Optimisation of pyruvate hyperpolarisation using SABRE by tuning the active magnetisation transfer catalyst.
Tickner, Ben J.; Semenova, Olga; Iali, Wissam; Rayner, Peter J.; Whitwood, Adrian C.; Duckett, Simon B.; Catalysis science & technology 10 (2020) 1343–1355; doi:10.1039/c9cy02498k

data_1557174
_publ_section_title
;
 Optimisation of pyruvate hyperpolarisation using SABRE by tuning the
 active magnetisation transfer catalyst.
;
_journal_issue                   5
_journal_name_full               'Catalysis science &amp; technology'
_journal_page_first              1343
_journal_page_last               1355
_journal_paper_doi               10.1039/c9cy02498k
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C56 H64 Cl2 Ir2 N4 S2, C H4 O'
_chemical_formula_sum            'C57 H68 Cl2 Ir2 N4 O S2'
_chemical_formula_weight         1344.57
_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     dual
_audit_creation_date             2019-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-04 deposited with the CCDC.	2019-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.2757(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9317(2)
_cell_length_b                   16.6000(3)
_cell_length_c                   25.5365(4)
_cell_measurement_reflns_used    9511
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.9880
_cell_measurement_theta_min      6.5490
_cell_volume                     5481.76(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -13.00  52.00   1.00    1.00    --    0.00  57.00 -60.00   65
  2  \w    -51.00 -20.00   1.00    1.00    --    0.00 124.00 101.00   31
  3  \w    -13.00  13.00   1.00    3.00    --   54.00 -57.00-150.00   26
  4  \w     27.00 105.00   1.00    3.00    --   54.00-125.00 120.00   78
  5  \w    -19.00  98.00   1.00    3.00    --   54.00 -19.00 -60.00  117
  6  \w     40.00  74.00   1.00    3.00    --   54.00 -57.00 120.00   34
  7  \w     92.00 119.00   1.00    3.00    --   54.00  77.00 -90.00   27
  8  \w     39.00  97.00   1.00    3.00    --  108.00-111.00-120.00   58
  9  \w    124.00 176.00   1.00    3.00    --  108.00  50.00-150.00   52
 10  \w     38.00  92.00   1.00    3.00    --  108.00-111.00 120.00   54
 11  \w     77.00 103.00   1.00    3.00    --  108.00 -50.00 -30.00   26
 12  \w     36.00  88.00   1.00    3.00    --  108.00-111.00-180.00   52
 13  \w     38.00  73.00   1.00    3.00    --  108.00 -50.00 -30.00   35
 14  \w    106.00 171.00   1.00    3.00    --  108.00  63.00   0.00   65
 15  \w     77.00 113.00   1.00    3.00    --  108.00-111.00 -90.00   36
 16  \w     90.00 176.00   1.00    3.00    --  108.00  63.00 120.00   86
 17  \w    113.00 139.00   1.00    3.00    --  108.00 -12.00-150.00   26
 18  \w     36.00  73.00   1.00    3.00    --  108.00 -12.00-150.00   37
;
_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      0.0536477000
_diffrn_orient_matrix_UB_12      -0.0704874000
_diffrn_orient_matrix_UB_13      0.0284325000
_diffrn_orient_matrix_UB_21      -0.0369154000
_diffrn_orient_matrix_UB_22      0.0333776000
_diffrn_orient_matrix_UB_23      0.0530168000
_diffrn_orient_matrix_UB_31      -0.0996791000
_diffrn_orient_matrix_UB_32      -0.0503459000
_diffrn_orient_matrix_UB_33      -0.0047444000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20688
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         3.462
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.192
_exptl_absorpt_correction_T_max  0.674
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_recrystallization_method 'crystallisation from methanol'
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.916
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         9782
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0265P)^2^+13.1045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8700
_reflns_number_total             9782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cy02498k2.cif
_cod_data_source_block           sbd1906
_cod_depositor_comments
;Adding full bibliography for 1557173--1557174.cif.

 Adding full bibliography for 1557173--1557174.cif.
;
_cod_original_cell_volume        5481.76(15)
_cod_database_code               1557174
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C57 H64 Cl2 Ir2 N4 O S2'
_chemical_oxdiff_usercomment     'Ben Tickner BT Ma1'
_shelx_estimated_absorpt_t_max   0.476
_shelx_estimated_absorpt_t_min   0.286
_reflns_odcompleteness_completeness 99.73
_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) groups
2. Restrained distances
 C46A-Cl1A \\sim Cl1A-C48A
 with sigma of 0.02
 C43A-C44A \\sim C44-C43
 with sigma of 0.02
 S1-C43 \\sim S1-C43A
 with sigma of 0.02
 C49A-C43A \\sim C43A-C45A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C49A) = Uanis(C49)
Uanis(C48) = Uanis(C48A)
Uanis(C47A) = Uanis(C47)
Uanis(C46A) = Uanis(C46)
Uanis(C45A) = Uanis(C45)
Uanis(C44A) = Uanis(C44)
Uanis(C43A) = Uanis(C43)
4. Others
 Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=
 Sof(H46A)=Sof(C47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(Cl1A)=1-FVAR(1)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=
 Sof(C47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(Cl1)=FVAR(1)
5.a Riding coordinates:
 Ir1(H,HA), Ir2(HB,HC)
5.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C43A(H43C,H43D), C50(H50A,H50B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C17(H17), C23(H23), C24(H24),
 C27(H27), C29(H29), C36(H36), C38(H38), C45A(H45A), C46A(H46A), C48A(H48A),
 C49A(H49A), C45(H45), C46(H46), C48(H48), C49(H49), C52(H52), C53(H53),
 C55(H55), C56(H56)
5.d Fitted hexagon refined as free rotating group:
 C44A(C45A,C46A,C47A,C48A,C49A)
5.e 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), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C57(H57A,H57B,H57C)
5.f Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              89407
_olex2_date_sample_data_collection 2019-09-20
_olex2_date_sample_submission    2019-09-19
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id 'BT Ma1'
_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 1.277
_oxdiff_exptl_absorpt_empirical_full_min 0.810