Complete Deconstruction of SF6 by an Aluminium(I) Compound
Sheldon, Daniel James; Crimmin, Mark Richard; Chemical Communications  (2021) –; doi:10.1039/D1CC02838C

data_7128506
_publ_section_title
;
 Complete Deconstruction of SF6 by an Aluminium(I) Compound
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC02838C
_journal_year                    2021
_chemical_formula_moiety         'C58 H82 Al2 N4 S2'
_chemical_formula_sum            'C58 H82 Al2 N4 S2'
_chemical_formula_weight         953.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-07-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2021-05-20 deposited with the CCDC.	2021-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3187(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3453(5)
_cell_length_b                   14.7350(3)
_cell_length_c                   16.3947(3)
_cell_measurement_reflns_used    3971
_cell_measurement_temperature    173.10(14)
_cell_measurement_theta_max      73.0690
_cell_measurement_theta_min      3.5880
_cell_volume                     5398.00(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.10(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.952
_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     31.00 113.00   1.00   10.63    --   42.23  38.00   0.00   82
  2  \w     77.00 164.00   1.00   42.33    --  105.13  77.00  30.00   87
  3  \w     82.00 170.00   1.00   42.33    --  105.13  61.00  90.00   88
  4  \w     41.00 122.00   1.00   42.33    --  105.13 -61.00   0.00   81
  5  \w     39.00 133.00   1.00   42.33    --  105.13 -61.00-120.00   94
  6  \w    -11.00  75.00   1.00   10.63    --   42.23 -99.00-150.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0619778000
_diffrn_orient_matrix_UB_12      0.0437532000
_diffrn_orient_matrix_UB_13      -0.0121480000
_diffrn_orient_matrix_UB_21      0.0295280000
_diffrn_orient_matrix_UB_22      -0.0801311000
_diffrn_orient_matrix_UB_23      0.0453363000
_diffrn_orient_matrix_UB_31      0.0068466000
_diffrn_orient_matrix_UB_32      -0.0511042000
_diffrn_orient_matrix_UB_33      -0.0812481000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8773
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.438
_diffrn_reflns_theta_min         3.593
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.507
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: C6D6'
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.174
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0967P)^2^+6.4619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4243
_reflns_number_total             5181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02838c3.cif
_cod_data_source_block           mrc2029
_cod_original_cell_volume        5398.01(18)
_cod_database_code               7128506
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C58 H68 N4 Al2 S2'
_chemical_oxdiff_usercomment     DJ
_reflns_odcompleteness_completeness 98.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C27(H27), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C10(H10), C9(H9), C20(H20), C23(H23), C21(H21)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C25(H25A,H25B,H25C), C5(H5A,H5B,H5C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C14(H14A,H14B,
 H14C), C13(H13A,H13B,H13C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              91516
_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 1.134
_oxdiff_exptl_absorpt_empirical_full_min 0.879