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_7240856
_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         'C37 H12 F14 N4, 2(C2 H6 O)'
_chemical_formula_sum            'C41 H24 F14 N4 O2'
_chemical_formula_weight         870.64
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-13
_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                94.1124(12)
_cell_angle_beta                 90.7528(12)
_cell_angle_gamma                96.7722(12)
_cell_formula_units_Z            4
_cell_length_a                   7.6090(3)
_cell_length_b                   18.3265(7)
_cell_length_c                   25.6198(10)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      66.63
_cell_measurement_theta_min      3.09
_cell_volume                     3537.7(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_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            23668
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.685
_diffrn_reflns_theta_max         66.685
_diffrn_reflns_theta_min         2.881
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.354
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.60
_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 78110 reflections, Rint = 0.0353
 (64251 with I > 3sig(I), Rint = 0.0342)
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       plate
_exptl_crystal_F_000             1760
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol'
_exptl_crystal_size_max          0.571
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         23668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0455P)^2^+1.1610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21454
_reflns_number_total             23668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0md00127a2.cif
_cod_data_source_block           Compound_16
_cod_database_code               7240856
_publcif_datablock.id            {c033bb44-a450-4844-aecf-c3eea158bb6e}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.512
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6069(5)
 0.3931(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3.a Fixed occupancy and ADP/Uiso:
 H2, H3, H4, H1A, H3AA, H4A
3.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C39A(H39C,H39D), C41(H41A,H41B), C41A(H41C,H41D)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3A), C7(H7), C8(H8), C12(H12), C13(H13), C16(H16), C17(H17),
 C35(H35), C2A(H2AA), C3A(H3AB), C7A(H7A), C8A(H8A), C12A(H12A), C13A(H13A),
 C16A(H16A), C17A(H17A), C35A(H35A)
3.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C38A(H38D,H38E,H38F), C40(H40A,H40B,H40C), C40A(H40D,
 H40E,H40F)
3.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O1A(H1AA), O2(H2B), O2A(H2AB)
;
_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'