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_1557173
_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         'C54 H48 Ir P3, 0.28(C H4 O)'
_chemical_formula_sum            'C54.28 H49.13 Ir O0.28 P3'
_chemical_formula_weight         991.09
_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     dual
_audit_creation_date             2019-09-17
_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                 94.4442(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.31801(12)
_cell_length_b                   12.99024(10)
_cell_length_c                   19.71788(16)
_cell_measurement_reflns_used    9261
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      71.0080
_cell_measurement_theta_min      4.9940
_cell_volume                     4422.50(6)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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      1.00  26.00   1.00    1.00    --    0.00  57.00 150.00   25
  2  \w    -10.00  27.00   1.00    1.00    --    0.00  93.00  61.00   37
  3  \w    -39.00 -13.00   1.00    1.00    --    0.00  93.00  61.00   26
  4  \w    -21.00  45.00   1.00    1.00    --    0.00  57.00-180.00   66
  5  \w     24.00 109.00   1.00    1.25    --   54.00-125.00 -90.00   85
  6  \w     28.00 114.00   1.00    1.25    --   54.00  37.00 -30.00   86
  7  \w     50.00 100.00   1.00    1.25    --   54.00  57.00-180.00   50
  8  \w    -13.00  73.00   1.00    1.25    --   54.00 -57.00   0.00   86
  9  \w    106.00 176.00   1.00    2.50    --  108.00 111.00 150.00   70
 10  \w     47.00 100.00   1.00    2.50    --  108.00-111.00 -60.00   53
 11  \w     55.00 103.00   1.00    2.50    --  108.00 -50.00-120.00   48
 12  \w     39.00 111.00   1.00    2.50    --  108.00-111.00  90.00   72
 13  \w     69.00 125.00   1.00    2.50    --  108.00 -50.00 150.00   56
 14  \w     95.00 162.00   1.00    2.50    --  108.00  63.00 -30.00   67
 15  \w     84.00 150.00   1.00    2.50    --  108.00 178.00 -60.00   66
 16  \w     86.00 163.00   1.00    2.50    --  108.00  50.00 -60.00   77
 17  \w     70.00  95.00   1.00    2.50    --  108.00-111.00-120.00   25
;
_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      0.0378139000
_diffrn_orient_matrix_UB_12      0.0190542000
_diffrn_orient_matrix_UB_13      0.0722370000
_diffrn_orient_matrix_UB_21      0.0197567000
_diffrn_orient_matrix_UB_22      -0.1153091000
_diffrn_orient_matrix_UB_23      0.0068760000
_diffrn_orient_matrix_UB_31      0.0784119000
_diffrn_orient_matrix_UB_32      0.0199077000
_diffrn_orient_matrix_UB_33      -0.0295763000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17542
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         4.079
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.149
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.375
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       plate
_exptl_crystal_F_000             1996.4
_exptl_crystal_recrystallization_method 'crystallisation from methanol'
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.000059(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         7896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+0.6768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7174
_reflns_number_total             7896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cy02498k2.cif
_cod_data_source_block           sbd1905
_cod_depositor_comments
;Adding full bibliography for 1557173--1557174.cif.

 Adding full bibliography for 1557173--1557174.cif.
;
_cod_database_code               1557173
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C54.3 H49.1 Ir1 O0.3 P3'
_chemical_oxdiff_usercomment     'Ben Tickner PPh3'
_reflns_odcompleteness_completeness 99.95
_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 O(H) groups
2. Others
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(O1)=Sof(H1)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
3.b Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C)
3.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              62826
_olex2_date_sample_data_collection 2019-09-06
_olex2_date_sample_submission    2019-09-03
_olex2_exptl_crystal_mounting_method 'oil on micromount'
_olex2_submission_original_sample_id 'BT PPh3'
_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 1.213
_oxdiff_exptl_absorpt_empirical_full_min 0.794