122.6(2) . . ?
C11 N3 C10 115.4(2) . . ?
C12 N4 C2 123.7(2) . . ?
C12 N5 C13 122.0(2) . . ?
C12 N5 C14 120.2(2) . . ?
C14 N5 C13 114.8(2) . . ?
C12 N6 C15 122.5(2) . . ?
C12 N6 C16 123.2(2) . . ?
C16 N6 C15 114.3(2) . . ?
C5 N7 C4 116.0(2) . 3_565 ?
N1 C1 C2 118.0(2) . . ?
C6 C1 N1 120.1(2) . . ?
C6 C1 C2 121.6(2) . . ?
N4 C2 C1 115.8(2) . . ?
C3 C2 N4 126.7(2) . . ?
C3 C2 C1 117.3(2) . . ?
C2 C3 H3 118.9 . . ?
C2 C3 C4 122.3(2) . . ?
C4 C3 H3 118.9 . . ?
N7 C4 C3 119.1(2) 3_565 . ?
N7 C4 C5 121.4(2) 3_565 . ?
C3 C4 C5 119.5(2) . . ?
N7 C5 C4 122.6(2) . . ?
N7 C5 C6 119.2(2) . . ?
C6 C5 C4 118.3(2) . . ?
C1 C6 C5 121.1(2) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
N2 C7 N1 120.0(2) . . ?
N2 C7 N3 120.4(2) . . ?
N3 C7 N1 119.6(2) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 N5 117.8(2) . . ?
N4 C12 N6 126.4(2) . . ?
N6 C12 N5 115.8(2) . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
N6 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C17 H17A 108.9 . . ?
N1 C17 H17B 108.9 . . ?
N1 C17 C18 113.4(2) . . ?
H17A C17 H17B 107.7 . . ?
C18 C17 H17A 108.9 . . ?
C18 C17 H17B 108.9 . . ?
C19 C18 C17 122.2(2) . . ?
C23 C18 C17 119.6(2) . . ?
C23 C18 C19 118.2(3) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.6(3) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 119.7 . . ?
C19 C20 C21 120.7(3) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 120.3 . . ?
C22 C21 C20 119.5(3) . . ?
C22 C21 H21 120.3 . . ?
C21 C22 H22 120.2 . . ?
C21 C22 C23 119.5(3) . . ?
C23 C22 H22 120.2 . . ?
C18 C23 C22 121.5(3) . . ?
C18 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?

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
N1 C1 C2 N4 0.0(3) . . . . ?
N1 C1 C2 C3 -174.9(2) . . . . ?
N1 C1 C6 C5 174.2(2) . . . . ?
N1 C17 C18 C19 -42.1(3) . . . . ?
N1 C17 C18 C23 138.2(2) . . . . ?
N4 C2 C3 C4 -173.4(2) . . . . ?
N7 C4 C5 N7 0.6(4) 3_565 . . . ?
N7 C4 C5 C6 -179.8(2) 3_565 . . . ?
N7 C5 C6 C1 180.0(2) . . . . ?
C1 N1 C7 N2 -37.8(3) . . . . ?
C1 N1 C7 N3 144.5(2) . . . . ?
C1 N1 C17 C18 -49.7(3) . . . . ?
C1 C2 C3 C4 0.9(4) . . . . ?
C2 N4 C12 N5 152.2(2) . . . . ?
C2 N4 C12 N6 -29.4(4) . . . . ?
C2 C1 C6 C5 -0.2(4) . . . . ?
C2 C3 C4 N7 179.1(2) . . . 3_565 ?
C2 C3 C4 C5 -0.8(4) . . . . ?
C3 C4 C5 N7 -179.5(2) . . . . ?
C3 C4 C5 C6 0.1(4) . . . . ?
C4 N7 C5 C4 -0.6(4) 3_565 . . . ?
C4 N7 C5 C6 179.8(2) 3_565 . . . ?
C4 C5 C6 C1 0.3(4) . . . . ?
C6 C1 C2 N4 174.5(2) . . . . ?
C6 C1 C2 C3 -0.5(4) . . . . ?
C7 N1 C1 C2 -48.4(3) . . . . ?
C7 N1 C1 C6 137.1(2) . . . . ?
C7 N1 C17 C18 141.6(2) . . . . ?
C8 N2 C7 N1 148.4(2) . . . . ?
C8 N2 C7 N3 -33.9(4) . . . . ?
C9 N2 C7 N1 -32.5(3) . . . . ?
C9 N2 C7 N3 145.2(2) . . . . ?
C10 N3 C7 N1 144.9(2) . . . . ?
C10 N3 C7 N2 -32.9(4) . . . . ?
C11 N3 C7 N1 -33.1(4) . . . . ?
C11 N3 C7 N2 149.2(2) . . . . ?
C12 N4 C2 C1 160.0(2) . . . . ?
C12 N4 C2 C3 -25.6(4) . . . . ?
C13 N5 C12 N4 135.8(3) . . . . ?
C13 N5 C12 N6 -42.8(3) . . . . ?
C14 N5 C12 N4 -23.5(4) . . . . ?
C14 N5 C12 N6 157.9(2) . . . . ?
C15 N6 C12 N4 152.8(3) . . . . ?
C15 N6 C12 N5 -28.8(3) . . . . ?
C16 N6 C12 N4 -25.0(4) . . . . ?
C16 N6 C12 N5 153.4(2) . . . . ?
C17 N1 C1 C2 143.1(2) . . . . ?
C17 N1 C1 C6 -31.4(3) . . . . ?
C17 N1 C7 N2 130.6(2) . . . . ?
C17 N1 C7 N3 -47.2(3) . . . . ?
C17 C18 C19 C20 -176.7(3) . . . . ?
C17 C18 C23 C22 178.0(3) . . . . ?
C18 C19 C20 C21 -2.0(5) . . . . ?
C19 C18 C23 C22 -1.8(4) . . . . ?
C19 C20 C21 C22 -0.5(5) . . . . ?
C20 C21 C22 C23 1.7(5) . . . . ?
C21 C22 C23 C18 -0.6(5) . . . . ?
C23 C18 C19 C20 3.1(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.279
_oxdiff_exptl_absorpt_empirical_full_min 0.848
_cell_oxdiff_length_a            18.13636(12)
_cell_oxdiff_length_b            13.78219(12)
_cell_oxdiff_length_c            11.10352(9)
_cell_oxdiff_angle_alpha         89.9844(7)
_cell_oxdiff_angle_beta          102.7537(6)
_cell_oxdiff_angle_gamma         90.0143(6)
_cell_oxdiff_volume              2706.95(4)
_cell_oxdiff_measurement_reflns_used 70873
_symmetry_cell_setting           monoclinic
#_space_group_name_H-M_alt       'P 21/c'
#_space_group_IT_number          14
_chemical_absolute_configuration .
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_hi_rl4
_database_code_depnum_ccdc_archive 'CCDC 1845739'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
#==============================================================================
_audit_creation_date             2017-05-10

_audit_block_code                hi_rl4
_audit_block_refno               2879
_audit_block_usercomment         'rlfp05b, plate, dark red'


_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:34:44 for OlexSys, GUI svn.r5337)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C36 H58 Cl6 Cu2 N16 Ni2'
_chemical_formula_sum            'C36 H58 Cl6 Cu2 N16 Ni2'
_chemical_formula_weight         1172.18
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_diffrn_ambient_temperature      120(1)
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'
Cl Cl 0.1484 0.1585 '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'
Ni Ni 0.3393 1.1124 '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/c 1'
_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                   12.4307(2)
_cell_length_b                   13.47874(19)
_cell_length_c                   15.9132(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.7608(19)
_cell_angle_gamma                90
_cell_volume                     2552.99(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18152
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      31.0110
_cell_measurement_theta_min      2.6610
_shelx_estimated_absorpt_T_max   0.832
_shelx_estimated_absorpt_T_min   0.832
_exptl_absorpt_coefficient_mu    1.906
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1204
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -14 -14 0.0563
-6 -2 -18 0.0640
-17 3 4 0.0222
1 15 13 0.0520
-3 2 22 0.0603
5 15 -14 0.0328
16 -2 1 0.0184
-2 -14 15 0.0640
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.054
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0060 -13.9806 -13.9681 -0.1680 0.5693 0.7986
-5.9943 -1.9860 -17.9642 -0.4663 -0.1068 0.8839
-16.9524 3.0119 3.9684 -0.9676 -0.1789 -0.0627
1.0055 14.9800 12.9706 0.1635 -0.6309 -0.7653
-2.9795 1.9931 21.9428 -0.0369 0.1129 -0.9832
4.9796 14.9858 -13.9587 0.2316 -0.8941 0.4102
16.0000 -2.0000 1.0000 0.9438 0.1746 -0.1639
-2.0000 -14.0000 15.0000 -0.0483 0.8657 -0.4949

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            78702
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.402
_diffrn_reflns_theta_min         2.283
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      7.00  96.00   0.50   15.00    --   27.02  57.00-120.00  178
  2  ω    -20.00  69.00   0.50   15.00    --   27.02 -99.00 -60.00  178
  3  ω    -42.00  48.00   0.50   15.00    --   27.02 -57.00   0.00  180
  4  ω    -42.00  48.00   0.50   15.00    --   27.02 -57.00-180.00  180
  5  ω      7.00  96.00   0.50   15.00    --   27.02  57.00 -30.00  178
  6  ω     -3.00  97.00   0.50   15.00    --   27.02  77.00 150.00  200
  7  ω    -20.00  69.00   0.50   15.00    --   27.02 -99.00 120.00  178
  8  ω     -3.00  97.00   0.50   15.00    --   27.02  77.00  60.00  200
  9  ω     -3.00  97.00   0.50   15.00    --   27.02  77.00 -90.00  200
 10  ω      7.00  96.00   0.50   15.00    --   27.02  57.00  30.00  178
 11  ω    -42.00  48.00   0.50   15.00    --   27.02 -57.00  90.00  180
 12  ω    -20.00  69.00   0.50   15.00    --   27.02 -99.00   0.00  178
 13  ω    -20.00  16.00   0.50   15.00    --   27.02 -99.00-120.00   72
 14  ω      2.00  99.00   0.50   15.00    --   27.02  38.00 150.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0588088000
_diffrn_orient_matrix_UB_12      0.0016407000
_diffrn_orient_matrix_UB_13      0.0061524000
_diffrn_orient_matrix_UB_21      0.0038540000
_diffrn_orient_matrix_UB_22      -0.0513186000
_diffrn_orient_matrix_UB_23      0.0103319000
_diffrn_orient_matrix_UB_31      -0.0088808000
_diffrn_orient_matrix_UB_32      -0.0115593000
_diffrn_orient_matrix_UB_33      -0.0449635000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6911
_reflns_number_total             8896
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2017/1
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         8896
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0428
_refine_ls_restrained_S_all      1.052
_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)+(0.0306P)²+2.3727P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0917
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Ni-Cl2A \\sim Ni-Cl2B
 with sigma of 0.02
3. Others
 Sof(Cl2B)=1-FVAR(1)
 Sof(Cl2A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
Cu Cu 0.69992(2) 0.31741(2) 0.52864(2) 0.02613(7) Uani 1 1 d . . . . .
Ni Ni 0.17998(2) 0.25926(2) 0.18366(2) 0.01625(6) Uani 1 1 d D . . . .
Cl1 Cl 0.11087(5) 0.10493(4) 0.18135(4) 0.02712(12) Uani 1 1 d . . . . .
Cl2A Cl 0.1532(8) 0.31935(17) 0.0491(3) 0.0258(7) Uani 0.73(3) 1 d D . P A 1
Cl2B Cl 0.114(3) 0.3185(5) 0.0467(5) 0.030(3) Uani 0.27(3) 1 d D . P A 2
Cl3 Cl 0.66077(6) 0.18874(5) 0.59956(6) 0.0500(2) Uani 1 1 d . . . . .
N1 N 0.32835(14) 0.24521(11) 0.27045(10) 0.0156(3) Uani 1 1 d . . . . .
N2 N 0.39601(16) 0.10536(13) 0.21947(12) 0.0223(4) Uani 1 1 d . . . . .
N3 N 0.40553(14) 0.11327(12) 0.36636(11) 0.0164(3) Uani 1 1 d . . . . .
N4 N 0.17915(14) 0.38518(12) 0.24737(11) 0.0166(3) Uani 1 1 d . . . . .
N5 N 0.00110(14) 0.44361(13) 0.18078(11) 0.0191(3) Uani 1 1 d . . . . .
N6 N 0.15129(15) 0.54858(12) 0.19110(12) 0.0198(3) Uani 1 1 d . . . . .
N7 N 0.58377(13) 0.42614(12) 0.50947(10) 0.0145(3) Uani 1 1 d . . . . .
N8 N 0.83063(18) 0.33919(16) 0.48973(14) 0.0336(5) Uani 1 1 d . . . . .
C1 C 0.35884(16) 0.32368(13) 0.32913(12) 0.0138(3) Uani 1 1 d . . . . .
C2 C 0.27591(15) 0.40230(13) 0.31548(12) 0.0145(3) Uani 1 1 d . . . . .
C3 C 0.29572(16) 0.48283(14) 0.37106(13) 0.0162(4) Uani 1 1 d . . . . .
H3 H 0.239577 0.532440 0.364306 0.019 Uiso 1 1 calc R . . . .
C4 C 0.39851(16) 0.49279(13) 0.43812(12) 0.0144(3) Uani 1 1 d . . . . .
C5 C 0.48286(15) 0.41781(13) 0.44815(12) 0.0135(3) Uani 1 1 d . . . . .
C6 C 0.45955(16) 0.33334(13) 0.39316(12) 0.0151(3) Uani 1 1 d . . . . .
H6 H 0.514414 0.282477 0.400629 0.018 Uiso 1 1 calc R . . . .
C7 C 0.37799(16) 0.15558(14) 0.28681(13) 0.0157(3) Uani 1 1 d . . . . .
C8 C 0.3821(2) -0.00187(17) 0.21110(17) 0.0324(5) Uani 1 1 d . . . . .
H8A H 0.454792 -0.032879 0.215531 0.049 Uiso 1 1 calc GR . . . .
H8B H 0.329000 -0.017861 0.154042 0.049 Uiso 1 1 calc GR . . . .
H8C H 0.352984 -0.026998 0.258095 0.049 Uiso 1 1 calc GR . . . .
C9 C 0.4040(2) 0.15682(19) 0.14088(15) 0.0324(5) Uani 1 1 d . . . . .
H9A H 0.332354 0.151226 0.094784 0.049 Uiso 1 1 calc GR . . . .
H9B H 0.463836 0.126835 0.120522 0.049 Uiso 1 1 calc GR . . . .
H9C H 0.421215 0.226978 0.154538 0.049 Uiso 1 1 calc GR . . . .
C10 C 0.49942(18) 0.04435(16) 0.39549(15) 0.0238(4) Uani 1 1 d . . . . .
H10A H 0.470768 -0.022034 0.402140 0.036 Uiso 1 1 calc GR . . . .
H10B H 0.549284 0.066563 0.451970 0.036 Uiso 1 1 calc GR . . . .
H10C H 0.541285 0.042218 0.351921 0.036 Uiso 1 1 calc GR . . . .
C11 C 0.35009(17) 0.13847(15) 0.43268(14) 0.0204(4) Uani 1 1 d . . . . .
H11A H 0.401336 0.177521 0.479286 0.031 Uiso 1 1 calc GR . . . .
H11B H 0.329329 0.077455 0.457682 0.031 Uiso 1 1 calc GR . . . .
H11C H 0.282330 0.177371 0.405676 0.031 Uiso 1 1 calc GR . . . .
C12 C 0.11110(16) 0.46027(14) 0.20788(12) 0.0161(4) Uani 1 1 d . . . . .
C13 C -0.0741(2) 0.49439(18) 0.10510(15) 0.0303(5) Uani 1 1 d . . . . .
H13A H -0.120703 0.542080 0.125396 0.045 Uiso 1 1 calc GR . . . .
H13B H -0.122548 0.445561 0.066429 0.045 Uiso 1 1 calc GR . . . .
H13C H -0.029511 0.529530 0.072808 0.045 Uiso 1 1 calc GR . . . .
C14 C -0.04963(19) 0.36005(17) 0.21275(15) 0.0259(4) Uani 1 1 d . . . . .
H14A H -0.062672 0.306001 0.169797 0.039 Uiso 1 1 calc GR . . . .
H14B H -0.121350 0.380645 0.221308 0.039 Uiso 1 1 calc GR . . . .
H14C H 0.000901 0.337146 0.268714 0.039 Uiso 1 1 calc GR . . . .
C15 C 0.0955(2) 0.64291(16) 0.19426(18) 0.0309(5) Uani 1 1 d . . . . .
H15A H 0.065728 0.669223 0.134638 0.046 Uiso 1 1 calc GR . . . .
H15B H 0.149571 0.690078 0.230132 0.046 Uiso 1 1 calc GR . . . .
H15C H 0.033708 0.632917 0.220130 0.046 Uiso 1 1 calc GR . . . .
C16 C 0.26076(18) 0.55605(17) 0.17519(15) 0.0257(4) Uani 1 1 d . . . . .
H16A H 0.315379 0.583587 0.227243 0.039 Uiso 1 1 calc GR . . . .
H16B H 0.255122 0.599607 0.124798 0.039 Uiso 1 1 calc GR . . . .
H16C H 0.285394 0.489961 0.162854 0.039 Uiso 1 1 calc GR . . . .
C17 C 0.9103(2) 0.35958(17) 0.47205(15) 0.0291(5) Uani 1 1 d . . . . .
C18 C 1.0110(2) 0.38794(17) 0.44915(16) 0.0302(5) Uani 1 1 d . . . . .
H18A H 0.992907 0.441326 0.405520 0.045 Uiso 1 1 calc GR . . . .
H18B H 1.039868 0.330535 0.424667 0.045 Uiso 1 1 calc GR . . . .
H18C H 1.068054 0.411102 0.501813 0.045 Uiso 1 1 calc GR . . . .


_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
Cu Cl3 2.1988(8) . ?
Cu N7 2.0178(16) . ?
Cu N8 1.921(2) . ?
Ni Cl1 2.2467(6) . ?
Ni Cl2A 2.223(3) . ?
Ni Cl2B 2.243(5) . ?
Ni N1 1.9687(16) . ?
Ni N4 1.9786(16) . ?
N1 C1 1.389(2) . ?
N1 C7 1.347(2) . ?
N2 C7 1.340(3) . ?
N2 C8 1.457(3) . ?
N2 C9 1.458(3) . ?
N3 C7 1.340(2) . ?
N3 C10 1.459(2) . ?
N3 C11 1.457(3) . ?
N4 C2 1.387(2) . ?
N4 C12 1.352(2) . ?
N5 C12 1.329(3) . ?
N5 C13 1.464(3) . ?
N5 C14 1.452(3) . ?
N6 C12 1.347(2) . ?
N6 C15 1.456(3) . ?
N6 C16 1.458(3) . ?
N7 C4 1.354(2) 3_666 ?
N7 C5 1.354(2) . ?
N8 C17 1.139(3) . ?
C1 C2 1.450(2) . ?
C1 C6 1.374(3) . ?
C2 C3 1.377(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.415(3) . ?
C4 C5 1.432(3) . ?
C5 C6 1.414(3) . ?
C6 H6 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.452(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 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
N7 Cu Cl3 113.32(5) . . ?
N8 Cu Cl3 128.24(7) . . ?
N8 Cu N7 118.37(8) . . ?
Cl2A Ni Cl1 111.80(14) . . ?
Cl2B Ni Cl1 106.4(3) . . ?
N1 Ni Cl1 101.47(5) . . ?
N1 Ni Cl2A 124.1(3) . . ?
N1 Ni Cl2B 136.2(8) . . ?
N1 Ni N4 82.26(6) . . ?
N4 Ni Cl1 138.08(5) . . ?
N4 Ni Cl2A 99.18(8) . . ?
N4 Ni Cl2B 97.9(3) . . ?
C1 N1 Ni 114.65(12) . . ?
C7 N1 Ni 120.40(13) . . ?
C7 N1 C1 122.13(16) . . ?
C7 N2 C8 122.09(19) . . ?
C7 N2 C9 120.94(18) . . ?
C8 N2 C9 115.41(19) . . ?
C7 N3 C10 122.30(17) . . ?
C7 N3 C11 122.67(16) . . ?
C11 N3 C10 114.86(16) . . ?
C2 N4 Ni 114.32(12) . . ?
C12 N4 Ni 119.93(13) . . ?
C12 N4 C2 121.61(16) . . ?
C12 N5 C13 122.76(18) . . ?
C12 N5 C14 121.83(17) . . ?
C14 N5 C13 114.31(17) . . ?
C12 N6 C15 123.87(18) . . ?
C12 N6 C16 120.90(17) . . ?
C15 N6 C16 115.05(17) . . ?
C4 N7 Cu 120.73(12) 3_666 . ?
C4 N7 C5 117.61(16) 3_666 . ?
C5 N7 Cu 121.51(12) . . ?
C17 N8 Cu 173.4(2) . . ?
N1 C1 C2 114.28(16) . . ?
C6 C1 N1 125.76(17) . . ?
C6 C1 C2 119.87(16) . . ?
N4 C2 C1 114.47(16) . . ?
C3 C2 N4 125.98(17) . . ?
C3 C2 C1 119.48(16) . . ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 120.96(17) . . ?
C4 C3 H3 119.5 . . ?
N7 C4 C3 119.49(17) 3_666 . ?
N7 C4 C5 121.15(16) 3_666 . ?
C3 C4 C5 119.34(16) . . ?
N7 C5 C4 121.23(16) . . ?
N7 C5 C6 119.65(17) . . ?
C6 C5 C4 119.12(16) . . ?
C1 C6 C5 121.04(17) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
N2 C7 N1 118.12(18) . . ?
N3 C7 N1 122.83(17) . . ?
N3 C7 N2 118.98(17) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 N4 118.13(17) . . ?
N5 C12 N6 119.39(17) . . ?
N6 C12 N4 122.38(18) . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
N6 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N8 C17 C18 178.7(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 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
Cu N7 C5 C4 176.55(13) . . . . ?
Cu N7 C5 C6 -3.0(2) . . . . ?
Ni N1 C1 C2 -0.4(2) . . . . ?
Ni N1 C1 C6 -177.12(16) . . . . ?
Ni N1 C7 N2 57.2(2) . . . . ?
Ni N1 C7 N3 -119.96(18) . . . . ?
Ni N4 C2 C1 -1.6(2) . . . . ?
Ni N4 C2 C3 -178.49(16) . . . . ?
Ni N4 C12 N5 59.4(2) . . . . ?
Ni N4 C12 N6 -116.99(18) . . . . ?
N1 C1 C2 N4 1.2(2) . . . . ?
N1 C1 C2 C3 178.40(18) . . . . ?
N1 C1 C6 C5 178.46(18) . . . . ?
N4 C2 C3 C4 -179.51(18) . . . . ?
N7 C4 C5 N7 -1.0(3) 3_666 . . . ?
N7 C4 C5 C6 178.58(17) 3_666 . . . ?
N7 C5 C6 C1 -178.66(18) . . . . ?
C1 N1 C7 N2 -142.85(19) . . . . ?
C1 N1 C7 N3 40.0(3) . . . . ?
C1 C2 C3 C4 3.7(3) . . . . ?
C2 N4 C12 N5 -144.85(19) . . . . ?
C2 N4 C12 N6 38.8(3) . . . . ?
C2 C1 C6 C5 1.9(3) . . . . ?
C2 C3 C4 N7 178.67(18) . . . 3_666 ?
C2 C3 C4 C5 -0.1(3) . . . . ?
C3 C4 C5 N7 177.72(18) . . . . ?
C3 C4 C5 C6 -2.7(3) . . . . ?
C4 N7 C5 C4 1.0(3) 3_666 . . . ?
C4 N7 C5 C6 -178.61(17) 3_666 . . . ?
C4 C5 C6 C1 1.8(3) . . . . ?
C6 C1 C2 N4 178.22(17) . . . . ?
C6 C1 C2 C3 -4.6(3) . . . . ?
C7 N1 C1 C2 -161.37(18) . . . . ?
C7 N1 C1 C6 21.9(3) . . . . ?
C8 N2 C7 N1 -141.6(2) . . . . ?
C8 N2 C7 N3 35.7(3) . . . . ?
C9 N2 C7 N1 23.5(3) . . . . ?
C9 N2 C7 N3 -159.2(2) . . . . ?
C10 N3 C7 N1 -151.23(19) . . . . ?
C10 N3 C7 N2 31.6(3) . . . . ?
C11 N3 C7 N1 23.7(3) . . . . ?
C11 N3 C7 N2 -153.41(19) . . . . ?
C12 N4 C2 C1 -158.60(18) . . . . ?
C12 N4 C2 C3 24.5(3) . . . . ?
C13 N5 C12 N4 -150.1(2) . . . . ?
C13 N5 C12 N6 26.4(3) . . . . ?
C14 N5 C12 N4 17.3(3) . . . . ?
C14 N5 C12 N6 -166.23(19) . . . . ?
C15 N6 C12 N4 -145.7(2) . . . . ?
C15 N6 C12 N5 38.0(3) . . . . ?
C16 N6 C12 N4 29.1(3) . . . . ?
C16 N6 C12 N5 -147.2(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.384
_oxdiff_exptl_absorpt_empirical_full_min 0.779
_cell_oxdiff_length_a            12.4303(4)
_cell_oxdiff_length_b            13.4771(2)
_cell_oxdiff_length_c            15.9174(5)
_cell_oxdiff_angle_alpha         89.983(2)
_cell_oxdiff_angle_beta          106.782(3)
_cell_oxdiff_angle_gamma         90.029(2)
_cell_oxdiff_volume              2552.99(13)
_cell_oxdiff_measurement_reflns_used 18152
_symmetry_cell_setting           monoclinic
#_space_group_name_H-M_alt       'P 21/c'
#_space_group_IT_number          14
_chemical_absolute_configuration .
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
####################################################################### 
# 
# 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_rlgu11ks
_database_code_depnum_ccdc_archive 'CCDC 1845741'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
#==============================================================================

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H58 Cl6 Cu4 N16'
_chemical_formula_weight         1181.84

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.248(2)
_cell_length_b                   13.649(3)
_cell_length_c                   15.785(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.46(3)
_cell_angle_gamma                90
_cell_volume                     2543.3(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    43023
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      30.10

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_F_000             1208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.009
_shelx_estimated_absorpt_T_min   0.433
_shelx_estimated_absorpt_T_max   0.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'O-Scan    '
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42047
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.005
_diffrn_reflns_theta_max         30.096
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7466
_reflns_number_gt                5253
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'COLLECT (Bruker AXS, 1997-2009)'
_computing_cell_refinement       'DENZO/SKALEPACK (Bruker AXS, 1997-2009)'
_computing_data_reduction        'DENZO/SKALEPACK (Bruker AXS, 1997-2009)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XPMA (Zsolnai, Huttner, 1994)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0354P)²+1.8746P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7466
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.0956
_refine_ls_wR_factor_gt          0.0832
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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
Cu1 Cu 0.18181(2) 0.76382(2) 0.18357(2) 0.01928(8) Uani 1 1 d . . . . .
Cu2 Cu 0.30006(3) 1.18320(2) 0.47106(2) 0.02814(9) Uani 1 1 d . . . . .
Cl1 Cl 0.11107(6) 0.81940(5) 0.04699(4) 0.02740(15) Uani 1 1 d . . . . .
Cl2 Cl 0.12056(5) 0.60803(4) 0.17688(4) 0.02437(14) Uani 1 1 d . . . . .
Cl3 Cl 0.34133(6) 1.31165(5) 0.40076(6) 0.0448(2) Uani 1 1 d . . . . .
N1 N 0.32553(17) 0.74603(14) 0.27376(13) 0.0190(4) Uani 1 1 d . . . . .
N2 N 0.39734(18) 0.60853(15) 0.22219(13) 0.0230(5) Uani 1 1 d . . . . .
N3 N 0.40250(16) 0.61545(14) 0.36985(13) 0.0187(4) Uani 1 1 d . . . . .
N4 N 0.18056(17) 0.88827(14) 0.24573(13) 0.0198(4) Uani 1 1 d . . . . .
N5 N -0.00050(17) 0.94519(15) 0.18483(13) 0.0211(4) Uani 1 1 d . . . . .
N6 N 0.14985(17) 1.05024(15) 0.19131(13) 0.0209(4) Uani 1 1 d . . . . .
N7 N 0.41733(16) 1.07481(14) 0.48923(12) 0.0183(4) Uani 1 1 d . . . . .
N8 N 0.1674(2) 1.15820(18) 0.51170(16) 0.0342(6) Uani 1 1 d . . . . .
C1 C 0.3575(2) 0.82432(17) 0.33135(15) 0.0178(5) Uani 1 1 d . . . . .
C2 C 0.27648(19) 0.90494(17) 0.31511(15) 0.0181(5) Uani 1 1 d . . . . .
C3 C 0.2971(2) 0.98501(17) 0.36998(15) 0.0197(5) Uani 1 1 d . . . . .
H3 H 0.2430 1.0343 0.3625 0.024 Uiso 1 1 calc R U . . .
C4 C 0.3987(2) 0.99382(17) 0.43745(15) 0.0181(5) Uani 1 1 d . . . . .
C5 C 0.48205(19) 0.91757(16) 0.44893(15) 0.0174(5) Uani 1 1 d . . . . .
C6 C 0.4576(2) 0.83328(17) 0.39566(15) 0.0192(5) Uani 1 1 d . . . . .
H6 H 0.5104 0.7827 0.4042 0.023 Uiso 1 1 calc R U . . .
C7 C 0.3759(2) 0.65739(17) 0.28979(16) 0.0192(5) Uani 1 1 d . . . . .
C8 C 0.4040(3) 0.6610(2) 0.14282(18) 0.0336(7) Uani 1 1 d . . . . .
H8A H 0.3318 0.6583 0.1000 0.050 Uiso 1 1 calc R U . . .
H8B H 0.4604 0.6310 0.1192 0.050 Uiso 1 1 calc R U . . .
H8C H 0.4241 0.7281 0.1572 0.050 Uiso 1 1 calc R U . . .
C9 C 0.3849(3) 0.50223(19) 0.21284(18) 0.0320(6) Uani 1 1 d . . . . .
H9A H 0.4576 0.4731 0.2176 0.048 Uiso 1 1 calc R U . . .
H9B H 0.3348 0.4869 0.1564 0.048 Uiso 1 1 calc R U . . .
H9C H 0.3541 0.4769 0.2583 0.048 Uiso 1 1 calc R U . . .
C10 C 0.3462(2) 0.64066(19) 0.43739(16) 0.0232(5) Uani 1 1 d . . . . .
H10A H 0.3960 0.6798 0.4818 0.035 Uiso 1 1 calc R U . . .
H10B H 0.3270 0.5818 0.4634 0.035 Uiso 1 1 calc R U . . .
H10C H 0.2784 0.6770 0.4114 0.035 Uiso 1 1 calc R U . . .
C11 C 0.4976(2) 0.54745(19) 0.39779(17) 0.0268(6) Uani 1 1 d . . . . .
H11A H 0.4696 0.4833 0.4056 0.040 Uiso 1 1 calc R U . . .
H11B H 0.5472 0.5696 0.4523 0.040 Uiso 1 1 calc R U . . .
H11C H 0.5386 0.5448 0.3538 0.040 Uiso 1 1 calc R U . . .
C12 C 0.1099(2) 0.96258(17) 0.20856(15) 0.0197(5) Uani 1 1 d . . . . .
C13 C -0.0500(2) 0.8594(2) 0.21539(18) 0.0276(6) Uani 1 1 d . . . . .
H13A H -0.0646 0.8100 0.1706 0.041 Uiso 1 1 calc R U . . .
H13B H -0.1198 0.8776 0.2280 0.041 Uiso 1 1 calc R U . . .
H13C H 0.0017 0.8343 0.2677 0.041 Uiso 1 1 calc R U . . .
C14 C -0.0784(2) 0.9964(2) 0.11134(18) 0.0302(6) Uani 1 1 d . . . . .
H14A H -0.1226 1.0428 0.1338 0.045 Uiso 1 1 calc R U . . .
H14B H -0.1280 0.9498 0.0747 0.045 Uiso 1 1 calc R U . . .
H14C H -0.0358 1.0302 0.0774 0.045 Uiso 1 1 calc R U . . .
C15 C 0.0933(2) 1.14339(19) 0.19746(19) 0.0292(6) Uani 1 1 d . . . . .
H15A H 0.0627 1.1697 0.1396 0.044 Uiso 1 1 calc R U . . .
H15B H 0.1469 1.1887 0.2320 0.044 Uiso 1 1 calc R U . . .
H15C H 0.0330 1.1328 0.2248 0.044 Uiso 1 1 calc R U . . .
C16 C 0.2598(2) 1.05889(19) 0.17233(17) 0.0269(6) Uani 1 1 d . . . . .
H16A H 0.3135 1.0869 0.2221 0.040 Uiso 1 1 calc R U . . .
H16B H 0.2527 1.1003 0.1220 0.040 Uiso 1 1 calc R U . . .
H16C H 0.2853 0.9951 0.1604 0.040 Uiso 1 1 calc R U . . .
C17 C 0.0870(3) 1.1371(2) 0.52976(17) 0.0291(6) Uani 1 1 d . . . . .
C18 C -0.0155(2) 1.1070(2) 0.55290(17) 0.0312(6) Uani 1 1 d . . . . .
H18A H -0.0716 1.0869 0.5008 0.047 Uiso 1 1 calc R U . . .
H18B H -0.0442 1.1610 0.5796 0.047 Uiso 1 1 calc R U . . .
H18C H 0.0016 1.0533 0.5936 0.047 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
Cu1 N1 1.962(2) . ?
Cu1 N4 1.964(2) . ?
Cu1 Cl1 2.2312(9) . ?
Cu1 Cl2 2.2479(8) . ?
Cu2 N8 1.929(3) . ?
Cu2 N7 2.0284(19) . ?
Cu2 Cl3 2.2045(9) . ?
N1 C7 1.351(3) . ?
N1 C1 1.390(3) . ?
N2 C7 1.342(3) . ?
N2 C9 1.462(3) . ?
N2 C8 1.464(3) . ?
N3 C7 1.346(3) . ?
N3 C10 1.457(3) . ?
N3 C11 1.463(3) . ?
N4 C12 1.361(3) . ?
N4 C2 1.395(3) . ?
N5 C12 1.324(3) . ?
N5 C13 1.458(3) . ?
N5 C14 1.468(3) . ?
N6 C12 1.348(3) . ?
N6 C16 1.460(3) . ?
N6 C15 1.464(3) . ?
N7 C5 1.357(3) 3_676 ?
N7 C4 1.357(3) . ?
N8 C17 1.134(4) . ?
C1 C6 1.373(3) . ?
C1 C2 1.458(3) . ?
C2 C3 1.375(3) . ?
C3 C4 1.411(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.435(3) . ?
C5 N7 1.357(3) 3_676 ?
C5 C6 1.409(3) . ?
C6 H6 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.457(4) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 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
N1 Cu1 N4 82.50(8) . . ?
N1 Cu1 Cl1 141.77(7) . . ?
N4 Cu1 Cl1 97.81(6) . . ?
N1 Cu1 Cl2 98.09(6) . . ?
N4 Cu1 Cl2 142.63(7) . . ?
Cl1 Cu1 Cl2 103.73(3) . . ?
N8 Cu2 N7 116.82(9) . . ?
N8 Cu2 Cl3 129.37(7) . . ?
N7 Cu2 Cl3 113.73(6) . . ?
C7 N1 C1 122.07(19) . . ?
C7 N1 Cu1 121.56(15) . . ?
C1 N1 Cu1 114.93(15) . . ?
C7 N2 C9 122.4(2) . . ?
C7 N2 C8 120.3(2) . . ?
C9 N2 C8 115.3(2) . . ?
C7 N3 C10 122.9(2) . . ?
C7 N3 C11 121.8(2) . . ?
C10 N3 C11 115.1(2) . . ?
C12 N4 C2 121.5(2) . . ?
C12 N4 Cu1 121.20(15) . . ?
C2 N4 Cu1 114.60(15) . . ?
C12 N5 C13 122.2(2) . . ?
C12 N5 C14 122.5(2) . . ?
C13 N5 C14 113.8(2) . . ?
C12 N6 C16 121.2(2) . . ?
C12 N6 C15 123.6(2) . . ?
C16 N6 C15 115.0(2) . . ?
C5 N7 C4 118.1(2) 3_676 . ?
C5 N7 Cu2 121.27(15) 3_676 . ?
C4 N7 Cu2 120.63(15) . . ?
C17 N8 Cu2 173.7(2) . . ?
C6 C1 N1 126.3(2) . . ?
C6 C1 C2 119.7(2) . . ?
N1 C1 C2 113.89(19) . . ?
C3 C2 N4 126.8(2) . . ?
C3 C2 C1 119.1(2) . . ?
N4 C2 C1 114.0(2) . . ?
C2 C3 C4 121.3(2) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
N7 C4 C3 119.8(2) . . ?
N7 C4 C5 121.0(2) . . ?
C3 C4 C5 119.2(2) . . ?
N7 C5 C6 120.0(2) 3_676 . ?
N7 C5 C4 121.0(2) 3_676 . ?
C6 C5 C4 119.1(2) . . ?
C1 C6 C5 121.3(2) . . ?
C1 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
N2 C7 N3 119.1(2) . . ?
N2 C7 N1 118.2(2) . . ?
N3 C7 N1 122.7(2) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 N6 120.0(2) . . ?
N5 C12 N4 118.2(2) . . ?
N6 C12 N4 121.7(2) . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N6 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N8 C17 C18 178.3(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 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
C7 N1 C1 C6 18.7(4) . . . . ?
Cu1 N1 C1 C6 -174.8(2) . . . . ?
C7 N1 C1 C2 -165.2(2) . . . . ?
Cu1 N1 C1 C2 1.3(3) . . . . ?
C12 N4 C2 C3 19.1(4) . . . . ?
Cu1 N4 C2 C3 -179.2(2) . . . . ?
C12 N4 C2 C1 -164.6(2) . . . . ?
Cu1 N4 C2 C1 -2.9(3) . . . . ?
C6 C1 C2 C3 -6.0(4) . . . . ?
N1 C1 C2 C3 177.7(2) . . . . ?
C6 C1 C2 N4 177.4(2) . . . . ?
N1 C1 C2 N4 1.1(3) . . . . ?
N4 C2 C3 C4 -179.2(2) . . . . ?
C1 C2 C3 C4 4.7(4) . . . . ?
C5 N7 C4 C3 -177.4(2) 3_676 . . . ?
Cu2 N7 C4 C3 0.4(3) . . . . ?
C5 N7 C4 C5 1.2(4) 3_676 . . . ?
Cu2 N7 C4 C5 178.94(17) . . . . ?
C2 C3 C4 N7 178.6(2) . . . . ?
C2 C3 C4 C5 0.0(4) . . . . ?
N7 C4 C5 N7 -1.2(4) . . . 3_676 ?
C3 C4 C5 N7 177.3(2) . . . 3_676 ?
N7 C4 C5 C6 177.9(2) . . . . ?
C3 C4 C5 C6 -3.5(3) . . . . ?
N1 C1 C6 C5 178.4(2) . . . . ?
C2 C1 C6 C5 2.5(4) . . . . ?
N7 C5 C6 C1 -178.7(2) 3_676 . . . ?
C4 C5 C6 C1 2.2(4) . . . . ?
C9 N2 C7 N3 36.3(3) . . . . ?
C8 N2 C7 N3 -160.6(2) . . . . ?
C9 N2 C7 N1 -142.0(2) . . . . ?
C8 N2 C7 N1 21.1(3) . . . . ?
C10 N3 C7 N2 -155.2(2) . . . . ?
C11 N3 C7 N2 30.5(3) . . . . ?
C10 N3 C7 N1 23.0(3) . . . . ?
C11 N3 C7 N1 -151.3(2) . . . . ?
C1 N1 C7 N2 -139.8(2) . . . . ?
Cu1 N1 C7 N2 54.6(3) . . . . ?
C1 N1 C7 N3 42.0(3) . . . . ?
Cu1 N1 C7 N3 -123.6(2) . . . . ?
C13 N5 C12 N6 -168.6(2) . . . . ?
C14 N5 C12 N6 25.9(4) . . . . ?
C13 N5 C12 N4 15.0(3) . . . . ?
C14 N5 C12 N4 -150.5(2) . . . . ?
C16 N6 C12 N5 -147.5(2) . . . . ?
C15 N6 C12 N5 38.0(3) . . . . ?
C16 N6 C12 N4 28.7(3) . . . . ?
C15 N6 C12 N4 -145.8(2) . . . . ?
C2 N4 C12 N5 -141.4(2) . . . . ?
Cu1 N4 C12 N5 58.1(3) . . . . ?
C2 N4 C12 N6 42.4(3) . . . . ?
Cu1 N4 C12 N6 -118.1(2) . . . . ?

_refine_diff_density_max         0.525
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.096

