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_1565594
_publ_section_title
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 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         'C10 H12 B2 F4 O4 S, C H2 Cl'
_chemical_formula_sum            'C11 H14 B2 Cl F4 O4 S'
_chemical_formula_weight         375.35
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                86.56(3)
_cell_angle_beta                 85.43(2)
_cell_angle_gamma                70.61(3)
_cell_formula_units_Z            2
_cell_length_a                   7.591(4)
_cell_length_b                   10.496(4)
_cell_length_c                   10.791(5)
_cell_measurement_reflns_used    10786
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      41.33
_cell_measurement_theta_min      2.85
_cell_volume                     807.9(7)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            69665
_diffrn_reflns_theta_full        41.33
_diffrn_reflns_theta_max         41.33
_diffrn_reflns_theta_min         2.85
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.419
_exptl_absorpt_correction_T_max  0.8535
_exptl_absorpt_correction_T_min  0.7222
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             382
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.81
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         10786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0669
_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^)+(0.1009P)^2^+0.1811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1788
_refine_ls_wR_factor_ref         0.2078
_reflns_number_gt                6303
_reflns_number_total             10786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1494_0m_aC11H14O4B2F4SCl.cif
_cod_data_source_block           1494_0m_a
_cod_original_cell_volume        808.0(6)
_cod_database_code               1565594
_olex2_refinement_description
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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:
 C11(H11A,H11B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5C,H5B,H5A), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C)
;
_olex2_submission_special_instructions 'No special instructions were received'