Bridged Difurans: Stabilizing Furan with p-Block Elements
Cao, Hongda; Brettell-Adams, Ian A.; Qu, Fengrui; Rupar, Paul A.; Organometallics 36 (2017) 2565–; doi:10.1021/acs.organomet.7b00135

data_4087345
_publ_section_title
;
 Bridged Difurans: Stabilizing Furan with p-Block Elements
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              2565
_journal_paper_doi               10.1021/acs.organomet.7b00135
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C16 H12 F3 O5 P S'
_chemical_formula_sum            'C16 H12 F3 O5 P S'
_chemical_formula_weight         404.29
_chemical_name_common            DFP-Me
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 118.667(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9262(6)
_cell_length_b                   12.3641(6)
_cell_length_c                   12.7478(6)
_cell_measurement_reflns_used    4069
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      22.7965
_cell_measurement_theta_min      2.4369
_cell_volume                     1787.63(16)
_computing_cell_refinement       'APEX2 V2013.10.0 (Bruker, 2013)'
_computing_data_collection       'APEX2 V2013.10.0 (Bruker, 2013)'
_computing_data_reduction        'APEX2 V2013.10.0 (Bruker, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Shelrick, 2015)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20727
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.796
_diffrn_source                   'fine focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.325
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       plate
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0783P)^2^+3.3182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2522
_reflns_number_total             3506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00135_si_003.cif
_cod_data_source_block           HDC03_a
_cod_original_cell_volume        1787.63(15)
_cod_database_code               4087345
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              26008
_shelx_hkl_checksum              55821