Novel tetranuclear Pd<sup>II</sup> and Pt<sup>II</sup> anticancer complexes derived from pyrene thiosemicarbazones.
Oliveira, Carolina G.; Romero-Canelón, Isolda; Coverdale, James P. C.; Maia, Pedro Ivo S.; Clarkson, Guy J.; Deflon, Victor M.; Sadler, Peter J.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9595–9604; doi:10.1039/d0dt01133a

data_7704742
_publ_section_title
;
 Novel tetranuclear Pd<sup>II</sup> and Pt<sup>II</sup> anticancer
 complexes derived from pyrene thiosemicarbazones.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9595
_journal_page_last               9604
_journal_paper_doi               10.1039/d0dt01133a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C96 H83 N12 Pt4 S4, C H Cl3, 2(C3 H6 O)'
_chemical_formula_sum            'C103 H96 Cl3 N12 O2 Pt4 S4'
_chemical_formula_weight         2548.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-12 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.045(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8631(8)
_cell_length_b                   26.4584(12)
_cell_length_c                   21.3233(8)
_cell_measurement_reflns_used    6278
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.99
_cell_measurement_theta_min      2.29
_cell_volume                     10640.4(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1224
_diffrn_reflns_av_unetI/netI     0.1492
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            87773
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.443
_diffrn_reflns_theta_min         1.227
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.447
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1145 before and 0.0655 after correction. The Ratio of minimum to maximum transmission is 0.8019. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             4964
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.347
_refine_diff_density_min         -1.471
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1211
_refine_ls_number_reflns         21672
_refine_ls_number_restraints     369
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1518
_refine_ls_R_factor_gt           0.0659
_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^)+(0.0698P)^2^+29.7710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11278
_reflns_number_total             21672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01133a2.cif
_cod_data_source_block           ocg6_sq
_cod_depositor_comments          'Adding full bibliography for 7704742.cif.'
_cod_database_code               7704742
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C422-C423 = C423-C424 = C424-C425 = C425-C426 = C426-C427 = C427-C422
 1.55 with sigma of 0.01
 N421-C22A = C22A-C23A = C23A-C24A = C24A-C25A = C25A-C26A = C26A-C27A = C27A-
 C22A
 1.55 with sigma of 0.01
 C22A-C24A = C23A-C25A = C24A-C26A = C25A-C27A = C26A-C22A
 2.53 with sigma of 0.016
 N421-C23A = N421-C27A
 2.46 with sigma of 0.02
3. Restrained planarity
 C422, C424, C425, C427
 with sigma of 0.1
 C423, C424, C426, C427
 with sigma of 0.1
 C27A, C26A, C24A, C23A
 with sigma of 0.1
 C22A, C27A, C25A, C24A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C422 \\sim C423 \\sim C424 \\sim C425 \\sim C426 \\sim C427: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C322 \\sim C323 \\sim C324 \\sim C325 \\sim C326 \\sim C327: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
N221 \\sim C222 \\sim C223 \\sim C224 \\sim C225 \\sim C226 \\sim C227: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Cl11 \\sim Cl12 \\sim Cl13 \\sim C10: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C6 \\sim O5 \\sim C5 \\sim C4: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C203 \\sim C204 \\sim C205 \\sim C206 \\sim C207 \\sim C208 \\sim C209 \\sim
C210: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C216, C217, N218, N219, C220, N221
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C308, C307, C306, C301, C302, C313
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C203, C216, C215, C214, C213
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N421, C22A, C27A, C26A, C25A, C24A, C23A
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0008
 C412, C411, C410, C409, C408, C407, C406, C405
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: H421(0.6) H42A(0.4) C422(0.6) H422(0.6) C423(0.6) H42B(0.6)
 H42C(0.6) C424(0.6) H42D(0.6) H42E(0.6) C425(0.6) H42F(0.6) H42G(0.6)
 C426(0.6) H42H(0.6) H42I(0.6) C427(0.6) H42J(0.6) H42K(0.6) C22A(0.4)
 H22K(0.4) C27A(0.4) H27A(0.4) H27B(0.4) C26A(0.4) H26A(0.4) H26B(0.4)
 C25A(0.4) H25A(0.4) H25B(0.4) C24A(0.4) H24A(0.4) H24B(0.4) C23A(0.4)
 H23A(0.4) H23B(0.4)
7.a Ternary CH refined with riding coordinates:
 C122(H122), C222(H222), C322(H322), C422(H422), C10(H10), C22A(H22K)
7.b Secondary CH2 refined with riding coordinates:
 C327(H32A,H32B), C123(H12A,H12B), C124(H12C,H12D), C125(H12E,H12F), C126(H12G,
 H12H), C127(H12I,H12J), C223(H22A,H22B), C224(H22C,H22D), C225(H22E,H22F),
 C226(H22G,H22H), C227(H22I,H22J), C323(H32C,H32D), C324(H32E,H32F), C325(H32G,
 H32H), C326(H32I,H32J), C423(H42B,H42C), C424(H42D,H42E), C425(H42F,H42G),
 C426(H42H,H42I), C427(H42J,H42K), C27A(H27A,H27B), C26A(H26A,H26B), C25A(H25A,
 H25B), C24A(H24A,H24B), C23A(H23A,H23B)
7.c Aromatic/amide H refined with riding coordinates:
 C104(H104), C105(H105), C107(H107), C108(H108), C109(H109), C111(H111),
 C112(H112), C114(H114), C117(H117), N121(H121), C204(H204), C205(H205),
 C207(H207), C208(H208), C209(H209), C211(H211), C212(H212), C214(H214),
 C217(H217), N221(H221), C304(H304), C305(H305), C307(H307), C308(H308),
 C311(H311), C312(H312), C314(H314), C317(H317), N321(H321), C404(H404),
 C405(H405), C407(H407), C408(H408), C409(H409), C411(H411), C412(H412),
 C414(H414), C417(H417), N421(H421), N421(H42A)
7.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              79837
_shelx_fab_checksum              74749
_olex2_submission_special_instructions 'No special instructions were received'