Pnictogen-bonding catalysis: brevetoxin-type polyether cyclizations
Gini, Andrea; Paraja, Miguel; Galmés, Bartomeu; Besnard, Celine; Poblador-Bahamonde, Amalia I.; Sakai, Naomi; Frontera, Antonio; Matile, Stefan; Chemical Science  (2020) –; doi:10.1039/D0SC02551H

data_1558417
_publ_section_title
;
 Pnictogen-bonding catalysis: brevetoxin-type polyether cyclizations
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02551H
_journal_year                    2020
_chemical_formula_moiety         'C18 H6 F9 Sb'
_chemical_formula_sum            'C18 H6 F9 Sb'
_chemical_formula_weight         514.98
_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     dual
_audit_creation_date             2019-11-11
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-04-26 deposited with the CCDC.	2020-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                98.5536(12)
_cell_angle_beta                 93.9179(11)
_cell_angle_gamma                102.0249(12)
_cell_formula_units_Z            4
_cell_length_a                   7.11145(10)
_cell_length_b                   14.5572(2)
_cell_length_c                   16.9641(2)
_cell_measurement_reflns_used    25590
_cell_measurement_temperature    140.01(10)
_cell_measurement_theta_max      32.8420
_cell_measurement_theta_min      1.7650
_cell_volume                     1689.55(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4670
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -50.00  27.00   0.50    3.50    --   18.57 -57.00-150.00  154
  2  \w    -13.00  91.00   0.50    3.50    --   18.57  77.00 120.00  208
  3  \w      0.00  88.00   0.50    3.50    --   18.57  57.00   0.00  176
  4  \w    -55.00  50.00   0.50    3.50    --   18.57 -77.00  30.00  210
  5  \w    -18.00  58.00   0.50    3.50    --   18.57 -99.00 150.00  152
  6  \w     35.00 105.00   0.50    3.50    --   18.57 178.00  30.00  140
  7  \w      2.00  56.00   0.50    3.50    --   18.57  57.00-120.00  108
  8  \w    -76.00 -51.00   0.50    3.50    --  -18.73 128.00-152.74   50
  9  \w    -76.00  -2.00   0.50    3.50    --  -18.73 -38.00-150.00  148
 10  \w    -78.00 -46.00   0.50    3.50    --  -18.73 131.00 125.09   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0903701000
_diffrn_orient_matrix_UB_12      0.0133282000
_diffrn_orient_matrix_UB_13      0.0006932000
_diffrn_orient_matrix_UB_21      -0.0475049000
_diffrn_orient_matrix_UB_22      -0.0484291000
_diffrn_orient_matrix_UB_23      -0.0024125000
_diffrn_orient_matrix_UB_31      0.0093210000
_diffrn_orient_matrix_UB_32      0.0054827000
_diffrn_orient_matrix_UB_33      0.0424326000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38775
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.938
_diffrn_reflns_theta_min         2.046
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.727
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.295
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.664
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.215
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         11671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+0.6497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10439
_reflns_number_total             11671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02551h2.cif
_cod_data_source_block           catalyst_1
_cod_database_code               1558417
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.393
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C34(H34), C30(H30), C15(H15), C9(H9), C19(H19), C43(H43), C37(H37), C41(H41),
 C6(H6), C13(H13), C47(H47), C2(H2)
;
_shelx_res_checksum              14776
_shelx_hkl_checksum              72979
_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 1.508
_oxdiff_exptl_absorpt_empirical_full_min 0.845