#------------------------------------------------------------------------------
#$Date: 2020-12-19 05:06:01 +0200 (Sat, 19 Dec 2020) $
#$Revision: 259981 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/60/7706060.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7706060
loop_
_publ_author_name
'Li, Shanhe'
'Khan, Muhammad Hamid'
'Wang, Xiaojun'
'Cai, Meiling'
'Zhang, Juzheng'
'Jiang, Ming'
'Zhang, Zhenlei'
'Wen, Xiao-An'
'Liang, Hong'
'Yang, Feng'
_publ_section_title
;
 Synthesis of a series of novel In(III) 2,6-diacetylpyridine
 bis(thiosemicarbazide) complexes: structure, anticancer function and
 mechanism.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17207
_journal_page_last               17220
_journal_paper_doi               10.1039/d0dt02266g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C15 H22 Cl2 In N7 S2, C H4 O'
_chemical_formula_sum            'C16 H26 Cl2 In N7 O S2'
_chemical_formula_weight         582.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-28 deposited with the CCDC.	2020-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.698(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7761(3)
_cell_length_b                   14.2179(6)
_cell_length_c                   16.7170(11)
_cell_measurement_reflns_used    1966
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.7690
_cell_measurement_theta_min      3.7560
_cell_volume                     2296.9(2)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00  88.00   1.00    9.00    --   17.77  77.00 -30.00  100
  2  ω    -50.00  50.00   1.00    9.00    --  -19.72  77.00  90.00  100
  3  ω    -50.00  50.00   1.00    9.00    --  -19.72  77.00 -30.00  100
  4  ω    -49.00 -14.00   1.00    9.00    --  -19.72  77.00-150.00   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0658401000
_diffrn_orient_matrix_UB_12      -0.0206542000
_diffrn_orient_matrix_UB_13      0.0124665000
_diffrn_orient_matrix_UB_21      -0.0313096000
_diffrn_orient_matrix_UB_22      -0.0450306000
_diffrn_orient_matrix_UB_23      -0.0004764000
_diffrn_orient_matrix_UB_31      0.0087924000
_diffrn_orient_matrix_UB_32      -0.0057183000
_diffrn_orient_matrix_UB_33      -0.0410605000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7683
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.883
_diffrn_reflns_theta_min         3.762
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.466
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85779
_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_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2683
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.332
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0485
_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)+(0.0267P)²+5.3085P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2183
_reflns_number_total             2683
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02266g2.cif
_cod_data_source_block           20191230-yf-cml-1
_cod_database_code               7706060
_shelx_shelxl_version_number     2018/3
_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.
;
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H5A-H1A
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H3(0.5) O1(0.5) H1A(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5)
6.a Riding coordinates:
 C5(H5A,H5B,H5C), O1(H1A)
6.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_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 1.180
_oxdiff_exptl_absorpt_empirical_full_min 0.910
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
In1 In 0.500000 0.63949(3) 0.750000 0.02974(16) Uani 1 2 d S TU P . .
Cl1 Cl 0.65624(14) 0.62429(9) 0.64275(9) 0.0495(4) Uani 1 1 d . U . . .
S02 S 0.37108(13) 0.78073(9) 0.67374(9) 0.0440(4) Uani 1 1 d . U . . .
N1 N 0.500000 0.4778(4) 0.750000 0.0348(13) Uani 1 2 d S TU P . .
N2 N 0.3089(4) 0.5770(3) 0.6600(2) 0.0331(9) Uani 1 1 d . U . . .
N3 N 0.2112(4) 0.6330(3) 0.6163(2) 0.0404(10) Uani 1 1 d . U . . .
H3 H 0.139151 0.609150 0.587560 0.049 Uiso 0.5 1 calc R . . . .
N4 N 0.1328(4) 0.7774(3) 0.5746(3) 0.0455(11) Uani 1 1 d . U . . .
C1 C 0.500000 0.2853(6) 0.750000 0.062(2) Uani 1 2 d S TU P . .
H1 H 0.499999 0.219878 0.750002 0.074 Uiso 1 2 calc RS T P . .
C2 C 0.3952(6) 0.3328(4) 0.7030(4) 0.0525(15) Uani 1 1 d . U . . .
H2 H 0.322956 0.300498 0.672166 0.063 Uiso 1 1 calc R . . . .
C3 C 0.3997(5) 0.4307(3) 0.7028(3) 0.0397(11) Uani 1 1 d . U . . .
C4 C 0.2959(5) 0.4880(4) 0.6507(3) 0.0410(12) Uani 1 1 d . U . . .
C5 C 0.1808(6) 0.4434(4) 0.5931(4) 0.0691(19) Uani 1 1 d . U . . .
H5A H 0.091273 0.460483 0.605511 0.104 Uiso 1 1 d DR . . . .
H5B H 0.188503 0.463183 0.539061 0.104 Uiso 1 1 d R . . . .
H5C H 0.192053 0.376483 0.597261 0.104 Uiso 1 1 d R . . . .
C6 C 0.2313(5) 0.7266(4) 0.6197(3) 0.0385(11) Uani 1 1 d . U . . .
C7 C 0.1428(6) 0.8786(4) 0.5691(4) 0.0596(16) Uani 1 1 d . U . . .
H7A H 0.133195 0.906128 0.620415 0.089 Uiso 1 1 calc GR . . . .
H7B H 0.070692 0.901496 0.528440 0.089 Uiso 1 1 calc GR . . . .
H7C H 0.231246 0.895224 0.554955 0.089 Uiso 1 1 calc GR . . . .
C8 C 0.0117(6) 0.7314(5) 0.5282(4) 0.0656(18) Uani 1 1 d . U . . .
H8A H 0.041128 0.690939 0.488117 0.098 Uiso 1 1 calc GR . . . .
H8B H -0.050165 0.778301 0.502138 0.098 Uiso 1 1 calc GR . . . .
H8C H -0.034987 0.694842 0.564133 0.098 Uiso 1 1 calc GR . . . .
O1 O -0.0368(8) 0.5594(6) 0.6543(6) 0.071(3) Uani 0.5 1 d . U . . .
H1A H -0.115670 0.580643 0.646169 0.107 Uiso 0.5 1 d DR . . A .
C9 C -0.015(4) 0.5238(8) 0.7356(16) 0.068(6) Uani 0.5 1 d . U . A -1
H9A H -0.055480 0.462471 0.736681 0.102 Uiso 0.5 1 calc GR . . A -1
H9B H -0.056579 0.565466 0.770056 0.102 Uiso 0.5 1 calc GR . . A -1
H9C H 0.082886 0.519648 0.754536 0.102 Uiso 0.5 1 calc GR . . A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 In1 Cl1 170.22(6) . 2_656 ?
Cl1 In1 S02 96.51(5) . 2_656 ?
Cl1 In1 S02 91.05(4) 2_656 2_656 ?
Cl1 In1 S02 96.51(5) 2_656 . ?
Cl1 In1 S02 91.05(4) . . ?
S02 In1 S02 78.87(6) . 2_656 ?
N1 In1 Cl1 85.11(3) . 2_656 ?
N1 In1 Cl1 85.11(3) . . ?
N1 In1 S02 140.56(3) . 2_656 ?
N1 In1 S02 140.57(3) . . ?
N1 In1 N2 68.14(10) . 2_656 ?
N1 In1 N2 68.14(10) . . ?
N2 In1 Cl1 91.16(9) 2_656 2_656 ?
N2 In1 Cl1 85.20(9) . 2_656 ?
N2 In1 Cl1 91.16(9) . . ?
N2 In1 Cl1 85.19(9) 2_656 . ?
N2 In1 S02 72.73(10) . . ?
N2 In1 S02 150.69(10) . 2_656 ?
N2 In1 S02 150.69(10) 2_656 . ?
N2 In1 S02 72.73(10) 2_656 2_656 ?
N2 In1 N2 136.3(2) 2_656 . ?
C6 S02 In1 101.65(19) . . ?
C3 N1 In1 120.0(3) . . ?
C3 N1 In1 120.0(3) 2_656 . ?
C3 N1 C3 120.0(6) 2_656 . ?
N3 N2 In1 122.5(3) . . ?
C4 N2 In1 120.0(3) . . ?
C4 N2 N3 117.5(4) . . ?
N2 N3 H3 121.1 . . ?
C6 N3 N2 117.9(4) . . ?
C6 N3 H3 121.1 . . ?
C6 N4 C7 121.4(5) . . ?
C6 N4 C8 120.7(5) . . ?
C7 N4 C8 117.8(5) . . ?
C2 C1 H1 119.5 2_656 . ?
C2 C1 H1 119.5 . . ?
C2 C1 C2 121.0(7) 2_656 . ?
C1 C2 H2 120.9 . . ?
C1 C2 C3 118.2(6) . . ?
C3 C2 H2 120.9 . . ?
N1 C3 C2 121.3(5) . . ?
N1 C3 C4 116.5(4) . . ?
C2 C3 C4 122.2(5) . . ?
N2 C4 C3 115.3(5) . . ?
N2 C4 C5 123.1(5) . . ?
C3 C4 C5 121.7(5) . . ?
C4 C5 H5A 111.9 . . ?
C4 C5 H5B 108.7 . . ?
C4 C5 H5C 107.7 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 S02 124.7(4) . . ?
N4 C6 S02 120.4(4) . . ?
N4 C6 N3 114.9(5) . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 O1 H1A 106.8 . . ?
O1 C9 H9A 109.5 . . ?
O1 C9 H9B 109.5 . . ?
O1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
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
In1 Cl1 2.5343(12) . ?
In1 Cl1 2.5344(12) 2_656 ?
In1 S02 2.6001(14) 2_656 ?
In1 S02 2.6001(14) . ?
In1 N1 2.298(5) . ?
In1 N2 2.386(4) 2_656 ?
In1 N2 2.386(4) . ?
S02 C6 1.703(5) . ?
N1 C3 1.341(6) 2_656 ?
N1 C3 1.341(6) . ?
N2 N3 1.367(5) . ?
N2 C4 1.279(6) . ?
N3 H3 0.8600 . ?
N3 C6 1.346(6) . ?
N4 C6 1.340(6) . ?
N4 C7 1.446(7) . ?
N4 C8 1.467(7) . ?
C1 H1 0.9300 . ?
C1 C2 1.371(7) . ?
C1 C2 1.371(7) 2_656 ?
C2 H2 0.9300 . ?
C2 C3 1.392(7) . ?
C3 C4 1.479(7) . ?
C4 C5 1.505(7) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9602 . ?
C5 H5C 0.9597 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
O1 H1A 0.8200 . ?
O1 C9 1.44(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
