Mechanistic insight into novel sulfoxide containing SABRE polarisation transfer catalysts.
Tickner, Ben J.; Lewis, Jennifer S.; John, Richard O.; Whitwood, Adrian C.; Duckett, Simon B.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15198–15206; doi:10.1039/c9dt02951f

data_7701249
_publ_section_title
;
 Mechanistic insight into novel sulfoxide containing SABRE polarisation
 transfer catalysts.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15198
_journal_page_last               15206
_journal_paper_doi               10.1039/c9dt02951f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C48 H64 Ir2 N4 O6 S2, 1.27(H2 O), 2(C H2 Cl2)'
_chemical_formula_sum            'C50 H70.54 Cl4 Ir2 N4 O7.27 S2'
_chemical_formula_weight         1434.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-18 deposited with the CCDC.    2019-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                85.912(6)
_cell_angle_beta                 69.210(6)
_cell_angle_gamma                76.361(5)
_cell_formula_units_Z            1
_cell_length_a                   9.7187(5)
_cell_length_b                   12.0086(7)
_cell_length_c                   13.3295(11)
_cell_measurement_reflns_used    4601
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.3310
_cell_measurement_theta_min      4.9870
_cell_volume                     1413.22(17)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -17.00  11.00   1.00    1.00    --    0.00  57.00-180.00   28
  2  \w     21.00  60.00   1.00    1.00    --    0.00  57.00  30.00   39
  3  \w    -15.00  17.00   1.00    1.00    --    0.00 -57.00-120.00   32
  4  \w    -63.00 -27.00   1.00    1.00    --    0.00 -57.00-120.00   36
  5  \w    -19.00  12.00   1.00    1.00    --    0.00  57.00  30.00   31
  6  \w    -15.00  51.00   1.00    4.00    --   54.00 -57.00  30.00   66
  7  \w     45.00 127.00   1.00    4.00    --   54.00  19.00 120.00   82
  8  \w     39.00 123.00   1.00    4.00    --   54.00  57.00-180.00   84
  9  \w     18.00  71.00   1.00    4.00    --   54.00 -57.00-180.00   53
 10  \w    -14.00  82.00   1.00    4.00    --   54.00 -77.00 -60.00   96
 11  \w     76.00 123.00   1.00    4.00    --   54.00  57.00 -30.00   47
 12  \w     26.00 107.00   1.00    4.00    --   54.00-125.00-180.00   81
 13  \w     70.00 111.00   1.00    8.00    --  108.00-111.00  30.00   41
 14  \w     89.00 151.00   1.00    8.00    --  108.00 178.00-150.00   62
 15  \w    100.00 174.00   1.00    8.00    --  108.00  63.00 -90.00   74
 16  \w     41.00 124.00   1.00    8.00    --  108.00 -63.00 -30.00   83
 17  \w     71.00 113.00   1.00    8.00    --  108.00-111.00-120.00   42
 18  \w     39.00  95.00   1.00    8.00    --  108.00 -25.00   0.00   56
 19  \w     40.00 114.00   1.00    8.00    --  108.00 -63.00-180.00   74
 20  \w    125.00 155.00   1.00    8.00    --  108.00  50.00 120.00   30
 21  \w     46.00 134.00   1.00    8.00    --  108.00 -37.00-120.00   88
 22  \w    124.00 177.00   1.00    8.00    --  108.00  50.00-180.00   53
 23  \w     57.00  96.00   1.00    8.00    --  108.00-111.00 -30.00   39
 24  \w    100.00 158.00   1.00    8.00    --  108.00 111.00 -60.00   58
 25  \w     42.00 141.00   1.00    8.00    --  108.00 -25.00 120.00   99
 26  \w     44.00 108.00   1.00    8.00    --  108.00-111.00-180.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1739642000
_diffrn_orient_matrix_UB_12      -0.0310023000
_diffrn_orient_matrix_UB_13      -0.0464436000
_diffrn_orient_matrix_UB_21      -0.0049517000
_diffrn_orient_matrix_UB_22      0.0136495000
_diffrn_orient_matrix_UB_23      -0.1145500000
_diffrn_orient_matrix_UB_31      0.0021454000
_diffrn_orient_matrix_UB_32      0.1276042000
_diffrn_orient_matrix_UB_33      0.0027161000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9141
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.063
_diffrn_reflns_theta_max         67.063
_diffrn_reflns_theta_min         3.547
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.827
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.388
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       plate
_exptl_crystal_F_000             710.7
_exptl_crystal_recrystallization_method
'crystallisation from dichloromethane, hexane and water'
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.507
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5051
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0361P)^2^+2.0011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4567
_reflns_number_total             5051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02951f2.cif
_cod_data_source_block           sbd1902b
_cod_depositor_comments          'Adding full bibliography for 7701249.cif.'
_cod_original_cell_volume        1413.21(17)
_cod_database_code               7701249
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H70.5 Cl4 Ir2 N4 O8.25 S2'
_chemical_oxdiff_usercomment     'Jenny Lewis JSL Ox 2'
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.249
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Ir1-HA
 1.6 with sigma of 0.01
 Cl2-C25 \\sim Cl2A-C25A \\sim Cl1-C25 \\sim Cl1A-C25A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1A) = Uanis(Cl1)
Uanis(C25A) = Uanis(C25)
Uanis(Cl2A) = Uanis(Cl2)
4. Others
 Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(Cl1A)=Sof(Cl2A)=1-FVAR(1)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(Cl1)=Sof(Cl2)=FVAR(1)
 Sof(O4)=Sof(H4A)=Sof(H4B)=FVAR(2)
5.a Free rotating group:
 O4(H4A,H4B)
5.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C25A(H25C,H25D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C9(H9), C16(H16), C18(H18)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C)
;
_shelx_res_checksum              82765
_olex2_date_sample_data_collection 2019-06-19
_olex2_date_sample_submission    2019-06-17
_olex2_exptl_crystal_mounting_method 'oil on 75 micrometre micromount'
_olex2_submission_original_sample_id 'JSL Ox 2'
_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 1.852
_oxdiff_exptl_absorpt_empirical_full_min 0.801