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_7125141
_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 H120 Cl3 Ir3 N12 Si3, 1.81(C3 H12 O3)'
_chemical_formula_sum            'C89.42 H141.68 Cl3 Ir3 N12 O5.42 Si3'
_chemical_formula_weight         2238.76
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-14
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.98535(15)
_cell_length_b                   27.98535(15)
_cell_length_c                   27.98535(15)
_cell_measurement_reflns_used    17456
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      31.8600
_cell_measurement_theta_min      3.7100
_cell_volume                     21917.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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 0.997
_diffrn_measured_fraction_theta_max 0.943
_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  96.50   0.75  145.00    --   25.48  19.00  30.00  154
;
_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      -0.0253245000
_diffrn_orient_matrix_UB_12      -0.0000228000
_diffrn_orient_matrix_UB_13      0.0009789000
_diffrn_orient_matrix_UB_21      -0.0005278000
_diffrn_orient_matrix_UB_22      -0.0219035000
_diffrn_orient_matrix_UB_23      -0.0127571000
_diffrn_orient_matrix_UB_31      0.0008716000
_diffrn_orient_matrix_UB_32      -0.0127597000
_diffrn_orient_matrix_UB_33      0.0218753000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            61051
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.118
_diffrn_reflns_theta_min         3.336
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.788
_exptl_absorpt_correction_T_max  0.628
_exptl_absorpt_correction_T_min  0.567
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             9036
_exptl_crystal_recrystallization_method d4-methanool
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.156
_refine_diff_density_max         2.035
_refine_diff_density_min         -1.487
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         12096
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+191.4852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8930
_reflns_number_total             12096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07109k2.cif
_cod_data_source_block           sbd1603
_cod_original_cell_volume        21917.6(3)
_cod_database_code               7125141
_chemical_oxdiff_formula         C91H148Cl3Ir3N12O7Si3
_chemical_oxdiff_usercomment     'Alexandra Olaru SiMe3pyrimidine'
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H17A,H17B,H17C} of C17, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, {H30A,H30B,H30C} of C30, {H29A,H29B,H29C} of C29, {H28A,
  H28B,H28C} of C28, {H27A,H27B,H27C} of C27, {H26A,H26B,H26C} of C26, {H31A,
  H31B,H31C} of C31, {H5A,H5B,H5C} of C5, {H6A,H6B,H6C} of C6, {H7A,H7B,H7C} of
  C7, {H18A,H18B,H18C} of C18, {H19A,H19B,H19C} of C19
2. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(O3)=Sof(H3A)=FVAR(1)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(O2)=Sof(H2)=FVAR(2)
 Fixed Sof: H29A(0.33333) H29B(0.33333) H29C(0.33333) H1A(0.33333)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C13(H13), C15(H15), C22(H22), C24(H24)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C)
4.d Idealised tetrahedral OH refined with riding coordinates:
 O3(H3A)
4.e Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O2(H2)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-01-07
_olex2_date_sample_submission    2016-01-04
_olex2_exptl_crystal_mounting_method 'oil on micromount'
_olex2_submission_original_sample_id SiMe3pyrimidine
_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 1.118
_oxdiff_exptl_absorpt_empirical_full_min 0.950