Silver(I) complexes of 3-methoxy-4-hydroxybenzaldehyde thiosemicarbazones and triphenylphosphine: structural, cytotoxicity, and apoptotic studies.
Silva, Débora E S; Becceneri, Amanda B.; Santiago, João V B; Gomes Neto, José A; Ellena, Javier; Cominetti, Márcia R; Pereira, José C M; Hannon, Michael J.; Netto, Adelino V. G.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16474–16487; doi:10.1039/d0dt01134g

data_7705231
_publ_section_title
;
 Silver(I) complexes of 3-methoxy-4-hydroxybenzaldehyde thiosemicarbazones
 and triphenylphosphine: structural, cytotoxicity, and apoptotic studies.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16474
_journal_page_last               16487
_journal_paper_doi               10.1039/d0dt01134g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C52 H54 Ag Cl N4 O2 P2 S'
_chemical_formula_sum            'C47 H49 Ag Cl2 N6 O2 P2 S0.12'
_chemical_formula_weight         974.64
_chemical_name_systematic        'DES 6'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-20
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-03-23 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.951(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.5169(10)
_cell_length_b                   10.2681(3)
_cell_length_c                   43.6410(13)
_cell_measurement_reflns_used    24530
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.9960
_cell_measurement_theta_min      2.7220
_cell_volume                     11143.5(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_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      298
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.947
_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    -69.00 117.00   0.75   12.18    --   27.63  54.00   0.00  248
  2  \w    -69.00 117.00   0.75   12.18    --   27.63  54.00  60.00  248
  3  \w    -69.00 117.00   0.75   12.18    --   27.63  54.00   0.00  248
  4  \w    -69.00   1.50   0.75   12.18    --   27.63  54.00-150.00   94
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0040719000
_diffrn_orient_matrix_UB_12      0.0192397000
_diffrn_orient_matrix_UB_13      0.0159820000
_diffrn_orient_matrix_UB_21      -0.0281839000
_diffrn_orient_matrix_UB_22      0.0004834000
_diffrn_orient_matrix_UB_23      -0.0012918000
_diffrn_orient_matrix_UB_31      0.0010755000
_diffrn_orient_matrix_UB_32      -0.0663213000
_diffrn_orient_matrix_UB_33      0.0046229000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            94501
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.487
_diffrn_reflns_theta_min         2.549
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             4016
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         22366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0530
_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/[\s^2^(Fo^2^)+(0.0567P)^2^+3.2233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10718
_reflns_number_total             22366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01134g2.cif
_cod_data_source_block           des6
_cod_depositor_comments
'Adding full bibliography for 7705230--7705231.cif.'
_cod_database_code               7705231
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C52 H30 N4 O2 S1 Cl1 P2 Ag1'
_chemical_oxdiff_usercomment     'Adelino - Unesp Arq. - 18-04-18'
_reflns_odcompleteness_completeness 99.85
_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 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.a Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C55(H55A,H55B), C58(H58A,H58B), C63(H63A,H63B), C66(H66A,
 H66B), C65(H65A,H65B), C64(H64A,H64B)
2.b Aromatic/amide H refined with riding coordinates:
 N49(H49), C10(H10), C29(H29), C14(H14), C11(H11), C26(H26), C39(H39),
 C42(H42), C47(H47), C35(H35), C13(H13), C20(H20), C22(H22), C30(H30), C38(H38),
  C46(H46), C25(H25), C33(H33), C31(H31), C12(H12), C32(H32), C16(H16), C4(H4),
 C37(H37), C45(H45), C24(H24), C23(H23), C5(H5), C19(H19), C6(H6), C17(H17),
 C36(H36), C18(H18), C2(H2), C61(H61)
2.c X=CH2 refined with riding coordinates:
 N52(H52A,H52B)
2.d Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C)
;
_shelx_res_checksum              64344
_shelx_fab_checksum              50992
_olex2_date_sample_data_collection 2018-04-19
_olex2_date_sample_submission    2018-04-18
_olex2_submission_original_sample_id DES6
_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 1.181
_oxdiff_exptl_absorpt_empirical_full_min 0.824