Hypervalent diorganoantimony(iii) fluorides via diorganoantimony(iii) cations ‒ a general method of synthesis
Preda, Ana Maria; Raţ, Ciprian I.; Silvestru, Cristian; Lang, Heinrich; Rüffer, Tobias; Mehring, Michael; RSC Advances 5 (2015) 99832–; doi:10.1039/C5RA21788A

data_7236023
_publ_section_title
;
 Hypervalent diorganoantimony(iii) fluorides via diorganoantimony(iii)
 cations -- a general method of synthesis
;
_journal_issue                   121
_journal_name_full               'RSC Advances'
_journal_page_first              99832
_journal_paper_doi               10.1039/C5RA21788A
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C38 H44 F N2 Sb'
_chemical_formula_sum            'C38 H44 F N2 Sb'
_chemical_formula_weight         669.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-04-04 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.847(11)
_cell_length_b                   21.755(16)
_cell_length_c                   10.693(8)
_cell_measurement_reflns_used    5582
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      21.98
_cell_measurement_theta_min      2.32
_cell_volume                     3454(4)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21151
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.661
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.8129
_exptl_absorpt_correction_T_min  0.7769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, 2001.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.260
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 2071 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         6049
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+0.1810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                5253
_reflns_number_total             6049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra21788a2.cif
_cod_data_source_block           577r
_cod_original_cell_volume        3454(5)
_cod_database_code               7236023
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.813
_shelxl_version_number           2014/6
_shelx_res_checksum              35256