# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_drr18_s1677
_database_code_depnum_ccdc_archive 'CCDC 1959772'
loop_
_audit_author_name
_audit_author_address
'William Lewis'
;University of Sydney
Australia
;
_audit_update_record             
;
2019-10-17 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
_sydney_internal_submission_code drr18_s1677
_sydney_internal_submission_date 2018-09-21
_sydney_internal_submission_number s1677
_sydney_internal_client_code     dm1
_sydney_internal_client_email    mahendiran.dharmasivam@sydney.edu.au
_sydney_internal_client_name     'Mahendiran Dharmasivam'
_sydney_internal_supervisor_code drr
_sydney_internal_supervisor_name 'Des Richardson'
_sydney_internal_collection_date 2018-09-24
_sydney_internal_collection_user wlew0588
_sydney_internal_process_date    2018-09-27
_sydney_internal_process_user    wlew0588
_sydney_internal_solution_date   2018-09-27
_sydney_internal_solution_user   wlew0588
_sydney_internal_refine_date     2018-10-04
_sydney_internal_refine_user     wlew0588
_sydney_internal_check_and_archive_date 2018-10-05
_sydney_internal_check_user      wlew0588
_refine_special_details          ?
_vrf_PLAT026_drr18_s1677         
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        38% Check 
RESPONSE: The crystal used was small and weakly diffracting, which has resulted in 
an overall weak dataset.
;
_vrf_PLAT341_drr18_s1677         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01686 Ang.  
RESPONSE: The weak, low-quality dataset has resulted in low precision of the C-C 
bond lengths, however the identity of the complex is not in question.
;
_audit_creation_date             2018-10-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H34 N10 Ni S2, 2(Cl), H2 O'
_chemical_formula_sum            'C30 H36 Cl2 N10 Ni O S2'
_chemical_formula_weight         746.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30H34N10S2Ni H2Cl2 H2O'
_chemical_oxdiff_usercomment     ' '
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'
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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.141(3)
_cell_length_b                   14.090(4)
_cell_length_c                   14.188(3)
_cell_angle_alpha                94.82(2)
_cell_angle_beta                 92.36(2)
_cell_angle_gamma                107.67(3)
_cell_volume                     1730.8(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    738
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.7590
_cell_measurement_theta_min      5.1360
_shelx_estimated_absorpt_T_max   0.943
_shelx_estimated_absorpt_T_min   0.757
_exptl_absorpt_coefficient_mu    3.690
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             776
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0060
0 -1 0 0.0100
1 -2 5 0.0024
5 -3 -3 0.0478
-5 3 3 0.0288
-1 2 -5 0.0295

_exptl_crystal_recrystallization_method 'crystallised from methanol'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.016
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
-0.0028 1.0027 -0.0030 0.0181 -0.0277 0.1106
0.0028 -1.0027 0.0030 -0.0181 0.0277 -0.1106
1.0366 -2.0054 4.9845 -0.5852 -0.0423 -0.0421
4.9895 -2.9761 -3.0832 0.0934 -0.8292 -0.3346
-4.9895 2.9761 3.0832 -0.0934 0.8292 0.3346
-1.0366 2.0054 -4.9845 0.5852 0.0423 0.0421

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1703
_diffrn_reflns_av_unetI/netI     0.2578
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11803
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.368
_diffrn_reflns_theta_min         4.322
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.5861
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -45.00  34.00   1.00   30.00    --  -39.89  38.00 120.00   79
  2  ω    -79.00 -51.00   1.00   30.00    --  -39.89 178.00-150.00   28
  3  ω    -57.00  26.00   1.00   30.00    --  -39.89  57.00 -60.00   83
  4  ω    -84.00  36.00   1.00   30.00    --  -39.89  19.00-120.00  120
  5  ω     57.00 130.00   1.00   30.00    --   39.89 178.00 120.00   73
  6  ω     80.00 130.00   1.00   30.00    --   39.89 178.00 -90.00   50
  7  ω     57.00  86.00   1.00  120.00    --  108.56 -30.00 -60.00   29
  8  ω     37.00  94.00   1.00  120.00    --  108.56 -45.00  60.00   57
  9  ω     36.00  97.00   1.00  120.00    --  108.56 -45.00 120.00   61
 10  ω     43.00 118.00   1.00  120.00    --  108.56-125.00 150.00   75
 11  ω     31.00  87.00   1.00  120.00    --  108.56 -30.00-180.00   56
 12  ω     27.00 110.00   1.00  120.00    --  108.56 -95.00 -60.00   83
 13  ω     98.00 125.00   1.00  120.00    --  108.56 125.00 -90.00   27
 14  ω     85.00 178.00   1.00  120.00    --  108.56  30.00   0.00   93
 15  ω     34.00  98.00   1.00  120.00    --  108.56 -45.00 -90.00   64
 16  ω     59.00 117.00   1.00  120.00    --  108.56-125.00 -90.00   58
 17  ω     35.00  93.00   1.00  120.00    --  108.56 -45.00   0.00   58
 18  ω     69.00  97.00   1.00  120.00    --  108.56-125.00-150.00   28
 19  ω     57.00  82.00   1.00  120.00    --  108.56 -61.00-150.00   25
 20  ω    102.00 129.00   1.00  120.00    --  108.56 125.00-180.00   27
 21  ω     50.00 101.00   1.00  120.00    --  108.56 -95.00  30.00   51
 22  ω     85.00 177.00   1.00  120.00    --  108.56  30.00  90.00   92
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0345128000
_diffrn_orient_matrix_UB_12      0.0176234000
_diffrn_orient_matrix_UB_13      -0.1031422000
_diffrn_orient_matrix_UB_21      -0.1729235000
_diffrn_orient_matrix_UB_22      -0.0280451000
_diffrn_orient_matrix_UB_23      0.0161855000
_diffrn_orient_matrix_UB_31      0.0186916000
_diffrn_orient_matrix_UB_32      0.1104828000
_diffrn_orient_matrix_UB_33      0.0321221000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2584
_reflns_number_total             6761
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6761
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2326
_refine_ls_R_factor_gt           0.1045
_refine_ls_restrained_S_all      0.967
_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)+(0.0781P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2267
_refine_ls_wR_factor_ref         0.2878
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C35(H35A,H35B)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N22(H22), C1(H1), C2(H2A), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10),
 C11(H11), C21(H21), C22(H22A), C23(H23), C24(H24), C28(H28), C29(H29),
 C30(H30), C31(H31)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C34(H34A,H34B,H34C), C36(H36A,H36B,
 H36C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.2782(2) 0.50700(16) 0.24779(12) 0.0439(5) Uani 1 1 d . . . . .
S1 S 0.5375(3) 0.6150(2) 0.28546(17) 0.0450(7) Uani 1 1 d . . . . .
S21 S 0.3240(3) 0.4479(2) 0.09327(17) 0.0455(7) Uani 1 1 d . . . . .
N1 N 0.0391(9) 0.4612(7) 0.2123(5) 0.040(2) Uani 1 1 d . . . . .
N2 N 0.1120(10) 0.8018(7) 0.1737(6) 0.046(2) Uani 1 1 d . . . . .
H2 H 0.134212 0.807125 0.235272 0.056 Uiso 1 1 calc R . . . .
N3 N 0.2539(10) 0.6364(8) 0.2125(5) 0.046(2) Uani 1 1 d . . . . .
N4 N 0.3648(10) 0.7247(8) 0.2137(6) 0.050(2) Uani 1 1 d . . . . .
N5 N 0.6150(10) 0.8086(8) 0.2560(6) 0.048(2) Uani 1 1 d . . . . .
N21 N 0.2357(9) 0.5109(7) 0.3911(5) 0.042(2) Uani 1 1 d . . . . .
N22 N 0.2397(10) 0.1738(7) 0.3618(6) 0.045(2) Uani 1 1 d . . . . .
H22 H 0.168262 0.166796 0.315910 0.054 Uiso 1 1 calc R . . . .
N23 N 0.2906(9) 0.3711(7) 0.2765(6) 0.042(2) Uani 1 1 d . . . . .
N24 N 0.3160(9) 0.3024(8) 0.2117(5) 0.046(2) Uani 1 1 d . . . . .
N25 N 0.3449(10) 0.2638(8) 0.0564(6) 0.048(2) Uani 1 1 d . . . . .
C1 C -0.0627(13) 0.3758(9) 0.2221(6) 0.042(3) Uani 1 1 d . . . . .
H1 H -0.029029 0.325641 0.248586 0.051 Uiso 1 1 calc R . . . .
C2 C -0.2168(13) 0.3546(10) 0.1959(8) 0.053(3) Uani 1 1 d . . . . .
H2A H -0.288723 0.292236 0.205935 0.063 Uiso 1 1 calc R . . . .
C3 C -0.2633(12) 0.4263(10) 0.1547(7) 0.053(3) Uani 1 1 d . . . . .
H3 H -0.367932 0.413046 0.133012 0.063 Uiso 1 1 calc R . . . .
C4 C -0.1579(12) 0.5173(9) 0.1451(7) 0.044(3) Uani 1 1 d . . . . .
H4 H -0.189282 0.568217 0.118491 0.053 Uiso 1 1 calc R . . . .
C5 C -0.0064(12) 0.5338(9) 0.1745(6) 0.046(3) Uani 1 1 d . . . . .
C6 C 0.1185(11) 0.6302(9) 0.1721(7) 0.041(3) Uani 1 1 d . . . . .
C7 C 0.0914(11) 0.7141(9) 0.1241(8) 0.044(3) Uani 1 1 d . . . . .
C8 C 0.0504(12) 0.7036(9) 0.0269(7) 0.046(3) Uani 1 1 d . . . . .
H8 H 0.030167 0.640630 -0.009481 0.055 Uiso 1 1 calc R . . . .
C9 C 0.0397(11) 0.7856(10) -0.0151(7) 0.051(3) Uani 1 1 d . . . . .
H9 H 0.014429 0.780187 -0.081403 0.061 Uiso 1 1 calc R . . . .
C10 C 0.0662(13) 0.8775(10) 0.0399(9) 0.053(3) Uani 1 1 d . . . . .
H10 H 0.060424 0.935136 0.011584 0.064 Uiso 1 1 calc R . . . .
C11 C 0.1004(13) 0.8822(10) 0.1346(9) 0.055(3) Uani 1 1 d . . . . .
H11 H 0.116151 0.943342 0.173226 0.066 Uiso 1 1 calc R . . . .
C12 C 0.5025(11) 0.7205(9) 0.2508(6) 0.042(3) Uani 1 1 d . . . . .
C14 C 0.7685(12) 0.8180(9) 0.2959(8) 0.051(3) Uani 1 1 d . . . . .
H14A H 0.764668 0.808493 0.363439 0.076 Uiso 1 1 calc GR . . . .
H14B H 0.837971 0.884781 0.288125 0.076 Uiso 1 1 calc GR . . . .
H14C H 0.806355 0.767127 0.262868 0.076 Uiso 1 1 calc GR . . . .
C15 C 0.5936(13) 0.8991(9) 0.2219(8) 0.048(3) Uani 1 1 d . . . . .
H15A H 0.504473 0.879742 0.174461 0.057 Uiso 1 1 calc R . . . .
H15B H 0.685981 0.934560 0.190025 0.057 Uiso 1 1 calc R . . . .
C16 C 0.5672(16) 0.9684(11) 0.3001(9) 0.066(4) Uani 1 1 d . . . . .
H16A H 0.540265 1.023267 0.273229 0.099 Uiso 1 1 calc GR . . . .
H16B H 0.661160 0.995821 0.342159 0.099 Uiso 1 1 calc GR . . . .
H16C H 0.482878 0.931715 0.336269 0.099 Uiso 1 1 calc GR . . . .
C21 C 0.2005(10) 0.5827(9) 0.4428(7) 0.042(3) Uani 1 1 d . . . . .
H21 H 0.189508 0.638530 0.413361 0.050 Uiso 1 1 calc R . . . .
C22 C 0.1790(12) 0.5782(9) 0.5410(8) 0.049(3) Uani 1 1 d . . . . .
H22A H 0.155235 0.629951 0.578426 0.059 Uiso 1 1 calc R . . . .
C23 C 0.1943(12) 0.4960(10) 0.5786(7) 0.052(3) Uani 1 1 d . . . . .
H23 H 0.181739 0.490942 0.644325 0.063 Uiso 1 1 calc R . . . .
C24 C 0.2275(11) 0.4189(9) 0.5247(6) 0.045(3) Uani 1 1 d . . . . .
H24 H 0.236496 0.361671 0.552491 0.054 Uiso 1 1 calc R . . . .
C25 C 0.2471(11) 0.4283(9) 0.4289(8) 0.046(3) Uani 1 1 d . . . . .
C26 C 0.2832(11) 0.3536(9) 0.3649(7) 0.040(3) Uani 1 1 d . . . . .
C27 C 0.3180(11) 0.2679(9) 0.3992(7) 0.044(3) Uani 1 1 d . . . . .
C28 C 0.4338(12) 0.2758(10) 0.4693(7) 0.047(3) Uani 1 1 d . . . . .
H28 H 0.492278 0.340308 0.498033 0.057 Uiso 1 1 calc R . . . .
C29 C 0.4655(13) 0.1935(10) 0.4981(7) 0.055(3) Uani 1 1 d . . . . .
H29 H 0.546314 0.201099 0.545147 0.066 Uiso 1 1 calc R . . . .
C30 C 0.3796(15) 0.0994(11) 0.4583(7) 0.060(4) Uani 1 1 d . . . . .
H30 H 0.400431 0.041694 0.477949 0.072 Uiso 1 1 calc R . . . .
C31 C 0.2627(13) 0.0897(10) 0.3894(7) 0.051(3) Uani 1 1 d . . . . .
H31 H 0.200200 0.025500 0.362288 0.061 Uiso 1 1 calc R . . . .
C32 C 0.3279(11) 0.3327(8) 0.1230(6) 0.038(2) Uani 1 1 d . . . . .
C34 C 0.3790(14) 0.2864(11) -0.0385(7) 0.062(4) Uani 1 1 d . . . . .
H34A H 0.449526 0.250993 -0.062038 0.092 Uiso 1 1 calc GR . . . .
H34B H 0.427287 0.358683 -0.038840 0.092 Uiso 1 1 calc GR . . . .
H34C H 0.283520 0.264937 -0.079567 0.092 Uiso 1 1 calc GR . . . .
C35 C 0.3132(13) 0.1578(10) 0.0701(7) 0.053(3) Uani 1 1 d . . . . .
H35A H 0.265761 0.117045 0.010058 0.064 Uiso 1 1 calc R . . . .
H35B H 0.237343 0.140603 0.118711 0.064 Uiso 1 1 calc R . . . .
C36 C 0.4553(15) 0.1293(11) 0.1008(11) 0.075(4) Uani 1 1 d . . . . .
H36A H 0.535617 0.152432 0.056869 0.112 Uiso 1 1 calc GR . . . .
H36B H 0.427870 0.056391 0.100255 0.112 Uiso 1 1 calc GR . . . .
H36C H 0.493581 0.160831 0.164998 0.112 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.1604(4) 0.8320(3) 0.38687(19) 0.0595(8) Uani 1 1 d . . . . .
Cl2 Cl -0.0310(3) 0.0843(2) 0.21613(18) 0.0543(8) Uani 1 1 d . . . . .
O1 O -0.0797(16) 0.2201(8) 0.3987(7) 0.090(3) Uani 1 1 d . . . . .
H1A H -0.098829 0.174422 0.352666 0.134 Uiso 1 1 d G . . . .
H1B H -0.104094 0.188722 0.447176 0.134 Uiso 1 1 d G . . . .


_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 S1 2.406(3) . ?
Ni1 S21 2.378(3) . ?
Ni1 N1 2.108(8) . ?
Ni1 N3 2.003(10) . ?
Ni1 N21 2.085(7) . ?
Ni1 N23 2.026(9) . ?
S1 C12 1.719(12) . ?
S21 C32 1.720(12) . ?
N1 C1 1.300(13) . ?
N1 C5 1.356(13) . ?
N2 H2 0.8800 . ?
N2 C7 1.327(14) . ?
N2 C11 1.333(14) . ?
N3 N4 1.343(13) . ?
N3 C6 1.317(12) . ?
N4 C12 1.364(13) . ?
N5 C12 1.345(14) . ?
N5 C14 1.455(13) . ?
N5 C15 1.465(14) . ?
N21 C21 1.326(14) . ?
N21 C25 1.352(14) . ?
N22 H22 0.8800 . ?
N22 C27 1.352(14) . ?
N22 C31 1.351(14) . ?
N23 N24 1.356(13) . ?
N23 C26 1.300(13) . ?
N24 C32 1.361(13) . ?
N25 C32 1.346(14) . ?
N25 C34 1.435(13) . ?
N25 C35 1.464(15) . ?
C1 H1 0.9500 . ?
C1 C2 1.377(15) . ?
C2 H2A 0.9500 . ?
C2 C3 1.372(16) . ?
C3 H3 0.9500 . ?
C3 C4 1.371(16) . ?
C4 H4 0.9500 . ?
C4 C5 1.373(14) . ?
C5 C6 1.491(16) . ?
C6 C7 1.490(15) . ?
C7 C8 1.398(15) . ?
C8 H8 0.9500 . ?
C8 C9 1.371(15) . ?
C9 H9 0.9500 . ?
C9 C10 1.404(17) . ?
C10 H10 0.9500 . ?
C10 C11 1.358(17) . ?
C11 H11 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.492(16) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C21 H21 0.9500 . ?
C21 C22 1.420(15) . ?
C22 H22A 0.9500 . ?
C22 C23 1.356(15) . ?
C23 H23 0.9500 . ?
C23 C24 1.393(16) . ?
C24 H24 0.9500 . ?
C24 C25 1.390(14) . ?
C25 C26 1.455(15) . ?
C26 C27 1.453(15) . ?
C27 C28 1.395(14) . ?
C28 H28 0.9500 . ?
C28 C29 1.368(16) . ?
C29 H29 0.9500 . ?
C29 C30 1.377(17) . ?
C30 H30 0.9500 . ?
C30 C31 1.386(16) . ?
C31 H31 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.529(16) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
O1 H1A 0.8501 . ?
O1 H1B 0.8500 . ?

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
S21 Ni1 S1 95.20(11) . . ?
N1 Ni1 S1 160.0(3) . . ?
N1 Ni1 S21 91.0(2) . . ?
N3 Ni1 S1 80.4(3) . . ?
N3 Ni1 S21 96.2(2) . . ?
N3 Ni1 N1 80.1(4) . . ?
N3 Ni1 N21 102.6(3) . . ?
N3 Ni1 N23 176.0(4) . . ?
N21 Ni1 S1 90.7(2) . . ?
N21 Ni1 S21 161.0(3) . . ?
N21 Ni1 N1 89.5(3) . . ?
N23 Ni1 S1 103.1(2) . . ?
N23 Ni1 S21 81.6(3) . . ?
N23 Ni1 N1 96.5(4) . . ?
N23 Ni1 N21 79.5(4) . . ?
C12 S1 Ni1 95.1(4) . . ?
C32 S21 Ni1 95.4(3) . . ?
C1 N1 Ni1 128.6(7) . . ?
C1 N1 C5 119.4(9) . . ?
C5 N1 Ni1 112.0(7) . . ?
C7 N2 H2 118.5 . . ?
C7 N2 C11 122.9(10) . . ?
C11 N2 H2 118.5 . . ?
N4 N3 Ni1 127.2(7) . . ?
C6 N3 Ni1 115.5(9) . . ?
C6 N3 N4 116.6(10) . . ?
N3 N4 C12 111.7(10) . . ?
C12 N5 C14 120.4(10) . . ?
C12 N5 C15 123.5(9) . . ?
C14 N5 C15 116.1(10) . . ?
C21 N21 Ni1 126.8(7) . . ?
C21 N21 C25 121.4(9) . . ?
C25 N21 Ni1 111.8(7) . . ?
C27 N22 H22 117.5 . . ?
C31 N22 H22 117.5 . . ?
C31 N22 C27 125.0(10) . . ?
N24 N23 Ni1 124.6(7) . . ?
C26 N23 Ni1 115.9(8) . . ?
C26 N23 N24 119.4(9) . . ?
N23 N24 C32 112.9(9) . . ?
C32 N25 C34 122.1(10) . . ?
C32 N25 C35 123.6(9) . . ?
C34 N25 C35 113.9(10) . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.2(11) . . ?
C2 C1 H1 118.4 . . ?
C1 C2 H2A 121.1 . . ?
C3 C2 C1 117.9(12) . . ?
C3 C2 H2A 121.1 . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.7(10) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.2(10) . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 120.7(11) . . ?
N1 C5 C6 114.6(9) . . ?
C4 C5 C6 124.7(10) . . ?
N3 C6 C5 116.6(10) . . ?
N3 C6 C7 122.1(10) . . ?
C5 C6 C7 121.3(9) . . ?
N2 C7 C6 119.4(9) . . ?
N2 C7 C8 119.1(11) . . ?
C8 C7 C6 121.4(11) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 C7 118.9(11) . . ?
C9 C8 H8 120.5 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 119.9(10) . . ?
C10 C9 H9 120.1 . . ?
C9 C10 H10 120.8 . . ?
C11 C10 C9 118.5(12) . . ?
C11 C10 H10 120.8 . . ?
N2 C11 C10 120.6(12) . . ?
N2 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
N4 C12 S1 125.4(9) . . ?
N5 C12 S1 121.3(7) . . ?
N5 C12 N4 113.2(10) . . ?
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 . . ?
N5 C15 H15A 109.1 . . ?
N5 C15 H15B 109.1 . . ?
N5 C15 C16 112.4(10) . . ?
H15A C15 H15B 107.9 . . ?
C16 C15 H15A 109.1 . . ?
C16 C15 H15B 109.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N21 C21 H21 119.2 . . ?
N21 C21 C22 121.5(10) . . ?
C22 C21 H21 119.2 . . ?
C21 C22 H22A 121.7 . . ?
C23 C22 C21 116.5(11) . . ?
C23 C22 H22A 121.7 . . ?
C22 C23 H23 118.7 . . ?
C22 C23 C24 122.6(9) . . ?
C24 C23 H23 118.7 . . ?
C23 C24 H24 121.1 . . ?
C25 C24 C23 117.8(11) . . ?
C25 C24 H24 121.1 . . ?
N21 C25 C24 120.1(11) . . ?
N21 C25 C26 116.5(9) . . ?
C24 C25 C26 123.4(11) . . ?
N23 C26 C25 115.9(10) . . ?
N23 C26 C27 122.2(10) . . ?
C27 C26 C25 121.7(9) . . ?
N22 C27 C26 120.7(9) . . ?
N22 C27 C28 115.6(11) . . ?
C28 C27 C26 123.7(11) . . ?
C27 C28 H28 119.0 . . ?
C29 C28 C27 122.0(12) . . ?
C29 C28 H28 119.0 . . ?
C28 C29 H29 120.2 . . ?
C28 C29 C30 119.6(11) . . ?
C30 C29 H29 120.2 . . ?
C29 C30 H30 120.3 . . ?
C29 C30 C31 119.4(12) . . ?
C31 C30 H30 120.3 . . ?
N22 C31 C30 118.4(12) . . ?
N22 C31 H31 120.8 . . ?
C30 C31 H31 120.8 . . ?
N24 C32 S21 125.4(8) . . ?
N25 C32 S21 120.5(8) . . ?
N25 C32 N24 114.1(10) . . ?
N25 C34 H34A 109.5 . . ?
N25 C34 H34B 109.5 . . ?
N25 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N25 C35 H35A 108.7 . . ?
N25 C35 H35B 108.7 . . ?
N25 C35 C36 114.2(10) . . ?
H35A C35 H35B 107.6 . . ?
C36 C35 H35A 108.7 . . ?
C36 C35 H35B 108.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
H1A O1 H1B 104.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2 Cl1 0.88 2.14 3.013(9) 170.7 . yes
N22 H22 Cl2 0.88 2.21 3.038(9) 155.9 . yes
O1 H1A Cl2 0.85 2.43 3.217(11) 153.8 . yes
O1 H1B Cl1 0.85 2.45 3.252(10) 156.7 2_566 yes

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
Ni1 S1 C12 N4 -1.3(8) . . . . ?
Ni1 S1 C12 N5 -179.4(7) . . . . ?
Ni1 S21 C32 N24 -3.4(9) . . . . ?
Ni1 S21 C32 N25 177.1(8) . . . . ?
Ni1 N1 C1 C2 -179.9(8) . . . . ?
Ni1 N1 C5 C4 178.7(7) . . . . ?
Ni1 N1 C5 C6 -3.6(10) . . . . ?
Ni1 N3 N4 C12 -5.4(11) . . . . ?
Ni1 N3 C6 C5 11.3(11) . . . . ?
Ni1 N3 C6 C7 -167.3(7) . . . . ?
Ni1 N21 C21 C22 -177.9(7) . . . . ?
Ni1 N21 C25 C24 177.9(8) . . . . ?
Ni1 N21 C25 C26 -0.9(11) . . . . ?
Ni1 N23 N24 C32 -1.9(11) . . . . ?
Ni1 N23 C26 C25 7.7(12) . . . . ?
Ni1 N23 C26 C27 -168.7(8) . . . . ?
N1 C1 C2 C3 2.1(16) . . . . ?
N1 C5 C6 N3 -4.8(12) . . . . ?
N1 C5 C6 C7 173.7(8) . . . . ?
N2 C7 C8 C9 3.1(16) . . . . ?
N3 N4 C12 S1 3.9(12) . . . . ?
N3 N4 C12 N5 -177.9(8) . . . . ?
N3 C6 C7 N2 -60.9(13) . . . . ?
N3 C6 C7 C8 116.6(12) . . . . ?
N4 N3 C6 C5 -177.4(8) . . . . ?
N4 N3 C6 C7 4.0(13) . . . . ?
N21 C21 C22 C23 -0.9(15) . . . . ?
N21 C25 C26 N23 -4.4(14) . . . . ?
N21 C25 C26 C27 172.0(9) . . . . ?
N22 C27 C28 C29 0.1(14) . . . . ?
N23 N24 C32 S21 3.8(12) . . . . ?
N23 N24 C32 N25 -176.6(8) . . . . ?
N23 C26 C27 N22 -57.6(14) . . . . ?
N23 C26 C27 C28 120.8(12) . . . . ?
N24 N23 C26 C25 -176.7(9) . . . . ?
N24 N23 C26 C27 6.9(15) . . . . ?
C1 N1 C5 C4 -1.2(14) . . . . ?
C1 N1 C5 C6 176.6(8) . . . . ?
C1 C2 C3 C4 -3.0(16) . . . . ?
C2 C3 C4 C5 1.9(15) . . . . ?
C3 C4 C5 N1 0.3(15) . . . . ?
C3 C4 C5 C6 -177.3(9) . . . . ?
C4 C5 C6 N3 172.8(9) . . . . ?
C4 C5 C6 C7 -8.6(15) . . . . ?
C5 N1 C1 C2 0.0(14) . . . . ?
C5 C6 C7 N2 120.6(10) . . . . ?
C5 C6 C7 C8 -61.8(14) . . . . ?
C6 N3 N4 C12 -175.5(8) . . . . ?
C6 C7 C8 C9 -174.5(9) . . . . ?
C7 N2 C11 C10 0.0(17) . . . . ?
C7 C8 C9 C10 -1.6(16) . . . . ?
C8 C9 C10 C11 -0.7(16) . . . . ?
C9 C10 C11 N2 1.6(17) . . . . ?
C11 N2 C7 C6 175.2(9) . . . . ?
C11 N2 C7 C8 -2.4(15) . . . . ?
C12 N5 C15 C16 99.0(12) . . . . ?
C14 N5 C12 S1 -3.1(12) . . . . ?
C14 N5 C12 N4 178.6(9) . . . . ?
C14 N5 C15 C16 -81.7(12) . . . . ?
C15 N5 C12 S1 176.1(8) . . . . ?
C15 N5 C12 N4 -2.2(13) . . . . ?
C21 N21 C25 C24 -2.4(15) . . . . ?
C21 N21 C25 C26 178.8(9) . . . . ?
C21 C22 C23 C24 -0.7(17) . . . . ?
C22 C23 C24 C25 0.7(17) . . . . ?
C23 C24 C25 N21 0.8(15) . . . . ?
C23 C24 C25 C26 179.6(10) . . . . ?
C24 C25 C26 N23 176.8(10) . . . . ?
C24 C25 C26 C27 -6.8(16) . . . . ?
C25 N21 C21 C22 2.4(15) . . . . ?
C25 C26 C27 N22 126.2(11) . . . . ?
C25 C26 C27 C28 -55.4(15) . . . . ?
C26 N23 N24 C32 -177.2(9) . . . . ?
C26 C27 C28 C29 -178.4(9) . . . . ?
C27 N22 C31 C30 -3.1(15) . . . . ?
C27 C28 C29 C30 -1.2(16) . . . . ?
C28 C29 C30 C31 0.3(16) . . . . ?
C29 C30 C31 N22 1.7(16) . . . . ?
C31 N22 C27 C26 -179.4(9) . . . . ?
C31 N22 C27 C28 2.2(14) . . . . ?
C32 N25 C35 C36 -96.1(12) . . . . ?
C34 N25 C32 S21 7.8(14) . . . . ?
C34 N25 C32 N24 -171.8(10) . . . . ?
C34 N25 C35 C36 90.7(12) . . . . ?
C35 N25 C32 S21 -164.9(8) . . . . ?
C35 N25 C32 N24 15.5(14) . . . . ?

loop_
_audit_author_email
mahendiran.dharmasivam@sydney.edu.au
?
d.richardson@sydney.edu.au
_olex2_date_sample_data_collection 2018-10-24
_olex2_date_sample_submission    2018-09-19
_olex2_exptl_crystal_mounting_method 'in paratone on a loop'
_olex2_submission_original_sample_id Ni(Dp4e4mT)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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.396
_oxdiff_exptl_absorpt_empirical_full_min 0.328
####################################################################### 
# 
# 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_drr19_s1943
_database_code_depnum_ccdc_archive 'CCDC 1982608'
loop_
_audit_author_name
_audit_author_address
'William Lewis'
;University of Sydney
Australia
;
_audit_update_record             
;
2020-02-07 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
_sydney_internal_submission_code drr19_s1943
_sydney_internal_submission_date 2019-11-07
_sydney_internal_submission_number s1943
_sydney_internal_client_code     dm1
_sydney_internal_client_email    mdha3758@chem.usyd.edu.au
_sydney_internal_client_name     'Mahendiran Dharmasivam'
_sydney_internal_supervisor_code drr
_sydney_internal_supervisor_name 'Des Richardson'
_sydney_internal_collection_date 2019-11-29
_sydney_internal_collection_user wlew0588
_sydney_internal_process_date    2019-12-12
_sydney_internal_process_user    wlew0588
_sydney_internal_solution_date   2019-12-12
_sydney_internal_solution_user   wlew0588
_sydney_internal_refine_date     2019-12-13
_sydney_internal_refine_user     wlew0588
_sydney_internal_check_and_archive_date 2019-12-17
_sydney_internal_check_user      wlew0588
_refine_special_details          
;
The N(Me)(Et) arm of the deprotonated ligand is disordered over two orientaions. 
The methyl group of the major component and the CH2 of the minor component share a 
site, while all other atoms have separated sites. The occupancies of the two 
components were refined competitively, converging to a ratio of 0.67:0.33. 
Chemically equivalent bond lengths of the disordered atoms were restrained to 
be approxiamtely equal, and C16, N6A, C19A and C19 were restrained to 
approximately flat geometry. The minor component atom N6A was refined 
isotropically, and all other disordered atoms were refined with enhanced 
rigid bond restraints.
;
_audit_creation_date             2019-12-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H33 Cu N10 S2, Cl O4, H2 O'
_chemical_formula_sum            'C30 H35 Cl Cu N10 O5 S2'
_chemical_formula_weight         778.79
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H34ClCuN10O5S2
_chemical_oxdiff_usercomment     C19H21N4O2SCu
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5625(3)
_cell_length_b                   13.6735(4)
_cell_length_c                   13.8397(5)
_cell_angle_alpha                73.376(3)
_cell_angle_beta                 77.366(3)
_cell_angle_gamma                86.693(3)
_cell_volume                     1691.94(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7494
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.6270
_cell_measurement_theta_min      4.7270
_shelx_estimated_absorpt_T_max   0.864
_shelx_estimated_absorpt_T_min   0.738
_exptl_absorpt_coefficient_mu    3.265
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0410
0 -1 0 0.0345
0 1 0 0.0345
-1 -1 -5 0.0214
-5 1 -4 0.0270
-1 -1 -1 0.0293
-2 0 5 0.0219
1 1 5 0.0246
5 4 0 0.0301

_exptl_crystal_recrystallization_method 'crystallised from an ethanol solution'
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.046
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
0.9992 0.0011 0.0023 -0.1333 0.0971 -0.0010
-0.0003 -0.9996 -0.0016 -0.0052 -0.0070 0.1172
0.0003 0.9996 0.0016 0.0052 0.0070 -0.1172
-0.9915 -0.9962 -4.9959 0.3606 0.4279 -0.0065
-4.9895 0.9978 -4.0037 0.8578 -0.0527 -0.2118
-0.9979 -0.9998 -1.0023 0.1746 0.0023 0.0932
-2.0065 -0.0066 4.9872 0.0342 -0.7261 0.1268
0.9915 0.9962 4.9959 -0.3606 -0.4279 0.0065
4.9974 4.0037 0.0181 -0.6460 0.5132 -0.4738

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15295
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.773
_diffrn_reflns_theta_min         4.069
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.5861
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  38.00   1.00    7.50    --  -38.19  57.00 -90.00   82
  2  ω   -116.00  -9.00   1.00    7.50    --  -38.19 -38.00 120.00  107
  3  ω     -5.00  45.00   1.00    7.50    --  -38.19  19.00-120.00   50
  4  ω     -5.00  45.00   1.00    7.50    --  -38.19  19.00 -90.00   50
  5  ω   -126.00 -37.00   1.00    7.50    --  -38.19 178.00-180.00   89
  6  ω     -2.00  24.00   1.00    7.50    --   38.19  91.00-178.73   26
  7  ω      0.00  31.00   1.00    7.50    --   38.19  87.00 136.23   31
  8  ω    103.00 178.00   1.00   30.00    --  107.94  77.00-150.00   75
  9  ω     32.00  93.00   1.00   30.00    --  107.94 -61.00  90.00   61
 10  ω     28.00 109.00   1.00   30.00    --  107.94-111.00-150.00   81
 11  ω     31.00  72.00   1.00   30.00    --  107.94 -45.00-180.00   41
 12  ω     28.00 109.00   1.00   30.00    --  107.94-111.00  30.00   81
 13  ω     32.00  93.00   1.00   30.00    --  107.94 -61.00 -60.00   61
 14  ω     23.00 106.00   1.00   30.00    --  107.94 -95.00-120.00   83
 15  ω     28.00  57.00   1.00   30.00    --  107.94 -30.00   0.00   29
 16  ω    104.00 178.00   1.00   30.00    --  107.94 111.00-120.00   74
 17  ω     28.00 109.00   1.00   30.00    --  107.94-111.00 -60.00   81
 18  ω     28.00  57.00   1.00   30.00    --  107.94 -30.00  90.00   29
 19  ω     28.00  57.00   1.00   30.00    --  107.94 -30.00 150.00   29
 20  ω     28.00  57.00   1.00   30.00    --  107.94 -30.00-150.00   29
 21  ω     28.00 109.00   1.00   30.00    --  107.94-111.00 150.00   81
 22  ω     31.00  72.00   1.00   30.00    --  107.94 -45.00-120.00   41
 23  ω     20.00  52.00   1.00   30.00    --  107.94  -6.00 -34.00   32
 24  ω     35.00  69.00   1.00   30.00    --  107.94 -45.00 120.00   34
 25  ω     26.00 126.00   1.00   30.00    --  107.94 -77.00  30.00  100
 26  ω     38.00 159.00   1.00   30.00    --  107.94  15.00   0.00  121
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1333317000
_diffrn_orient_matrix_UB_12      0.0052945000
_diffrn_orient_matrix_UB_13      -0.0467692000
_diffrn_orient_matrix_UB_21      0.0973713000
_diffrn_orient_matrix_UB_22      0.0071334000
_diffrn_orient_matrix_UB_23      -0.1063983000
_diffrn_orient_matrix_UB_31      -0.0009640000
_diffrn_orient_matrix_UB_32      -0.1172479000
_diffrn_orient_matrix_UB_33      0.0248776000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5677
_reflns_number_total             6469
_reflns_odcompleteness_completeness 97.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6469
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0406
_refine_ls_restrained_S_all      1.036
_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)+(0.0664P)²+1.1950P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1148
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N6A-C19 \\sim N6-C17
 with sigma of 0.02
 N6-C19 \\sim N6A-C19A
 with sigma of 0.02
 C17-C18 \\sim C18A-C19
 with sigma of 0.02
3. Restrained planarity
 N6A, C16, C19, C19A
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 N6, N6A, C17, C18, C18A, C19, C19A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N6A)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(H19D)=Sof(H19E)=
 Sof(C19A)=Sof(H19F)=Sof(H19G)=Sof(H19H)=1-FVAR(1)
 Sof(N6)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
6.a Free rotating group:
 O5(H5A,H5B)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C17(H17A,H17B), C19(H19D,H19E)
6.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29),
  C30(H30)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F),
 C19(H19A,H19B,H19C), C19A(H19F,H19G,H19H)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.04616(3) 0.31818(3) 0.11137(2) 0.02560(11) Uani 1 1 d . . . . .
S1 S -0.03543(6) 0.38534(4) -0.04014(4) 0.02783(14) Uani 1 1 d . . . . .
S2 S -0.17627(6) 0.28602(6) 0.21212(5) 0.04236(18) Uani 1 1 d . . . . .
N1 N -0.0345(2) 0.29464(15) -0.18727(15) 0.0278(4) Uani 1 1 d . . . . .
N2 N 0.0611(2) 0.19952(14) -0.05413(14) 0.0236(4) Uani 1 1 d . . . . .
H2 H 0.079685 0.152291 -0.086956 0.028 Uiso 1 1 calc R U . . .
N3 N 0.09511(19) 0.18287(14) 0.04009(14) 0.0232(4) Uani 1 1 d . . . . .
N4 N 0.1619(2) 0.02156(14) -0.06360(15) 0.0245(4) Uani 1 1 d . . . . .
N5 N 0.0782(3) 0.05113(18) 0.26041(17) 0.0389(5) Uani 1 1 d . . . . .
N6 N -0.2182(4) 0.2585(5) 0.4190(3) 0.0340(9) Uani 0.668(8) 1 d D . P A 1
N6A N -0.2246(9) 0.2234(6) 0.4162(6) 0.026(2) Uiso 0.332(8) 1 d D . P A 2
N7 N 0.0092(2) 0.28683(16) 0.33570(15) 0.0282(4) Uani 1 1 d . . . . .
N8 N 0.1024(2) 0.30945(14) 0.24359(14) 0.0249(4) Uani 1 1 d . . . . .
N9 N 0.2560(2) 0.36044(14) 0.05744(14) 0.0243(4) Uani 1 1 d . . . . .
N10 N 0.3559(2) 0.44927(15) 0.29666(15) 0.0281(4) Uani 1 1 d . . . . .
C1 C -0.0010(2) 0.28817(17) -0.09758(17) 0.0251(4) Uani 1 1 d . . . . .
C2 C -0.1028(3) 0.38586(19) -0.24444(19) 0.0325(5) Uani 1 1 d . . . . .
H2A H -0.151020 0.424645 -0.196176 0.039 Uiso 1 1 calc R U . . .
H2B H -0.176545 0.364388 -0.274552 0.039 Uiso 1 1 calc R U . . .
C3 C 0.0061(3) 0.4541(2) -0.3298(2) 0.0434(7) Uani 1 1 d . . . . .
H3A H 0.052170 0.416391 -0.378611 0.065 Uiso 1 1 calc R U . . .
H3B H 0.078755 0.475917 -0.300032 0.065 Uiso 1 1 calc R U . . .
H3C H -0.042266 0.514189 -0.365840 0.065 Uiso 1 1 calc R U . . .
C4 C 0.0087(3) 0.21501(18) -0.23964(18) 0.0326(5) Uani 1 1 d . . . . .
H4A H 0.112867 0.206469 -0.250304 0.049 Uiso 1 1 calc R U . . .
H4B H -0.019559 0.234845 -0.306523 0.049 Uiso 1 1 calc R U . . .
H4C H -0.038463 0.150504 -0.197097 0.049 Uiso 1 1 calc R U . . .
C5 C 0.1581(2) 0.09779(17) 0.07551(17) 0.0240(4) Uani 1 1 d . . . . .
C6 C 0.2031(2) 0.01555(16) 0.02558(17) 0.0241(4) Uani 1 1 d . . . . .
C7 C 0.2034(2) -0.05135(18) -0.10966(19) 0.0283(5) Uani 1 1 d . . . . .
H7 H 0.173981 -0.047348 -0.171950 0.034 Uiso 1 1 calc R U . . .
C8 C 0.2878(3) -0.13324(19) -0.0710(2) 0.0336(5) Uani 1 1 d . . . . .
H8 H 0.316216 -0.183583 -0.106463 0.040 Uiso 1 1 calc R U . . .
C9 C 0.3291(3) -0.13979(19) 0.0198(2) 0.0358(5) Uani 1 1 d . . . . .
H9 H 0.386483 -0.195059 0.048155 0.043 Uiso 1 1 calc R U . . .
C10 C 0.2863(3) -0.06503(18) 0.06949(19) 0.0295(5) Uani 1 1 d . . . . .
H10 H 0.313256 -0.068554 0.132524 0.035 Uiso 1 1 calc R U . . .
C11 C 0.1888(3) 0.08423(17) 0.17998(18) 0.0273(5) Uani 1 1 d . . . . .
C12 C 0.1041(4) 0.0399(2) 0.3541(2) 0.0489(7) Uani 1 1 d . . . . .
H12 H 0.027448 0.017955 0.412076 0.059 Uiso 1 1 calc R U . . .
C13 C 0.2350(4) 0.0583(2) 0.3716(2) 0.0484(7) Uani 1 1 d . . . . .
H13 H 0.247415 0.049613 0.439835 0.058 Uiso 1 1 calc R U . . .
C14 C 0.3474(4) 0.0894(2) 0.2887(3) 0.0463(7) Uani 1 1 d . . . . .
H14 H 0.439461 0.101271 0.298591 0.056 Uiso 1 1 calc R U . . .
C15 C 0.3238(3) 0.1031(2) 0.1900(2) 0.0367(5) Uani 1 1 d . . . . .
H15 H 0.399140 0.124904 0.130985 0.044 Uiso 1 1 calc R U . . .
C16 C -0.1238(3) 0.2717(2) 0.32843(19) 0.0354(5) Uani 1 1 d . . . . .
C17 C -0.3736(4) 0.2463(4) 0.4292(4) 0.0318(10) Uani 0.668(8) 1 d D . P A 1
H17A H -0.399292 0.281154 0.362206 0.038 Uiso 0.668(8) 1 calc R U P A 1
H17B H -0.426206 0.280131 0.480672 0.038 Uiso 0.668(8) 1 calc R U P A 1
C18 C -0.4214(5) 0.1356(4) 0.4618(4) 0.0398(11) Uani 0.668(8) 1 d D . P A 1
H18A H -0.369285 0.101374 0.411469 0.060 Uiso 0.668(8) 1 calc R U P A 1
H18B H -0.524537 0.132569 0.464972 0.060 Uiso 0.668(8) 1 calc R U P A 1
H18C H -0.401374 0.101500 0.529874 0.060 Uiso 0.668(8) 1 calc R U P A 1
C18A C -0.2237(10) 0.3389(6) 0.5191(6) 0.039(2) Uani 0.332(8) 1 d D . P A 2
H18D H -0.166155 0.390127 0.461625 0.059 Uiso 0.332(8) 1 calc R U P A 2
H18E H -0.212552 0.348369 0.584568 0.059 Uiso 0.332(8) 1 calc R U P A 2
H18F H -0.324842 0.346697 0.514614 0.059 Uiso 0.332(8) 1 calc R U P A 2
C19 C -0.1769(3) 0.2396(3) 0.5140(2) 0.0458(7) Uani 1 1 d D . . . .
H19A H -0.100585 0.188504 0.517766 0.069 Uiso 0.668(8) 1 calc R U P A 1
H19B H -0.259445 0.214150 0.570339 0.069 Uiso 0.668(8) 1 calc R U P A 1
H19C H -0.141690 0.303056 0.520076 0.069 Uiso 0.668(8) 1 calc R U P A 1
H19D H -0.221904 0.187478 0.577621 0.055 Uiso 0.332(8) 1 calc R U P A 2
H19E H -0.071446 0.234516 0.505712 0.055 Uiso 0.332(8) 1 calc R U P A 2
C19A C -0.3685(9) 0.1971(11) 0.4148(8) 0.041(3) Uani 0.332(8) 1 d D . P A 2
H19F H -0.415374 0.257691 0.378215 0.062 Uiso 0.332(8) 1 calc R U P A 2
H19G H -0.423401 0.171783 0.485760 0.062 Uiso 0.332(8) 1 calc R U P A 2
H19H H -0.364275 0.143885 0.379480 0.062 Uiso 0.332(8) 1 calc R U P A 2
C20 C 0.2317(2) 0.34025(16) 0.23705(17) 0.0241(4) Uani 1 1 d . . . . .
C21 C 0.3253(2) 0.35829(16) 0.13372(17) 0.0238(4) Uani 1 1 d . . . . .
C22 C 0.3323(3) 0.37297(17) -0.03892(17) 0.0268(4) Uani 1 1 d . . . . .
H22 H 0.283391 0.374776 -0.092195 0.032 Uiso 1 1 calc R U . . .
C23 C 0.4800(3) 0.38335(16) -0.06337(18) 0.0279(5) Uani 1 1 d . . . . .
H23 H 0.531522 0.393055 -0.132425 0.033 Uiso 1 1 calc R U . . .
C24 C 0.5512(2) 0.37936(16) 0.01446(18) 0.0277(5) Uani 1 1 d . . . . .
H24 H 0.652752 0.384870 -0.000347 0.033 Uiso 1 1 calc R U . . .
C25 C 0.4735(2) 0.36725(16) 0.11437(18) 0.0255(4) Uani 1 1 d . . . . .
H25 H 0.520792 0.365117 0.168576 0.031 Uiso 1 1 calc R U . . .
C26 C 0.2813(2) 0.36162(17) 0.32381(17) 0.0245(4) Uani 1 1 d . . . . .
C27 C 0.3937(3) 0.47817(19) 0.3720(2) 0.0337(5) Uani 1 1 d . . . . .
H27 H 0.445801 0.540186 0.354014 0.040 Uiso 1 1 calc R U . . .
C28 C 0.3607(3) 0.4220(2) 0.47532(19) 0.0354(5) Uani 1 1 d . . . . .
H28 H 0.386640 0.446305 0.526799 0.042 Uiso 1 1 calc R U . . .
C29 C 0.2894(3) 0.33029(19) 0.50134(18) 0.0311(5) Uani 1 1 d . . . . .
H29 H 0.269483 0.288717 0.570767 0.037 Uiso 1 1 calc R U . . .
C30 C 0.2472(2) 0.29945(18) 0.42456(18) 0.0273(4) Uani 1 1 d . . . . .
H30 H 0.196148 0.237265 0.440669 0.033 Uiso 1 1 calc R U . . .
Cl1 Cl -0.44274(6) -0.21950(4) 0.23966(4) 0.03026(14) Uani 1 1 d . . . . .
O1 O -0.4176(3) -0.15032(17) 0.29510(18) 0.0556(6) Uani 1 1 d . . . . .
O2 O -0.4036(2) -0.17172(14) 0.13109(14) 0.0370(4) Uani 1 1 d . . . . .
O3 O -0.3567(2) -0.30945(15) 0.26594(15) 0.0439(5) Uani 1 1 d . . . . .
O4 O -0.5913(2) -0.24834(18) 0.26611(17) 0.0511(5) Uani 1 1 d . . . . .
O5 O -0.1977(4) -0.0679(3) 0.3782(2) 0.0809(9) Uani 1 1 d G . . . .
H5A H -0.266068 -0.074362 0.348056 0.121 Uiso 1 1 d G U . . .
H5B H -0.136792 -0.026131 0.330412 0.121 Uiso 1 1 d G 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 S1 2.3195(6) . ?
Cu1 S2 2.2630(7) . ?
Cu1 N3 2.3147(19) . ?
Cu1 N8 1.9874(19) . ?
Cu1 N9 2.0371(19) . ?
S1 C1 1.716(2) . ?
S2 C16 1.744(3) . ?
N1 C1 1.326(3) . ?
N1 C2 1.475(3) . ?
N1 C4 1.466(3) . ?
N2 H2 0.8800 . ?
N2 N3 1.366(3) . ?
N2 C1 1.356(3) . ?
N3 C5 1.296(3) . ?
N4 C6 1.355(3) . ?
N4 C7 1.328(3) . ?
N5 C11 1.347(3) . ?
N5 C12 1.337(4) . ?
N6 C16 1.346(4) . ?
N6 C17 1.476(5) . ?
N6 C19 1.404(5) . ?
N6A C16 1.394(9) . ?
N6A C19 1.594(9) . ?
N6A C19A 1.449(11) . ?
N7 N8 1.351(3) . ?
N7 C16 1.330(3) . ?
N8 C20 1.305(3) . ?
N9 C21 1.356(3) . ?
N9 C22 1.341(3) . ?
N10 C26 1.346(3) . ?
N10 C27 1.338(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.514(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.478(3) . ?
C5 C11 1.496(3) . ?
C6 C10 1.394(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.390(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.376(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.384(4) . ?
C10 H10 0.9500 . ?
C11 C15 1.375(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.375(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.373(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.392(4) . ?
C15 H15 0.9500 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.517(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18A H18D 0.9800 . ?
C18A H18E 0.9800 . ?
C18A H18F 0.9800 . ?
C18A C19 1.421(9) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 H19D 0.9900 . ?
C19 H19E 0.9900 . ?
C19A H19F 0.9800 . ?
C19A H19G 0.9800 . ?
C19A H19H 0.9800 . ?
C20 C21 1.473(3) . ?
C20 C26 1.489(3) . ?
C21 C25 1.390(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.384(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.382(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.388(3) . ?
C25 H25 0.9500 . ?
C26 C30 1.388(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.392(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.378(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.391(3) . ?
C30 H30 0.9500 . ?
Cl1 O1 1.436(2) . ?
Cl1 O2 1.4301(18) . ?
Cl1 O3 1.443(2) . ?
Cl1 O4 1.436(2) . ?
O5 H5A 0.8698 . ?
O5 H5B 0.8701 . ?

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
S2 Cu1 S1 94.30(2) . . ?
S2 Cu1 N3 104.99(5) . . ?
N3 Cu1 S1 80.17(5) . . ?
N8 Cu1 S1 160.26(6) . . ?
N8 Cu1 S2 83.66(6) . . ?
N8 Cu1 N3 119.38(7) . . ?
N8 Cu1 N9 80.16(8) . . ?
N9 Cu1 S1 98.83(5) . . ?
N9 Cu1 S2 162.69(6) . . ?
N9 Cu1 N3 88.41(7) . . ?
C1 S1 Cu1 102.18(8) . . ?
C16 S2 Cu1 95.80(9) . . ?
C1 N1 C2 122.3(2) . . ?
C1 N1 C4 120.96(19) . . ?
C4 N1 C2 116.45(19) . . ?
N3 N2 H2 119.7 . . ?
C1 N2 H2 119.7 . . ?
C1 N2 N3 120.62(18) . . ?
N2 N3 Cu1 114.61(13) . . ?
C5 N3 Cu1 127.94(15) . . ?
C5 N3 N2 117.28(19) . . ?
C7 N4 C6 118.48(19) . . ?
C12 N5 C11 116.3(3) . . ?
C16 N6 C17 122.6(4) . . ?
C16 N6 C19 123.2(3) . . ?
C19 N6 C17 113.6(3) . . ?
C16 N6A C19 108.0(5) . . ?
C16 N6A C19A 124.0(7) . . ?
C19A N6A C19 124.6(7) . . ?
C16 N7 N8 112.98(19) . . ?
N7 N8 Cu1 123.32(15) . . ?
C20 N8 Cu1 116.59(15) . . ?
C20 N8 N7 119.47(19) . . ?
C21 N9 Cu1 112.98(15) . . ?
C22 N9 Cu1 126.93(16) . . ?
C22 N9 C21 119.1(2) . . ?
C27 N10 C26 117.4(2) . . ?
N1 C1 S1 122.05(17) . . ?
N1 C1 N2 115.6(2) . . ?
N2 C1 S1 122.38(17) . . ?
N1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
N1 C2 C3 111.4(2) . . ?
H2A C2 H2B 108.0 . . ?
C3 C2 H2A 109.3 . . ?
C3 C2 H2B 109.3 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 C6 128.3(2) . . ?
N3 C5 C11 114.1(2) . . ?
C6 C5 C11 117.63(18) . . ?
N4 C6 C5 118.10(19) . . ?
N4 C6 C10 121.6(2) . . ?
C10 C6 C5 120.3(2) . . ?
N4 C7 H7 118.5 . . ?
N4 C7 C8 123.1(2) . . ?
C8 C7 H7 118.5 . . ?
C7 C8 H8 120.7 . . ?
C9 C8 C7 118.6(2) . . ?
C9 C8 H8 120.7 . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.3(2) . . ?
C10 C9 H9 120.3 . . ?
C6 C10 H10 120.5 . . ?
C9 C10 C6 119.0(2) . . ?
C9 C10 H10 120.5 . . ?
N5 C11 C5 115.8(2) . . ?
N5 C11 C15 123.8(2) . . ?
C15 C11 C5 120.3(2) . . ?
N5 C12 H12 118.0 . . ?
N5 C12 C13 124.0(3) . . ?
C13 C12 H12 118.0 . . ?
C12 C13 H13 120.6 . . ?
C14 C13 C12 118.8(3) . . ?
C14 C13 H13 120.6 . . ?
C13 C14 H14 120.6 . . ?
C13 C14 C15 118.8(3) . . ?
C15 C14 H14 120.6 . . ?
C11 C15 C14 118.3(3) . . ?
C11 C15 H15 120.8 . . ?
C14 C15 H15 120.8 . . ?
N6 C16 S2 122.8(2) . . ?
N6A C16 S2 114.7(4) . . ?
N7 C16 S2 124.06(19) . . ?
N7 C16 N6 112.5(3) . . ?
N7 C16 N6A 120.1(4) . . ?
N6 C17 H17A 108.9 . . ?
N6 C17 H17B 108.9 . . ?
N6 C17 C18 113.3(4) . . ?
H17A C17 H17B 107.7 . . ?
C18 C17 H17A 108.9 . . ?
C18 C17 H17B 108.9 . . ?
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 . . ?
H18D C18A H18E 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C19 C18A H18D 109.5 . . ?
C19 C18A H18E 109.5 . . ?
C19 C18A H18F 109.5 . . ?
N6 C19 H19A 109.5 . . ?
N6 C19 H19B 109.5 . . ?
N6 C19 H19C 109.5 . . ?
N6A C19 H19D 110.5 . . ?
N6A C19 H19E 110.5 . . ?
C18A C19 N6A 106.1(5) . . ?
C18A C19 H19D 110.5 . . ?
C18A C19 H19E 110.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
H19D C19 H19E 108.7 . . ?
N6A C19A H19F 109.5 . . ?
N6A C19A H19G 109.5 . . ?
N6A C19A H19H 109.5 . . ?
H19F C19A H19G 109.5 . . ?
H19F C19A H19H 109.5 . . ?
H19G C19A H19H 109.5 . . ?
N8 C20 C21 114.4(2) . . ?
N8 C20 C26 123.9(2) . . ?
C21 C20 C26 121.5(2) . . ?
N9 C21 C20 114.6(2) . . ?
N9 C21 C25 121.4(2) . . ?
C25 C21 C20 124.0(2) . . ?
N9 C22 H22 118.9 . . ?
N9 C22 C23 122.2(2) . . ?
C23 C22 H22 118.9 . . ?
C22 C23 H23 120.6 . . ?
C24 C23 C22 118.8(2) . . ?
C24 C23 H23 120.6 . . ?
C23 C24 H24 120.2 . . ?
C23 C24 C25 119.6(2) . . ?
C25 C24 H24 120.2 . . ?
C21 C25 H25 120.6 . . ?
C24 C25 C21 118.8(2) . . ?
C24 C25 H25 120.6 . . ?
N10 C26 C20 113.87(19) . . ?
N10 C26 C30 123.1(2) . . ?
C30 C26 C20 123.0(2) . . ?
N10 C27 H27 118.3 . . ?
N10 C27 C28 123.3(2) . . ?
C28 C27 H27 118.3 . . ?
C27 C28 H28 120.7 . . ?
C29 C28 C27 118.6(2) . . ?
C29 C28 H28 120.7 . . ?
C28 C29 H29 120.5 . . ?
C28 C29 C30 119.1(2) . . ?
C30 C29 H29 120.5 . . ?
C26 C30 C29 118.5(2) . . ?
C26 C30 H30 120.8 . . ?
C29 C30 H30 120.8 . . ?
O1 Cl1 O3 108.96(13) . . ?
O2 Cl1 O1 109.78(13) . . ?
O2 Cl1 O3 109.30(12) . . ?
O2 Cl1 O4 108.93(12) . . ?
O4 Cl1 O1 110.52(15) . . ?
O4 Cl1 O3 109.34(14) . . ?
H5A O5 H5B 104.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2 N4 0.88 1.88 2.593(3) 136.8 . yes
O5 H5A O1 0.87 2.19 3.015(4) 158.5 . yes
O5 H5B N5 0.87 2.25 3.060(4) 154.3 . yes

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 S1 C1 N1 178.78(18) . . . . ?
Cu1 S1 C1 N2 -0.7(2) . . . . ?
Cu1 S2 C16 N6 174.6(4) . . . . ?
Cu1 S2 C16 N6A -163.3(4) . . . . ?
Cu1 S2 C16 N7 4.5(2) . . . . ?
Cu1 N3 C5 C6 -173.14(16) . . . . ?
Cu1 N3 C5 C11 6.2(3) . . . . ?
Cu1 N8 C20 C21 -11.2(2) . . . . ?
Cu1 N8 C20 C26 165.56(16) . . . . ?
Cu1 N9 C21 C20 -8.1(2) . . . . ?
Cu1 N9 C21 C25 168.71(16) . . . . ?
Cu1 N9 C22 C23 -167.78(16) . . . . ?
N2 N3 C5 C6 1.9(3) . . . . ?
N2 N3 C5 C11 -178.69(19) . . . . ?
N3 N2 C1 S1 2.0(3) . . . . ?
N3 N2 C1 N1 -177.47(19) . . . . ?
N3 C5 C6 N4 -7.8(3) . . . . ?
N3 C5 C6 C10 171.7(2) . . . . ?
N3 C5 C11 N5 81.2(3) . . . . ?
N3 C5 C11 C15 -100.2(3) . . . . ?
N4 C6 C10 C9 0.8(4) . . . . ?
N4 C7 C8 C9 0.7(4) . . . . ?
N5 C11 C15 C14 -1.4(4) . . . . ?
N5 C12 C13 C14 -0.5(5) . . . . ?
N7 N8 C20 C21 177.48(18) . . . . ?
N7 N8 C20 C26 -5.8(3) . . . . ?
N8 N7 C16 S2 -3.3(3) . . . . ?
N8 N7 C16 N6 -174.3(3) . . . . ?
N8 N7 C16 N6A 163.9(4) . . . . ?
N8 C20 C21 N9 12.7(3) . . . . ?
N8 C20 C21 C25 -164.0(2) . . . . ?
N8 C20 C26 N10 -134.6(2) . . . . ?
N8 C20 C26 C30 42.3(3) . . . . ?
N9 C21 C25 C24 0.5(3) . . . . ?
N9 C22 C23 C24 0.8(3) . . . . ?
N10 C26 C30 C29 1.4(3) . . . . ?
N10 C27 C28 C29 2.2(4) . . . . ?
C1 N1 C2 C3 99.1(3) . . . . ?
C1 N2 N3 Cu1 -2.2(2) . . . . ?
C1 N2 N3 C5 -178.0(2) . . . . ?
C2 N1 C1 S1 0.4(3) . . . . ?
C2 N1 C1 N2 179.9(2) . . . . ?
C4 N1 C1 S1 173.92(18) . . . . ?
C4 N1 C1 N2 -6.6(3) . . . . ?
C4 N1 C2 C3 -74.7(3) . . . . ?
C5 C6 C10 C9 -178.7(2) . . . . ?
C5 C11 C15 C14 -180.0(2) . . . . ?
C6 N4 C7 C8 -0.4(3) . . . . ?
C6 C5 C11 N5 -99.4(2) . . . . ?
C6 C5 C11 C15 79.2(3) . . . . ?
C7 N4 C6 C5 179.2(2) . . . . ?
C7 N4 C6 C10 -0.4(3) . . . . ?
C7 C8 C9 C10 -0.2(4) . . . . ?
C8 C9 C10 C6 -0.5(4) . . . . ?
C11 N5 C12 C13 -1.2(4) . . . . ?
C11 C5 C6 N4 172.8(2) . . . . ?
C11 C5 C6 C10 -7.7(3) . . . . ?
C12 N5 C11 C5 -179.2(2) . . . . ?
C12 N5 C11 C15 2.2(4) . . . . ?
C12 C13 C14 C15 1.3(4) . . . . ?
C13 C14 C15 C11 -0.4(4) . . . . ?
C16 N6 C17 C18 94.3(6) . . . . ?
C16 N6A C19 C18A 81.0(6) . . . . ?
C16 N7 N8 Cu1 -0.4(3) . . . . ?
C16 N7 N8 C20 170.3(2) . . . . ?
C17 N6 C16 S2 5.3(7) . . . . ?
C17 N6 C16 N7 176.5(4) . . . . ?
C19 N6 C16 S2 175.3(4) . . . . ?
C19 N6 C16 N7 -13.6(7) . . . . ?
C19 N6 C17 C18 -76.5(5) . . . . ?
C19 N6A C16 S2 -167.0(3) . . . . ?
C19 N6A C16 N7 24.7(7) . . . . ?
C19A N6A C16 S2 -7.1(9) . . . . ?
C19A N6A C16 N7 -175.4(7) . . . . ?
C19A N6A C19 C18A -78.7(9) . . . . ?
C20 C21 C25 C24 177.0(2) . . . . ?
C20 C26 C30 C29 -175.1(2) . . . . ?
C21 N9 C22 C23 0.3(3) . . . . ?
C21 C20 C26 N10 41.9(3) . . . . ?
C21 C20 C26 C30 -141.2(2) . . . . ?
C22 N9 C21 C20 -177.78(19) . . . . ?
C22 N9 C21 C25 -1.0(3) . . . . ?
C22 C23 C24 C25 -1.3(3) . . . . ?
C23 C24 C25 C21 0.7(3) . . . . ?
C26 N10 C27 C28 0.5(4) . . . . ?
C26 C20 C21 N9 -164.07(19) . . . . ?
C26 C20 C21 C25 19.2(3) . . . . ?
C27 N10 C26 C20 174.5(2) . . . . ?
C27 N10 C26 C30 -2.3(3) . . . . ?
C27 C28 C29 C30 -3.0(4) . . . . ?
C28 C29 C30 C26 1.3(4) . . . . ?

loop_
_audit_author_email
mahendiran.dharmasivam@sydney.edu.au
?
d.richardson@sydney.edu.au
_olex2_date_sample_data_collection 2019-11-29
_olex2_date_sample_submission    2019-11-07
_olex2_exptl_crystal_mounting_method 'in paratone on a micromount'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.371
_oxdiff_exptl_absorpt_empirical_full_min 0.853
####################################################################### 
# 
# 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_drr18_s1671
_database_code_depnum_ccdc_archive 'CCDC 1959773'
loop_
_audit_author_name
_audit_author_address
'William Lewis'
;University of Sydney
Australia
;
_audit_update_record             
;
2019-10-17 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
_sydney_internal_submission_code drr18_s1671
_sydney_internal_submission_date 2018-09-03
_sydney_internal_submission_number s1671
_sydney_internal_client_code     dm1
_sydney_internal_client_email    mahendiran.dharmasivam@sydney.edu.au
_sydney_internal_client_name     'Mahendiran Dharmasivam'
_sydney_internal_supervisor_code drr
_sydney_internal_supervisor_name 'Des Richardson'
_sydney_internal_collection_date 2018-09-10
_sydney_internal_collection_user wlew0588
_sydney_internal_process_date    2018-09-10
_sydney_internal_process_user    wlew0588
_sydney_internal_solution_date   2018-09-10
_sydney_internal_solution_user   wlew0588
_sydney_internal_refine_date     2018-09-10
_sydney_internal_refine_user     wlew0588
_sydney_internal_check_and_archive_date 2018-09-11
_sydney_internal_check_user      wlew0588
_refine_special_details          
;
One of the two coordinated ligands exhibits disorder in two different locations - 
the non-coordinating pyridine ring is rotationally disordered over two orientations, 
and the termincal carbon atom of the ethyl group is disordered over two positions. 
The occupancies of the disorder components were refeind competitively, converging 
to ratios of 0.57:0.43 and 0.58:0.42, respectively. The location of the nitrogen 
atoms of the disordered pyridine rings was determined by examining both thermal 
parameter information and residual density information to locate the hydrogen atoms 
of the CH of the opposite CH of the ring. All hydrogen atoms were subsequently 
placed in calculated positions and refined with a riding model. 

Enhanced rigid bond and similarity restraints were applied to the thermal parameters 
of the disordered atoms and the atoms to which they are bonded.
;
_audit_creation_date             2018-09-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H32 N10 S2 Zn'
_chemical_formula_sum            'C30 H32 N10 S2 Zn'
_chemical_formula_weight         662.14
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H34N10S2Zn
_chemical_oxdiff_usercomment     drr18_s1671
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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7315(10)
_cell_length_b                   10.8268(12)
_cell_length_c                   14.7436(13)
_cell_angle_alpha                109.844(9)
_cell_angle_beta                 91.411(7)
_cell_angle_gamma                103.463(9)
_cell_volume                     1556.9(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5736
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.4040
_cell_measurement_theta_min      4.2060
_shelx_estimated_absorpt_T_max   0.659
_shelx_estimated_absorpt_T_min   0.344
_exptl_absorpt_coefficient_mu    2.656
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.196
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             688
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 1 6 0.1574
0 0 1 0.2015
5 -1 -4 0.1677
5 -1 -1 0.1430
5 -1 1 0.1904
-1 1 -5 0.1774
-5 2 -5 0.2488
0 1 0 0.0521
0 -1 0 0.1189
-1 -5 -3 0.1155
0 -3 5 0.2305
-4 -5 5 0.1967
5 3 0 0.1259
4 -1 5 0.2466
3 -5 -2 0.0639
1 -4 -5 0.1108
-3 5 2 0.1231
-1 3 5 0.1437

_exptl_crystal_recrystallization_method 
'crystallised from a solution in methanol'
_exptl_crystal_size_max          0.511
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.171
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
-5.0041 1.0017 5.9990 0.8011 -0.5293 0.0841
-0.0007 0.0007 0.9999 0.0490 -0.0476 0.0885
5.0027 -1.0003 -3.9992 -0.7032 0.4340 0.0930
5.0005 -0.9981 -0.9994 -0.5564 0.2911 0.3586
4.9991 -0.9967 1.0004 -0.4585 0.1958 0.5357
-0.9968 0.9960 -5.0003 -0.1892 0.0748 -0.5123
-4.9968 1.9940 -5.0009 0.2052 -0.1486 -0.8650
-0.0006 1.0002 -0.0008 -0.0575 -0.1434 0.0248
0.0006 -1.0002 0.0008 0.0575 0.1434 -0.0248
-0.9948 -5.0038 -2.9958 0.2534 0.8401 -0.4840
-0.0019 -2.9970 5.0019 0.4171 0.1921 0.3683
-4.0001 -4.9998 5.0037 0.9840 0.3990 -0.0588
4.9975 3.0035 -0.0026 -0.7373 -0.3303 0.5463
3.9964 -0.9943 5.0001 -0.1497 -0.0148 0.7954
3.0038 -5.0008 -1.9961 -0.1495 0.8724 -0.0179
1.0057 -4.0039 -4.9965 -0.1279 0.8320 -0.4475
-3.0038 5.0008 1.9961 0.1495 -0.8724 0.0179
-1.0051 3.0037 4.9973 0.1854 -0.6885 0.4227

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10830
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.230
_diffrn_reflns_theta_min         4.264
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.5861
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -86.00  32.00   2.00    2.00    --  -40.45  19.00 150.00   59
  2  ω    -24.00  32.00   2.00    2.00    --  -40.45  38.00-180.00   28
  3  ω    -50.00  36.00   2.00    2.00    --  -40.45  38.00  30.00   43
  4  ω     66.00  92.00   2.00    2.00    --   40.45-178.00 -30.00   13
  5  ω     58.00 126.00   2.00    2.00    --   40.45 178.00   0.00   34
  6  ω     82.00 128.00   2.00    2.00    --   40.45 178.00-180.00   23
  7  ω    100.00 128.00   2.00    2.00    --   40.45-178.00 -30.00   14
  8  ω     69.00  97.00   2.00    2.00    --  107.93 -45.00-150.00   14
  9  ω     77.00 177.00   2.00    2.00    --  107.93  30.00  90.00   50
 10  ω     52.00 122.00   2.00    2.00    --  107.93 -61.00   0.00   35
 11  ω     54.00 100.00   2.00    2.00    --  107.93-125.00-180.00   23
 12  ω     80.00 178.00   2.00    2.00    --  107.93  30.00   0.00   49
 13  ω     65.00  91.00   2.00    2.00    --  107.93 -30.00  30.00   13
 14  ω     35.00  75.00   2.00    2.00    --  107.93 -45.00 -30.00   20
 15  ω     30.00  80.00   2.00    2.00    --  107.93 -30.00  90.00   25
 16  ω     84.00 116.00   2.00    2.00    --  107.93-125.00  90.00   16
 17  ω     26.00 102.00   2.00    2.00    --  107.93 -95.00 -30.00   38
 18  ω     29.00 125.00   2.00    2.00    --  107.93 -77.00-180.00   48
 19  ω     30.00  88.00   2.00    2.00    --  107.93 -30.00-180.00   29
 20  ω     90.00 116.00   2.00    2.00    --  107.93-125.00-150.00   13
 21  ω     92.00 116.00   2.00    2.00    --  107.93-125.00 -60.00   12
 22  ω     56.00  82.00   2.00    2.00    --  107.93 -30.00 -90.00   13
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1129602000
_diffrn_orient_matrix_UB_12      -0.0574715000
_diffrn_orient_matrix_UB_13      0.0489172000
_diffrn_orient_matrix_UB_21      0.0200798000
_diffrn_orient_matrix_UB_22      -0.1434277000
_diffrn_orient_matrix_UB_23      -0.0475297000
_diffrn_orient_matrix_UB_31      0.0943901000
_diffrn_orient_matrix_UB_32      0.0249158000
_diffrn_orient_matrix_UB_33      0.0885936000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5433
_reflns_number_total             6092
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6092
_refine_ls_number_restraints     249
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0362
_refine_ls_restrained_S_all      1.044
_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)+(0.0444P)²+1.2470P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0969
_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
 C16-C15 \\sim C35A-C34 \\sim C35-C34
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N22 \\sim N22A \\sim C27 \\sim C28 \\sim C28A \\sim C29 \\sim C29A \\sim C30
\\sim C30A \\sim C31 \\sim C31A \\sim C34 \\sim C35 \\sim C35A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N22, N22A, C27, C28, C28A, C29, C29A, C30, C30A, C31, C31A, C34, C35, C35A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N22A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C31A)=Sof(H31A)=1-FVAR(1)
 Sof(N22)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C31)=Sof(H31)=FVAR(1)
 Sof(C30A)=Sof(H30A)=1-FVAR(2)
 Sof(C30)=Sof(H30)=FVAR(2)
 Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(3)
 Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C34(H34A,H34B), C34(H34C,H34D)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C21(H21),
 C22(H22), C23(H23), C24(H24), C28(H28), C28A(H28A), C29(H29), C29A(H29A),
 C30(H30), C30A(H30A), C31(H31), C31A(H31A)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C35(H35A,H35B,H35C), C35A(H35D,H35E,
 H35F), C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.26798(3) 0.91159(3) 0.21748(2) 0.02180(9) Uani 1 1 d . . . . .
S1 S 0.32499(5) 1.15806(6) 0.25832(4) 0.02635(13) Uani 1 1 d . . . . .
S21 S 0.46098(5) 0.88098(6) 0.28445(4) 0.02907(13) Uani 1 1 d . . . . .
N1 N 0.20721(17) 0.69644(18) 0.11494(13) 0.0225(4) Uani 1 1 d . . . . .
N2 N 0.10761(18) 0.7501(2) -0.14680(13) 0.0277(4) Uani 1 1 d . . . . .
N3 N 0.28460(16) 0.92304(17) 0.07622(12) 0.0196(3) Uani 1 1 d . . . . .
N4 N 0.31873(16) 1.04204(17) 0.05978(12) 0.0204(3) Uani 1 1 d . . . . .
N5 N 0.39219(18) 1.27152(18) 0.12611(13) 0.0261(4) Uani 1 1 d . . . . .
N21 N 0.05927(16) 0.90035(18) 0.20485(13) 0.0225(4) Uani 1 1 d . . . . .
N22 N -0.0743(4) 0.6413(4) 0.3644(3) 0.0374(10) Uani 0.567(4) 1 d . U P A 1
N22A N -0.0438(6) 0.8405(6) 0.4797(4) 0.0308(12) Uani 0.433(4) 1 d . U P A 2
N23 N 0.19478(17) 0.84524(19) 0.33168(12) 0.0238(4) Uani 1 1 d . . . . .
N24 N 0.26852(17) 0.8153(2) 0.39300(13) 0.0266(4) Uani 1 1 d . . . . .
N25 N 0.47263(19) 0.8219(2) 0.44459(14) 0.0327(4) Uani 1 1 d . . . . .
C1 C 0.1763(2) 0.5838(2) 0.13713(17) 0.0266(5) Uani 1 1 d . . . . .
H1 H 0.177545 0.593242 0.203630 0.032 Uiso 1 1 calc R . . . .
C2 C 0.1426(2) 0.4542(2) 0.06789(17) 0.0288(5) Uani 1 1 d . . . . .
H2 H 0.120408 0.376521 0.086231 0.035 Uiso 1 1 calc R . . . .
C3 C 0.1422(2) 0.4410(2) -0.02897(17) 0.0280(5) Uani 1 1 d . . . . .
H3 H 0.119879 0.353438 -0.078313 0.034 Uiso 1 1 calc R . . . .
C4 C 0.1745(2) 0.5564(2) -0.05323(16) 0.0255(4) Uani 1 1 d . . . . .
H4 H 0.174962 0.548949 -0.119298 0.031 Uiso 1 1 calc R . . . .
C5 C 0.20641(19) 0.6833(2) 0.02044(15) 0.0209(4) Uani 1 1 d . . . . .
C6 C 0.24250(19) 0.8116(2) 0.00157(14) 0.0194(4) Uani 1 1 d . . . . .
C7 C 0.2278(2) 0.8067(2) -0.10072(15) 0.0213(4) Uani 1 1 d . . . . .
C8 C 0.3324(2) 0.8539(2) -0.14408(15) 0.0235(4) Uani 1 1 d . . . . .
H8 H 0.415472 0.894982 -0.108442 0.028 Uiso 1 1 calc R . . . .
C9 C 0.3127(2) 0.8398(2) -0.24091(16) 0.0274(5) Uani 1 1 d . . . . .
H9 H 0.382654 0.869483 -0.273178 0.033 Uiso 1 1 calc R . . . .
C10 C 0.1901(2) 0.7819(2) -0.28958(16) 0.0310(5) Uani 1 1 d . . . . .
H10 H 0.174000 0.770855 -0.355880 0.037 Uiso 1 1 calc R . . . .
C11 C 0.0912(2) 0.7403(3) -0.23964(17) 0.0334(5) Uani 1 1 d . . . . .
H11 H 0.006603 0.702522 -0.273113 0.040 Uiso 1 1 calc R . . . .
C12 C 0.34557(19) 1.1534(2) 0.14125(15) 0.0218(4) Uani 1 1 d . . . . .
C14 C 0.4290(2) 1.2733(2) 0.03184(17) 0.0308(5) Uani 1 1 d . . . . .
H14A H 0.360876 1.293620 -0.001875 0.046 Uiso 1 1 calc GR . . . .
H14B H 0.441008 1.184327 -0.007071 0.046 Uiso 1 1 calc GR . . . .
H14C H 0.509702 1.343199 0.041151 0.046 Uiso 1 1 calc GR . . . .
C15 C 0.4153(2) 1.4050(2) 0.20350(18) 0.0332(5) Uani 1 1 d D . . . .
H15A H 0.356435 1.398040 0.253214 0.040 Uiso 1 1 calc R . . . .
H15B H 0.394513 1.470299 0.175908 0.040 Uiso 1 1 calc R . . . .
C16 C 0.5528(3) 1.4594(3) 0.2518(2) 0.0463(7) Uani 1 1 d D . . . .
H16A H 0.611941 1.463441 0.202712 0.069 Uiso 1 1 calc GR . . . .
H16B H 0.571829 1.399184 0.284080 0.069 Uiso 1 1 calc GR . . . .
H16C H 0.563565 1.550668 0.299910 0.069 Uiso 1 1 calc GR . . . .
C21 C -0.0055(2) 0.9317(2) 0.14053(16) 0.0256(4) Uani 1 1 d . . . . .
H21 H 0.041179 0.965941 0.096526 0.031 Uiso 1 1 calc R . . . .
C22 C -0.1379(2) 0.9164(2) 0.13528(17) 0.0292(5) Uani 1 1 d . . . . .
H22 H -0.181217 0.938413 0.088193 0.035 Uiso 1 1 calc R . . . .
C23 C -0.2049(2) 0.8684(3) 0.20044(17) 0.0313(5) Uani 1 1 d . . . . .
H23 H -0.295510 0.857065 0.198888 0.038 Uiso 1 1 calc R . . . .
C24 C -0.1391(2) 0.8368(2) 0.26793(16) 0.0292(5) Uani 1 1 d . . . . .
H24 H -0.183972 0.804246 0.313396 0.035 Uiso 1 1 calc R . . . .
C25 C -0.0059(2) 0.8534(2) 0.26848(15) 0.0234(4) Uani 1 1 d . . . . .
C26 C 0.0715(2) 0.8216(2) 0.33730(15) 0.0234(4) Uani 1 1 d . . . . .
C27 C 0.0058(2) 0.7635(2) 0.40736(16) 0.0255(4) Uani 1 1 d . U . . .
C28 C 0.0125(6) 0.8454(5) 0.5022(4) 0.0266(10) Uani 0.567(4) 1 d . U P A 1
H28 H 0.066302 0.935419 0.526388 0.032 Uiso 0.567(4) 1 calc R . P A 1
C28A C 0.0064(6) 0.6286(6) 0.4048(5) 0.0387(13) Uani 0.433(4) 1 d . U P A 2
H28A H 0.050366 0.574552 0.358673 0.046 Uiso 0.433(4) 1 calc R . P A 2
C29 C -0.0627(6) 0.7914(7) 0.5613(5) 0.0294(12) Uani 0.567(4) 1 d . U P A 1
H29 H -0.058041 0.842248 0.628520 0.035 Uiso 0.567(4) 1 calc R . P A 1
C29A C -0.0583(7) 0.5800(7) 0.4708(5) 0.0443(14) Uani 0.433(4) 1 d . U P A 2
H29A H -0.063177 0.489897 0.467810 0.053 Uiso 0.433(4) 1 calc R . P A 2
C30 C -0.1441(18) 0.6635(12) 0.5218(13) 0.0309(19) Uani 0.52(6) 1 d . U P A 1
H30 H -0.198854 0.625464 0.560457 0.037 Uiso 0.52(6) 1 calc R . P A 1
C30A C -0.115(2) 0.6618(15) 0.5404(13) 0.037(2) Uani 0.48(6) 1 d . U P A 2
H30A H -0.161126 0.628845 0.585268 0.044 Uiso 0.48(6) 1 calc R . P A 2
C31 C -0.1442(5) 0.5913(5) 0.4241(3) 0.0430(12) Uani 0.567(4) 1 d . U P A 1
H31 H -0.196918 0.500899 0.397919 0.052 Uiso 0.567(4) 1 calc R . P A 1
C31A C -0.1050(7) 0.7912(10) 0.5440(6) 0.0303(16) Uani 0.433(4) 1 d . U P A 2
H31A H -0.142114 0.848858 0.593572 0.036 Uiso 0.433(4) 1 calc R . P A 2
C32 C 0.3943(2) 0.8379(2) 0.37830(16) 0.0260(5) Uani 1 1 d . . . . .
C34 C 0.4208(2) 0.7754(3) 0.52135(17) 0.0380(6) Uani 1 1 d D U . . .
H34A H 0.349916 0.817759 0.545433 0.046 Uiso 0.58(3) 1 calc R . P B 1
H34B H 0.489289 0.805304 0.576139 0.046 Uiso 0.58(3) 1 calc R . P B 1
H34C H 0.331325 0.784302 0.527202 0.046 Uiso 0.42(3) 1 calc R . P B 2
H34D H 0.473462 0.832131 0.584129 0.046 Uiso 0.42(3) 1 calc R . P B 2
C35 C 0.3722(14) 0.6277(8) 0.4878(9) 0.052(2) Uani 0.58(3) 1 d D U P B 1
H35A H 0.300735 0.598147 0.436255 0.078 Uiso 0.58(3) 1 calc GR . P B 1
H35B H 0.341816 0.600609 0.542062 0.078 Uiso 0.58(3) 1 calc GR . P B 1
H35C H 0.441601 0.585259 0.462548 0.078 Uiso 0.58(3) 1 calc GR . P B 1
C35A C 0.422(2) 0.6267(10) 0.4974(13) 0.057(3) Uani 0.42(3) 1 d D U P B 2
H35D H 0.368040 0.570555 0.436193 0.085 Uiso 0.42(3) 1 calc GR . P B 2
H35E H 0.389309 0.596116 0.549581 0.085 Uiso 0.42(3) 1 calc GR . P B 2
H35F H 0.511047 0.618239 0.490977 0.085 Uiso 0.42(3) 1 calc GR . P B 2
C36 C 0.6116(2) 0.8428(3) 0.44109(19) 0.0368(6) Uani 1 1 d . . . . .
H36A H 0.628537 0.767681 0.387333 0.055 Uiso 1 1 calc GR . . . .
H36B H 0.652342 0.845944 0.502348 0.055 Uiso 1 1 calc GR . . . .
H36C H 0.647199 0.928634 0.431239 0.055 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
Zn1 S1 2.4472(7) . ?
Zn1 S21 2.4115(6) . ?
Zn1 N1 2.2339(19) . ?
Zn1 N3 2.1374(17) . ?
Zn1 N21 2.2143(17) . ?
Zn1 N23 2.1428(18) . ?
S1 C12 1.731(2) . ?
S21 C32 1.725(2) . ?
N1 C1 1.339(3) . ?
N1 C5 1.351(3) . ?
N2 C7 1.344(3) . ?
N2 C11 1.340(3) . ?
N3 N4 1.360(2) . ?
N3 C6 1.300(3) . ?
N4 C12 1.348(3) . ?
N5 C12 1.355(3) . ?
N5 C14 1.459(3) . ?
N5 C15 1.467(3) . ?
N21 C21 1.339(3) . ?
N21 C25 1.348(3) . ?
N22 C27 1.329(4) . ?
N22 C31 1.342(6) . ?
N22A C27 1.322(6) . ?
N22A C31A 1.351(10) . ?
N23 N24 1.353(2) . ?
N23 C26 1.298(3) . ?
N24 C32 1.351(3) . ?
N25 C32 1.354(3) . ?
N25 C34 1.460(3) . ?
N25 C36 1.460(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.383(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.386(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.385(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.391(3) . ?
C5 C6 1.474(3) . ?
C6 C7 1.494(3) . ?
C7 C8 1.386(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.388(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.379(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.383(3) . ?
C11 H11 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.513(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C21 H21 0.9500 . ?
C21 C22 1.388(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.382(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.383(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.398(3) . ?
C25 C26 1.472(3) . ?
C26 C27 1.493(3) . ?
C27 C28 1.367(5) . ?
C27 C28A 1.449(6) . ?
C28 H28 0.9500 . ?
C28 C29 1.383(8) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.384(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.372(17) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.370(15) . ?
C30 H30 0.9500 . ?
C30 C31 1.386(16) . ?
C30A H30A 0.9500 . ?
C30A C31A 1.36(2) . ?
C31 H31 0.9500 . ?
C31A H31A 0.9500 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 H34C 0.9900 . ?
C34 H34D 0.9900 . ?
C34 C35 1.462(8) . ?
C34 C35A 1.531(12) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C35A H35D 0.9800 . ?
C35A H35E 0.9800 . ?
C35A H35F 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 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
S21 Zn1 S1 101.08(2) . . ?
N1 Zn1 S1 153.92(5) . . ?
N1 Zn1 S21 93.14(5) . . ?
N3 Zn1 S1 79.56(5) . . ?
N3 Zn1 S21 112.21(5) . . ?
N3 Zn1 N1 74.83(7) . . ?
N3 Zn1 N21 91.80(6) . . ?
N3 Zn1 N23 160.22(7) . . ?
N21 Zn1 S1 91.78(5) . . ?
N21 Zn1 S21 154.33(5) . . ?
N21 Zn1 N1 84.24(6) . . ?
N23 Zn1 S1 114.63(5) . . ?
N23 Zn1 S21 79.71(5) . . ?
N23 Zn1 N1 89.22(7) . . ?
N23 Zn1 N21 74.73(7) . . ?
C12 S1 Zn1 95.79(7) . . ?
C32 S21 Zn1 96.45(7) . . ?
C1 N1 Zn1 127.56(15) . . ?
C1 N1 C5 118.59(19) . . ?
C5 N1 Zn1 113.82(14) . . ?
C11 N2 C7 116.70(19) . . ?
N4 N3 Zn1 123.55(13) . . ?
C6 N3 Zn1 117.90(14) . . ?
C6 N3 N4 117.82(17) . . ?
C12 N4 N3 113.92(17) . . ?
C12 N5 C14 121.62(18) . . ?
C12 N5 C15 122.79(19) . . ?
C14 N5 C15 115.52(19) . . ?
C21 N21 Zn1 126.81(15) . . ?
C21 N21 C25 118.96(18) . . ?
C25 N21 Zn1 114.21(13) . . ?
C27 N22 C31 114.8(3) . . ?
C27 N22A C31A 121.4(6) . . ?
N24 N23 Zn1 123.41(13) . . ?
C26 N23 Zn1 118.27(14) . . ?
C26 N23 N24 118.06(18) . . ?
C32 N24 N23 113.37(17) . . ?
C32 N25 C34 121.23(19) . . ?
C32 N25 C36 122.7(2) . . ?
C34 N25 C36 116.01(19) . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.2(2) . . ?
C2 C1 H1 118.4 . . ?
C1 C2 H2 120.9 . . ?
C1 C2 C3 118.2(2) . . ?
C3 C2 H2 120.9 . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(2) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.1(2) . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 121.52(19) . . ?
N1 C5 C6 115.56(18) . . ?
C4 C5 C6 122.92(19) . . ?
N3 C6 C5 117.22(18) . . ?
N3 C6 C7 124.01(18) . . ?
C5 C6 C7 118.76(18) . . ?
N2 C7 C6 114.90(18) . . ?
N2 C7 C8 123.56(19) . . ?
C8 C7 C6 121.51(19) . . ?
C7 C8 H8 120.8 . . ?
C7 C8 C9 118.3(2) . . ?
C9 C8 H8 120.8 . . ?
C8 C9 H9 120.5 . . ?
C10 C9 C8 119.0(2) . . ?
C10 C9 H9 120.5 . . ?
C9 C10 H10 120.8 . . ?
C9 C10 C11 118.5(2) . . ?
C11 C10 H10 120.8 . . ?
N2 C11 C10 123.9(2) . . ?
N2 C11 H11 118.1 . . ?
C10 C11 H11 118.1 . . ?
N4 C12 S1 126.76(16) . . ?
N4 C12 N5 114.18(19) . . ?
N5 C12 S1 119.05(16) . . ?
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 . . ?
N5 C15 H15A 108.9 . . ?
N5 C15 H15B 108.9 . . ?
N5 C15 C16 113.3(2) . . ?
H15A C15 H15B 107.7 . . ?
C16 C15 H15A 108.9 . . ?
C16 C15 H15B 108.9 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N21 C21 H21 118.5 . . ?
N21 C21 C22 123.0(2) . . ?
C22 C21 H21 118.5 . . ?
C21 C22 H22 120.9 . . ?
C23 C22 C21 118.2(2) . . ?
C23 C22 H22 120.9 . . ?
C22 C23 H23 120.2 . . ?
C22 C23 C24 119.5(2) . . ?
C24 C23 H23 120.2 . . ?
C23 C24 H24 120.4 . . ?
C23 C24 C25 119.2(2) . . ?
C25 C24 H24 120.4 . . ?
N21 C25 C24 121.1(2) . . ?
N21 C25 C26 116.03(18) . . ?
C24 C25 C26 122.9(2) . . ?
N23 C26 C25 116.55(19) . . ?
N23 C26 C27 124.06(19) . . ?
C25 C26 C27 119.39(18) . . ?
N22 C27 C26 113.1(2) . . ?
N22 C27 C28 126.1(3) . . ?
N22A C27 C26 119.7(3) . . ?
N22A C27 C28A 118.1(4) . . ?
C28 C27 C26 119.4(3) . . ?
C28A C27 C26 121.8(3) . . ?
C27 C28 H28 121.5 . . ?
C27 C28 C29 117.0(5) . . ?
C29 C28 H28 121.5 . . ?
C27 C28A H28A 120.6 . . ?
C29A C28A C27 118.9(5) . . ?
C29A C28A H28A 120.6 . . ?
C28 C29 H29 120.3 . . ?
C30 C29 C28 119.3(8) . . ?
C30 C29 H29 120.3 . . ?
C28A C29A H29A 120.0 . . ?
C30A C29A C28A 119.9(9) . . ?
C30A C29A H29A 120.0 . . ?
C29 C30 H30 120.9 . . ?
C29 C30 C31 118.2(9) . . ?
C31 C30 H30 120.9 . . ?
C29A C30A H30A 120.6 . . ?
C31A C30A C29A 118.8(12) . . ?
C31A C30A H30A 120.6 . . ?
N22 C31 C30 124.0(6) . . ?
N22 C31 H31 118.0 . . ?
C30 C31 H31 118.0 . . ?
N22A C31A C30A 122.3(10) . . ?
N22A C31A H31A 118.8 . . ?
C30A C31A H31A 118.8 . . ?
N24 C32 S21 126.65(16) . . ?
N24 C32 N25 114.74(19) . . ?
N25 C32 S21 118.60(17) . . ?
N25 C34 H34A 109.2 . . ?
N25 C34 H34B 109.2 . . ?
N25 C34 H34C 109.8 . . ?
N25 C34 H34D 109.8 . . ?
N25 C34 C35 112.2(5) . . ?
N25 C34 C35A 109.5(6) . . ?
H34A C34 H34B 107.9 . . ?
H34C C34 H34D 108.2 . . ?
C35 C34 H34A 109.2 . . ?
C35 C34 H34B 109.2 . . ?
C35A C34 H34C 109.8 . . ?
C35A C34 H34D 109.8 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C35A H35D 109.5 . . ?
C34 C35A H35E 109.5 . . ?
C34 C35A H35F 109.5 . . ?
H35D C35A H35E 109.5 . . ?
H35D C35A H35F 109.5 . . ?
H35E C35A H35F 109.5 . . ?
N25 C36 H36A 109.5 . . ?
N25 C36 H36B 109.5 . . ?
N25 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 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
Zn1 S1 C12 N4 7.23(18) . . . . ?
Zn1 S1 C12 N5 -173.41(15) . . . . ?
Zn1 S21 C32 N24 7.1(2) . . . . ?
Zn1 S21 C32 N25 -174.08(18) . . . . ?
Zn1 N1 C1 C2 -178.41(16) . . . . ?
Zn1 N1 C5 C4 178.16(15) . . . . ?
Zn1 N1 C5 C6 -1.3(2) . . . . ?
Zn1 N3 N4 C12 2.1(2) . . . . ?
Zn1 N3 C6 C5 -9.7(2) . . . . ?
Zn1 N3 C6 C7 169.72(15) . . . . ?
Zn1 N21 C21 C22 177.33(16) . . . . ?
Zn1 N21 C25 C24 -178.23(16) . . . . ?
Zn1 N21 C25 C26 1.8(2) . . . . ?
Zn1 N23 N24 C32 3.1(3) . . . . ?
Zn1 N23 C26 C25 -4.7(3) . . . . ?
Zn1 N23 C26 C27 174.42(16) . . . . ?
N1 C1 C2 C3 0.6(3) . . . . ?
N1 C5 C6 N3 7.2(3) . . . . ?
N1 C5 C6 C7 -172.29(17) . . . . ?
N2 C7 C8 C9 -1.3(3) . . . . ?
N3 N4 C12 S1 -7.0(3) . . . . ?
N3 N4 C12 N5 173.64(16) . . . . ?
N3 C6 C7 N2 -121.2(2) . . . . ?
N3 C6 C7 C8 60.6(3) . . . . ?
N4 N3 C6 C5 179.74(16) . . . . ?
N4 N3 C6 C7 -0.8(3) . . . . ?
N21 C21 C22 C23 0.9(3) . . . . ?
N21 C25 C26 N23 1.8(3) . . . . ?
N21 C25 C26 C27 -177.41(18) . . . . ?
N22 C27 C28 C29 6.4(7) . . . . ?
N22A C27 C28A C29A 7.7(8) . . . . ?
N23 N24 C32 S21 -7.4(3) . . . . ?
N23 N24 C32 N25 173.71(19) . . . . ?
N23 C26 C27 N22 -114.7(3) . . . . ?
N23 C26 C27 N22A 110.5(4) . . . . ?
N23 C26 C27 C28 77.6(4) . . . . ?
N23 C26 C27 C28A -62.8(4) . . . . ?
N24 N23 C26 C25 -179.10(18) . . . . ?
N24 N23 C26 C27 0.1(3) . . . . ?
C1 N1 C5 C4 -0.1(3) . . . . ?
C1 N1 C5 C6 -179.50(18) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
C2 C3 C4 C5 -0.2(3) . . . . ?
C3 C4 C5 N1 0.4(3) . . . . ?
C3 C4 C5 C6 179.78(19) . . . . ?
C4 C5 C6 N3 -172.26(19) . . . . ?
C4 C5 C6 C7 8.3(3) . . . . ?
C5 N1 C1 C2 -0.5(3) . . . . ?
C5 C6 C7 N2 58.2(3) . . . . ?
C5 C6 C7 C8 -120.0(2) . . . . ?
C6 N3 N4 C12 172.05(17) . . . . ?
C6 C7 C8 C9 176.73(19) . . . . ?
C7 N2 C11 C10 1.5(4) . . . . ?
C7 C8 C9 C10 1.2(3) . . . . ?
C8 C9 C10 C11 0.1(3) . . . . ?
C9 C10 C11 N2 -1.5(4) . . . . ?
C11 N2 C7 C6 -178.2(2) . . . . ?
C11 N2 C7 C8 0.0(3) . . . . ?
C12 N5 C15 C16 94.4(3) . . . . ?
C14 N5 C12 S1 171.14(16) . . . . ?
C14 N5 C12 N4 -9.4(3) . . . . ?
C14 N5 C15 C16 -82.6(3) . . . . ?
C15 N5 C12 S1 -5.7(3) . . . . ?
C15 N5 C12 N4 173.77(18) . . . . ?
C21 N21 C25 C24 0.2(3) . . . . ?
C21 N21 C25 C26 -179.74(19) . . . . ?
C21 C22 C23 C24 -0.2(3) . . . . ?
C22 C23 C24 C25 -0.4(3) . . . . ?
C23 C24 C25 N21 0.4(3) . . . . ?
C23 C24 C25 C26 -179.6(2) . . . . ?
C24 C25 C26 N23 -178.1(2) . . . . ?
C24 C25 C26 C27 2.7(3) . . . . ?
C25 N21 C21 C22 -0.9(3) . . . . ?
C25 C26 C27 N22 64.5(3) . . . . ?
C25 C26 C27 N22A -70.3(4) . . . . ?
C25 C26 C27 C28 -103.2(4) . . . . ?
C25 C26 C27 C28A 116.3(4) . . . . ?
C26 N23 N24 C32 177.2(2) . . . . ?
C26 C27 C28 C29 172.3(4) . . . . ?
C26 C27 C28A C29A -178.9(5) . . . . ?
C27 N22 C31 C30 5.7(13) . . . . ?
C27 N22A C31A C30A 2.3(16) . . . . ?
C27 C28 C29 C30 -3.5(13) . . . . ?
C27 C28A C29A C30A -3.6(16) . . . . ?
C28 C29 C30 C31 2(2) . . . . ?
C28A C29A C30A C31A -1(3) . . . . ?
C29 C30 C31 N22 -4(2) . . . . ?
C29A C30A C31A N22A 2(3) . . . . ?
C31 N22 C27 C26 -174.0(4) . . . . ?
C31 N22 C27 C28 -7.3(6) . . . . ?
C31A N22A C27 C26 179.4(5) . . . . ?
C31A N22A C27 C28A -7.0(8) . . . . ?
C32 N25 C34 C35 82.1(7) . . . . ?
C32 N25 C34 C35A 104.7(10) . . . . ?
C34 N25 C32 S21 -175.23(19) . . . . ?
C34 N25 C32 N24 3.7(3) . . . . ?
C36 N25 C32 S21 1.4(3) . . . . ?
C36 N25 C32 N24 -179.6(2) . . . . ?
C36 N25 C34 C35 -94.8(7) . . . . ?
C36 N25 C34 C35A -72.2(10) . . . . ?

loop_
_audit_author_email
mahendiran.dharmasivam@sydney.edu.au
?
d.richardson@sydney.edu.au
_olex2_date_sample_data_collection 2018-09-10
_olex2_date_sample_submission    2018-09-03
_olex2_exptl_crystal_mounting_method 'in paratone on a loop'
_olex2_submission_original_sample_id drr180903a
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.277
_oxdiff_exptl_absorpt_empirical_full_min 0.786
####################################################################### 
# 
# 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_drr18_s1692
_database_code_depnum_ccdc_archive 'CCDC 1959775'
loop_
_audit_author_name
_audit_author_address
'William Lewis'
;University of Sydney
Australia
;
_audit_update_record             
;
2019-10-17 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
_refine_special_details          
;
Atoms N9, C27, N10, C28, C29 and C30 are disordered over two positions. Additionally 
the ethyl and methyl groups have swapped positions between the two components. The 
occupancies of the two components were refined competitively, converging to a ratio 
of 0.83:0.17. Bond distacnes of the two components were restrained to be approximately 
equal, as well as a small number of 1,3-distances. The minor component atoms were 
refined isotropically, and similarity restraints were applied to their isotropic 
thermal parameters.

The nitrate anion is disordered along a pocket, which is across a centre of symmetry. 
It was possible to model the nitrate over four discrete positions The occupancies of 
the four components were refined competitively, converging to a ratio of 
0.46:0.36:0.09:0.09. N-O and O--O distances were restrained to the mean values 
derived from a search of Conquest. Each nitrate was also restrained to approxiamtely 
flat geometry. The thermal parameters for each of the two smallest components 
were set to common refining values for all four atoms. Enhanced rigid bond and 
similarity restraints were applied to the thermal parameters of all nitrate atoms. 

The solvent water molecuel is disordered over three positions, likely due to 
hydrogen bonding to the nitrate anion. The hydrogen atoms could not be located 
for any of these components, and sensible positions could not be determined, so 
these hydrogen atoms were excluded from the model, although they were included 
in the formula and calculation of derived parameters. The occupancies of the 
three components were refined competitively, converging to a ratio of 
0.82:0.13:0.05. Enhanced rigid bond and similarity restraints were applied to 
the thermal parameters of these atoms.
;
_audit_creation_date             2018-11-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Ga(Dp4e4mT)2
_chemical_formula_moiety         'C30 H32 Ga N10 S2, 1(N O3), 1(O)'
_chemical_formula_sum            'C30 H34 Ga N11 O4 S2'
_chemical_formula_weight         746.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H34GaN11O4S2
_chemical_oxdiff_usercomment     ' '
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'
Ga Ga -1.2846 0.7763 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7832(3)
_cell_length_b                   11.7181(3)
_cell_length_c                   17.1171(4)
_cell_angle_alpha                92.486(2)
_cell_angle_beta                 102.138(2)
_cell_angle_gamma                94.766(2)
_cell_volume                     1713.04(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13149
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.7190
_cell_measurement_theta_min      4.4400
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.682
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             772
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0527
1 0 0 0.0527
1 5 -3 0.0427
0 -5 3 0.0453
-1 1 5 0.0232
1 -1 -5 0.0232
0 5 4 0.0338
-5 2 -1 0.0476
0 5 -3 0.0469
0 0 1 0.0251

_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.046
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
-0.9996 -0.0005 0.0042 0.1665 -0.0384 -0.0568
0.9996 0.0005 -0.0042 -0.1665 0.0384 0.0568
1.0066 4.9957 -3.0531 0.0500 0.0087 0.7233
-0.0069 -4.9952 3.0489 -0.2165 0.0297 -0.6664
-0.9894 1.0211 4.9807 0.1541 0.4483 -0.0660
0.9894 -1.0211 -4.9807 -0.1541 -0.4483 0.0660
0.0180 5.0234 3.9339 0.1469 0.5861 0.4883
-4.9951 1.9965 -0.9990 0.9171 -0.1862 -0.0227
0.0069 4.9952 -3.0489 0.2165 -0.0297 0.6664
0.0016 0.0040 0.9975 -0.0099 0.0880 -0.0254

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29333
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.209
_diffrn_reflns_theta_min         3.793
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.5861
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      1.00  26.00   1.00    5.00    --   40.00  92.00-133.89   25
  2  ω   -130.00 -92.00   1.00    5.00    --  -40.45   0.00-120.00   38
  3  ω    -86.00  42.00   1.00    5.00    --  -40.45   0.00-120.00  128
  4  ω    -50.00  35.00   1.00    5.00    --  -40.45  38.00 -60.00   85
  5  ω   -112.00 -15.00   1.00    5.00    --  -40.45 -38.00 150.00   97
  6  ω      2.00  27.00   1.00    5.00    --   40.45  91.00 -21.88   25
  7  ω     69.00 127.00   1.00    5.00    --   40.45-178.00-120.00   58
  8  ω     12.00  39.00   1.00    5.00    --   40.45  57.00  60.00   27
  9  ω     11.00  40.00   1.00    5.00    --   40.45  57.00-150.00   29
 10  ω     56.00 123.00   1.00    5.00    --   40.45-178.00  90.00   67
 11  ω     73.00 124.00   1.00    5.00    --   40.45 178.00 -30.00   51
 12  ω      7.00  32.00   1.00    5.00    --   44.00  89.00  86.94   25
 13  ω     13.00  38.00   1.00    5.00    --   48.00  83.00 168.17   25
 14  ω     12.00  38.00   1.00    5.00    --   48.00  84.00-127.99   26
 15  ω     18.00  43.00   1.00    5.00    --   52.00  79.00 124.66   25
 16  ω     17.00  42.00   1.00    5.00    --   52.00  81.00 -31.39   25
 17  ω     18.00  43.00   1.00    5.00    --   52.00  79.00  37.94   25
 18  ω     33.00  60.00   1.00    5.00    --   64.00  76.00 -48.79   27
 19  ω     30.00  57.00   1.00    5.00    --   64.00  77.00 115.69   27
 20  ω     33.00  60.00   1.00    5.00    --   64.00  77.00 150.42   27
 21  ω     34.00  61.00   1.00    5.00    --   64.00  76.00  29.10   27
 22  ω     31.00  57.00   1.00    5.00    --   64.00  75.00  68.42   26
 23  ω     31.00  57.00   1.00    5.00    --   64.00  76.00 -95.23   26
 24  ω     35.00  77.00   1.00    5.00    --   68.00  77.00-150.39   42
 25  ω     92.00 146.00   1.00    5.00    --   68.00  77.00-150.39   54
 26  ω     35.00  62.00   1.00    5.00    --   68.00  76.00 -25.45   27
 27  ω     41.00  71.00   1.00    5.00    --   72.00  75.00 119.14   30
 28  ω     38.00  65.00   1.00    5.00    --   72.00  77.00  69.82   27
 29  ω     44.00  71.00   1.00   20.00    --   76.00  70.00 -77.75   27
 30  ω     44.00  71.00   1.00   20.00    --   76.00  76.00  -5.27   27
 31  ω     50.00 125.00   1.00   20.00    --   80.00  75.00 159.56   75
 32  ω     49.00 101.00   1.00   20.00    --   80.00  70.00 136.15   52
 33  ω     51.00  76.00   1.00   20.00    --   80.00  59.00  44.28   25
 34  ω     48.00  73.00   1.00   20.00    --   80.00  75.00 -37.75   25
 35  ω     50.00  78.00   1.00   20.00    --   84.00  77.00 -88.53   28
 36  ω     53.00  80.00   1.00   20.00    --   84.00  66.00  75.85   27
 37  ω     62.00  87.00   1.00   20.00    --   92.00  66.00  38.24   25
 38  ω     77.00 175.00   1.00   20.00    --  108.56  77.00  60.00   98
 39  ω     27.00 107.00   1.00   20.00    --  108.56 -95.00  60.00   80
 40  ω     75.00 176.00   1.00   20.00    --  108.56  77.00   0.00  101
 41  ω     75.00 154.00   1.00   20.00    --  108.56  77.00-120.00   79
 42  ω     56.00 115.00   1.00   20.00    --  108.56-125.00  30.00   59
 43  ω    121.00 151.00   1.00   20.00    --  108.56  61.00-180.00   30
 44  ω     91.00 118.00   1.00   20.00    --  108.56-125.00 -90.00   27
 45  ω     78.00 107.00   1.00   20.00    --  108.56  61.00-180.00   29
 46  ω     76.00 164.00   1.00   20.00    --  108.56  77.00-150.00   88
 47  ω     75.00 102.00   1.00   20.00    --  108.56  77.00-180.00   27
 48  ω     52.00  93.00   1.00   20.00    --  108.56 -45.00  30.00   41
 49  ω     76.00 148.00   1.00   20.00    --  108.56  77.00 -90.00   72
 50  ω    113.00 172.00   1.00   20.00    --  108.56  77.00 150.00   59
 51  ω     75.00 101.00   1.00   20.00    --  108.56  77.00 150.00   26
 52  ω     28.00 109.00   1.00   20.00    --  108.56 -95.00 150.00   81
 53  ω     75.00 168.00   1.00   20.00    --  108.56  77.00  90.00   93
 54  ω    114.00 163.00   1.00   20.00    --  108.56  77.00 -30.00   49
 55  ω     53.00 141.00   1.00   20.00    --  108.56 -77.00-150.00   88
 56  ω     75.00 111.00   1.00   20.00    --  108.56  77.00 -30.00   36
 57  ω     78.00 137.00   1.00   20.00    --  108.56  61.00-150.00   59
 58  ω     75.00 175.00   1.00   20.00    --  108.56  77.00 -60.00  100
 59  ω     77.00 174.00   1.00   20.00    --  108.56  77.00  30.00   97
 60  ω     64.00  94.00   1.00   20.00    --  108.56 -45.00 120.00   30
 61  ω     75.00 164.00   1.00   20.00    --  108.56  77.00 120.00   89
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1666141000
_diffrn_orient_matrix_UB_12      0.0375555000
_diffrn_orient_matrix_UB_13      -0.0098501000
_diffrn_orient_matrix_UB_21      0.0387569000
_diffrn_orient_matrix_UB_22      0.0476789000
_diffrn_orient_matrix_UB_23      0.0879292000
_diffrn_orient_matrix_UB_31      0.0567005000
_diffrn_orient_matrix_UB_32      0.1174249000
_diffrn_orient_matrix_UB_33      -0.0260682000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6008
_reflns_number_total             6839
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.288
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         6839
_refine_ls_number_restraints     358
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0432
_refine_ls_restrained_S_all      1.040
_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)+(0.0749P)²+1.9419P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1265
_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. Restrained distances
 O3-O1 = O1-O2 = O2-O3 = O3A-O1A = O1A-O2A = O2A-O3A = O1C-O2C = O2C-O3C = O3C-
 O1C = O3B-O2B = O2B-O1B = O1B-O3B
 2.148 with sigma of 0.001
 O3A-N11A = O2-N11 = O3-N11 = O1A-N11A = O1-N11 = O2A-N11A = N11C-O1C = N11C-
 O2C = N11C-O3C = N11B-O3B = N11B-O2B = N11B-O1B
 1.245 with sigma of 0.001
 S2-C27A \\sim S2-C27
 with sigma of 0.02
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 C28A-C27A \\sim C27-C28
 with sigma of 0.02
 C28-C29 \\sim C28A-C29A
 with sigma of 0.02
 C29-C27 \\sim C27A-C29A
 with sigma of 0.02
 N9-N8 \\sim N9A-N8
 with sigma of 0.02
 N9A-C27A \\sim N9-C27
 with sigma of 0.02
 N10-C27 \\sim N10A-C27A
 with sigma of 0.02
 N10A-C28A \\sim N10-C28
 with sigma of 0.02
 N10A-C29A \\sim N10-C29
 with sigma of 0.02
 C30A-N10A \\sim C30-N10
 with sigma of 0.02
3. Restrained planarity
 O1, O2, O3, N11
 with sigma of 0.1
 O1B, O2B, O3B, N11B
 with sigma of 0.01
 O1C, O2C, O3C, N11C
 with sigma of 0.01
 O1A, O2A, O3A, N11A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O4 \\sim O4A \\sim O4B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N9A \\sim N10A \\sim C27A \\sim C28A \\sim C29A \\sim C30A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
O1 \\sim O2 \\sim O3 \\sim N11 \\sim O1A \\sim O2A \\sim O3A \\sim N11A \\sim
O1B \\sim O2B \\sim O3B \\sim N11B \\sim O1C \\sim O2C \\sim O3C \\sim N11C:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O1, O2, O3, N11, O1A, O2A, O3A, N11A, O1B, O2B, O3B, N11B, O1C, O2C, O3C,
 N11C, O4, O4A, O4B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(O1)+Sof(O2)+Sof(O3)+Sof(N11)]+1*[Sof(O1A)+Sof(O2A)+Sof(O3A)+Sof(N11A)]+
 1*[Sof(O1C)+Sof(O2C)+Sof(O3C)+Sof(N11C)]+1*[Sof(O1B)+Sof(O2B)+Sof(O3B)+
 Sof(N11B)]=1 with esd of 0.001
 1*[Sof(O4)]+1*[Sof(O4A)]+1*[Sof(O4B)]=1 with esd of 0.001
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(N11)=FVAR(1)
 Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(N11A)=FVAR(2)
 Sof(O1C)=Sof(O2C)=Sof(O3C)=Sof(N11C)=FVAR(3)
 Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(N11B)=FVAR(4)
 U11(O1B)=U11(O2B)=U11(O3B)=U11(N11B)=FVAR(5)
 U22(O1B)=U22(O2B)=U22(O3B)=U22(N11B)=FVAR(6)
 U33(O1B)=U33(O2B)=U33(O3B)=U33(N11B)=FVAR(7)
 U23(O1B)=U23(O2B)=U23(O3B)=U23(N11B)=FVAR(8)
 U13(O1B)=U13(O2B)=U13(O3B)=U13(N11B)=FVAR(9)
 U12(O1B)=U12(O2B)=U12(O3B)=U12(N11B)=FVAR(10)
 U11(O1C)=U11(O2C)=U11(O3C)=U11(N11C)=FVAR(11)
 U22(O1C)=U22(O2C)=U22(O3C)=U22(N11C)=FVAR(12)
 U33(O1C)=U33(O2C)=U33(O3C)=U33(N11C)=FVAR(13)
 U23(O1C)=U23(O2C)=U23(O3C)=U23(N11C)=FVAR(14)
 U13(O1C)=U13(O2C)=U13(O3C)=U13(N11C)=FVAR(15)
 U12(O1C)=U12(O2C)=U12(O3C)=U12(N11C)=FVAR(16)
 Sof(N9A)=Sof(N10A)=Sof(C27A)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-
 FVAR(17)
 Sof(N9)=Sof(N10)=Sof(C27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=
 Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(17)
7.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C29(H29A,H29B), C29A(H29C,H29D)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26)
7.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C28(H28A,H28B,H28C), C28A(H28D,H28E,
 H28F), C30(H30A,H30B,H30C), C30A(H30D,H30E,H30F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.21134(3) 0.33735(3) 0.20877(2) 0.01954(11) Uani 1 1 d . . . . .
S1 S -0.06083(7) 0.28278(5) 0.17039(4) 0.02449(15) Uani 1 1 d . . . . .
S2 S 0.28966(7) 0.26105(5) 0.09495(4) 0.02460(15) Uani 1 1 d D . . . .
N1 N 0.4436(2) 0.34523(19) 0.27395(12) 0.0230(4) Uani 1 1 d . . . . .
N2 N 0.4777(3) 0.0065(2) 0.35399(13) 0.0266(5) Uani 1 1 d . . . . .
N3 N 0.2083(2) 0.19568(18) 0.27395(12) 0.0212(4) Uani 1 1 d . . . . .
N4 N 0.0769(2) 0.12501(19) 0.26995(13) 0.0242(4) Uani 1 1 d . . . . .
N5 N -0.1849(3) 0.0943(2) 0.22433(15) 0.0318(5) Uani 1 1 d . . . . .
N6 N 0.1797(2) 0.45988(19) 0.29328(12) 0.0221(4) Uani 1 1 d . . . . .
N7 N 0.2745(3) 0.7822(2) 0.19880(14) 0.0294(5) Uani 1 1 d . . . . .
N8 N 0.2149(2) 0.48579(18) 0.14827(12) 0.0207(4) Uani 1 1 d D . . . .
N9 N 0.2294(9) 0.4871(4) 0.0713(3) 0.0215(11) Uani 0.833(9) 1 d D . P A 1
N9A N 0.257(5) 0.483(3) 0.0751(15) 0.028(8) Uiso 0.167(9) 1 d D U P A 2
N10 N 0.2712(5) 0.3814(3) -0.03483(16) 0.0250(7) Uani 0.833(9) 1 d D . P A 1
N10A N 0.336(3) 0.3778(14) -0.0259(10) 0.036(5) Uiso 0.167(9) 1 d D U P A 2
C1 C 0.5566(3) 0.4286(3) 0.27239(17) 0.0299(6) Uani 1 1 d . . . . .
H1 H 0.532101 0.490937 0.241894 0.036 Uiso 1 1 calc R . . . .
C2 C 0.7088(3) 0.4249(3) 0.31478(19) 0.0360(7) Uani 1 1 d . . . . .
H2 H 0.785514 0.483865 0.313131 0.043 Uiso 1 1 calc R . . . .
C3 C 0.7440(3) 0.3313(3) 0.35964(17) 0.0322(6) Uani 1 1 d . . . . .
H3 H 0.845520 0.326147 0.388086 0.039 Uiso 1 1 calc R . . . .
C4 C 0.6270(3) 0.2454(2) 0.36188(15) 0.0262(5) Uani 1 1 d . . . . .
H4 H 0.649085 0.182653 0.392335 0.031 Uiso 1 1 calc R . . . .
C5 C 0.4760(3) 0.2538(2) 0.31817(14) 0.0223(5) Uani 1 1 d . . . . .
C6 C 0.3410(3) 0.1701(2) 0.31717(14) 0.0217(5) Uani 1 1 d . . . . .
C7 C 0.3559(3) 0.0647(2) 0.36244(14) 0.0235(5) Uani 1 1 d . . . . .
C8 C 0.2505(3) 0.0298(2) 0.40871(15) 0.0274(5) Uani 1 1 d . . . . .
H8 H 0.167884 0.072669 0.413127 0.033 Uiso 1 1 calc R . . . .
C9 C 0.2709(3) -0.0708(3) 0.44832(16) 0.0320(6) Uani 1 1 d . . . . .
H9 H 0.201562 -0.096970 0.479290 0.038 Uiso 1 1 calc R . . . .
C10 C 0.3966(4) -0.1311(2) 0.44076(16) 0.0321(6) Uani 1 1 d . . . . .
H10 H 0.413720 -0.198375 0.466853 0.038 Uiso 1 1 calc R . . . .
C11 C 0.4962(3) -0.0894(2) 0.39356(16) 0.0305(6) Uani 1 1 d . . . . .
H11 H 0.580707 -0.130172 0.389051 0.037 Uiso 1 1 calc R . . . .
C12 C -0.0527(3) 0.1607(2) 0.22524(15) 0.0242(5) Uani 1 1 d . . . . .
C13 C -0.1794(4) -0.0098(3) 0.2689(2) 0.0479(9) Uani 1 1 d . . . . .
H13A H -0.122670 -0.063850 0.245659 0.072 Uiso 1 1 calc GR . . . .
H13B H -0.283958 -0.043179 0.266627 0.072 Uiso 1 1 calc GR . . . .
H13C H -0.127905 0.009330 0.323759 0.072 Uiso 1 1 calc GR . . . .
C14 C -0.3376(3) 0.1170(3) 0.17722(17) 0.0301(6) Uani 1 1 d . . . . .
H14A H -0.338736 0.198969 0.171467 0.036 Uiso 1 1 calc R . . . .
H14B H -0.417684 0.093430 0.206086 0.036 Uiso 1 1 calc R . . . .
C15 C -0.3768(4) 0.0564(3) 0.0959(2) 0.0476(8) Uani 1 1 d . . . . .
H15A H -0.302619 0.083703 0.065428 0.071 Uiso 1 1 calc GR . . . .
H15B H -0.480059 0.071102 0.069040 0.071 Uiso 1 1 calc GR . . . .
H15C H -0.372807 -0.024643 0.101001 0.071 Uiso 1 1 calc GR . . . .
C16 C 0.1600(3) 0.4367(3) 0.36620(16) 0.0289(6) Uani 1 1 d . . . . .
H16 H 0.166173 0.362065 0.382081 0.035 Uiso 1 1 calc R . . . .
C17 C 0.1308(4) 0.5208(3) 0.41897(17) 0.0347(6) Uani 1 1 d . . . . .
H17 H 0.120074 0.503670 0.470204 0.042 Uiso 1 1 calc R . . . .
C18 C 0.1179(4) 0.6296(3) 0.39399(18) 0.0350(6) Uani 1 1 d . . . . .
H18 H 0.096226 0.687211 0.428033 0.042 Uiso 1 1 calc R . . . .
C19 C 0.1373(3) 0.6541(3) 0.31773(17) 0.0318(6) Uani 1 1 d . . . . .
H19 H 0.128093 0.727793 0.300228 0.038 Uiso 1 1 calc R . . . .
C20 C 0.1706(3) 0.5673(2) 0.26823(15) 0.0230(5) Uani 1 1 d . . . . .
C21 C 0.1944(3) 0.5808(2) 0.18581(15) 0.0221(5) Uani 1 1 d . . . . .
C22 C 0.1907(3) 0.6947(2) 0.15082(15) 0.0238(5) Uani 1 1 d . . . . .
C23 C 0.1050(3) 0.7097(2) 0.07444(16) 0.0260(5) Uani 1 1 d . . . . .
H23 H 0.051332 0.647268 0.041915 0.031 Uiso 1 1 calc R . . . .
C24 C 0.1010(3) 0.8197(2) 0.04773(17) 0.0302(6) Uani 1 1 d . . . . .
H24 H 0.043195 0.832417 -0.002715 0.036 Uiso 1 1 calc R . . . .
C25 C 0.1843(4) 0.9101(2) 0.09732(18) 0.0331(6) Uani 1 1 d . . . . .
H25 H 0.182867 0.984811 0.081059 0.040 Uiso 1 1 calc R . . . .
C26 C 0.2698(4) 0.8874(2) 0.17154(17) 0.0343(6) Uani 1 1 d . . . . .
H26 H 0.327171 0.948402 0.204222 0.041 Uiso 1 1 calc R . . . .
C27 C 0.2606(6) 0.3852(3) 0.0420(2) 0.0216(10) Uani 0.833(9) 1 d D . P A 1
C27A C 0.299(3) 0.3848(16) 0.0456(11) 0.028(7) Uiso 0.167(9) 1 d D U P A 2
C28 C 0.2562(7) 0.4856(4) -0.0809(3) 0.0414(13) Uani 0.833(9) 1 d D . P A 1
H28A H 0.205956 0.540453 -0.054333 0.062 Uiso 0.833(9) 1 calc GR . P A 1
H28B H 0.194768 0.465419 -0.133775 0.062 Uiso 0.833(9) 1 calc GR . P A 1
H28C H 0.358292 0.518276 -0.084369 0.062 Uiso 0.833(9) 1 calc GR . P A 1
C28A C 0.374(3) 0.2717(17) -0.0618(13) 0.040(6) Uiso 0.167(9) 1 d D U P A 2
H28D H 0.432359 0.229498 -0.020926 0.060 Uiso 0.167(9) 1 calc GR . P A 2
H28E H 0.434744 0.289508 -0.100808 0.060 Uiso 0.167(9) 1 calc GR . P A 2
H28F H 0.278760 0.226272 -0.087372 0.060 Uiso 0.167(9) 1 calc GR . P A 2
C29 C 0.3098(6) 0.2782(3) -0.0759(2) 0.0302(9) Uani 0.833(9) 1 d D . P A 1
H29A H 0.266461 0.278623 -0.132919 0.036 Uiso 0.833(9) 1 calc R . P A 1
H29B H 0.263155 0.210367 -0.056283 0.036 Uiso 0.833(9) 1 calc R . P A 1
C29A C 0.249(4) 0.458(2) -0.0867(17) 0.068(9) Uiso 0.167(9) 1 d D U P A 2
H29C H 0.218555 0.419682 -0.139919 0.082 Uiso 0.167(9) 1 calc R . P A 2
H29D H 0.155897 0.481113 -0.070622 0.082 Uiso 0.167(9) 1 calc R . P A 2
C30 C 0.4875(5) 0.2737(4) -0.0618(3) 0.0493(13) Uani 0.833(9) 1 d D . P A 1
H30A H 0.510103 0.209459 -0.092824 0.074 Uiso 0.833(9) 1 calc GR . P A 1
H30B H 0.529081 0.265453 -0.006051 0.074 Uiso 0.833(9) 1 calc GR . P A 1
H30C H 0.534552 0.343294 -0.077806 0.074 Uiso 0.833(9) 1 calc GR . P A 1
C30A C 0.368(4) 0.560(2) -0.085(2) 0.089(10) Uiso 0.167(9) 1 d D U P A 2
H30D H 0.316239 0.623836 -0.106487 0.134 Uiso 0.167(9) 1 calc GR . P A 2
H30E H 0.442803 0.540312 -0.115526 0.134 Uiso 0.167(9) 1 calc GR . P A 2
H30F H 0.421810 0.580157 -0.030121 0.134 Uiso 0.167(9) 1 calc GR . P A 2
O1 O 0.1688(5) 0.2221(5) 0.5985(2) 0.0418(14) Uani 0.464(5) 1 d D U P B 1
O2 O 0.0454(6) 0.2257(9) 0.4762(3) 0.0366(19) Uani 0.464(5) 1 d D U P B 1
O3 O 0.2921(5) 0.2773(5) 0.5087(3) 0.0568(16) Uani 0.464(5) 1 d D U P B 1
N11 N 0.1669(4) 0.2483(6) 0.5287(2) 0.0413(15) Uani 0.464(5) 1 d D U P B 1
O1A O 0.2444(6) 0.3148(4) 0.5814(3) 0.0351(15) Uani 0.355(5) 1 d D U P C 2
O2A O 0.1118(7) 0.1526(5) 0.5826(4) 0.050(2) Uani 0.355(5) 1 d D U P C 2
O3A O 0.0599(10) 0.2549(8) 0.4808(4) 0.022(2) Uani 0.355(5) 1 d D U P C 2
N11A N 0.1457(7) 0.2372(5) 0.5460(3) 0.0314(17) Uani 0.355(5) 1 d D U P C 2
O1B O 0.2853(16) 0.3100(17) 0.5497(12) 0.037(2) Uani 0.091(3) 1 d D U P D 4
O2B O 0.442(2) 0.3589(19) 0.4735(7) 0.037(2) Uani 0.091(3) 1 d D U P D 4
O3B O 0.4942(19) 0.4219(15) 0.5969(8) 0.037(2) Uani 0.091(3) 1 d D U P D 4
N11B N 0.4073(13) 0.3636(10) 0.5400(7) 0.037(2) Uani 0.091(3) 1 d D U P D 4
O1C O 0.463(3) 0.3870(9) 0.4807(10) 0.034(2) Uani 0.094(3) 1 d D U P E -3
O2C O 0.483(2) 0.5425(13) 0.5552(6) 0.034(2) Uani 0.094(3) 1 d D U P E -3
O3C O 0.520(2) 0.5495(13) 0.4351(7) 0.034(2) Uani 0.094(3) 1 d D U P E -3
N11C N 0.4889(13) 0.4930(9) 0.4904(6) 0.034(2) Uani 0.094(3) 1 d D U P E -3
O4 O 0.5943(3) 0.7003(2) 0.25633(18) 0.0384(9) Uani 0.815(8) 1 d . U P F 1
O4A O 0.529(3) 0.6727(15) 0.2919(13) 0.050(5) Uani 0.133(8) 1 d . U P G 2
O4B O 0.797(4) 0.687(3) 0.2704(19) 0.024(5) Uani 0.053(5) 1 d . U P H 3


_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
Ga1 S1 2.3673(6) . ?
Ga1 S2 2.3628(7) . ?
Ga1 N1 2.102(2) . ?
Ga1 N3 2.041(2) . ?
Ga1 N6 2.071(2) . ?
Ga1 N8 2.064(2) . ?
S1 C12 1.743(3) . ?
S2 C27 1.756(3) . ?
S2 C27A 1.714(16) . ?
N1 C1 1.338(4) . ?
N1 C5 1.353(3) . ?
N2 C7 1.344(3) . ?
N2 C11 1.341(4) . ?
N3 N4 1.351(3) . ?
N3 C6 1.307(3) . ?
N4 C12 1.341(3) . ?
N5 C12 1.340(4) . ?
N5 C13 1.466(4) . ?
N5 C14 1.464(3) . ?
N6 C16 1.332(3) . ?
N6 C20 1.351(3) . ?
N7 C22 1.348(3) . ?
N7 C26 1.337(4) . ?
N8 N9 1.351(4) . ?
N8 N9A 1.379(17) . ?
N8 C21 1.306(3) . ?
N9 C27 1.346(5) . ?
N9A C27A 1.347(18) . ?
N10 C27 1.337(4) . ?
N10 C28 1.481(5) . ?
N10 C29 1.472(4) . ?
N10A C27A 1.329(15) . ?
N10A C28A 1.458(16) . ?
N10A C29A 1.552(17) . ?
C1 H1 0.9300 . ?
C1 C2 1.386(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.385(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.393(3) . ?
C5 C6 1.472(4) . ?
C6 C7 1.487(4) . ?
C7 C8 1.388(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.390(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.384(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.385(4) . ?
C11 H11 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.494(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16 0.9300 . ?
C16 C17 1.383(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.369(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.390(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.385(4) . ?
C20 C21 1.482(3) . ?
C21 C22 1.486(4) . ?
C22 C23 1.391(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.386(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.382(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.382(4) . ?
C26 H26 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C28A H28D 0.9600 . ?
C28A H28E 0.9600 . ?
C28A H28F 0.9600 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.534(6) . ?
C29A H29C 0.9700 . ?
C29A H29D 0.9700 . ?
C29A C30A 1.52(2) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C30A H30D 0.9600 . ?
C30A H30E 0.9600 . ?
C30A H30F 0.9600 . ?
O1 N11 1.2437(10) . ?
O2 N11 1.2433(10) . ?
O3 N11 1.2435(10) . ?
O1A N11A 1.2441(10) . ?
O2A N11A 1.2439(10) . ?
O3A N11A 1.2438(10) . ?
O1B N11B 1.2413(9) . ?
O2B N11B 1.2413(9) . ?
O3B N11B 1.2413(9) . ?
O1C N11C 1.2414(9) . ?
O2C N11C 1.2413(9) . ?
O3C N11C 1.2414(9) . ?

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
S2 Ga1 S1 99.24(2) . . ?
N1 Ga1 S1 159.68(6) . . ?
N1 Ga1 S2 89.78(6) . . ?
N3 Ga1 S1 82.85(6) . . ?
N3 Ga1 S2 100.56(6) . . ?
N3 Ga1 N1 77.58(8) . . ?
N3 Ga1 N6 99.39(8) . . ?
N3 Ga1 N8 177.01(8) . . ?
N6 Ga1 S1 91.91(6) . . ?
N6 Ga1 S2 158.19(6) . . ?
N6 Ga1 N1 85.95(8) . . ?
N8 Ga1 S1 97.70(6) . . ?
N8 Ga1 S2 82.27(6) . . ?
N8 Ga1 N1 101.56(8) . . ?
N8 Ga1 N6 77.67(8) . . ?
C12 S1 Ga1 94.38(9) . . ?
C27 S2 Ga1 94.17(13) . . ?
C27A S2 Ga1 98.2(6) . . ?
C1 N1 Ga1 125.73(18) . . ?
C1 N1 C5 120.1(2) . . ?
C5 N1 Ga1 114.11(17) . . ?
C11 N2 C7 116.9(2) . . ?
N4 N3 Ga1 122.28(15) . . ?
C6 N3 Ga1 117.96(18) . . ?
C6 N3 N4 119.6(2) . . ?
C12 N4 N3 114.6(2) . . ?
C12 N5 C13 119.9(2) . . ?
C12 N5 C14 123.2(2) . . ?
C14 N5 C13 116.9(2) . . ?
C16 N6 Ga1 124.04(19) . . ?
C16 N6 C20 120.6(2) . . ?
C20 N6 Ga1 115.30(16) . . ?
C26 N7 C22 117.6(2) . . ?
N9 N8 Ga1 122.9(2) . . ?
N9A N8 Ga1 119.0(11) . . ?
C21 N8 Ga1 117.57(17) . . ?
C21 N8 N9 119.5(3) . . ?
C21 N8 N9A 122.9(12) . . ?
C27 N9 N8 113.0(4) . . ?
C27A N9A N8 120(2) . . ?
C27 N10 C28 120.6(3) . . ?
C27 N10 C29 122.6(3) . . ?
C29 N10 C28 116.7(3) . . ?
C27A N10A C28A 123.0(14) . . ?
C27A N10A C29A 114.1(15) . . ?
C28A N10A C29A 114.5(14) . . ?
N1 C1 H1 119.0 . . ?
N1 C1 C2 122.1(3) . . ?
C2 C1 H1 119.0 . . ?
C1 C2 H2 120.8 . . ?
C3 C2 C1 118.4(3) . . ?
C3 C2 H2 120.8 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.6(2) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.5(3) . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 120.3(2) . . ?
N1 C5 C6 115.0(2) . . ?
C4 C5 C6 124.7(2) . . ?
N3 C6 C5 115.0(2) . . ?
N3 C6 C7 123.0(2) . . ?
C5 C6 C7 122.0(2) . . ?
N2 C7 C6 114.6(2) . . ?
N2 C7 C8 123.4(2) . . ?
C8 C7 C6 122.0(2) . . ?
C7 C8 H8 120.7 . . ?
C7 C8 C9 118.6(3) . . ?
C9 C8 H8 120.7 . . ?
C8 C9 H9 120.7 . . ?
C10 C9 C8 118.7(3) . . ?
C10 C9 H9 120.7 . . ?
C9 C10 H10 120.7 . . ?
C9 C10 C11 118.7(3) . . ?
C11 C10 H10 120.7 . . ?
N2 C11 C10 123.7(3) . . ?
N2 C11 H11 118.2 . . ?
C10 C11 H11 118.2 . . ?
N4 C12 S1 125.7(2) . . ?
N5 C12 S1 119.31(19) . . ?
N5 C12 N4 115.0(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 108.9 . . ?
N5 C14 H14B 108.9 . . ?
N5 C14 C15 113.2(3) . . ?
H14A C14 H14B 107.7 . . ?
C15 C14 H14A 108.9 . . ?
C15 C14 H14B 108.9 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 H16 119.1 . . ?
N6 C16 C17 121.8(3) . . ?
C17 C16 H16 119.1 . . ?
C16 C17 H17 120.8 . . ?
C18 C17 C16 118.4(3) . . ?
C18 C17 H17 120.8 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.0(3) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 120.5 . . ?
C20 C19 C18 119.0(3) . . ?
C20 C19 H19 120.5 . . ?
N6 C20 C19 120.1(2) . . ?
N6 C20 C21 114.9(2) . . ?
C19 C20 C21 125.0(2) . . ?
N8 C21 C20 114.5(2) . . ?
N8 C21 C22 124.6(2) . . ?
C20 C21 C22 120.9(2) . . ?
N7 C22 C21 115.2(2) . . ?
N7 C22 C23 122.6(2) . . ?
C23 C22 C21 122.3(2) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 C22 118.7(2) . . ?
C24 C23 H23 120.6 . . ?
C23 C24 H24 120.5 . . ?
C25 C24 C23 118.9(3) . . ?
C25 C24 H24 120.5 . . ?
C24 C25 H25 120.7 . . ?
C24 C25 C26 118.7(3) . . ?
C26 C25 H25 120.7 . . ?
N7 C26 C25 123.4(3) . . ?
N7 C26 H26 118.3 . . ?
C25 C26 H26 118.3 . . ?
N9 C27 S2 126.3(3) . . ?
N10 C27 S2 118.5(3) . . ?
N10 C27 N9 115.2(3) . . ?
N9A C27A S2 120.9(16) . . ?
N10A C27A S2 117.6(13) . . ?
N10A C27A N9A 121.2(15) . . ?
N10 C28 H28A 109.5 . . ?
N10 C28 H28B 109.5 . . ?
N10 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N10A C28A H28D 109.5 . . ?
N10A C28A H28E 109.5 . . ?
N10A C28A H28F 109.5 . . ?
H28D C28A H28E 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 109.5 . . ?
N10 C29 H29A 109.4 . . ?
N10 C29 H29B 109.4 . . ?
N10 C29 C30 111.0(3) . . ?
H29A C29 H29B 108.0 . . ?
C30 C29 H29A 109.4 . . ?
C30 C29 H29B 109.4 . . ?
N10A C29A H29C 111.0 . . ?
N10A C29A H29D 111.0 . . ?
H29C C29A H29D 109.0 . . ?
C30A C29A N10A 103.8(16) . . ?
C30A C29A H29C 111.0 . . ?
C30A C29A H29D 111.0 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29A C30A H30D 109.5 . . ?
C29A C30A H30E 109.5 . . ?
C29A C30A H30F 109.5 . . ?
H30D C30A H30E 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 109.5 . . ?
O2 N11 O1 119.57(13) . . ?
O2 N11 O3 119.56(12) . . ?
O3 N11 O1 119.59(12) . . ?
O2A N11A O1A 119.39(13) . . ?
O3A N11A O1A 119.49(13) . . ?
O3A N11A O2A 119.49(13) . . ?
O2B N11B O1B 120.01(11) . . ?
O2B N11B O3B 119.98(11) . . ?
O3B N11B O1B 120.01(10) . . ?
O2C N11C O1C 119.99(10) . . ?
O3C N11C O1C 120.03(10) . . ?
O3C N11C O2C 119.97(10) . . ?

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
Ga1 S1 C12 N4 -0.3(2) . . . . ?
Ga1 S1 C12 N5 179.7(2) . . . . ?
Ga1 S2 C27 N9 9.1(5) . . . . ?
Ga1 S2 C27 N10 -171.6(3) . . . . ?
Ga1 S2 C27A N9A -4(3) . . . . ?
Ga1 S2 C27A N10A -178(2) . . . . ?
Ga1 N1 C1 C2 -177.3(2) . . . . ?
Ga1 N1 C5 C4 177.43(19) . . . . ?
Ga1 N1 C5 C6 -4.1(3) . . . . ?
Ga1 N3 N4 C12 -5.3(3) . . . . ?
Ga1 N3 C6 C5 4.8(3) . . . . ?
Ga1 N3 C6 C7 -175.41(18) . . . . ?
Ga1 N6 C16 C17 -176.4(2) . . . . ?
Ga1 N6 C20 C19 175.0(2) . . . . ?
Ga1 N6 C20 C21 -3.5(3) . . . . ?
Ga1 N8 N9 C27 -7.7(7) . . . . ?
Ga1 N8 N9A C27A -2(5) . . . . ?
Ga1 N8 C21 C20 -0.2(3) . . . . ?
Ga1 N8 C21 C22 -178.86(18) . . . . ?
N1 C1 C2 C3 0.3(5) . . . . ?
N1 C5 C6 N3 -0.2(3) . . . . ?
N1 C5 C6 C7 179.9(2) . . . . ?
N2 C7 C8 C9 -0.2(4) . . . . ?
N3 N4 C12 S1 3.3(3) . . . . ?
N3 N4 C12 N5 -176.7(2) . . . . ?
N3 C6 C7 N2 133.7(3) . . . . ?
N3 C6 C7 C8 -45.6(4) . . . . ?
N4 N3 C6 C5 -179.1(2) . . . . ?
N4 N3 C6 C7 0.7(4) . . . . ?
N6 C16 C17 C18 1.7(4) . . . . ?
N6 C20 C21 N8 2.5(3) . . . . ?
N6 C20 C21 C22 -178.8(2) . . . . ?
N7 C22 C23 C24 -2.4(4) . . . . ?
N8 N9 C27 S2 -2.7(8) . . . . ?
N8 N9 C27 N10 178.0(5) . . . . ?
N8 N9A C27A S2 4(5) . . . . ?
N8 N9A C27A N10A 178(3) . . . . ?
N8 C21 C22 N7 -134.8(3) . . . . ?
N8 C21 C22 C23 46.1(4) . . . . ?
N9 N8 C21 C20 176.5(4) . . . . ?
N9 N8 C21 C22 -2.1(5) . . . . ?
N9A N8 C21 C20 -172(2) . . . . ?
N9A N8 C21 C22 9(2) . . . . ?
C1 N1 C5 C4 -0.4(4) . . . . ?
C1 N1 C5 C6 178.0(2) . . . . ?
C1 C2 C3 C4 -0.9(5) . . . . ?
C2 C3 C4 C5 0.8(4) . . . . ?
C3 C4 C5 N1 -0.1(4) . . . . ?
C3 C4 C5 C6 -178.4(2) . . . . ?
C4 C5 C6 N3 178.1(2) . . . . ?
C4 C5 C6 C7 -1.7(4) . . . . ?
C5 N1 C1 C2 0.3(4) . . . . ?
C5 C6 C7 N2 -46.4(3) . . . . ?
C5 C6 C7 C8 134.2(3) . . . . ?
C6 N3 N4 C12 178.8(2) . . . . ?
C6 C7 C8 C9 179.0(2) . . . . ?
C7 N2 C11 C10 0.9(4) . . . . ?
C7 C8 C9 C10 0.8(4) . . . . ?
C8 C9 C10 C11 -0.5(4) . . . . ?
C9 C10 C11 N2 -0.4(4) . . . . ?
C11 N2 C7 C6 -179.9(2) . . . . ?
C11 N2 C7 C8 -0.6(4) . . . . ?
C12 N5 C14 C15 92.3(4) . . . . ?
C13 N5 C12 S1 178.8(2) . . . . ?
C13 N5 C12 N4 -1.2(4) . . . . ?
C13 N5 C14 C15 -84.7(4) . . . . ?
C14 N5 C12 S1 1.9(4) . . . . ?
C14 N5 C12 N4 -178.1(2) . . . . ?
C16 N6 C20 C19 -1.4(4) . . . . ?
C16 N6 C20 C21 -179.9(2) . . . . ?
C16 C17 C18 C19 -1.3(5) . . . . ?
C17 C18 C19 C20 -0.4(4) . . . . ?
C18 C19 C20 N6 1.8(4) . . . . ?
C18 C19 C20 C21 -179.9(3) . . . . ?
C19 C20 C21 N8 -175.9(2) . . . . ?
C19 C20 C21 C22 2.8(4) . . . . ?
C20 N6 C16 C17 -0.4(4) . . . . ?
C20 C21 C22 N7 46.6(3) . . . . ?
C20 C21 C22 C23 -132.5(3) . . . . ?
C21 N8 N9 C27 175.7(4) . . . . ?
C21 N8 N9A C27A 170(3) . . . . ?
C21 C22 C23 C24 176.7(2) . . . . ?
C22 N7 C26 C25 -0.1(5) . . . . ?
C22 C23 C24 C25 1.1(4) . . . . ?
C23 C24 C25 C26 0.6(4) . . . . ?
C24 C25 C26 N7 -1.1(5) . . . . ?
C26 N7 C22 C21 -177.2(2) . . . . ?
C26 N7 C22 C23 1.9(4) . . . . ?
C27 N10 C29 C30 -85.2(5) . . . . ?
C27A N10A C29A C30A 100(3) . . . . ?
C28 N10 C27 S2 -176.6(4) . . . . ?
C28 N10 C27 N9 2.7(7) . . . . ?
C28 N10 C29 C30 90.1(5) . . . . ?
C28A N10A C27A S2 -3(3) . . . . ?
C28A N10A C27A N9A -177(3) . . . . ?
C28A N10A C29A C30A -111(3) . . . . ?
C29 N10 C27 S2 -1.5(6) . . . . ?
C29 N10 C27 N9 177.8(5) . . . . ?
C29A N10A C27A S2 143.8(19) . . . . ?
C29A N10A C27A N9A -30(4) . . . . ?

loop_
_audit_author_email
mahendiran.dharmasivam@sydney.edu.au
?
d.richardson@sydney.edu.au
_olex2_date_sample_data_collection 2018-10-17
_olex2_date_sample_submission    2018-10-04
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with paratone-N oil'
_olex2_submission_original_sample_id drr181004c
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.155
_oxdiff_exptl_absorpt_empirical_full_min 0.884
####################################################################### 
# 
# 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_2232codp4e4mt
_database_code_depnum_ccdc_archive 'CCDC 2299821'
loop_
_audit_author_name
_audit_author_address
'Paul Bernhardt'
;The University of Queensland
Australia
;
_audit_update_record             
;
2023-10-08 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_2232codp4e4mt       
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: theta limit of the dual source diffractometer reached
;
_vrf_PLAT934_2232codp4e4mt       
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          3 Check
RESPONSE: disorder of anions and solvent molecules affects overall precision
;
# Added during the CSD deposition process: Sunday 08 October 2023 07:08 AM
# end Validation Reply Form


_audit_creation_date             2023-10-03T11:16:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_formula_sum            'C31 H38 Cl Co N10 O2 S2'
_chemical_formula_weight         741.21

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
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                   22.7746(12)
_cell_length_b                   14.2349(7)
_cell_length_c                   23.3316(9)
_cell_angle_alpha                90
_cell_angle_beta                 91.509(4)
_cell_angle_gamma                90
_cell_volume                     7561.3(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    4459
_cell_measurement_theta_min      4.06
_cell_measurement_theta_max      61.09
_cell_measurement_wavelength     1.54184

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

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3088

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

_exptl_absorpt_coefficient_mu    5.579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.285
_shelx_estimated_absorpt_T_max   0.285

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

_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_ambient_temperature      190(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.02
_diffrn_orient_matrix_ub_11      0.065529
_diffrn_orient_matrix_ub_12      -0.020512
_diffrn_orient_matrix_ub_13      -0.008909
_diffrn_orient_matrix_ub_21      -0.002877
_diffrn_orient_matrix_ub_22      0.055921
_diffrn_orient_matrix_ub_23      -0.056569
_diffrn_orient_matrix_ub_31      0.016604
_diffrn_orient_matrix_ub_32      0.090352
_diffrn_orient_matrix_ub_33      0.03294
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  
'Agilent Technologies Xcalibur, EosS2, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_number            17313
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.662
_diffrn_reflns_theta_max         61.616
_diffrn_reflns_theta_full        61.616
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_reflns_Friedel_coverage         0
_reflns_number_total             5808
_reflns_number_gt                4760
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

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

_computing_data_collection       'CrysalisPro (Agilent Technologies,     )'
_computing_cell_refinement       'CrysalisPro (Agilent Technologies,     )'
_computing_data_reduction        'CrysalisPro (Agilent Technologies,     )'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

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

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_atom_sites_solution_hydrogens   mixed

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

_shelx_SHELXL_version_number     2018/1
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1517P)²+25.4368P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5808
_refine_ls_number_parameters     433
_refine_ls_number_restraints     3
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0792
_refine_ls_wR_factor_ref         0.2456
_refine_ls_wR_factor_gt          0.2323
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.106

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'

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
Cl1 Cl 0.3333(2) 0.3796(4) 0.3929(2) 0.0966(13) Uani 0.5 1 d . . P . .
Cl2 Cl 0.3426(2) 0.3751(4) 0.5789(3) 0.1161(17) Uani 0.5 1 d . . P . .
C1 C 0.3535(6) 0.5099(10) 0.4784(6) 0.065(3) Uiso 0.5 1 d D . P . .
H1Z H 0.391306 0.542468 0.476548 0.097 Uiso 0.5 1 calc R U P . .
H1Y H 0.345672 0.476228 0.442381 0.097 Uiso 0.5 1 calc R U P . .
H1C H 0.354709 0.465136 0.510298 0.097 Uiso 0.5 1 calc R U P . .
C2 C 0.3064(9) 0.5792(14) 0.4874(10) 0.110(6) Uiso 0.5 1 d D . P . .
H2Z H 0.320742 0.621735 0.518286 0.132 Uiso 0.5 1 calc R U P . .
H2Y H 0.303296 0.617473 0.452026 0.132 Uiso 0.5 1 calc R U P . .
O1 O 0.2531(10) 0.555(3) 0.5001(12) 0.240(13) Uiso 0.5 1 d D . P . .
H1 H 0.253985 0.521087 0.529485 0.361 Uiso 0.5 1 calc R U P . .
O2 O 0.7080(8) 0.8052(13) 0.3913(8) 0.138(5) Uiso 0.5 1 d . . P . .
H2M H 0.690156 0.746691 0.389675 0.207 Uiso 0.5 1 d R U P . .
H2N H 0.70975 0.821613 0.428306 0.207 Uiso 0.5 1 d R U P . .
O3 O 0.2155(11) 0.380(2) 0.5051(10) 0.194(9) Uiso 0.5 1 d . . P . .
H3M H 0.194414 0.324854 0.513197 0.291 Uiso 0.5 1 d R U P . .
H3N H 0.253091 0.365064 0.518045 0.291 Uiso 0.5 1 d R U P . .
O4 O 0.6374(11) 0.7480(18) 0.5344(11) 0.190(9) Uiso 0.5 1 d . . P . .
H4N H 0.668796 0.779348 0.517913 0.284 Uiso 0.5 1 d R U P . .
H4M H 0.645775 0.676089 0.52124 0.284 Uiso 0.5 1 d R U P . .
C1A C 0.4694(3) 0.3935(4) 0.3397(3) 0.0548(15) Uani 1 1 d . . . . .
H1A H 0.429259 0.382421 0.32983 0.066 Uiso 1 1 calc R U . . .
C2A C 0.4834(3) 0.4540(5) 0.3842(3) 0.0614(17) Uani 1 1 d . . . . .
H2A H 0.453306 0.48308 0.405383 0.074 Uiso 1 1 calc R U . . .
C3A C 0.5426(4) 0.4719(4) 0.3977(3) 0.0662(19) Uani 1 1 d . . . . .
H3A H 0.553146 0.513872 0.427908 0.079 Uiso 1 1 calc R U . . .
C4A C 0.5855(3) 0.4280(4) 0.3665(3) 0.0550(15) Uani 1 1 d . . . . .
H4A H 0.625887 0.440848 0.37417 0.066 Uiso 1 1 calc R U . . .
C5A C 0.5685(3) 0.3644(4) 0.3237(2) 0.0458(13) Uani 1 1 d . . . . .
C6A C 0.6092(3) 0.3089(4) 0.2898(2) 0.0465(13) Uani 1 1 d . . . . .
C7A C 0.6738(3) 0.3083(4) 0.3007(3) 0.0522(15) Uani 1 1 d . . . . .
C8A C 0.7126(3) 0.3192(5) 0.2565(3) 0.0623(17) Uani 1 1 d . . . . .
H8A H 0.698666 0.327812 0.218083 0.075 Uiso 1 1 calc R U . . .
C9A C 0.7722(3) 0.3173(5) 0.2698(4) 0.080(2) Uani 1 1 d . . . . .
H9A H 0.800022 0.324053 0.240438 0.096 Uiso 1 1 calc R U . . .
C10A C 0.7908(4) 0.3053(6) 0.3264(5) 0.088(3) Uani 1 1 d . . . . .
H10A H 0.83132 0.304015 0.336993 0.106 Uiso 1 1 calc R U . . .
C11A C 0.7486(4) 0.2956(5) 0.3662(4) 0.083(3) Uani 1 1 d . . . . .
H11A H 0.761591 0.28693 0.40489 0.099 Uiso 1 1 calc R U . . .
C12A C 0.5815(3) 0.1425(4) 0.1842(3) 0.0525(15) Uani 1 1 d . . . . .
C13A C 0.6772(4) 0.0786(8) 0.1528(4) 0.102(3) Uani 1 1 d . . . . .
H13A H 0.690363 0.02916 0.126843 0.153 Uiso 1 1 calc R U . . .
H13B H 0.692182 0.139486 0.139955 0.153 Uiso 1 1 calc R U . . .
H13C H 0.692201 0.065734 0.191725 0.153 Uiso 1 1 calc R U . . .
C14A C 0.5813(4) 0.0067(6) 0.1198(3) 0.076(2) Uani 1 1 d . . . . .
H14A H 0.604323 -0.052052 0.12362 0.091 Uiso 1 1 calc R U . . .
H14B H 0.542427 -0.004559 0.136593 0.091 Uiso 1 1 calc R U . . .
C15A C 0.5732(5) 0.0288(8) 0.0599(4) 0.103(3) Uani 1 1 d . . . . .
H15A H 0.552839 -0.02329 0.040392 0.154 Uiso 1 1 calc R U . . .
H15B H 0.549588 0.086109 0.055789 0.154 Uiso 1 1 calc R U . . .
H15C H 0.611518 0.038591 0.042808 0.154 Uiso 1 1 calc R U . . .
Co1A Co 0.5 0.25554(8) 0.25 0.0416(4) Uani 1 2 d S T P . .
N1A N 0.5111(2) 0.3500(3) 0.30988(19) 0.0459(11) Uani 1 1 d . . . . .
N2A N 0.5827(2) 0.2549(3) 0.25148(19) 0.0438(11) Uani 1 1 d . . . . .
N3A N 0.6155(2) 0.1990(3) 0.2185(2) 0.0501(12) Uani 1 1 d . . . . .
N4A N 0.6114(3) 0.0810(4) 0.1523(3) 0.0691(16) Uani 1 1 d . . . . .
N5A N 0.6902(3) 0.2970(4) 0.3557(3) 0.0691(16) Uani 1 1 d . . . . .
S1A S 0.50580(6) 0.14554(10) 0.18239(6) 0.0483(4) Uani 1 1 d . . . . .
C1B C 0.4090(3) 0.6524(4) 0.2223(3) 0.0505(14) Uani 1 1 d . . . . .
H1B H 0.415493 0.663928 0.18282 0.061 Uiso 1 1 calc R U . . .
C2B C 0.3672(3) 0.5866(5) 0.2372(3) 0.0599(16) Uani 1 1 d . . . . .
H2B H 0.345132 0.553802 0.208486 0.072 Uiso 1 1 calc R U . . .
C3B C 0.3582(3) 0.5697(4) 0.2940(3) 0.0583(16) Uani 1 1 d . . . . .
H3B H 0.330105 0.524149 0.304959 0.07 Uiso 1 1 calc R U . . .
C4B C 0.3901(3) 0.6190(4) 0.3355(3) 0.0532(15) Uani 1 1 d . . . . .
H4B H 0.38419 0.607616 0.37508 0.064 Uiso 1 1 calc R U . . .
C5B C 0.4308(3) 0.6853(4) 0.3183(2) 0.0452(13) Uani 1 1 d . . . . .
C6B C 0.4667(2) 0.7435(4) 0.3570(2) 0.0428(12) Uani 1 1 d . . . . .
C7B C 0.4594(3) 0.7443(4) 0.4198(2) 0.0530(15) Uani 1 1 d . . . . .
C8B C 0.5072(4) 0.7321(5) 0.4570(3) 0.074(2) Uani 1 1 d . . . . .
H8B H 0.545331 0.720401 0.443108 0.089 Uiso 1 1 calc R U . . .
C9B C 0.4971(6) 0.7376(7) 0.5159(4) 0.100(3) Uani 1 1 d . . . . .
H9B H 0.528354 0.728805 0.543087 0.121 Uiso 1 1 calc R U . . .
C10B C 0.4417(7) 0.7559(6) 0.5333(4) 0.106(4) Uani 1 1 d . . . . .
H10B H 0.433919 0.761032 0.572993 0.128 Uiso 1 1 calc R U . . .
C11B C 0.3975(5) 0.7668(6) 0.4934(4) 0.090(3) Uani 1 1 d . . . . .
H11B H 0.35914 0.778859 0.506545 0.109 Uiso 1 1 calc R U . . .
C12B C 0.5701(2) 0.9128(4) 0.3292(2) 0.0433(13) Uani 1 1 d . . . . .
C13B C 0.6036(4) 0.9830(6) 0.4189(3) 0.074(2) Uani 1 1 d . . . . .
H13D H 0.630311 1.032879 0.432042 0.111 Uiso 1 1 calc R U . . .
H13E H 0.563683 0.997078 0.431174 0.111 Uiso 1 1 calc R U . . .
H13F H 0.616394 0.922853 0.435429 0.111 Uiso 1 1 calc R U . . .
C14B C 0.6365(3) 1.0497(5) 0.3265(3) 0.0589(16) Uani 1 1 d . . . . .
H14C H 0.627109 1.111562 0.343299 0.071 Uiso 1 1 calc R U . . .
H14D H 0.622757 1.050619 0.28585 0.071 Uiso 1 1 calc R U . . .
C15B C 0.7016(3) 1.0371(6) 0.3284(4) 0.081(2) Uani 1 1 d . . . . .
H15D H 0.720036 1.088318 0.307287 0.121 Uiso 1 1 calc R U . . .
H15E H 0.71597 1.037925 0.368368 0.121 Uiso 1 1 calc R U . . .
H15F H 0.71161 0.976875 0.310817 0.121 Uiso 1 1 calc R U . . .
Co1B Co 0.5 0.79650(8) 0.25 0.0390(3) Uani 1 2 d S T P . .
N1B N 0.4403(2) 0.7001(3) 0.26174(19) 0.0442(11) Uani 1 1 d . . . . .
N2B N 0.50295(19) 0.7985(3) 0.33051(19) 0.0408(10) Uani 1 1 d . . . . .
N3B N 0.5374(2) 0.8589(3) 0.3618(2) 0.0479(11) Uani 1 1 d . . . . .
N4B N 0.6039(2) 0.9771(3) 0.3567(2) 0.0527(12) Uani 1 1 d . . . . .
N5B N 0.4049(3) 0.7617(4) 0.4372(2) 0.0684(16) Uani 1 1 d . . . . .
S1B S 0.56984(6) 0.90588(10) 0.25468(6) 0.0445(4) Uani 1 1 d . . . . .



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

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.475(16) . ?
C1 H1Z 0.98 . ?
C1 H1Y 0.98 . ?
C1 H1C 0.98 . ?
C2 O1 1.304(17) . ?
C2 H2Z 0.99 . ?
C2 H2Y 0.99 . ?
O1 H1 0.84 . ?
O2 H2M 0.926 . ?
O2 H2N 0.8948 . ?
O3 H3M 0.9372 . ?
O3 H3N 0.9228 . ?
O4 H4N 0.9337 . ?
O4 H4M 1.0872 . ?
C1A N1A 1.342(8) . ?
C1A C2A 1.381(9) . ?
C1A H1A 0.95 . ?
C2A C3A 1.399(11) . ?
C2A H2A 0.95 . ?
C3A C4A 1.383(10) . ?
C3A H3A 0.95 . ?
C4A C5A 1.396(8) . ?
C4A H4A 0.95 . ?
C5A N1A 1.354(7) . ?
C5A C6A 1.467(8) . ?
C6A N2A 1.314(7) . ?
C6A C7A 1.485(8) . ?
C7A N5A 1.336(9) . ?
C7A C8A 1.386(9) . ?
C8A C9A 1.385(10) . ?
C8A H8A 0.95 . ?
C9A C10A 1.388(13) . ?
C9A H9A 0.95 . ?
C10A C11A 1.359(13) . ?
C10A H10A 0.95 . ?
C11A N5A 1.348(10) . ?
C11A H11A 0.95 . ?
C12A N4A 1.345(8) . ?
C12A N3A 1.360(8) . ?
C12A S1A 1.725(7) . ?
C13A N4A 1.499(10) . ?
C13A H13A 0.98 . ?
C13A H13B 0.98 . ?
C13A H13C 0.98 . ?
C14A C15A 1.440(12) . ?
C14A N4A 1.462(9) . ?
C14A H14A 0.99 . ?
C14A H14B 0.99 . ?
C15A H15A 0.98 . ?
C15A H15B 0.98 . ?
C15A H15C 0.98 . ?
Co1A N2A 1.884(5) 2_655 ?
Co1A N2A 1.884(5) . ?
Co1A N1A 1.951(5) . ?
Co1A N1A 1.951(5) 2_655 ?
Co1A S1A 2.2290(16) 2_655 ?
Co1A S1A 2.2290(16) . ?
N2A N3A 1.346(7) . ?
C1B N1B 1.335(7) . ?
C1B C2B 1.387(9) . ?
C1B H1B 0.95 . ?
C2B C3B 1.367(10) . ?
C2B H2B 0.95 . ?
C3B C4B 1.386(9) . ?
C3B H3B 0.95 . ?
C4B C5B 1.391(8) . ?
C4B H4B 0.95 . ?
C5B N1B 1.359(7) . ?
C5B C6B 1.460(8) . ?
C6B N2B 1.306(7) . ?
C6B C7B 1.478(8) . ?
C7B N5B 1.339(9) . ?
C7B C8B 1.385(10) . ?
C8B C9B 1.401(12) . ?
C8B H8B 0.95 . ?
C9B C10B 1.361(16) . ?
C9B H9B 0.95 . ?
C10B C11B 1.361(16) . ?
C10B H10B 0.95 . ?
C11B N5B 1.329(10) . ?
C11B H11B 0.95 . ?
C12B N3B 1.324(7) . ?
C12B N4B 1.348(7) . ?
C12B S1B 1.742(6) . ?
C13B N4B 1.455(9) . ?
C13B H13D 0.98 . ?
C13B H13E 0.98 . ?
C13B H13F 0.98 . ?
C14B N4B 1.463(8) . ?
C14B C15B 1.494(10) . ?
C14B H14C 0.99 . ?
C14B H14D 0.99 . ?
C15B H15D 0.98 . ?
C15B H15E 0.98 . ?
C15B H15F 0.98 . ?
Co1B N2B 1.878(4) . ?
Co1B N2B 1.878(4) 2_655 ?
Co1B N1B 1.957(5) 2_655 ?
Co1B N1B 1.957(5) . ?
Co1B S1B 2.2264(16) . ?
Co1B S1B 2.2264(16) 2_655 ?
N2B N3B 1.363(6) . ?

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
C2 C1 H1Z 109.5 . . ?
C2 C1 H1Y 109.5 . . ?
H1Z C1 H1Y 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1Z C1 H1C 109.5 . . ?
H1Y C1 H1C 109.5 . . ?
O1 C2 C1 123(2) . . ?
O1 C2 H2Z 106.6 . . ?
C1 C2 H2Z 106.6 . . ?
O1 C2 H2Y 106.6 . . ?
C1 C2 H2Y 106.6 . . ?
H2Z C2 H2Y 106.6 . . ?
C2 O1 H1 109.5 . . ?
H2M O2 H2N 106.5 . . ?
H3M O3 H3N 103 . . ?
H4N O4 H4M 101.1 . . ?
N1A C1A C2A 121.7(6) . . ?
N1A C1A H1A 119.2 . . ?
C2A C1A H1A 119.2 . . ?
C1A C2A C3A 119.0(6) . . ?
C1A C2A H2A 120.5 . . ?
C3A C2A H2A 120.5 . . ?
C4A C3A C2A 119.3(6) . . ?
C4A C3A H3A 120.3 . . ?
C2A C3A H3A 120.3 . . ?
C3A C4A C5A 118.8(6) . . ?
C3A C4A H4A 120.6 . . ?
C5A C4A H4A 120.6 . . ?
N1A C5A C4A 121.2(5) . . ?
N1A C5A C6A 114.3(5) . . ?
C4A C5A C6A 124.6(5) . . ?
N2A C6A C5A 113.4(5) . . ?
N2A C6A C7A 123.2(5) . . ?
C5A C6A C7A 123.3(5) . . ?
N5A C7A C8A 124.1(6) . . ?
N5A C7A C6A 114.6(6) . . ?
C8A C7A C6A 121.3(6) . . ?
C9A C8A C7A 118.1(7) . . ?
C9A C8A H8A 120.9 . . ?
C7A C8A H8A 120.9 . . ?
C8A C9A C10A 119.2(8) . . ?
C8A C9A H9A 120.4 . . ?
C10A C9A H9A 120.4 . . ?
C11A C10A C9A 117.4(7) . . ?
C11A C10A H10A 121.3 . . ?
C9A C10A H10A 121.3 . . ?
N5A C11A C10A 125.9(8) . . ?
N5A C11A H11A 117.1 . . ?
C10A C11A H11A 117.1 . . ?
N4A C12A N3A 115.0(6) . . ?
N4A C12A S1A 121.5(5) . . ?
N3A C12A S1A 123.5(5) . . ?
N4A C13A H13A 109.5 . . ?
N4A C13A H13B 109.5 . . ?
H13A C13A H13B 109.5 . . ?
N4A C13A H13C 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
C15A C14A N4A 113.1(8) . . ?
C15A C14A H14A 109 . . ?
N4A C14A H14A 109 . . ?
C15A C14A H14B 109 . . ?
N4A C14A H14B 109 . . ?
H14A C14A H14B 107.8 . . ?
C14A C15A H15A 109.5 . . ?
C14A C15A H15B 109.5 . . ?
H15A C15A H15B 109.5 . . ?
C14A C15A H15C 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
N2A Co1A N2A 179.4(3) 2_655 . ?
N2A Co1A N1A 97.3(2) 2_655 . ?
N2A Co1A N1A 83.11(19) . . ?
N2A Co1A N1A 83.11(19) 2_655 2_655 ?
N2A Co1A N1A 97.3(2) . 2_655 ?
N1A Co1A N1A 92.8(3) . 2_655 ?
N2A Co1A S1A 86.08(14) 2_655 2_655 ?
N2A Co1A S1A 93.52(14) . 2_655 ?
N1A Co1A S1A 89.21(14) . 2_655 ?
N1A Co1A S1A 169.16(14) 2_655 2_655 ?
N2A Co1A S1A 93.52(14) 2_655 . ?
N2A Co1A S1A 86.08(14) . . ?
N1A Co1A S1A 169.17(14) . . ?
N1A Co1A S1A 89.21(14) 2_655 . ?
S1A Co1A S1A 90.75(9) 2_655 . ?
C1A N1A C5A 119.9(5) . . ?
C1A N1A Co1A 127.5(4) . . ?
C5A N1A Co1A 112.4(4) . . ?
C6A N2A N3A 118.9(5) . . ?
C6A N2A Co1A 116.8(4) . . ?
N3A N2A Co1A 124.2(4) . . ?
N2A N3A C12A 111.8(5) . . ?
C12A N4A C14A 121.4(6) . . ?
C12A N4A C13A 122.1(6) . . ?
C14A N4A C13A 116.3(6) . . ?
C7A N5A C11A 115.3(7) . . ?
C12A S1A Co1A 94.5(2) . . ?
N1B C1B C2B 121.8(6) . . ?
N1B C1B H1B 119.1 . . ?
C2B C1B H1B 119.1 . . ?
C3B C2B C1B 119.0(6) . . ?
C3B C2B H2B 120.5 . . ?
C1B C2B H2B 120.5 . . ?
C2B C3B C4B 119.9(6) . . ?
C2B C3B H3B 120 . . ?
C4B C3B H3B 120 . . ?
C3B C4B C5B 118.9(6) . . ?
C3B C4B H4B 120.6 . . ?
C5B C4B H4B 120.6 . . ?
N1B C5B C4B 120.7(5) . . ?
N1B C5B C6B 114.4(5) . . ?
C4B C5B C6B 124.9(5) . . ?
N2B C6B C5B 113.4(5) . . ?
N2B C6B C7B 123.6(5) . . ?
C5B C6B C7B 122.9(5) . . ?
N5B C7B C8B 123.5(6) . . ?
N5B C7B C6B 115.5(6) . . ?
C8B C7B C6B 120.9(7) . . ?
C7B C8B C9B 117.5(9) . . ?
C7B C8B H8B 121.3 . . ?
C9B C8B H8B 121.3 . . ?
C10B C9B C8B 118.8(9) . . ?
C10B C9B H9B 120.6 . . ?
C8B C9B H9B 120.6 . . ?
C9B C10B C11B 119.4(9) . . ?
C9B C10B H10B 120.3 . . ?
C11B C10B H10B 120.3 . . ?
N5B C11B C10B 124.0(10) . . ?
N5B C11B H11B 118 . . ?
C10B C11B H11B 118 . . ?
N3B C12B N4B 116.4(5) . . ?
N3B C12B S1B 123.6(4) . . ?
N4B C12B S1B 120.0(4) . . ?
N4B C13B H13D 109.5 . . ?
N4B C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
N4B C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
N4B C14B C15B 114.6(6) . . ?
N4B C14B H14C 108.6 . . ?
C15B C14B H14C 108.6 . . ?
N4B C14B H14D 108.6 . . ?
C15B C14B H14D 108.6 . . ?
H14C C14B H14D 107.6 . . ?
C14B C15B H15D 109.5 . . ?
C14B C15B H15E 109.5 . . ?
H15D C15B H15E 109.5 . . ?
C14B C15B H15F 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
N2B Co1B N2B 178.3(3) . 2_655 ?
N2B Co1B N1B 98.28(19) . 2_655 ?
N2B Co1B N1B 82.95(19) 2_655 2_655 ?
N2B Co1B N1B 82.95(19) . . ?
N2B Co1B N1B 98.29(19) 2_655 . ?
N1B Co1B N1B 90.9(3) 2_655 . ?
N2B Co1B S1B 86.19(14) . . ?
N2B Co1B S1B 92.58(14) 2_655 . ?
N1B Co1B S1B 89.97(14) 2_655 . ?
N1B Co1B S1B 169.12(14) . . ?
N2B Co1B S1B 92.59(14) . 2_655 ?
N2B Co1B S1B 86.19(14) 2_655 2_655 ?
N1B Co1B S1B 169.12(14) 2_655 2_655 ?
N1B Co1B S1B 89.97(14) . 2_655 ?
S1B Co1B S1B 91.25(8) . 2_655 ?
C1B N1B C5B 119.7(5) . . ?
C1B N1B Co1B 128.3(4) . . ?
C5B N1B Co1B 111.9(4) . . ?
C6B N2B N3B 119.1(5) . . ?
C6B N2B Co1B 117.3(4) . . ?
N3B N2B Co1B 123.4(3) . . ?
C12B N3B N2B 112.5(5) . . ?
C12B N4B C13B 119.6(5) . . ?
C12B N4B C14B 122.8(5) . . ?
C13B N4B C14B 117.2(5) . . ?
C11B N5B C7B 116.8(8) . . ?
C12B S1B Co1B 94.14(18) . . ?



# END of CIF
####################################################################### 
# 
# 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_drr18_s1675
_database_code_depnum_ccdc_archive 'CCDC 1959776'
loop_
_audit_author_name
_audit_author_address
'William Lewis'
;University of Sydney
Australia
;
_audit_update_record             
;
2019-10-17 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
_sydney_internal_submission_code drr18_s1675
_sydney_internal_submission_date 2018-09-12
_sydney_internal_submission_number s1675
_sydney_internal_client_code     dm1
_sydney_internal_client_email    mahendiran.dharmasivam@sydney.edu.au
_sydney_internal_client_name     'Mahendiran Dharmasivam'
_sydney_internal_supervisor_code drr
_sydney_internal_supervisor_name 'Des Richardson'
_sydney_internal_collection_date 2018-09-17
_sydney_internal_collection_user wlew0588
_sydney_internal_process_date    2018-09-19
_sydney_internal_process_user    wlew0588
_sydney_internal_solution_date   2018-09-19
_sydney_internal_solution_user   wlew0588
_sydney_internal_refine_date     2018-09-19
_sydney_internal_refine_user     wlew0588
_sydney_internal_check_and_archive_date 2018-09-19
_sydney_internal_check_user      wlew0588
_refine_special_details          ?
_audit_creation_date             2018-09-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H16 Cl N5 Pd S'
_chemical_formula_sum            'C15 H16 Cl N5 Pd S'
_chemical_formula_weight         440.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H17ClN5SPd
_chemical_oxdiff_usercomment     drr18_s1675
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'
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'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0507(3)
_cell_length_b                   10.5184(3)
_cell_length_c                   17.5993(4)
_cell_angle_alpha                73.219(2)
_cell_angle_beta                 81.923(2)
_cell_angle_gamma                69.997(3)
_cell_volume                     1672.07(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20714
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.0620
_cell_measurement_theta_min      4.6270
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.634
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.301
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0557
-6 -4 -3 0.0412
-5 -4 -8 0.0269
0 0 -1 0.0528
5 0 -7 0.0758
6 4 7 0.0587
0 -1 0 0.0010
0 1 0 0.0199
2 2 11 0.0531

_exptl_crystal_recrystallization_method 'crystallised form methanol'
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.021
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
0.0004 0.0007 0.9988 0.0873 -0.0232 0.0141
-5.9959 -3.9919 -2.9908 -0.2524 -0.1455 0.9200
-4.9991 -3.9971 -7.9855 -0.6917 -0.1001 0.7028
-0.0004 -0.0007 -0.9988 -0.0873 0.0232 -0.0141
4.9903 -0.0135 -6.9943 -0.6261 -0.1914 -0.8331
5.9973 3.9947 6.9861 0.6014 0.0526 -0.8637
-0.0009 -1.0001 0.0007 -0.0022 -0.1601 0.0201
0.0009 1.0001 -0.0007 0.0022 0.1601 -0.0201
2.0027 2.0042 10.9848 0.9582 -0.0772 -0.1795

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41878
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.375
_diffrn_reflns_theta_min         4.631
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.5861
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -129.00 -34.00   1.00    2.00    --  -40.45 178.00-120.00   95
  2  ω    -50.00  35.00   1.00    2.00    --  -40.45  38.00-150.00   85
  3  ω   -129.00 -34.00   1.00    2.00    --  -40.45 178.00-180.00   95
  4  ω   -114.00 -11.00   1.00    2.00    --  -40.45 -57.00  60.00  103
  5  ω     46.00 123.00   1.00    2.00    --   40.45-166.00 -25.00   77
  6  ω     32.00  98.00   1.00    8.00    --  106.66 -45.00 150.00   66
  7  ω     32.00  98.00   1.00    8.00    --  106.66 -45.00  60.00   66
  8  ω     28.00 140.00   1.00    8.00    --  106.66 -77.00 -30.00  112
  9  ω     32.00 118.00   1.00    8.00    --  106.66-125.00   0.00   86
 10  ω     32.00  98.00   1.00    8.00    --  106.66 -45.00-150.00   66
 11  ω     29.00  91.00   1.00    8.00    --  106.66 -30.00 -30.00   62
 12  ω     29.00  91.00   1.00    8.00    --  106.66 -30.00  90.00   62
 13  ω     94.00 178.00   1.00    8.00    --  106.66 125.00  30.00   84
 14  ω     73.00 178.00   1.00    8.00    --  106.66  77.00 120.00  105
 15  ω     23.00 110.00   1.00    8.00    --  106.66 -95.00-180.00   87
 16  ω     23.00 110.00   1.00    8.00    --  106.66 -95.00  90.00   87
 17  ω     17.00 178.00   1.00    8.00    --  106.66   0.00 -60.00  161
 18  ω   -119.00  -7.00   1.00    2.00    --  -40.45 -77.00-150.00  112
 19  ω   -123.00 -44.00   1.00    2.00    --  -40.45-166.00 -25.00   79
 20  ω   -114.00 -11.00   1.00    2.00    --  -40.45 -57.00-120.00  103
 21  ω   -114.00 -11.00   1.00    2.00    --  -40.45 -57.00 -30.00  103
 22  ω   -114.00 -11.00   1.00    2.00    --  -40.45 -57.00 150.00  103
 23  ω     79.00 178.00   1.00    8.00    --  106.66  45.00  90.00   99
 24  ω     73.00 178.00   1.00    8.00    --  106.66  77.00  30.00  105
 25  ω     45.00 178.00   1.00    8.00    --  106.66  15.00  60.00  133
 26  ω     73.00 178.00   1.00    8.00    --  106.66  77.00 -60.00  105
 27  ω     73.00 178.00   1.00    8.00    --  106.66  77.00-150.00  105
 28  ω     76.00 178.00   1.00    8.00    --  106.66  61.00 -90.00  102
 29  ω     73.00 178.00   1.00    8.00    --  106.66  77.00   0.00  105
 30  ω     73.00 178.00   1.00    8.00    --  106.66  77.00  90.00  105
 31  ω     76.00 178.00   1.00    8.00    --  106.66  61.00 150.00  102
 32  ω     76.00 178.00   1.00    8.00    --  106.66  61.00-180.00  102
 33  ω   -116.00 -14.00   1.00    2.00    --  -40.45 -38.00-180.00  102
 34  ω   -119.00  -7.00   1.00    2.00    --  -40.45 -77.00-120.00  112
 35  ω   -119.00  -7.00   1.00    2.00    --  -40.45 -77.00 -30.00  112
 36  ω   -119.00  -7.00   1.00    2.00    --  -40.45 -77.00  30.00  112
 37  ω   -119.00  -7.00   1.00    2.00    --  -40.45 -77.00 120.00  112
 38  ω     76.00 178.00   1.00    8.00    --  106.66  61.00-120.00  102
 39  ω     76.00 178.00   1.00    8.00    --  106.66  61.00 120.00  102
 40  ω     73.00 178.00   1.00    8.00    --  106.66  77.00 -30.00  105
 41  ω     76.00 178.00   1.00    8.00    --  106.66  61.00  30.00  102
 42  ω     76.00 178.00   1.00    8.00    --  106.66  61.00  90.00  102
 43  ω     76.00 178.00   1.00    8.00    --  106.66  61.00 -60.00  102
 44  ω     73.00  98.00   1.00    8.00    --  106.66  77.00 150.00   25
 45  ω     76.00 178.00   1.00    8.00    --  106.66  61.00-150.00  102
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0030191000
_diffrn_orient_matrix_UB_12      0.0023074000
_diffrn_orient_matrix_UB_13      0.0873610000
_diffrn_orient_matrix_UB_21      -0.0706655000
_diffrn_orient_matrix_UB_22      0.1600993000
_diffrn_orient_matrix_UB_23      -0.0233577000
_diffrn_orient_matrix_UB_31      -0.1471814000
_diffrn_orient_matrix_UB_32      -0.0199749000
_diffrn_orient_matrix_UB_33      0.0141344000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5979
_reflns_number_total             6610
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.091
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.101
_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     419
_refine_ls_number_reflns         6610
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0307
_refine_ls_restrained_S_all      1.059
_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)+(0.0488P)²+1.4296P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0830
_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:
 C15(H15A,H15B), C35(H35A,H35B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C21(H21),
 C22(H22), C23(H23), C24(H24), C28(H28), C29(H29), C30(H30), C31(H31)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C34(H34A,H34B,H34C), C36(H36A,H36B,
 H36C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.27377(2) 0.16335(2) 0.41827(2) 0.02015(7) Uani 1 1 d . . . . .
Cl1 Cl 0.07164(8) 0.12828(8) 0.39346(4) 0.02941(16) Uani 1 1 d . . . . .
S1 S 0.34105(8) 0.22558(7) 0.28985(4) 0.02394(15) Uani 1 1 d . . . . .
N1 N 0.2534(3) 0.1154(2) 0.54028(14) 0.0236(5) Uani 1 1 d . . . . .
N2 N 0.4939(3) 0.3394(3) 0.58604(14) 0.0255(5) Uani 1 1 d . . . . .
N3 N 0.4395(3) 0.2053(2) 0.43885(14) 0.0205(5) Uani 1 1 d . . . . .
N4 N 0.5250(3) 0.2557(2) 0.37979(14) 0.0215(5) Uani 1 1 d . . . . .
N5 N 0.5638(3) 0.3181(3) 0.24531(14) 0.0249(5) Uani 1 1 d . . . . .
C1 C 0.1619(3) 0.0589(3) 0.58769(17) 0.0232(6) Uani 1 1 d . . . . .
H1 H 0.088633 0.046165 0.564899 0.028 Uiso 1 1 calc R . . . .
C2 C 0.1708(3) 0.0180(3) 0.66966(18) 0.0254(6) Uani 1 1 d . . . . .
H2 H 0.104092 -0.021539 0.702726 0.030 Uiso 1 1 calc R . . . .
C3 C 0.2785(4) 0.0357(3) 0.70240(17) 0.0260(6) Uani 1 1 d . . . . .
H3 H 0.287953 0.006563 0.758281 0.031 Uiso 1 1 calc R . . . .
C4 C 0.3726(3) 0.0967(3) 0.65274(17) 0.0252(6) Uani 1 1 d . . . . .
H4 H 0.446176 0.110950 0.674409 0.030 Uiso 1 1 calc R . . . .
C5 C 0.3584(3) 0.1364(3) 0.57155(17) 0.0201(6) Uani 1 1 d . . . . .
C6 C 0.4547(3) 0.1981(3) 0.51306(17) 0.0219(6) Uani 1 1 d . . . . .
C7 C 0.5539(3) 0.2566(3) 0.53615(16) 0.0213(6) Uani 1 1 d . . . . .
C8 C 0.6937(3) 0.2327(3) 0.50686(17) 0.0245(6) Uani 1 1 d . . . . .
H8 H 0.732989 0.171974 0.472903 0.029 Uiso 1 1 calc R . . . .
C9 C 0.7748(4) 0.2997(3) 0.52843(18) 0.0273(6) Uani 1 1 d . . . . .
H9 H 0.870692 0.285369 0.509445 0.033 Uiso 1 1 calc R . . . .
C10 C 0.7135(4) 0.3877(3) 0.57800(18) 0.0309(7) Uani 1 1 d . . . . .
H10 H 0.765742 0.435943 0.593048 0.037 Uiso 1 1 calc R . . . .
C11 C 0.5746(4) 0.4033(3) 0.60487(18) 0.0300(7) Uani 1 1 d . . . . .
H11 H 0.533342 0.463340 0.639024 0.036 Uiso 1 1 calc R . . . .
C12 C 0.4865(3) 0.2690(3) 0.30753(17) 0.0217(6) Uani 1 1 d . . . . .
C14 C 0.6845(4) 0.3574(4) 0.25659(19) 0.0301(7) Uani 1 1 d . . . . .
H14A H 0.772909 0.287986 0.244494 0.045 Uiso 1 1 calc GR . . . .
H14B H 0.682480 0.360755 0.311821 0.045 Uiso 1 1 calc GR . . . .
H14C H 0.678995 0.449726 0.221007 0.045 Uiso 1 1 calc GR . . . .
C15 C 0.5195(4) 0.3562(3) 0.16325(17) 0.0274(6) Uani 1 1 d . . . . .
H15A H 0.476754 0.287768 0.157447 0.033 Uiso 1 1 calc R . . . .
H15B H 0.603763 0.351923 0.126163 0.033 Uiso 1 1 calc R . . . .
C16 C 0.4127(4) 0.5028(4) 0.1416(2) 0.0387(8) Uani 1 1 d . . . . .
H16A H 0.387686 0.526228 0.086259 0.058 Uiso 1 1 calc GR . . . .
H16B H 0.454336 0.570542 0.148081 0.058 Uiso 1 1 calc GR . . . .
H16C H 0.327253 0.505963 0.176547 0.058 Uiso 1 1 calc GR . . . .
Pd2 Pd 0.19183(2) 0.86503(2) -0.00188(2) 0.02132(7) Uani 1 1 d . . . . .
Cl21 Cl 0.35198(9) 0.95957(8) -0.08437(4) 0.02865(16) Uani 1 1 d . . . . .
S21 S 0.09542(8) 0.82729(8) -0.09800(4) 0.02874(17) Uani 1 1 d . . . . .
N21 N 0.2463(3) 0.8787(2) 0.10281(14) 0.0229(5) Uani 1 1 d . . . . .
N22 N 0.0666(3) 0.5973(3) 0.27227(15) 0.0294(6) Uani 1 1 d . . . . .
N23 N 0.0632(3) 0.7774(2) 0.07079(14) 0.0226(5) Uani 1 1 d . . . . .
N24 N -0.0237(3) 0.7230(3) 0.04667(15) 0.0276(5) Uani 1 1 d . . . . .
N25 N -0.0936(4) 0.6860(4) -0.06077(18) 0.0433(8) Uani 1 1 d . . . . .
C21 C 0.3362(4) 0.9394(3) 0.11315(18) 0.0286(7) Uani 1 1 d . . . . .
H21 H 0.391139 0.973975 0.068637 0.034 Uiso 1 1 calc R . . . .
C22 C 0.3524(4) 0.9539(4) 0.18696(19) 0.0342(7) Uani 1 1 d . . . . .
H22 H 0.418030 0.996685 0.193179 0.041 Uiso 1 1 calc R . . . .
C23 C 0.2708(4) 0.9046(3) 0.25118(18) 0.0310(7) Uani 1 1 d . . . . .
H23 H 0.278034 0.915359 0.302070 0.037 Uiso 1 1 calc R . . . .
C24 C 0.1784(3) 0.8393(3) 0.24083(17) 0.0255(6) Uani 1 1 d . . . . .
H24 H 0.122815 0.803689 0.284661 0.031 Uiso 1 1 calc R . . . .
C25 C 0.1679(3) 0.8267(3) 0.16570(17) 0.0236(6) Uani 1 1 d . . . . .
C26 C 0.0708(3) 0.7628(3) 0.14742(17) 0.0235(6) Uani 1 1 d . . . . .
C27 C -0.0096(3) 0.6873(3) 0.21011(17) 0.0251(6) Uani 1 1 d . . . . .
C28 C -0.1533(3) 0.7104(3) 0.20530(17) 0.0243(6) Uani 1 1 d . . . . .
H28 H -0.202754 0.772789 0.159880 0.029 Uiso 1 1 calc R . . . .
C29 C -0.2228(4) 0.6403(3) 0.26827(19) 0.0282(6) Uani 1 1 d . . . . .
H29 H -0.321661 0.656736 0.267657 0.034 Uiso 1 1 calc R . . . .
C30 C -0.1461(4) 0.5461(3) 0.33196(19) 0.0327(7) Uani 1 1 d . . . . .
H30 H -0.190788 0.495532 0.375477 0.039 Uiso 1 1 calc R . . . .
C31 C -0.0029(4) 0.5273(4) 0.33080(19) 0.0341(7) Uani 1 1 d . . . . .
H31 H 0.049619 0.460655 0.374100 0.041 Uiso 1 1 calc R . . . .
C32 C -0.0156(4) 0.7416(4) -0.03214(18) 0.0309(7) Uani 1 1 d . . . . .
C34 C -0.0905(5) 0.6931(6) -0.1458(2) 0.0555(12) Uani 1 1 d . . . . .
H34A H -0.057406 0.770916 -0.177358 0.083 Uiso 1 1 calc GR . . . .
H34B H -0.185974 0.707982 -0.160862 0.083 Uiso 1 1 calc GR . . . .
H34C H -0.025906 0.605075 -0.155883 0.083 Uiso 1 1 calc GR . . . .
C35 C -0.1824(4) 0.6073(5) -0.0071(2) 0.0451(9) Uani 1 1 d . . . . .
H35A H -0.189789 0.535476 -0.030880 0.054 Uiso 1 1 calc R . . . .
H35B H -0.136555 0.558520 0.044234 0.054 Uiso 1 1 calc R . . . .
C36 C -0.3257(5) 0.7009(4) 0.0069(3) 0.0521(10) Uani 1 1 d . . . . .
H36A H -0.369276 0.753159 -0.044057 0.078 Uiso 1 1 calc GR . . . .
H36B H -0.319262 0.766622 0.034876 0.078 Uiso 1 1 calc GR . . . .
H36C H -0.383883 0.644973 0.039367 0.078 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
Pd1 Cl1 2.3042(7) . ?
Pd1 S1 2.2389(7) . ?
Pd1 N1 2.057(2) . ?
Pd1 N3 1.966(2) . ?
S1 C12 1.764(3) . ?
N1 C1 1.329(4) . ?
N1 C5 1.363(4) . ?
N2 C7 1.351(4) . ?
N2 C11 1.340(4) . ?
N3 N4 1.357(4) . ?
N3 C6 1.314(4) . ?
N4 C12 1.336(4) . ?
N5 C12 1.333(4) . ?
N5 C14 1.463(4) . ?
N5 C15 1.473(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.388(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.384(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.389(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.382(4) . ?
C5 C6 1.478(4) . ?
C6 C7 1.489(4) . ?
C7 C8 1.390(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.393(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.379(5) . ?
C11 H11 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.523(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
Pd2 Cl21 2.3005(8) . ?
Pd2 S21 2.2517(7) . ?
Pd2 N21 2.051(2) . ?
Pd2 N23 1.956(3) . ?
S21 C32 1.768(4) . ?
N21 C21 1.328(4) . ?
N21 C25 1.359(4) . ?
N22 C27 1.349(4) . ?
N22 C31 1.343(4) . ?
N23 N24 1.362(4) . ?
N23 C26 1.323(4) . ?
N24 C32 1.339(4) . ?
N25 C32 1.343(5) . ?
N25 C34 1.474(5) . ?
N25 C35 1.480(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.388(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.382(5) . ?
C23 H23 0.9500 . ?
C23 C24 1.387(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.388(4) . ?
C25 C26 1.473(4) . ?
C26 C27 1.477(4) . ?
C27 C28 1.391(5) . ?
C28 H28 0.9500 . ?
C28 C29 1.386(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.382(5) . ?
C30 H30 0.9500 . ?
C30 C31 1.382(5) . ?
C31 H31 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.475(6) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 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
S1 Pd1 Cl1 94.52(3) . . ?
N1 Pd1 Cl1 98.79(8) . . ?
N1 Pd1 S1 166.68(8) . . ?
N3 Pd1 Cl1 176.52(7) . . ?
N3 Pd1 S1 85.34(7) . . ?
N3 Pd1 N1 81.34(10) . . ?
C12 S1 Pd1 94.99(10) . . ?
C1 N1 Pd1 128.2(2) . . ?
C1 N1 C5 120.3(3) . . ?
C5 N1 Pd1 111.2(2) . . ?
C11 N2 C7 116.8(3) . . ?
N4 N3 Pd1 122.75(18) . . ?
C6 N3 Pd1 116.3(2) . . ?
C6 N3 N4 120.4(3) . . ?
C12 N4 N3 112.8(2) . . ?
C12 N5 C14 120.7(2) . . ?
C12 N5 C15 122.0(3) . . ?
C14 N5 C15 116.6(3) . . ?
N1 C1 H1 119.2 . . ?
N1 C1 C2 121.6(3) . . ?
C2 C1 H1 119.2 . . ?
C1 C2 H2 120.6 . . ?
C3 C2 C1 118.9(3) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.3(3) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 120.4(3) . . ?
N1 C5 C6 115.5(2) . . ?
C4 C5 C6 124.1(3) . . ?
N3 C6 C5 114.8(3) . . ?
N3 C6 C7 122.7(3) . . ?
C5 C6 C7 122.3(2) . . ?
N2 C7 C6 113.7(3) . . ?
N2 C7 C8 123.1(3) . . ?
C8 C7 C6 123.2(3) . . ?
C7 C8 H8 120.7 . . ?
C7 C8 C9 118.5(3) . . ?
C9 C8 H8 120.7 . . ?
C8 C9 H9 120.5 . . ?
C10 C9 C8 119.0(3) . . ?
C10 C9 H9 120.5 . . ?
C9 C10 H10 120.9 . . ?
C11 C10 C9 118.2(3) . . ?
C11 C10 H10 120.9 . . ?
N2 C11 C10 124.4(3) . . ?
N2 C11 H11 117.8 . . ?
C10 C11 H11 117.8 . . ?
N4 C12 S1 124.1(2) . . ?
N5 C12 S1 118.5(2) . . ?
N5 C12 N4 117.4(3) . . ?
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 . . ?
N5 C15 H15A 109.3 . . ?
N5 C15 H15B 109.3 . . ?
N5 C15 C16 111.4(3) . . ?
H15A C15 H15B 108.0 . . ?
C16 C15 H15A 109.3 . . ?
C16 C15 H15B 109.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
S21 Pd2 Cl21 96.10(3) . . ?
N21 Pd2 Cl21 97.44(7) . . ?
N21 Pd2 S21 166.46(8) . . ?
N23 Pd2 Cl21 177.30(7) . . ?
N23 Pd2 S21 85.14(7) . . ?
N23 Pd2 N21 81.32(10) . . ?
C32 S21 Pd2 94.96(10) . . ?
C21 N21 Pd2 128.1(2) . . ?
C21 N21 C25 120.1(2) . . ?
C25 N21 Pd2 111.55(19) . . ?
C31 N22 C27 116.6(3) . . ?
N24 N23 Pd2 123.32(19) . . ?
C26 N23 Pd2 116.7(2) . . ?
C26 N23 N24 119.8(3) . . ?
C32 N24 N23 112.7(3) . . ?
C32 N25 C34 122.5(3) . . ?
C32 N25 C35 121.2(3) . . ?
C34 N25 C35 116.3(3) . . ?
N21 C21 H21 119.0 . . ?
N21 C21 C22 122.1(3) . . ?
C22 C21 H21 119.0 . . ?
C21 C22 H22 120.7 . . ?
C23 C22 C21 118.5(3) . . ?
C23 C22 H22 120.7 . . ?
C22 C23 H23 120.2 . . ?
C22 C23 C24 119.5(3) . . ?
C24 C23 H23 120.2 . . ?
C23 C24 H24 120.4 . . ?
C23 C24 C25 119.3(3) . . ?
C25 C24 H24 120.4 . . ?
N21 C25 C24 120.5(3) . . ?
N21 C25 C26 115.6(3) . . ?
C24 C25 C26 123.9(3) . . ?
N23 C26 C25 114.5(3) . . ?
N23 C26 C27 123.2(3) . . ?
C25 C26 C27 122.3(3) . . ?
N22 C27 C26 114.8(3) . . ?
N22 C27 C28 123.2(3) . . ?
C28 C27 C26 122.0(3) . . ?
C27 C28 H28 120.7 . . ?
C29 C28 C27 118.5(3) . . ?
C29 C28 H28 120.7 . . ?
C28 C29 H29 120.5 . . ?
C30 C29 C28 119.1(3) . . ?
C30 C29 H29 120.5 . . ?
C29 C30 H30 120.8 . . ?
C31 C30 C29 118.4(3) . . ?
C31 C30 H30 120.8 . . ?
N22 C31 C30 124.1(3) . . ?
N22 C31 H31 118.0 . . ?
C30 C31 H31 118.0 . . ?
N24 C32 S21 123.8(3) . . ?
N24 C32 N25 116.6(3) . . ?
N25 C32 S21 119.5(2) . . ?
N25 C34 H34A 109.5 . . ?
N25 C34 H34B 109.5 . . ?
N25 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N25 C35 H35A 109.3 . . ?
N25 C35 H35B 109.3 . . ?
H35A C35 H35B 108.0 . . ?
C36 C35 N25 111.5(4) . . ?
C36 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

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
Pd1 S1 C12 N4 1.7(2) . . . . ?
Pd1 S1 C12 N5 -178.4(2) . . . . ?
Pd1 N1 C1 C2 172.7(2) . . . . ?
Pd1 N1 C5 C4 -173.3(2) . . . . ?
Pd1 N1 C5 C6 4.7(3) . . . . ?
Pd1 N3 N4 C12 -2.0(3) . . . . ?
Pd1 N3 C6 C5 9.9(3) . . . . ?
Pd1 N3 C6 C7 -166.0(2) . . . . ?
N1 C1 C2 C3 -0.5(4) . . . . ?
N1 C5 C6 N3 -9.6(4) . . . . ?
N1 C5 C6 C7 166.2(3) . . . . ?
N2 C7 C8 C9 -1.6(4) . . . . ?
N3 N4 C12 S1 -0.2(3) . . . . ?
N3 N4 C12 N5 179.9(2) . . . . ?
N3 C6 C7 N2 130.1(3) . . . . ?
N3 C6 C7 C8 -47.6(4) . . . . ?
N4 N3 C6 C5 -177.8(2) . . . . ?
N4 N3 C6 C7 6.3(4) . . . . ?
C1 N1 C5 C4 1.3(4) . . . . ?
C1 N1 C5 C6 179.2(2) . . . . ?
C1 C2 C3 C4 1.4(4) . . . . ?
C2 C3 C4 C5 -1.0(4) . . . . ?
C3 C4 C5 N1 -0.3(4) . . . . ?
C3 C4 C5 C6 -178.1(3) . . . . ?
C4 C5 C6 N3 168.2(3) . . . . ?
C4 C5 C6 C7 -15.9(4) . . . . ?
C5 N1 C1 C2 -0.8(4) . . . . ?
C5 C6 C7 N2 -45.4(4) . . . . ?
C5 C6 C7 C8 136.9(3) . . . . ?
C6 N3 N4 C12 -173.7(3) . . . . ?
C6 C7 C8 C9 176.0(3) . . . . ?
C7 N2 C11 C10 -1.3(5) . . . . ?
C7 C8 C9 C10 -0.1(4) . . . . ?
C8 C9 C10 C11 1.0(4) . . . . ?
C9 C10 C11 N2 -0.3(5) . . . . ?
C11 N2 C7 C6 -175.5(3) . . . . ?
C11 N2 C7 C8 2.2(4) . . . . ?
C12 N5 C15 C16 82.3(4) . . . . ?
C14 N5 C12 S1 179.2(2) . . . . ?
C14 N5 C12 N4 -0.9(4) . . . . ?
C14 N5 C15 C16 -88.2(3) . . . . ?
C15 N5 C12 S1 9.1(4) . . . . ?
C15 N5 C12 N4 -171.0(3) . . . . ?
Pd2 S21 C32 N24 2.0(3) . . . . ?
Pd2 S21 C32 N25 -175.3(3) . . . . ?
Pd2 N21 C21 C22 173.1(3) . . . . ?
Pd2 N21 C25 C24 -173.4(2) . . . . ?
Pd2 N21 C25 C26 4.6(3) . . . . ?
Pd2 N23 N24 C32 -2.7(4) . . . . ?
Pd2 N23 C26 C25 5.1(3) . . . . ?
Pd2 N23 C26 C27 -174.2(2) . . . . ?
N21 C21 C22 C23 -0.7(5) . . . . ?
N21 C25 C26 N23 -6.4(4) . . . . ?
N21 C25 C26 C27 172.9(3) . . . . ?
N22 C27 C28 C29 1.6(4) . . . . ?
N23 N24 C32 S21 0.0(4) . . . . ?
N23 N24 C32 N25 177.4(3) . . . . ?
N23 C26 C27 N22 134.2(3) . . . . ?
N23 C26 C27 C28 -47.1(4) . . . . ?
N24 N23 C26 C25 -179.7(2) . . . . ?
N24 N23 C26 C27 1.0(4) . . . . ?
C21 N21 C25 C24 1.5(4) . . . . ?
C21 N21 C25 C26 179.5(3) . . . . ?
C21 C22 C23 C24 1.6(5) . . . . ?
C22 C23 C24 C25 -1.0(5) . . . . ?
C23 C24 C25 N21 -0.6(5) . . . . ?
C23 C24 C25 C26 -178.4(3) . . . . ?
C24 C25 C26 N23 171.5(3) . . . . ?
C24 C25 C26 C27 -9.3(5) . . . . ?
C25 N21 C21 C22 -0.9(5) . . . . ?
C25 C26 C27 N22 -45.0(4) . . . . ?
C25 C26 C27 C28 133.7(3) . . . . ?
C26 N23 N24 C32 -177.5(3) . . . . ?
C26 C27 C28 C29 -177.0(3) . . . . ?
C27 N22 C31 C30 -2.5(5) . . . . ?
C27 C28 C29 C30 -2.5(4) . . . . ?
C28 C29 C30 C31 1.0(5) . . . . ?
C29 C30 C31 N22 1.6(5) . . . . ?
C31 N22 C27 C26 179.6(3) . . . . ?
C31 N22 C27 C28 0.8(5) . . . . ?
C32 N25 C35 C36 88.8(4) . . . . ?
C34 N25 C32 S21 0.1(5) . . . . ?
C34 N25 C32 N24 -177.4(4) . . . . ?
C34 N25 C35 C36 -94.2(5) . . . . ?
C35 N25 C32 S21 176.9(3) . . . . ?
C35 N25 C32 N24 -0.6(5) . . . . ?

loop_
_audit_author_email
mahendiran.dharmasivam@sydney.edu.au
?
d.richardson@sydney.edu.au
_olex2_date_sample_data_collection 2018-09-17
_olex2_date_sample_submission    2018-09-12
_olex2_exptl_crystal_mounting_method 'in paratone on a loop'
_olex2_submission_original_sample_id Pd(Dp4e4mT)Cl
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.721
_oxdiff_exptl_absorpt_empirical_full_min 0.681
