Synthesis and structure of boron difluoride binuclear β-diketonates
Svistunova, Iryna V.; Sharutin, Vladimir V.; Tretyakova, Galina O.; Puzyrkov, Zakhar N.; Inorganica Chimica Acta 501 (2020) 119230–; doi:10.1016/j.ica.2019.119230

data_1565595
_publ_section_title
;
 Synthesis and structure of boron difluoride binuclear \b-diketonates
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119230
_journal_paper_doi               10.1016/j.ica.2019.119230
_journal_volume                  501
_journal_year                    2020
_chemical_formula_moiety         'C20 H16 B2 F4 O4 S'
_chemical_formula_sum            'C20 H16 B2 F4 O4 S'
_chemical_formula_weight         450.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.368(3)
_cell_length_b                   18.822(7)
_cell_length_c                   25.534(9)
_cell_measurement_reflns_used    75569
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.91
_cell_volume                     4022(3)
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            75569
_diffrn_reflns_theta_full        29.21
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         2.91
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  0.9802
_exptl_absorpt_correction_T_min  0.8194
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.93
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+1.7016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                3816
_reflns_number_total             5427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1502_0m_aC20H16O4B2F4S.cif
_cod_data_source_block           1502_0m_a
_cod_original_cell_volume        4022(2)
_cod_database_code               1565595
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C26(H26), C23(H23), C22(H22), C16(H16), C15(H15),
 C14(H14), C13(H13), C12(H12)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5C,H5A,H5B)
;
_olex2_submission_special_instructions 'No special instructions were received'