#------------------------------------------------------------------------------
#$Date: 2019-11-16 06:31:23 +0200 (Sat, 16 Nov 2019) $
#$Revision: 227936 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/90/7059057.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_7059057
loop_
_publ_author_name
'Jin, Jinjin'
'Hu, Jiyong'
'Qin, Yue'
'Zhang, Junshuai'
'Zhao, Jin'an'
'Yue, Liang'
'Hou, Hongwei'
_publ_section_title
;
 In vitro and in vivo anticancer activity of thiourea tripyridyl dinuclear
 Cu(II) complex
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/C9NJ03371H
_journal_year                    2019
_chemical_formula_moiety         'C34 H26 Cu2 I2 N12 S2, 2(C2 H3 N)'
_chemical_formula_sum            'C38 H32 Cu2 I2 N14 S2'
_chemical_formula_weight         1129.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-11-21 deposited with the CCDC.	2019-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                105.415(3)
_cell_angle_beta                 107.187(3)
_cell_angle_gamma                94.746(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8160(3)
_cell_length_b                   10.8974(4)
_cell_length_c                   11.8642(4)
_cell_measurement_reflns_used    6435
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.0120
_cell_measurement_theta_min      4.0700
_cell_volume                     1033.52(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5281
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -114.00 -11.00   1.00    1.50    --  -40.36 -57.00  90.00  103
  2  ω    -67.00  36.00   1.00    1.50    --  -40.36  37.00  30.00  103
  3  ω    -70.00  34.00   1.00    1.50    --  -40.36  57.00-120.00  104
  4  ω      1.00  82.00   1.00    1.50    --   40.36 -99.00 -30.00   81
  5  ω     23.00  98.00   1.00    1.50    --   40.36-125.00  30.00   75
  6  ω     24.00 168.00   1.00    4.50    --  106.83 -15.00  30.00  144
  7  ω     23.00 109.00   1.00    4.50    --  106.83 -94.00-120.00   86
  8  ω     29.00 137.00   1.00    4.50    --  106.83 -30.00-150.00  108
  9  ω     23.00 109.00   1.00    4.50    --  106.83 -94.00 120.00   86
 10  ω     29.00 116.00   1.00    4.50    --  106.83-111.00  30.00   87
 11  ω     79.00 178.00   1.00    4.50    --  106.83  45.00  30.00   99
 12  ω     38.00 124.00   1.00    4.50    --  106.83 -61.00  90.00   86
 13  ω     93.00 145.00   1.00    4.50    --  106.83 -92.00-161.00   52
 14  ω    102.00 172.00   1.00    4.50    --  106.83 111.00-150.00   70
 15  ω     76.00 123.00   1.00    4.50    --  106.83 178.00 150.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1848412000
_diffrn_orient_matrix_UB_12      0.0186119000
_diffrn_orient_matrix_UB_13      0.0337882000
_diffrn_orient_matrix_UB_21      0.0184262000
_diffrn_orient_matrix_UB_22      0.0957630000
_diffrn_orient_matrix_UB_23      0.1268642000
_diffrn_orient_matrix_UB_31      0.0031906000
_diffrn_orient_matrix_UB_32      -0.1125515000
_diffrn_orient_matrix_UB_33      0.0559527000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7828
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.241
_diffrn_reflns_theta_min         4.095
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.333
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_description       rod
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.062
_refine_diff_density_min         -1.386
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0495P)²+2.1767P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3778
_reflns_number_total             3790
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj03371h2.cif
_cod_data_source_block           1
_cod_database_code               7059057
_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.
;
_shelx_estimated_absorpt_t_max   0.278
_shelx_estimated_absorpt_t_min   0.162
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2.a Aromatic/amide H refined with riding coordinates:
 N5(H5), C16(H16), C3(H3), C15(H15), C11(H11), C9(H9), C4(H4), C17(H17),
 C10(H10), C8(H8), C2(H2), C1(H1), C14(H14)
2.b Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c)
;
_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 4.124
_oxdiff_exptl_absorpt_empirical_full_min 0.591
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
I2 I 0.22735(2) 0.03550(2) 0.85954(2) 0.01695(9) Uani 1 1 d .
Cu1 Cu 0.35792(5) 0.27600(4) 0.89877(4) 0.00860(11) Uani 1 1 d .
S2 S 0.21528(9) 0.28819(7) 0.70685(6) 0.01095(16) Uani 1 1 d .
N3 N 0.2968(3) 0.4473(2) 0.9552(2) 0.0083(5) Uani 1 1 d .
N2 N 0.4556(3) 0.3172(2) 1.0854(2) 0.0106(5) Uani 1 1 d .
N4 N 0.2100(3) 0.5092(2) 0.8789(2) 0.0092(5) Uani 1 1 d .
N5 N 0.0732(3) 0.4878(2) 0.6750(2) 0.0103(5) Uani 1 1 d .
H5 H 0.064420 0.449529 0.599398 0.012 Uiso 1 1 calc R
C12 C 0.1667(4) 0.4396(3) 0.7610(3) 0.0093(6) Uani 1 1 d .
C6 C 0.3461(3) 0.5058(3) 1.0735(3) 0.0082(6) Uani 1 1 d .
C16 C -0.2095(4) 0.7716(3) 0.6982(3) 0.0126(6) Uani 1 1 d .
H16 H -0.281418 0.829467 0.696909 0.015 Uiso 1 1 calc R
C5 C 0.3070(4) 0.6360(3) 1.1210(3) 0.0087(6) Uani 1 1 d .
C7 C 0.4336(4) 0.4328(3) 1.1510(3) 0.0093(6) Uani 1 1 d .
C3 C 0.1137(4) 0.7651(3) 1.1654(3) 0.0145(6) Uani 1 1 d .
H3 H 0.015942 0.773970 1.178935 0.017 Uiso 1 1 calc R
C13 C -0.0112(4) 0.5917(3) 0.6928(3) 0.0097(6) Uani 1 1 d .
C15 C -0.1133(4) 0.7594(3) 0.8090(3) 0.0137(6) Uani 1 1 d .
H15 H -0.117184 0.811412 0.883843 0.016 Uiso 1 1 calc R
C11 C 0.5402(4) 0.2450(3) 1.1472(3) 0.0140(6) Uani 1 1 d .
H11 H 0.557505 0.166442 1.102514 0.017 Uiso 1 1 calc R
N7 N 0.5689(6) 0.1948(5) 0.5328(4) 0.0462(11) Uani 1 1 d .
C9 C 0.5748(4) 0.3989(3) 1.3427(3) 0.0153(6) Uani 1 1 d .
H9 H 0.612610 0.424580 1.428796 0.018 Uiso 1 1 calc R
C4 C 0.1616(4) 0.6453(3) 1.1420(3) 0.0132(6) Uani 1 1 d .
H4 H 0.096963 0.572494 1.140434 0.016 Uiso 1 1 calc R
C17 C -0.1955(4) 0.6953(3) 0.5895(3) 0.0144(6) Uani 1 1 d .
H17 H -0.256802 0.705714 0.515210 0.017 Uiso 1 1 calc R
C10 C 0.6027(4) 0.2833(3) 1.2751(3) 0.0165(7) Uani 1 1 d .
H10 H 0.662794 0.231897 1.315419 0.020 Uiso 1 1 calc R
C8 C 0.4892(4) 0.4764(3) 1.2794(3) 0.0116(6) Uani 1 1 d .
H8 H 0.469980 0.555058 1.322232 0.014 Uiso 1 1 calc R
C2 C 0.2139(4) 0.8707(3) 1.1683(3) 0.0154(6) Uani 1 1 d .
H2 H 0.183390 0.951629 1.181147 0.018 Uiso 1 1 calc R
C1 C 0.3614(4) 0.8544(3) 1.1517(3) 0.0151(6) Uani 1 1 d .
H1 H 0.430539 0.926689 1.157280 0.018 Uiso 1 1 calc R
C19 C 0.7782(7) 0.0462(5) 0.5067(4) 0.0419(11) Uani 1 1 d .
H19A H 0.763432 0.010801 0.420168 0.063 Uiso 1 1 calc GR
H19B H 0.763622 -0.022858 0.540717 0.063 Uiso 1 1 calc GR
H19C H 0.885080 0.095402 0.549117 0.063 Uiso 1 1 calc GR
C18 C 0.6609(6) 0.1296(4) 0.5219(4) 0.0323(9) Uani 1 1 d .
N1 N 0.4086(3) 0.7390(2) 1.1280(2) 0.0098(5) Uani 1 1 d .
N6 N -0.0980(3) 0.6067(3) 0.5853(2) 0.0126(5) Uani 1 1 d .
C14 C -0.0112(4) 0.6694(3) 0.8079(3) 0.0121(6) Uani 1 1 d .
H14 H 0.055513 0.660776 0.881402 0.014 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
S2 Cu1 I2 95.86(2) . .
N3 Cu1 I2 134.59(7) . .
N3 Cu1 S2 82.52(8) . .
N3 Cu1 N2 79.31(10) . .
N3 Cu1 N1 120.82(10) . 2_667
N2 Cu1 I2 95.35(7) . .
N2 Cu1 S2 161.71(8) . .
N2 Cu1 N1 92.58(10) . 2_667
N1 Cu1 I2 104.36(7) 2_667 .
N1 Cu1 S2 98.57(7) 2_667 .
C12 S2 Cu1 95.71(11) . .
N4 N3 Cu1 124.9(2) . .
C6 N3 Cu1 117.4(2) . .
C6 N3 N4 117.7(3) . .
C7 N2 Cu1 114.3(2) . .
C11 N2 Cu1 127.1(2) . .
C11 N2 C7 118.5(3) . .
C12 N4 N3 111.8(2) . .
C12 N5 C13 129.0(3) . .
N4 C12 S2 125.0(2) . .
N4 C12 N5 117.8(3) . .
N5 C12 S2 117.1(2) . .
N3 C6 C5 119.7(3) . .
N3 C6 C7 115.2(3) . .
C7 C6 C5 125.0(3) . .
C17 C16 C15 118.0(3) . .
C4 C5 C6 119.3(3) . .
N1 C5 C6 117.3(3) . .
N1 C5 C4 123.0(3) . .
N2 C7 C6 113.7(3) . .
N2 C7 C8 122.6(3) . .
C8 C7 C6 123.7(3) . .
C2 C3 C4 118.7(3) . .
N6 C13 N5 112.1(3) . .
N6 C13 C14 122.6(3) . .
C14 C13 N5 125.2(3) . .
C14 C15 C16 119.7(3) . .
N2 C11 C10 122.2(3) . .
C10 C9 C8 119.0(3) . .
C5 C4 C3 118.8(3) . .
N6 C17 C16 123.7(3) . .
C11 C10 C9 119.4(3) . .
C7 C8 C9 118.2(3) . .
C3 C2 C1 118.9(3) . .
N1 C1 C2 122.9(3) . .
N7 C18 C19 179.5(4) . .
C5 N1 Cu1 122.7(2) . 2_667
C1 N1 Cu1 119.9(2) . 2_667
C1 N1 C5 117.5(3) . .
C13 N6 C17 117.7(3) . .
C15 C14 C13 118.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I2 Cu1 2.6356(5) .
Cu1 S2 2.2977(8) .
Cu1 N3 1.985(3) .
Cu1 N2 2.031(3) .
Cu1 N1 2.186(3) 2_667
S2 C12 1.742(3) .
N3 N4 1.364(4) .
N3 C6 1.297(4) .
N2 C7 1.356(4) .
N2 C11 1.339(4) .
N4 C12 1.323(4) .
N5 C12 1.362(4) .
N5 C13 1.409(4) .
C6 C5 1.490(4) .
C6 C7 1.464(4) .
C16 C15 1.385(5) .
C16 C17 1.382(5) .
C5 C4 1.383(4) .
C5 N1 1.345(4) .
C7 C8 1.386(4) .
C3 C4 1.389(5) .
C3 C2 1.378(5) .
C13 N6 1.339(4) .
C13 C14 1.403(4) .
C15 C14 1.385(4) .
C11 C10 1.383(5) .
N7 C18 1.135(6) .
C9 C10 1.386(5) .
C9 C8 1.398(4) .
C17 N6 1.344(4) .
C2 C1 1.390(5) .
C1 N1 1.342(4) .
C19 C18 1.452(6) .
