Using signal amplification by reversible exchange (SABRE) to hyperpolarise <sup>119</sup>Sn and <sup>29</sup>Si NMR nuclei.
Olaru, Alexandra M.; Burt, Alister; Rayner, Peter J.; Hart, Sam J.; Whitwood, Adrian C.; Green, Gary G. R.; Duckett, Simon B.; Chemical communications (Cambridge, England) 52 (2016) 14482–14485; doi:10.1039/c6cc07109k

data_7125140
_publ_section_title
;
 Using signal amplification by reversible exchange (SABRE) to
 hyperpolarise <sup>119</sup>Sn and <sup>29</sup>Si NMR nuclei.
;
_journal_issue                   100
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14482
_journal_page_last               14485
_journal_paper_doi               10.1039/c6cc07109k
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C84 H114 Cl3 Ir3 N12 Si3'
_chemical_formula_sum            'C84 H114 Cl3 Ir3 N12 Si3'
_chemical_formula_weight         2059.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-30 deposited with the CCDC.
2016-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.152(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9974(5)
_cell_length_b                   14.9781(4)
_cell_length_c                   31.1032(9)
_cell_measurement_reflns_used    11405
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      70.8920
_cell_measurement_theta_min      5.1910
_cell_volume                     9756.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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    -19.00  13.00   1.00   10.00    --    0.00  61.00 -76.00   32
  2  \w     26.00  67.00   1.00   10.00    --    0.00  61.00 -76.00   41
  3  \w    -13.00  62.00   1.00   40.00    --   54.00 -57.00-150.00   75
  4  \w     31.00 123.00   1.00   40.00    --   54.00  77.00 120.00   92
  5  \w    -17.00  74.00   1.00   40.00    --   54.00 -37.00 -30.00   91
  6  \w     56.00 105.00   1.00   50.00    --  108.00 -50.00 -30.00   49
  7  \w     60.00  86.00   1.00   50.00    --  108.00 -37.00-180.00   26
  8  \w     38.00  74.00   1.00   50.00    --  108.00 -37.00 -60.00   36
  9  \w    100.00 170.00   1.00   50.00    --  108.00 111.00   0.00   70
 10  \w     44.00  87.00   1.00   50.00    --  108.00 -25.00-120.00   43
 11  \w     38.00  94.00   1.00   50.00    --  108.00 -25.00  30.00   56
 12  \w     47.00 115.00   1.00   50.00    --  108.00-111.00 -30.00   68
 13  \w     90.00 174.00   1.00   50.00    --  108.00  63.00  60.00   84
 14  \w     48.00  84.00   1.00   50.00    --  108.00 -25.00 120.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0455874000
_diffrn_orient_matrix_UB_12      0.0574572000
_diffrn_orient_matrix_UB_13      -0.0294834000
_diffrn_orient_matrix_UB_21      0.0577842000
_diffrn_orient_matrix_UB_22      0.0433645000
_diffrn_orient_matrix_UB_23      -0.0196965000
_diffrn_orient_matrix_UB_31      -0.0018893000
_diffrn_orient_matrix_UB_32      -0.0733917000
_diffrn_orient_matrix_UB_33      -0.0347554000
_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     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            33778
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.667
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.206
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       plate
_exptl_crystal_F_000             4104
_exptl_crystal_recrystallization_method 'MeOH evaporation'
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.021
_refine_diff_density_max         3.321
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         17287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0493P)^2^+29.3123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14835
_reflns_number_total             17287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07109k2.cif
_cod_data_source_block           sbd1622
_cod_original_cell_volume        9756.4(4)
_cod_database_code               7125140
_chemical_oxdiff_formula         'C86.75 H125 Cl3 Ir3 N12 O2.75 Si3'
_chemical_oxdiff_usercomment     'Alexandra Si-pmd-IMes'
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All Ir(H,H) groups
2.a Riding coordinates:
 Ir1(H,HA), Ir2(HB,HC), Ir3(HD,HE)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C17(H17), C22(H22), C23(H23),
 C25(H25), C30(H30), C31(H31), C34(H34), C36(H36), C43(H43), C45(H45), C50(H50),
  C51(H51), C53(H53), C58(H58), C59(H59), C62(H62), C64(H64), C71(H71),
 C73(H73), C78(H78), C79(H79), C81(H81)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,
 H49C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C66(H66A,
 H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C75(H75A,H75B,H75C),
 C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C82(H82A,H82B,H82C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C)
;
_shelx_res_checksum              26440
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-06-06
_olex2_date_sample_submission    2016-05-24
_olex2_exptl_crystal_mounting_method '200/mm micromount'
_olex2_submission_original_sample_id Si-pmd-IMes
_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 1.777
_oxdiff_exptl_absorpt_empirical_full_min 0.713