Structures of rhenium(I) complexes with 3-hydroxyflavone and benzhydroxamic acid as <i>O</i>,<i>O</i>'-bidentate ligands and confirmation of π-stacking by solid-state NMR spectroscopy
Schutte-Smith, Marietjie; Roodt, Andreas; Alberto, Roger; Twigge, Linette; Visser, Hendrik Gideon; Kirsten, Leo; Koen, Renier; Acta Crystallographica Section C 75 (2019) 378–387; doi:10.1107/S2053229619002717

data_2021531
_publ_section_title
;
 Structures of rhenium(I) complexes with 3-hydroxyflavone and
 benzhydroxamic acid as <i>O</i>,<i>O</i>'-bidentate ligands and
 confirmation of \p-stacking by solid-state NMR spectroscopy
;
_journal_coeditor_code           FN3295
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              378
_journal_page_last               387
_journal_paper_doi               10.1107/S2053229619002717
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C15 H10 O3'
_chemical_formula_moiety         'C15 H10 O3'
_chemical_formula_sum            'C15 H10 O3'
_chemical_formula_weight         238.23
_chemical_name_common
;
3-Hydroxyflavone
;
_chemical_name_systematic
;
2-Phenylchromen-4-one
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.3502(6)
_cell_length_b                   11.3531(14)
_cell_length_c                   18.063(2)
_cell_measurement_reflns_used    6732
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.88
_cell_volume                     1097.2(2)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2008) and XPREP (Bruker,
2008)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_refinement
;
WinGX (Farrugia, 2012) and SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>, 1999)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17120
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         3.763
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.211
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   -0.5(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+0.2600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                2376
_reflns_number_total             2621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3295sup1.cif
_cod_data_source_block           10RMSc3
_cod_depositor_comments
'Adding full bibliography for 2021529--2021531.cif.'
_cod_database_code               2021531
_cod_database_fobs_code          2021531
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              39640