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_7705230
_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         'C51 H52 Ag Cl N4 O3 P2 S, 0.25[C2H3N]'
_chemical_formula_sum            'C50 H53 Ag Cl2 N5 O3 P2 S0.12'
_chemical_formula_weight         1016.69
_chemical_name_systematic        DS05
_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             2019-09-30
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-03-23 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.785(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.4270(9)
_cell_length_b                   12.1243(5)
_cell_length_c                   33.2299(10)
_cell_measurement_reflns_used    15348
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5650
_cell_measurement_theta_min      2.9600
_cell_volume                     10063.3(6)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL n/a (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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     33.00  66.00   1.00   42.01    --   27.63  54.00 -30.00   33
  2  \w    -69.00 118.00   1.00   42.01    --   27.63  54.00  90.00  187
  3  \w    -46.00 -20.00   1.00   42.01    --   27.63  54.00 -30.00   26
;
_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      0.0011852000
_diffrn_orient_matrix_UB_12      0.0558922000
_diffrn_orient_matrix_UB_13      0.0063572000
_diffrn_orient_matrix_UB_21      -0.0052502000
_diffrn_orient_matrix_UB_22      0.0171394000
_diffrn_orient_matrix_UB_23      -0.0207926000
_diffrn_orient_matrix_UB_31      -0.0278643000
_diffrn_orient_matrix_UB_32      -0.0006529000
_diffrn_orient_matrix_UB_33      0.0000428000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            23269
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.515
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96167
_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    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         11513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+9.7236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8224
_reflns_number_total             11513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01134g2.cif
_cod_data_source_block           ds05_2
_cod_depositor_comments
'Adding full bibliography for 7705230--7705231.cif.'
_cod_database_code               7705230
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C51 H51 N4 O3 Cl1 P2 S1 Ag1 '
_chemical_oxdiff_usercomment     'Debora Javier 24-09-2019'
_reflns_odcompleteness_completeness 99.80
_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:
 C10(H10A,H10B), C9(H9A,H9B), C12(H12A,H12B), C16(H16A,H16B), C15(H15A,H15B),
 C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 N19(H19), C2(H2), C30(H30), C5(H5), C17(H17), C4(H4), C29(H29), C33(H33),
 C35(H35), C43(H43), C53(H53), C39(H39), C34(H34), C59(H59), C26(H26), C37(H37),
  C28(H28), C63(H63), C42(H42), C57(H57), C27(H27), C41(H41), C54(H54),
 C50(H50), C36(H36), C55(H55), C62(H62), C40(H40), C60(H60), C46(H46), C61(H61),
  C56(H56), C49(H49), C47(H47), C48(H48)
2.c X=CH2 refined with riding coordinates:
 N22(H22A,H22B)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              17130
_shelx_fab_checksum              90628
_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 1.051
_oxdiff_exptl_absorpt_empirical_full_min 0.958