Synthesis and cytotoxicity studies of Cu(I) and Ag(I) complexes based on sterically hindered β-diketonates with different degrees of fluorination
Pellei, Maura; Del Gobbo, Jo'; Caviglia, Miriam; Karade, Deepika V.; Gandin, Valentina; Marzano, Cristina; Noonikara Poyil, Anurag; Dias, Rasika; Santini, Carlo; Dalton Transactions  (2023) –; doi:10.1039/D3DT02179C

data_7713653
_publ_section_title
;
 Synthesis and cytotoxicity studies of Cu(I) and Ag(I) complexes based on
 sterically hindered \b-diketonates with different degrees of fluorination
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02179C
_journal_year                    2023
_chemical_formula_moiety         'C19 H8 F12 O2'
_chemical_formula_sum            'C19 H8 F12 O2'
_chemical_formula_weight         496.25
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-05 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.682(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.898(7)
_cell_length_b                   8.400(2)
_cell_length_c                   9.239(2)
_cell_measurement_reflns_used    1390
_cell_measurement_temperature    99.96
_cell_measurement_theta_max      29.90
_cell_measurement_theta_min      3.28
_cell_volume                     1807.7(8)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.96
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'PHOTON II 7 CPAD'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Smart ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.6 mm double-pinhole'
_diffrn_radiation_detector       'PHOTON II 7 CPAD'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4933
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.913
_diffrn_reflns_theta_min         1.748
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'KFF MO-2KC-90'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0582 before and 0.0340 after correction.
The Ratio of minimum to maximum transmission is 0.7627.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2578
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0773P)^2^+0.0583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1826
_reflns_number_total             2578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02179c2.cif
_cod_data_source_block           dia99_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        1807.8(8)
_cod_database_code               7713653
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.920
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 F4-C10 \\sim F4A-C10
 with sigma of 0.02
 C10-F4 \\sim C10-F5 \\sim C10-F6 \\sim C10-F6A \\sim C10-F4A \\sim C10-F5A
 with sigma of 0.02
 F6-C10 \\sim F6A-C10
 with sigma of 0.02
 F5-C10 \\sim F5A-C10
 with sigma of 0.02
 F4-F5 \\sim F4-F6 \\sim F5-F6 \\sim F6A-F4A \\sim F6A-F5A \\sim F4A-F5A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 F4A, C10, F5A, F6A, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, F4, F5, F6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F6A)=Sof(F4A)=Sof(F5A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Fixed Sof: H1(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C4(H4), C6(H6), C8(H8)
5.b Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              14729
_olex2_submission_special_instructions 'No special instructions were received'