Synthesis of a series of novel In(III) 2,6-diacetylpyridine bis(thiosemicarbazide) complexes: structure, anticancer function and mechanism.
Li, Shanhe; Khan, Muhammad Hamid; Wang, Xiaojun; Cai, Meiling; Zhang, Juzheng; Jiang, Ming; Zhang, Zhenlei; Wen, Xiao-An; Liang, Hong; Yang, Feng; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17207–17220; doi:10.1039/d0dt02266g

data_7706060
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -12.00  88.00   1.00    9.00    --   17.77  77.00 -30.00  100
  2  \w    -50.00  50.00   1.00    9.00    --  -19.72  77.00  90.00  100
  3  \w    -50.00  50.00   1.00    9.00    --  -19.72  77.00 -30.00  100
  4  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0267P)^2^+5.3085P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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)
;
_shelx_res_checksum              15569
_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