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_1565596
_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         'C11 H14 B2 F4 O5 S'
_chemical_formula_sum            'C11 H14 B2 F4 O5 S'
_chemical_formula_weight         355.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 116.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.371(9)
_cell_length_b                   12.765(11)
_cell_length_c                   11.993(9)
_cell_measurement_reflns_used    4100
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      3.19
_cell_volume                     1561(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53701
_diffrn_reflns_theta_full        28.90
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_T_max  0.9310
_exptl_absorpt_correction_T_min  0.9024
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0597P)^2^+0.4475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                3356
_reflns_number_total             4100
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C11H14O5SB2F4.cif
_cod_data_source_block           1491_0m_a
_cod_database_code               1565596
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C5(H5A,H5B,H5C), C4(H4B,H4A,H4C), C6(H6A,H6C,H6B)
;
_olex2_submission_special_instructions 'No special instructions were received'