A3- and A2B-fluorocorroles: synthesis, X-ray characterization and antiviral activity evaluation against human cytomegalovirus infection
Kappler-Gratias, Sandrine; Bucher, Léo; Desbois, Nicolas; Rousselin, Yoann; Bystricky, Kerstin; Gros, Claude P.; Gallardo, Franck; RSC Medicinal Chemistry  (2020) –; doi:10.1039/D0MD00127A

data_7240855
_publ_section_title
;
 A3- and A2B-fluorocorroles: synthesis, X-ray characterization and
 antiviral activity evaluation against human cytomegalovirus infection
;
_journal_name_full               'RSC Medicinal Chemistry'
_journal_paper_doi               10.1039/D0MD00127A
_journal_year                    2020
_chemical_formula_moiety         'C39 H17 F12 Mn N4 O, C2 H6 O'
_chemical_formula_sum            'C41 H23 F12 Mn N4 O2'
_chemical_formula_weight         886.57
_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     dual
_audit_creation_date             2018-10-10
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-16 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                95.3050(16)
_cell_angle_beta                 90.3264(16)
_cell_angle_gamma                97.8043(17)
_cell_formula_units_Z            4
_cell_length_a                   7.5565(3)
_cell_length_b                   17.8342(7)
_cell_length_c                   26.0523(10)
_cell_measurement_reflns_used    9726
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      66.67
_cell_measurement_theta_min      3.17
_cell_volume                     3462.9(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_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      100(1)
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture (Cu)'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'QUAZAR MX multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21719
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        66.680
_diffrn_reflns_theta_max         66.680
_diffrn_reflns_theta_min         2.900
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'high brilliance microfocus sealed tube, Cu'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.109
_exptl_absorpt_correction_T_max  0.58
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 46918 reflections, Rint = 0.0568
 (35482 with I > 3sig(I), Rint = 0.0531)
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       prism
_exptl_crystal_F_000             1784
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: mixture of ethanol and ethyl acetate'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1090
_refine_ls_number_reflns         21719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0526P)^2^+3.3290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18498
_reflns_number_total             21719
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {53378663-1ceb-4946-9d78-8a10e966723d}
_cod_data_source_file            d0md00127a2.cif
_cod_data_source_block           Compound_15
_cod_database_code               7240855
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.735
_shelx_estimated_absorpt_t_min   0.233
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7122(6)
 0.2878(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3.a Secondary CH2 refined with riding coordinates:
 C39A(H39A,H39B), C39(H39C,H39D), C40A(H40A,H40B), C40(H40C,H40D)
3.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C23(H23), C5A(H5A), C29(H29), C9(H9), C5(H5), C35A(H35A),
 C18A(H18A), C15A(H15A), C23A(H23A), C19(H19), C19A(H19A), C10A(H10A), C35(H35),
  C29A(H29A), C10(H10), C4(H4), C18(H18), C14(H14), C9A(H9A), C14A(H14A),
 C15(H15)
3.c Idealised Me refined as rotating group:
 C38A(H38A,H38B,H38C), C41(H41D,H41E,H41F), C41A(H41A,H41B,H41C), C38(H38D,
 H38E,H38F)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O1A(H1A), O2A(H2A), O2(H2)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_special_instructions 'No special instructions were received'