# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_p-31c
_database_code_depnum_ccdc_archive 'CCDC 2152097'
loop_
_audit_author_name
_audit_author_address
'Cong Wu'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2022-02-15 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_audit_creation_date             2022-02-15
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H24 N6 Ni1, O4 S0.981'
_chemical_formula_sum            'C6 H24 N6 Ni O4 S0.98'
_chemical_formula_weight         334.44
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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      trigonal
_space_group_IT_number           163
_space_group_name_H-M_alt        'P -3 1 c'
_space_group_name_Hall           '-P 3 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   8.9389(5)
_cell_length_b                   8.9389(5)
_cell_length_c                   9.6152(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     665.36(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1708
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5740
_cell_measurement_theta_min      4.5550
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.630
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             355
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3110
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.748
_diffrn_reflns_theta_min         4.239
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00 -53.00   0.50    0.88    --    0.10 -63.00  52.00   72
  2  ω    -59.00  -9.00   0.50    0.88    --    0.10 -82.00 150.00  100
  3  ω     -8.00  27.00   0.50    0.88    --    0.10 -82.00   0.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0507390000
_diffrn_orient_matrix_UB_12      0.0339329000
_diffrn_orient_matrix_UB_13      0.0271229000
_diffrn_orient_matrix_UB_21      -0.0250067000
_diffrn_orient_matrix_UB_22      -0.0585007000
_diffrn_orient_matrix_UB_23      0.0566294000
_diffrn_orient_matrix_UB_31      0.0720722000
_diffrn_orient_matrix_UB_32      0.0618091000
_diffrn_orient_matrix_UB_33      0.0387230000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                539
_reflns_number_total             573
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         573
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0299
_refine_ls_restrained_S_all      1.165
_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)+(0.0362P)²+0.3811P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0764
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Rigid body (RIGU) restrains
 O2, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: O1(0.33333) O2(0.33333)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.333333 0.666667 0.750000 0.0190(2) Uani 1 6 d S T P . .
N1 N 0.5408(2) 0.6858(2) 0.62806(17) 0.0320(4) Uani 1 1 d . . . . .
H1A H 0.552019 0.593286 0.641310 0.038 Uiso 1 1 calc R U . . .
H1B H 0.520716 0.691955 0.538186 0.038 Uiso 1 1 calc R U . . .
C1 C 0.6996(3) 0.8433(3) 0.6717(2) 0.0368(5) Uani 1 1 d . . . . .
H1C H 0.703665 0.944157 0.630143 0.044 Uiso 1 1 calc R U . . .
H1D H 0.800323 0.838171 0.641177 0.044 Uiso 1 1 calc R U . . .
O1 O 0.7985(16) 0.4896(13) 0.6827(10) 0.100(3) Uani 0.3333 1 d . . P . .
O2 O 0.5535(19) 0.2165(12) 0.6476(9) 0.100(4) Uani 0.3333 1 d . . P . .
S1 S 0.666667 0.333333 0.750000 0.0208(4) Uani 0.981(8) 6 d S T . . .


_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 N1 2.1278(17) 5_556 ?
Ni1 N1 2.1278(17) 4_666 ?
Ni1 N1 2.1278(17) 3_565 ?
Ni1 N1 2.1278(17) 2_665 ?
Ni1 N1 2.1278(17) 6_566 ?
Ni1 N1 2.1278(17) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.475(3) . ?
C1 C1 1.510(5) 6_566 ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
O1 O1 1.61(3) 5_656 ?
O1 O2 1.346(13) 2_655 ?
O1 O2 1.666(14) 4_666 ?
O1 O2 1.124(14) 3_665 ?
O1 S1 1.453(7) . ?
O2 O2 1.782(16) 3_665 ?
O2 O2 1.782(16) 2_655 ?
O2 S1 1.424(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
N1 Ni1 N1 81.97(9) 5_556 2_665 ?
N1 Ni1 N1 81.97(10) 6_566 . ?
N1 Ni1 N1 81.97(9) 3_565 4_666 ?
N1 Ni1 N1 92.55(7) 5_556 6_566 ?
N1 Ni1 N1 172.04(10) 2_665 4_666 ?
N1 Ni1 N1 93.46(10) 2_665 6_566 ?
N1 Ni1 N1 92.55(7) 2_665 . ?
N1 Ni1 N1 93.46(10) 5_556 3_565 ?
N1 Ni1 N1 92.55(7) 5_556 4_666 ?
N1 Ni1 N1 92.55(7) 2_665 3_565 ?
N1 Ni1 N1 92.55(7) 6_566 4_666 ?
N1 Ni1 N1 172.04(10) 6_566 3_565 ?
N1 Ni1 N1 93.46(10) . 4_666 ?
N1 Ni1 N1 172.04(10) 5_556 . ?
N1 Ni1 N1 92.55(7) 3_565 . ?
Ni1 N1 H1A 110.2 . . ?
Ni1 N1 H1B 110.2 . . ?
H1A N1 H1B 108.5 . . ?
C1 N1 Ni1 107.67(13) . . ?
C1 N1 H1A 110.2 . . ?
C1 N1 H1B 110.2 . . ?
N1 C1 C1 108.68(15) . 6_566 ?
N1 C1 H1C 110.0 . . ?
N1 C1 H1D 110.0 . . ?
C1 C1 H1C 110.0 6_566 . ?
C1 C1 H1D 110.0 6_566 . ?
H1C C1 H1D 108.3 . . ?
O1 O1 O2 40.1(6) 5_656 4_666 ?
O2 O1 O1 72.6(13) 3_665 5_656 ?
O2 O1 O1 116.4(6) 2_655 5_656 ?
O2 O1 O2 91.9(11) 3_665 2_655 ?
O2 O1 O2 93.2(9) 2_655 4_666 ?
O2 O1 O2 105.5(9) 3_665 4_666 ?
O2 O1 S1 65.6(6) 3_665 . ?
O2 O1 S1 61.0(4) 2_655 . ?
S1 O1 O1 56.3(6) . 5_656 ?
S1 O1 O2 53.8(4) . 4_666 ?
O1 O2 O1 67.3(15) 2_655 4_666 ?
O1 O2 O1 131.6(9) 2_655 3_665 ?
O1 O2 O1 86.1(11) 3_665 4_666 ?
O1 O2 O2 39.1(8) 3_665 2_655 ?
O1 O2 O2 49.0(8) 2_655 3_665 ?
O1 O2 O2 96.5(7) 3_665 3_665 ?
O1 O2 O2 101.5(7) 4_666 2_655 ?
O1 O2 O2 105.8(7) 2_655 2_655 ?
O1 O2 O2 93.7(8) 4_666 3_665 ?
O1 O2 S1 68.4(5) 2_655 . ?
O1 O2 S1 63.2(5) 3_665 . ?
O2 O2 O2 60.001(2) 2_655 3_665 ?
S1 O2 O1 55.5(4) . 4_666 ?
S1 O2 O2 51.3(3) . 3_665 ?
S1 O2 O2 51.3(3) . 2_655 ?
O1 S1 O1 90.8(13) 5_656 2_655 ?
O1 S1 O1 165.0(14) . 4_666 ?
O1 S1 O1 101.7(5) 3_665 2_655 ?
O1 S1 O1 67.3(12) 3_665 6_556 ?
O1 S1 O1 101.7(5) 6_556 5_656 ?
O1 S1 O1 165.0(15) 6_556 2_655 ?
O1 S1 O1 101.7(5) 6_556 4_666 ?
O1 S1 O1 101.7(5) 4_666 5_656 ?
O1 S1 O1 165.0(15) 3_665 5_656 ?
O1 S1 O1 101.7(5) 3_665 . ?
O1 S1 O1 67.3(12) . 5_656 ?
O1 S1 O1 90.8(13) 6_556 . ?
O1 S1 O1 90.8(13) 3_665 4_666 ?
O1 S1 O1 67.3(12) 4_666 2_655 ?
O1 S1 O1 101.7(5) . 2_655 ?
O2 S1 O1 55.8(6) . 3_665 ?
O2 S1 O1 55.8(6) 2_655 . ?
O2 S1 O1 46.0(6) 2_655 3_665 ?
O2 S1 O1 122.0(13) 4_666 3_665 ?
O2 S1 O1 55.8(6) 6_556 5_656 ?
O2 S1 O1 46.0(6) 3_665 . ?
O2 S1 O1 136.3(12) 4_666 2_655 ?
O2 S1 O1 122.0(13) 6_556 . ?
O2 S1 O1 46.0(6) 4_666 5_656 ?
O2 S1 O1 109.6(5) 3_665 3_665 ?
O2 S1 O1 136.3(12) 3_665 6_556 ?
O2 S1 O1 136.3(12) 6_556 3_665 ?
O2 S1 O1 109.6(5) 2_655 2_655 ?
O2 S1 O1 55.8(6) 5_656 4_666 ?
O2 S1 O1 70.8(6) 6_556 2_655 ?
O2 S1 O1 136.3(12) 2_655 4_666 ?
O2 S1 O1 136.3(12) . 5_656 ?
O2 S1 O1 70.8(6) . 4_666 ?
O2 S1 O1 70.8(6) 3_665 5_656 ?
O2 S1 O1 109.6(5) 4_666 4_666 ?
O2 S1 O1 70.8(6) 5_656 3_665 ?
O2 S1 O1 122.0(13) 3_665 4_666 ?
O2 S1 O1 109.6(5) 6_556 6_556 ?
O2 S1 O1 46.0(6) 6_556 4_666 ?
O2 S1 O1 122.0(13) 5_656 2_655 ?
O2 S1 O1 46.0(6) 5_656 6_556 ?
O2 S1 O1 46.0(6) . 2_655 ?
O2 S1 O1 70.8(6) 2_655 6_556 ?
O2 S1 O1 55.8(6) 3_665 2_655 ?
O2 S1 O1 122.0(13) . 6_556 ?
O2 S1 O1 136.3(12) 5_656 . ?
O2 S1 O1 109.6(5) 5_656 5_656 ?
O2 S1 O1 122.0(13) 2_655 5_656 ?
O2 S1 O1 109.6(5) . . ?
O2 S1 O1 70.8(6) 4_666 . ?
O2 S1 O1 55.8(6) 4_666 6_556 ?
O2 S1 O2 177.7(15) 5_656 3_665 ?
O2 S1 O2 101.1(9) 3_665 6_556 ?
O2 S1 O2 77.5(7) 5_656 4_666 ?
O2 S1 O2 77.5(7) 2_655 3_665 ?
O2 S1 O2 101.1(9) 5_656 . ?
O2 S1 O2 77.5(7) . 3_665 ?
O2 S1 O2 177.7(15) . 4_666 ?
O2 S1 O2 104.0(14) 4_666 3_665 ?
O2 S1 O2 104.0(14) 5_656 2_655 ?
O2 S1 O2 77.5(7) 5_656 6_556 ?
O2 S1 O2 77.5(7) 2_655 . ?
O2 S1 O2 177.7(15) 2_655 6_556 ?
O2 S1 O2 101.1(9) 2_655 4_666 ?
O2 S1 O2 104.0(14) . 6_556 ?
O2 S1 O2 77.5(7) 4_666 6_556 ?

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 N1 C1 C1 41.7(2) . . . 6_566 ?
O1 O1 S1 O1 -102.4(8) 5_656 . . 6_556 ?
O1 O1 S1 O1 85.9(13) 5_656 . . 2_655 ?
O1 O1 S1 O1 -169.3(12) 5_656 . . 3_665 ?
O1 O1 S1 O1 44.5(8) 5_656 . . 4_666 ?
O1 O1 S1 O2 84.7(15) 5_656 . . 3_665 ?
O1 O1 S1 O2 -49.3(7) 5_656 . . 4_666 ?
O1 O1 S1 O2 133.1(13) 5_656 . . . ?
O1 O1 S1 O2 -95.0(17) 5_656 . . 5_656 ?
O1 O1 S1 O2 -168.3(12) 5_656 . . 2_655 ?
O1 O1 S1 O2 11.4(11) 5_656 . . 6_556 ?
O1 O2 S1 O1 168.7(11) 2_655 . . 6_556 ?
O1 O2 S1 O1 -104.8(14) 3_665 . . 4_666 ?
O1 O2 S1 O1 -164.1(15) 4_666 . . . ?
O1 O2 S1 O1 -12.8(12) 3_665 . . 6_556 ?
O1 O2 S1 O1 -178.6(11) 2_655 . . 3_665 ?
O1 O2 S1 O1 178.6(11) 3_665 . . 2_655 ?
O1 O2 S1 O1 76.6(18) 2_655 . . 4_666 ?
O1 O2 S1 O1 -76.6(18) 4_666 . . 2_655 ?
O1 O2 S1 O1 104.8(14) 4_666 . . 3_665 ?
O1 O2 S1 O1 -87.5(6) 2_655 . . . ?
O1 O2 S1 O1 -10(2) 2_655 . . 5_656 ?
O1 O2 S1 O1 91.1(5) 3_665 . . . ?
O1 O2 S1 O1 168.3(13) 3_665 . . 5_656 ?
O1 O2 S1 O1 -86.9(6) 4_666 . . 5_656 ?
O1 O2 S1 O1 92.0(8) 4_666 . . 6_556 ?
O1 O2 S1 O2 124.5(6) 3_665 . . 3_665 ?
O1 O2 S1 O2 -133.8(7) 2_655 . . 2_655 ?
O1 O2 S1 O2 -57.3(10) 3_665 . . 5_656 ?
O1 O2 S1 O2 -130.7(15) 4_666 . . 3_665 ?
O1 O2 S1 O2 -54.1(9) 2_655 . . 3_665 ?
O1 O2 S1 O2 44.4(11) 2_655 . . 6_556 ?
O1 O2 S1 O2 47.5(6) 4_666 . . 5_656 ?
O1 O2 S1 O2 -137.0(9) 3_665 . . 6_556 ?
O1 O2 S1 O2 149.6(17) 4_666 . . 2_655 ?
O1 O2 S1 O2 -32.2(7) 4_666 . . 6_556 ?
O1 O2 S1 O2 124.1(15) 2_655 . . 5_656 ?
O1 O2 S1 O2 44.8(9) 3_665 . . 2_655 ?
O2 O1 S1 O1 135.2(13) 4_666 . . 2_655 ?
O2 O1 S1 O1 65.9(7) 2_655 . . 6_556 ?
O2 O1 S1 O1 93.8(10) 4_666 . . 4_666 ?
O2 O1 S1 O1 -105.8(5) 2_655 . . 2_655 ?
O2 O1 S1 O1 -40.1(9) 3_665 . . 4_666 ?
O2 O1 S1 O1 168.3(12) 2_655 . . 5_656 ?
O2 O1 S1 O1 172.9(13) 3_665 . . 6_556 ?
O2 O1 S1 O1 1.2(9) 3_665 . . 2_655 ?
O2 O1 S1 O1 -53.1(7) 4_666 . . 6_556 ?
O2 O1 S1 O1 106.0(6) 3_665 . . 3_665 ?
O2 O1 S1 O1 -147.2(6) 2_655 . . 4_666 ?
O2 O1 S1 O1 -1.1(8) 2_655 . . 3_665 ?
O2 O1 S1 O1 -84.7(15) 3_665 . . 5_656 ?
O2 O1 S1 O1 -120.0(14) 4_666 . . 3_665 ?
O2 O1 S1 O1 49.3(7) 4_666 . . 5_656 ?
O2 O1 S1 O2 60.7(10) 4_666 . . 6_556 ?
O2 O1 S1 O2 -179.7(2) 3_665 . . 5_656 ?
O2 O1 S1 O2 -134.0(16) 3_665 . . 4_666 ?
O2 O1 S1 O2 107.0(12) 3_665 . . 2_655 ?
O2 O1 S1 O2 73.3(14) 2_655 . . 5_656 ?
O2 O1 S1 O2 -119.0(12) 4_666 . . 2_655 ?
O2 O1 S1 O2 119.0(12) 2_655 . . 4_666 ?
O2 O1 S1 O2 48.4(8) 3_665 . . . ?
O2 O1 S1 O2 -107.0(12) 2_655 . . 3_665 ?
O2 O1 S1 O2 -58.6(8) 2_655 . . . ?
O2 O1 S1 O2 -45.7(19) 4_666 . . 5_656 ?
O2 O1 S1 O2 -177.6(16) 4_666 . . . ?
O2 O1 S1 O2 134.0(16) 4_666 . . 3_665 ?
O2 O1 S1 O2 179.7(2) 2_655 . . 6_556 ?
O2 O1 S1 O2 -73.3(13) 3_665 . . 6_556 ?
O2 O2 S1 O1 -137.3(10) 3_665 . . 6_556 ?
O2 O2 S1 O1 130.7(15) 3_665 . . 4_666 ?
O2 O2 S1 O1 -124.5(6) 3_665 . . 3_665 ?
O2 O2 S1 O1 123.5(18) 2_655 . . 5_656 ?
O2 O2 S1 O1 46.3(8) 2_655 . . . ?
O2 O2 S1 O1 133.8(7) 2_655 . . 2_655 ?
O2 O2 S1 O1 -149.6(17) 2_655 . . 4_666 ?
O2 O2 S1 O1 -33.4(7) 3_665 . . . ?
O2 O2 S1 O1 43.8(16) 3_665 . . 5_656 ?
O2 O2 S1 O1 -57.5(11) 2_655 . . 6_556 ?
O2 O2 S1 O1 54.1(9) 3_665 . . 2_655 ?
O2 O2 S1 O1 -44.8(9) 2_655 . . 3_665 ?
O2 O2 S1 O2 178.2(12) 3_665 . . 5_656 ?
O2 O2 S1 O2 98.5(11) 3_665 . . 6_556 ?
O2 O2 S1 O2 178.2(12) 2_655 . . 6_556 ?
O2 O2 S1 O2 -102.1(14) 2_655 . . 5_656 ?
O2 O2 S1 O2 79.7(4) 2_655 . . 3_665 ?
O2 O2 S1 O2 -79.7(4) 3_665 . . 2_655 ?

_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 1.391
_oxdiff_exptl_absorpt_empirical_full_min 0.867
####################################################################### 
# 
# 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_p-3
_database_code_depnum_ccdc_archive 'CCDC 2152100'
loop_
_audit_author_name
_audit_author_address
'Cong Wu'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2022-02-15 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_audit_creation_date             2022-02-15
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H24 Mn N6, O4 S'
_chemical_formula_sum            'C6 H24 Mn N6 O4 S'
_chemical_formula_weight         331.31
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'

_cell_length_a                   15.6935(5)
_cell_length_b                   15.6935(5)
_cell_length_c                   9.5255(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2031.69(16)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    2966
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.0440
_cell_measurement_theta_min      4.5010
_shelx_estimated_absorpt_T_max   0.894
_shelx_estimated_absorpt_T_min   0.803
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1050
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10980
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.710
_diffrn_reflns_theta_min         3.967
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -39.00 -13.00   0.50    8.00    --    0.10 -81.00 146.00   52
  2  ω    -89.00   0.00   0.50    8.00    --    0.10 -19.00   0.00  178
  3  ω    -63.00 -38.00   0.50    8.00    --    0.10 -82.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0398034000
_diffrn_orient_matrix_UB_12      -0.0382873000
_diffrn_orient_matrix_UB_13      0.0374074000
_diffrn_orient_matrix_UB_21      -0.0212794000
_diffrn_orient_matrix_UB_22      0.0303137000
_diffrn_orient_matrix_UB_23      0.0085927000
_diffrn_orient_matrix_UB_31      -0.0261998000
_diffrn_orient_matrix_UB_32      -0.0183924000
_diffrn_orient_matrix_UB_33      -0.0638026000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1323
_reflns_number_total             1809
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.632
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1809
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0544
_refine_ls_restrained_S_all      2.011
_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)+(0.0746P)²+3.7126P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1669
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
S1 \\sim O2 \\sim O1: within 2A with sigma of 0.1 and sigma for terminal atoms
of 0.2 within 2A
O1 \\sim S1 \\sim O2: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Uanis(O1) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N1(H1A,H1B), N2(H2A,H2B), C2(H2C,H2D), C1(H1C,H1D), C3(H3C,H3D)
;
_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
Mn1 Mn 0.000000 0.66715(3) 0.250000 0.0096(2) Uani 1 2 d S T P . .
S1 S 0.33562(5) 1.000000 0.250000 0.0110(2) Uani 1 2 d S TU P . .
N3 N 0.04670(16) 0.80189(15) 0.3848(2) 0.0160(4) Uani 1 1 d . . . . .
H3A H 0.029264 0.784336 0.473683 0.019 Uiso 1 1 calc R U . . .
H3B H 0.111719 0.840802 0.381360 0.019 Uiso 1 1 calc R U . . .
N1 N 0.08295(15) 0.60763(16) 0.3731(2) 0.0157(4) Uani 1 1 d . . . . .
H1A H 0.078819 0.616225 0.464633 0.019 Uiso 1 1 calc R U . . .
H1B H 0.057089 0.543544 0.356738 0.019 Uiso 1 1 calc R U . . .
N2 N 0.14383(16) 0.72962(17) 0.1282(2) 0.0178(5) Uani 1 1 d . . . . .
H2A H 0.131931 0.723689 0.036298 0.021 Uiso 1 1 calc R U . . .
H2B H 0.182342 0.793111 0.148156 0.021 Uiso 1 1 calc R U . . .
O2 O 0.25637(16) 0.94789(19) 0.3508(2) 0.0412(6) Uani 1 1 d . U . . .
C2 C 0.19247(19) 0.6737(2) 0.1697(3) 0.0181(5) Uani 1 1 d . . . . .
H2C H 0.260744 0.708598 0.139995 0.022 Uiso 1 1 calc R U . . .
H2D H 0.160182 0.609677 0.124620 0.022 Uiso 1 1 calc R U . . .
C1 C 0.18677(19) 0.6613(2) 0.3278(3) 0.0183(5) Uani 1 1 d . . . . .
H1C H 0.219118 0.625085 0.356078 0.022 Uiso 1 1 calc R U . . .
H1D H 0.220428 0.725353 0.372536 0.022 Uiso 1 1 calc R U . . .
C3 C -0.0025(2) 0.85408(19) 0.3297(3) 0.0189(5) Uani 1 1 d . . . . .
H3C H 0.029441 0.920685 0.366234 0.023 Uiso 1 1 calc R U . . .
H3D H -0.070734 0.820714 0.359728 0.023 Uiso 1 1 calc R U . . .
O1 O 0.3515(3) 0.9288(2) 0.1739(3) 0.0587(7) Uani 1 1 d . 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
Mn1 N3 2.260(2) 6 ?
Mn1 N3 2.260(2) . ?
Mn1 N1 2.271(2) . ?
Mn1 N1 2.271(2) 6 ?
Mn1 N2 2.278(2) . ?
Mn1 N2 2.278(2) 6 ?
S1 O2 1.456(2) . ?
S1 O2 1.456(2) 5_675 ?
S1 O1 1.454(2) . ?
S1 O1 1.454(2) 5_675 ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C3 1.475(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.476(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.476(3) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C1 1.516(4) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C3 C3 1.520(5) 6 ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Mn1 N3 78.66(11) 6 . ?
N3 Mn1 N1 166.54(8) . 6 ?
N3 Mn1 N1 96.15(8) . . ?
N3 Mn1 N1 96.15(8) 6 6 ?
N3 Mn1 N1 166.54(8) 6 . ?
N3 Mn1 N2 90.11(7) . 6 ?
N3 Mn1 N2 95.67(9) . . ?
N3 Mn1 N2 90.11(7) 6 . ?
N3 Mn1 N2 95.67(9) 6 6 ?
N1 Mn1 N1 91.48(11) 6 . ?
N1 Mn1 N2 77.97(8) 6 6 ?
N1 Mn1 N2 77.97(8) . . ?
N1 Mn1 N2 96.76(8) 6 . ?
N1 Mn1 N2 96.76(8) . 6 ?
N2 Mn1 N2 172.54(11) 6 . ?
O2 S1 O2 110.0(2) 5_675 . ?
O1 S1 O2 108.88(16) . . ?
O1 S1 O2 108.28(14) 5_675 . ?
O1 S1 O2 108.28(14) . 5_675 ?
O1 S1 O2 108.89(16) 5_675 5_675 ?
O1 S1 O1 112.5(3) . 5_675 ?
Mn1 N3 H3A 110.2 . . ?
Mn1 N3 H3B 110.2 . . ?
H3A N3 H3B 108.5 . . ?
C3 N3 Mn1 107.61(14) . . ?
C3 N3 H3A 110.2 . . ?
C3 N3 H3B 110.2 . . ?
Mn1 N1 H1A 110.1 . . ?
Mn1 N1 H1B 110.1 . . ?
H1A N1 H1B 108.4 . . ?
C1 N1 Mn1 108.12(14) . . ?
C1 N1 H1A 110.1 . . ?
C1 N1 H1B 110.1 . . ?
Mn1 N2 H2A 110.2 . . ?
Mn1 N2 H2B 110.2 . . ?
H2A N2 H2B 108.5 . . ?
C2 N2 Mn1 107.66(15) . . ?
C2 N2 H2A 110.2 . . ?
C2 N2 H2B 110.2 . . ?
N2 C2 H2C 109.9 . . ?
N2 C2 H2D 109.9 . . ?
N2 C2 C1 109.12(19) . . ?
H2C C2 H2D 108.3 . . ?
C1 C2 H2C 109.9 . . ?
C1 C2 H2D 109.9 . . ?
N1 C1 C2 109.94(19) . . ?
N1 C1 H1C 109.7 . . ?
N1 C1 H1D 109.7 . . ?
C2 C1 H1C 109.7 . . ?
C2 C1 H1D 109.7 . . ?
H1C C1 H1D 108.2 . . ?
N3 C3 C3 109.56(17) . 6 ?
N3 C3 H3C 109.8 . . ?
N3 C3 H3D 109.8 . . ?
C3 C3 H3C 109.8 6 . ?
C3 C3 H3D 109.8 6 . ?
H3C C3 H3D 108.2 . . ?

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
Mn1 N3 C3 C3 -43.1(3) . . . 6 ?
Mn1 N1 C1 C2 -42.1(2) . . . . ?
Mn1 N2 C2 C1 -44.4(2) . . . . ?
N2 C2 C1 N1 59.9(3) . . . . ?

_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 12.268
_oxdiff_exptl_absorpt_empirical_full_min 0.623
####################################################################### 
# 
# 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_p-31c_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2152099'
loop_
_audit_author_name
_audit_author_address
'Cong Wu'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2022-02-16 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_audit_creation_date             2022-02-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H24 Mn1 N6, O4 S1'
_chemical_formula_sum            'C6 H24 Mn N6 O4 S'
_chemical_formula_weight         331.31
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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      trigonal
_space_group_IT_number           163
_space_group_name_H-M_alt        'P -3 1 c'
_space_group_name_Hall           '-P 3 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   9.0947(4)
_cell_length_b                   9.0947(4)
_cell_length_c                   9.5725(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     685.70(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2218
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.7850
_cell_measurement_theta_min      4.4990
_shelx_estimated_absorpt_T_max   0.895
_shelx_estimated_absorpt_T_min   0.805
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             350
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3906
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.529
_diffrn_reflns_theta_min         4.258
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -37.00  -9.00   0.50    3.00    --    0.10 -43.00-127.00   56
  2  ω    -63.00  30.00   0.50    3.00    --    0.10 -82.00-120.00  186
  3  ω    -53.00 -28.00   0.50    3.00    --    0.10 -82.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                552
_reflns_number_total             608
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         608
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0290
_refine_ls_restrained_S_all      1.115
_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)+(0.0439P)²+0.1754P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0788
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Others
 Fixed Sof: O1(0.33333) O2(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Mn1 Mn 0.666667 0.333333 0.250000 0.02263(19) Uani 1 6 d S T P . .
N1 N 0.69510(18) 0.55724(18) 0.37605(13) 0.0350(3) Uani 1 1 d . . . . .
H1A H 0.605262 0.570089 0.363078 0.042 Uiso 1 1 calc R U . . .
H1B H 0.702636 0.539920 0.466624 0.042 Uiso 1 1 calc R U . . .
C1 C 0.8498(2) 0.7095(2) 0.32902(18) 0.0389(4) Uani 1 1 d . . . . .
H1C H 0.948684 0.711075 0.368840 0.047 Uiso 1 1 calc R U . . .
H1D H 0.848598 0.810275 0.360429 0.047 Uiso 1 1 calc R U . . .
S1 S 0.666667 0.333333 0.750000 0.0236(2) Uani 1 6 d S T P . .
O1 O 0.5543(12) 0.2184(8) 0.8555(6) 0.094(3) Uani 0.3333 1 d . . P A -1
O2 O 0.5145(11) 0.308(2) 0.8130(7) 0.129(4) Uani 0.3333 1 d . . P A -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 N1 2.2678(13) 6 ?
Mn1 N1 2.2679(13) 4_665 ?
Mn1 N1 2.2678(13) . ?
Mn1 N1 2.2678(13) 3_665 ?
Mn1 N1 2.2678(13) 5_655 ?
Mn1 N1 2.2678(13) 2_655 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.467(2) . ?
C1 C1 1.515(3) 5_655 ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
S1 O1 1.445(5) . ?
S1 O2 1.419(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
N1 Mn1 N1 77.91(7) 6 3_665 ?
N1 Mn1 N1 77.91(7) 5_655 . ?
N1 Mn1 N1 94.32(5) 5_655 4_665 ?
N1 Mn1 N1 94.32(5) 6 5_655 ?
N1 Mn1 N1 94.32(5) 6 4_665 ?
N1 Mn1 N1 94.49(7) 3_665 5_655 ?
N1 Mn1 N1 94.32(5) 3_665 . ?
N1 Mn1 N1 94.49(7) 6 2_655 ?
N1 Mn1 N1 94.32(5) 2_655 . ?
N1 Mn1 N1 94.32(5) 3_665 2_655 ?
N1 Mn1 N1 168.67(7) 3_665 4_665 ?
N1 Mn1 N1 168.66(7) 5_655 2_655 ?
N1 Mn1 N1 94.48(7) . 4_665 ?
N1 Mn1 N1 168.67(7) 6 . ?
N1 Mn1 N1 77.91(7) 2_655 4_665 ?
Mn1 N1 H1A 110.1 . . ?
Mn1 N1 H1B 110.1 . . ?
H1A N1 H1B 108.4 . . ?
C1 N1 Mn1 108.01(10) . . ?
C1 N1 H1A 110.1 . . ?
C1 N1 H1B 110.1 . . ?
N1 C1 C1 109.58(11) . 5_655 ?
N1 C1 H1C 109.8 . . ?
N1 C1 H1D 109.8 . . ?
C1 C1 H1C 109.8 5_655 . ?
C1 C1 H1D 109.8 5_655 . ?
H1C C1 H1D 108.2 . . ?

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
Mn1 N1 C1 C1 43.07(19) . . . 5_655 ?

_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
;
####################################################################### 
# 
# 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_p-31c_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2152101'
loop_
_audit_author_name
_audit_author_address
'Cong Wu'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2022-02-16 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_audit_creation_date             2022-02-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H24 Cd1 N6, O4 S1'
_chemical_formula_sum            'C6 H24 Cd N6 O4 S'
_chemical_formula_weight         388.77
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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      trigonal
_space_group_IT_number           163
_space_group_name_H-M_alt        'P -3 1 c'
_space_group_name_Hall           '-P 3 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   9.1957(3)
_cell_length_b                   9.1957(3)
_cell_length_c                   9.5096(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     696.41(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2774
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.0360
_cell_measurement_theta_min      4.4470
_shelx_estimated_absorpt_T_max   0.846
_shelx_estimated_absorpt_T_min   0.723
_exptl_absorpt_coefficient_mu    1.736
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3093
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.692
_diffrn_reflns_theta_min         4.286
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -34.00  -8.00   0.50    2.00    --    0.10 -29.00-171.00   52
  2  ω    -33.00  29.00   0.50    2.00    --    0.10 -77.00-150.00  124
  3  ω    -24.00   3.00   0.50    2.00    --    0.10 -82.00 120.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                597
_reflns_number_total             617
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         617
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0294
_refine_ls_restrained_S_all      1.067
_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)+(0.0554P)²+0.1381P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0756
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Others
 Fixed Sof: O1(0.33333) O2(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Cd1 Cd 0.666667 0.333333 0.750000 0.02541(17) Uani 1 6 d S T P . .
N1 N 0.6973(3) 0.5671(3) 0.6218(2) 0.0365(4) Uani 1 1 d . . . . .
H1A H 0.704147 0.551761 0.530147 0.044 Uiso 1 1 calc R U . . .
H1B H 0.609619 0.581241 0.636546 0.044 Uiso 1 1 calc R U . . .
C1 C 0.8519(4) 0.7140(3) 0.6712(2) 0.0392(5) Uani 1 1 d . . . . .
H1C H 0.854420 0.815572 0.639928 0.047 Uiso 1 1 calc R U . . .
H1D H 0.948310 0.712612 0.631239 0.047 Uiso 1 1 calc R U . . .
S1 S 0.666667 0.333333 0.250000 0.0245(3) Uani 1 6 d S T P . .
O1 O 0.7764(14) 0.447(2) 0.3569(13) 0.111(6) Uani 0.3333 1 d . . P A -2
O2 O 0.696(3) 0.4881(16) 0.3048(12) 0.119(6) Uani 0.3333 1 d . . P A -1


_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
Cd1 N1 2.362(2) 3_665 ?
Cd1 N1 2.362(2) 4_666 ?
Cd1 N1 2.362(2) . ?
Cd1 N1 2.362(2) 6_556 ?
Cd1 N1 2.362(2) 2_655 ?
Cd1 N1 2.362(2) 5_656 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.465(4) . ?
C1 C1 1.501(5) 5_656 ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
S1 O1 1.445(9) . ?
S1 O2 1.410(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N1 76.00(11) 3_665 6_556 ?
N1 Cd1 N1 95.76(8) 2_655 . ?
N1 Cd1 N1 76.00(11) 2_655 4_666 ?
N1 Cd1 N1 95.76(8) 3_665 2_655 ?
N1 Cd1 N1 168.14(11) 3_665 4_666 ?
N1 Cd1 N1 93.58(12) 6_556 2_655 ?
N1 Cd1 N1 168.14(11) 6_556 . ?
N1 Cd1 N1 93.58(12) 3_665 5_656 ?
N1 Cd1 N1 76.00(11) 5_656 . ?
N1 Cd1 N1 95.76(8) 6_556 5_656 ?
N1 Cd1 N1 95.76(8) 6_556 4_666 ?
N1 Cd1 N1 168.14(11) 2_655 5_656 ?
N1 Cd1 N1 93.58(12) . 4_666 ?
N1 Cd1 N1 95.76(8) 3_665 . ?
N1 Cd1 N1 95.76(8) 5_656 4_666 ?
Cd1 N1 H1A 110.3 . . ?
Cd1 N1 H1B 110.3 . . ?
H1A N1 H1B 108.6 . . ?
C1 N1 Cd1 107.01(16) . . ?
C1 N1 H1A 110.3 . . ?
C1 N1 H1B 110.3 . . ?
N1 C1 C1 110.58(18) . 5_656 ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
C1 C1 H1C 109.5 5_656 . ?
C1 C1 H1D 109.5 5_656 . ?
H1C C1 H1D 108.1 . . ?

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
Cd1 N1 C1 C1 -44.5(3) . . . 5_656 ?

_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
;
####################################################################### 
# 
# 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_p
_database_code_depnum_ccdc_archive 'CCDC 2152098'
loop_
_audit_author_name
_audit_author_address
'Cong Wu'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2022-02-15 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_audit_creation_date             2022-02-15
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H24 N6 Ni1, O4 S1'
_chemical_formula_sum            'C6 H24 N6 Ni O4 S'
_chemical_formula_weight         335.08
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   8.8526(4)
_cell_length_b                   8.8526(4)
_cell_length_c                   9.6749(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     656.63(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2452
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      29.7690
_cell_measurement_theta_min      4.6050
_shelx_estimated_absorpt_T_max   0.637
_shelx_estimated_absorpt_T_min   0.557
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             356
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3355
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.737
_diffrn_reflns_theta_min         4.213
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -79.00 -39.00   0.50    1.00    --    0.10 -63.00  52.00   80
  2  ω    -63.00  -1.00   0.50    1.00    --    0.10 -82.00 150.00  124
  3  ω     -9.00  16.00   0.50    1.00    --    0.10 -82.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0858847000
_diffrn_orient_matrix_UB_12      -0.0348713000
_diffrn_orient_matrix_UB_13      -0.0262593000
_diffrn_orient_matrix_UB_21      0.0328269000
_diffrn_orient_matrix_UB_22      0.0586268000
_diffrn_orient_matrix_UB_23      -0.0566110000
_diffrn_orient_matrix_UB_31      0.0102594000
_diffrn_orient_matrix_UB_32      -0.0624887000
_diffrn_orient_matrix_UB_33      -0.0384872000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1088
_reflns_number_total             1095
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1095
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0376
_refine_ls_restrained_S_all      1.125
_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)+(0.0348P)²+1.4366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.0992
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.699(3)
 0.301(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
3. Uiso/Uaniso restraints and constraints
O1 \\sim O2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
4. Rigid body (RIGU) restrains
 O2, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 S1, O1, O2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), C2(H2C,H2D), C1(H1C,H1D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.666667 0.333333 0.23732(9) 0.00812(18) Uani 1 3 d S T P . .
N2 N 0.8671(4) 0.5383(4) 0.1190(3) 0.0141(6) Uani 1 1 d . . . . .
H2A H 0.967522 0.539693 0.130699 0.017 Uiso 1 1 calc R U . . .
H2B H 0.839869 0.522697 0.029606 0.017 Uiso 1 1 calc R U . . .
N1 N 0.6975(4) 0.5462(4) 0.3607(3) 0.0163(6) Uani 1 1 d . . . . .
H1A H 0.610947 0.567546 0.344407 0.020 Uiso 1 1 calc R U . . .
H1B H 0.696069 0.521337 0.449997 0.020 Uiso 1 1 calc R U . . .
O1 O 0.6853(4) 0.1866(4) 0.8088(3) 0.0309(7) Uani 1 1 d . . . . .
C2 C 0.8835(5) 0.7045(4) 0.1673(4) 0.0165(7) Uani 1 1 d . . . . .
H2C H 0.792975 0.720917 0.125764 0.020 Uiso 1 1 calc R U . . .
H2D H 0.995838 0.801350 0.140051 0.020 Uiso 1 1 calc R U . . .
C1 C 0.8664(5) 0.6994(5) 0.3236(4) 0.0175(7) Uani 1 1 d . . . . .
H1C H 0.961179 0.690626 0.365681 0.021 Uiso 1 1 calc R U . . .
H1D H 0.871404 0.805294 0.356600 0.021 Uiso 1 1 calc R U . . .
O2 O 0.666667 0.333333 0.6059(5) 0.0466(16) Uani 1 3 d S T P . .
S1 S 0.666667 0.333333 0.75472(15) 0.0105(3) Uani 1 3 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 2.128(3) 3_665 ?
Ni1 N2 2.128(3) . ?
Ni1 N2 2.128(3) 2_655 ?
Ni1 N1 2.130(3) 3_665 ?
Ni1 N1 2.130(3) 2_655 ?
Ni1 N1 2.130(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.481(5) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.476(4) . ?
O1 S1 1.485(3) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C1 1.518(5) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
O2 S1 1.440(5) . ?

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
N2 Ni1 N2 93.80(11) 3_665 . ?
N2 Ni1 N2 93.80(11) 3_665 2_655 ?
N2 Ni1 N2 93.80(11) . 2_655 ?
N2 Ni1 N1 92.80(11) 3_665 2_655 ?
N2 Ni1 N1 82.18(11) . . ?
N2 Ni1 N1 82.18(11) 2_655 2_655 ?
N2 Ni1 N1 172.49(11) . 2_655 ?
N2 Ni1 N1 82.18(11) 3_665 3_665 ?
N2 Ni1 N1 172.49(11) 3_665 . ?
N2 Ni1 N1 92.80(11) . 3_665 ?
N2 Ni1 N1 172.49(11) 2_655 3_665 ?
N2 Ni1 N1 92.80(11) 2_655 . ?
N1 Ni1 N1 91.65(12) 3_665 . ?
N1 Ni1 N1 91.65(12) 3_665 2_655 ?
N1 Ni1 N1 91.65(12) 2_655 . ?
Ni1 N2 H2A 110.2 . . ?
Ni1 N2 H2B 110.2 . . ?
H2A N2 H2B 108.5 . . ?
C2 N2 Ni1 107.6(2) . . ?
C2 N2 H2A 110.2 . . ?
C2 N2 H2B 110.2 . . ?
Ni1 N1 H1A 110.2 . . ?
Ni1 N1 H1B 110.2 . . ?
H1A N1 H1B 108.5 . . ?
C1 N1 Ni1 107.4(2) . . ?
C1 N1 H1A 110.2 . . ?
C1 N1 H1B 110.2 . . ?
N2 C2 H2C 109.9 . . ?
N2 C2 H2D 109.9 . . ?
N2 C2 C1 109.0(3) . . ?
H2C C2 H2D 108.3 . . ?
C1 C2 H2C 109.9 . . ?
C1 C2 H2D 109.9 . . ?
N1 C1 C2 108.0(3) . . ?
N1 C1 H1C 110.1 . . ?
N1 C1 H1D 110.1 . . ?
C2 C1 H1C 110.1 . . ?
C2 C1 H1D 110.1 . . ?
H1C C1 H1D 108.4 . . ?
O1 S1 O1 108.28(14) . 3_665 ?
O1 S1 O1 108.29(14) . 2_655 ?
O1 S1 O1 108.28(14) 2_655 3_665 ?
O2 S1 O1 110.63(13) . 3_665 ?
O2 S1 O1 110.63(13) . . ?
O2 S1 O1 110.63(13) . 2_655 ?

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 N2 C2 C1 40.2(3) . . . . ?
Ni1 N1 C1 C2 43.5(3) . . . . ?
N2 C2 C1 N1 -57.1(4) . . . . ?

_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 1.323
_oxdiff_exptl_absorpt_empirical_full_min 0.869
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.699(3)
2 0.301(3)

####################################################################### 
# 
# 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_cdso4-140k
_database_code_depnum_ccdc_archive 'CCDC 2152102'
loop_
_audit_author_name
_audit_author_address
'Cong Wu'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2022-02-15 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_audit_creation_date             2022-02-15
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H24 Cd1 N6, O4 S1'
_chemical_formula_sum            'C6 H24 Cd N6 O4 S'
_chemical_formula_weight         388.77
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   9.1148(4)
_cell_length_b                   9.1148(4)
_cell_length_c                   9.5425(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     686.57(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3025
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      29.7640
_cell_measurement_theta_min      4.9340
_shelx_estimated_absorpt_T_max   0.844
_shelx_estimated_absorpt_T_min   0.720
_exptl_absorpt_coefficient_mu    1.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3365
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.385
_diffrn_reflns_theta_min         4.271
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     33.00  90.00   0.50    5.00    --    0.10  73.00  32.00  114
  2  ω    -46.00  26.00   0.50    5.00    --    0.10 -77.00   0.00  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0858065000
_diffrn_orient_matrix_UB_12      0.0238417000
_diffrn_orient_matrix_UB_13      0.0124431000
_diffrn_orient_matrix_UB_21      0.0261677000
_diffrn_orient_matrix_UB_22      0.0648341000
_diffrn_orient_matrix_UB_23      -0.0511343000
_diffrn_orient_matrix_UB_31      0.0051253000
_diffrn_orient_matrix_UB_32      0.0574949000
_diffrn_orient_matrix_UB_33      0.0524674000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1126
_reflns_number_total             1144
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.574
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.181
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1144
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0474
_refine_ls_restrained_S_all      1.150
_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)+(0.0526P)²+3.5139P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1156
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9572(17)
 0.0428(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), C2(H2C,H2D), C1(H1C,H1D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.666667 0.333333 0.77129(6) 0.01260(19) Uani 1 3 d S T P . .
S1 S 0.666667 0.333333 0.2483(2) 0.0120(3) Uani 1 3 d S T P . .
N2 N 0.4316(5) 0.1403(5) 0.6343(5) 0.0199(8) Uani 1 1 d . . . . .
H2A H 0.454568 0.161611 0.543520 0.024 Uiso 1 1 calc R U . . .
H2B H 0.407009 0.034410 0.651394 0.024 Uiso 1 1 calc R U . . .
N1 N 0.4329(5) 0.3192(5) 0.8885(4) 0.0177(8) Uani 1 1 d . . . . .
H1A H 0.441293 0.307772 0.980303 0.021 Uiso 1 1 calc R U . . .
H1B H 0.428666 0.413367 0.873586 0.021 Uiso 1 1 calc R U . . .
C2 C 0.2888(6) 0.1633(7) 0.6739(6) 0.0213(10) Uani 1 1 d . . . . .
H2C H 0.183994 0.069597 0.638425 0.026 Uiso 1 1 calc R U . . .
H2D H 0.303336 0.267163 0.632865 0.026 Uiso 1 1 calc R U . . .
O2 O 0.5072(6) 0.3173(7) 0.1958(6) 0.0401(11) Uani 1 1 d . . . . .
C1 C 0.2800(6) 0.1717(6) 0.8329(6) 0.0206(9) Uani 1 1 d . . . . .
H1C H 0.181038 0.179110 0.859026 0.025 Uiso 1 1 calc R U . . .
H1D H 0.268589 0.068973 0.873626 0.025 Uiso 1 1 calc R U . . .
O1 O 0.666667 0.333333 0.3987(9) 0.053(2) Uani 1 3 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N2 2.372(4) 2_655 ?
Cd1 N2 2.372(4) . ?
Cd1 N2 2.372(4) 3_665 ?
Cd1 N1 2.352(4) 2_655 ?
Cd1 N1 2.352(4) 3_665 ?
Cd1 N1 2.352(4) . ?
S1 O2 1.474(4) 3_665 ?
S1 O2 1.474(4) . ?
S1 O2 1.474(4) 2_655 ?
S1 O1 1.435(8) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.467(6) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.469(6) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C1 1.524(7) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cd1 N2 92.56(15) . 3_665 ?
N2 Cd1 N2 92.55(15) 2_655 . ?
N2 Cd1 N2 92.56(15) 2_655 3_665 ?
N1 Cd1 N2 92.54(15) 2_655 . ?
N1 Cd1 N2 167.96(15) 2_655 3_665 ?
N1 Cd1 N2 92.54(15) 3_665 2_655 ?
N1 Cd1 N2 76.33(14) 3_665 3_665 ?
N1 Cd1 N2 167.96(15) . 2_655 ?
N1 Cd1 N2 76.33(14) 2_655 2_655 ?
N1 Cd1 N2 167.96(15) 3_665 . ?
N1 Cd1 N2 76.33(14) . . ?
N1 Cd1 N2 92.54(15) . 3_665 ?
N1 Cd1 N1 99.26(13) 2_655 3_665 ?
N1 Cd1 N1 99.26(13) 3_665 . ?
N1 Cd1 N1 99.26(13) 2_655 . ?
O2 S1 O2 109.1(2) 2_655 3_665 ?
O2 S1 O2 109.1(2) 2_655 . ?
O2 S1 O2 109.1(2) 3_665 . ?
O1 S1 O2 109.9(2) . 2_655 ?
O1 S1 O2 109.9(2) . 3_665 ?
O1 S1 O2 109.9(2) . . ?
Cd1 N2 H2A 110.4 . . ?
Cd1 N2 H2B 110.4 . . ?
H2A N2 H2B 108.6 . . ?
C2 N2 Cd1 106.8(3) . . ?
C2 N2 H2A 110.4 . . ?
C2 N2 H2B 110.4 . . ?
Cd1 N1 H1A 110.3 . . ?
Cd1 N1 H1B 110.3 . . ?
H1A N1 H1B 108.5 . . ?
C1 N1 Cd1 107.3(3) . . ?
C1 N1 H1A 110.3 . . ?
C1 N1 H1B 110.3 . . ?
N2 C2 H2C 109.7 . . ?
N2 C2 H2D 109.7 . . ?
N2 C2 C1 109.6(4) . . ?
H2C C2 H2D 108.2 . . ?
C1 C2 H2C 109.7 . . ?
C1 C2 H2D 109.7 . . ?
N1 C1 C2 110.8(4) . . ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C2 C1 H1D 109.5 . . ?
H1C C1 H1D 108.1 . . ?

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
Cd1 N2 C2 C1 -45.5(4) . . . . ?
Cd1 N1 C1 C2 -43.6(4) . . . . ?
N2 C2 C1 N1 63.0(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 9.275
_oxdiff_exptl_absorpt_empirical_full_min 0.617
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9572(17)
2 0.0428(17)

