data_watanabe_lab180314bf4_sl_1_1
_audit_creation_date              2018-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_id_orcid     ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common             ?
_chemical_name_systematic         ?
_chemical_formula_moiety          'C4 H8 B F4 Li O2 S'
_chemical_formula_sum             'C4 H8 B F4 Li O2 S'
_chemical_formula_weight          213.91
_chemical_absolute_configuration  ?
_chemical_melting_point           ?
_chemical_oxdiff_formula          C4H8O2S1B1F4Li
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Li' 'Li' -0.0003 0.0001
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system       'orthorhombic'
_space_group_IT_number            19
_space_group_name_H-M_alt         'P 21 21 21'
_space_group_name_Hall            'P 2ac 2ab'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'

_cell_length_a                    5.1560(11)
_cell_length_b                    8.8536(17)
_cell_length_c                    18.337(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      837.1(3)
_cell_formula_units_Z             4
_cell_measurement_reflns_used     2540
_cell_measurement_temperature     223
_cell_measurement_theta_max       29.5470
_cell_measurement_theta_min       4.0750
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     0.412
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_correction_T_min   0.27488
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details    ?
_exptl_crystal_colour             'clear colourless'
_exptl_crystal_density_diffrn     1.697
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_description        needle
_exptl_crystal_F_000              432
_exptl_crystal_size_max           0.9
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.2
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0562
_diffrn_reflns_av_unetI/netI      0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_l_max        24
_diffrn_reflns_limit_l_min        -25
_diffrn_reflns_number             7196
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full         25.242
_diffrn_reflns_theta_max          30.180
_diffrn_reflns_theta_min          2.555
_diffrn_ambient_temperature       223
_diffrn_detector                  'CCD plate'
_diffrn_detector_area_resol_mean  ?
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.8698
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω      5.00  30.00   0.50    0.61    --   -0.10  81.00 -89.00   50
  2  ω    -80.00 -54.00   0.50    0.61    --   -0.10 -40.00 -37.00   52
  3  ω     -1.00  67.00   0.50    0.61    --   -0.10  77.00 -30.00  136
  4  ω    -17.00  65.00   0.50    0.61    --   -0.10  38.00 -90.00  164
  5  ω     19.00  44.00   0.50    0.61    --   -0.10  38.00-150.00   50
;
_diffrn_measurement_device        'four-circle diffractometer'
_diffrn_measurement_device_type   'XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method        'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11       0.0732053000
_diffrn_orient_matrix_UB_12       0.0601265000
_diffrn_orient_matrix_UB_13       -0.0152504000
_diffrn_orient_matrix_UB_21       -0.1163973000
_diffrn_orient_matrix_UB_22       0.0344667000
_diffrn_orient_matrix_UB_23       -0.0121817000
_diffrn_orient_matrix_UB_31       -0.0093633000
_diffrn_orient_matrix_UB_32       0.0400406000
_diffrn_orient_matrix_UB_33       0.0333358000
_diffrn_oxdiff_ac3_digest_frames
;
01ee2f307a1e36ac507d514787649e188100037ca69
;
_diffrn_oxdiff_ac3_digest_hkl
;
016f548c67c67a9023d2035ec356e33240c17b
;
_diffrn_radiation_monochromator   graphite
_diffrn_radiation_probe           x-ray
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    'fine-focus sealed X-ray tube'
_diffrn_source_type               'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage          0.632
_reflns_Friedel_fraction_full     0.985
_reflns_Friedel_fraction_max      0.823
_reflns_number_gt                 1913
_reflns_number_total              2164
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric  1
_reflns_odcompleteness_theta      26.32
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_cell_refinement        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction         'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_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     'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max          0.361
_refine_diff_density_min          -0.599
_refine_diff_density_rms          0.133
_refine_ls_abs_structure_details
;
 Flack x determined using 677 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    -0.10(7)
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    0.880
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_parameters      118
_refine_ls_number_reflns          2164
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0529
_refine_ls_R_factor_gt            0.0447
_refine_ls_restrained_S_all       0.880
_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/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.1128
_refine_ls_wR_factor_ref          0.1177
_refine_special_details           ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
;
_atom_sites_solution_hydrogens    geom
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 S1 S 1.06571(15) 0.53943(8) 0.57463(4) 0.0196(2) Uani 1 1 d . . . . .
 F1 F 0.5605(5) 0.8921(3) 0.62399(13) 0.0410(6) Uani 1 1 d . . . . .
 F2 F 0.4097(6) 1.1186(3) 0.58685(12) 0.0461(6) Uani 1 1 d . . . . .
 F3 F 0.3707(5) 1.0491(3) 0.70523(11) 0.0382(5) Uani 1 1 d . . . . .
 F4 F 0.1293(5) 0.9354(3) 0.61956(16) 0.0501(7) Uani 1 1 d . . . . .
 O1 O 1.2944(5) 0.5239(3) 0.52905(14) 0.0304(5) Uani 1 1 d . . . . .
 O2 O 0.8858(5) 0.6567(3) 0.55345(15) 0.0326(6) Uani 1 1 d . . . . .
 C1 C 1.1610(8) 0.5586(4) 0.6676(2) 0.0323(8) Uani 1 1 d . . . . .
 H1A H 1.3381 0.5980 0.6714 0.039 Uiso 1 1 calc R . . . .
 H1B H 1.0432 0.6263 0.6939 0.039 Uiso 1 1 calc R . . . .
 C2 C 1.1447(7) 0.3992(4) 0.69733(19) 0.0295(7) Uani 1 1 d . . . . .
 H2A H 1.1349 0.4005 0.7507 0.035 Uiso 1 1 calc R . . . .
 H2B H 1.2975 0.3406 0.6828 0.035 Uiso 1 1 calc R . . . .
 C3 C 0.8975(7) 0.3301(4) 0.66475(19) 0.0290(7) Uani 1 1 d . . . . .
 H3A H 0.8933 0.2210 0.6736 0.035 Uiso 1 1 calc R . . . .
 H3B H 0.7434 0.3756 0.6870 0.035 Uiso 1 1 calc R . . . .
 C4 C 0.9030(6) 0.3624(3) 0.58316(17) 0.0227(6) Uani 1 1 d . . . . .
 H4A H 0.7266 0.3687 0.5635 0.027 Uiso 1 1 calc R . . . .
 H4B H 0.9974 0.2829 0.5571 0.027 Uiso 1 1 calc R . . . .
 B1 B 0.3693(7) 1.0015(4) 0.6343(2) 0.0223(7) Uani 1 1 d . . . . .
 Li1 Li 0.8520(11) 0.8718(6) 0.5627(3) 0.0245(11) Uani 1 1 d . . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 S1 O1 1.452(2) . ?
 S1 O2 1.445(2) . ?
 S1 C1 1.783(4) . ?
 S1 C4 1.785(3) . ?
 S1 Li1 3.023(6) 4_566 ?
 F1 B1 1.395(4) . ?
 F1 Li1 1.885(6) . ?
 F2 B1 1.370(4) . ?
 F3 B1 1.367(4) . ?
 F4 B1 1.395(4) . ?
 F4 Li1 1.857(6) 1_455 ?
 O1 Li1 1.942(6) 4_566 ?
 O2 Li1 1.920(6) . ?
 C1 H1A 0.9800 . ?
 C1 H1B 0.9800 . ?
 C1 C2 1.516(5) . ?
 C2 H2A 0.9800 . ?
 C2 H2B 0.9800 . ?
 C2 C3 1.535(5) . ?
 C3 H3A 0.9800 . ?
 C3 H3B 0.9800 . ?
 C3 C4 1.523(4) . ?
 C4 H4A 0.9800 . ?
 C4 H4B 0.9800 . ?
 Li1 S1 3.023(5) 4_466 ?
 Li1 F4 1.857(6) 1_655 ?
 Li1 O1 1.942(6) 4_466 ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 S1 C1 109.62(18) . . ?
 O1 S1 C4 110.42(16) . . ?
 O1 S1 Li1 31.62(15) . 4_566 ?
 O2 S1 O1 115.75(16) . . ?
 O2 S1 C1 111.44(17) . . ?
 O2 S1 C4 110.67(16) . . ?
 O2 S1 Li1 84.41(17) . 4_566 ?
 C1 S1 C4 97.45(16) . . ?
 C1 S1 Li1 129.60(18) . 4_566 ?
 C4 S1 Li1 122.06(15) . 4_566 ?
 B1 F1 Li1 135.3(3) . . ?
 B1 F4 Li1 156.8(3) . 1_455 ?
 S1 O1 Li1 125.3(2) . 4_566 ?
 S1 O2 Li1 138.3(2) . . ?
 S1 C1 H1A 111.0 . . ?
 S1 C1 H1B 111.0 . . ?
 H1A C1 H1B 109.0 . . ?
 C2 C1 S1 103.9(2) . . ?
 C2 C1 H1A 111.0 . . ?
 C2 C1 H1B 111.0 . . ?
 C1 C2 H2A 110.5 . . ?
 C1 C2 H2B 110.5 . . ?
 C1 C2 C3 106.1(3) . . ?
 H2A C2 H2B 108.7 . . ?
 C3 C2 H2A 110.5 . . ?
 C3 C2 H2B 110.5 . . ?
 C2 C3 H3A 110.3 . . ?
 C2 C3 H3B 110.3 . . ?
 H3A C3 H3B 108.6 . . ?
 C4 C3 C2 107.0(3) . . ?
 C4 C3 H3A 110.3 . . ?
 C4 C3 H3B 110.3 . . ?
 S1 C4 H4A 110.7 . . ?
 S1 C4 H4B 110.7 . . ?
 C3 C4 S1 105.0(2) . . ?
 C3 C4 H4A 110.7 . . ?
 C3 C4 H4B 110.7 . . ?
 H4A C4 H4B 108.8 . . ?
 F1 B1 F4 108.0(3) . . ?
 F2 B1 F1 109.4(3) . . ?
 F2 B1 F4 109.2(3) . . ?
 F3 B1 F1 109.9(3) . . ?
 F3 B1 F2 111.7(3) . . ?
 F3 B1 F4 108.6(3) . . ?
 F1 Li1 S1 94.7(2) . 4_466 ?
 F1 Li1 O1 110.4(3) . 4_466 ?
 F1 Li1 O2 102.7(3) . . ?
 F4 Li1 S1 139.9(3) 1_655 4_466 ?
 F4 Li1 F1 104.5(3) 1_655 . ?
 F4 Li1 O1 117.4(3) 1_655 4_466 ?
 F4 Li1 O2 106.3(3) 1_655 . ?
 O1 Li1 S1 23.07(11) 4_466 4_466 ?
 O2 Li1 S1 103.2(2) . 4_466 ?
 O2 Li1 O1 114.1(3) . 4_466 ?

_shelx_SHELXL_version_number      '2014/7'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.336
_oxdiff_exptl_absorpt_empirical_full_min 0.432
