Tunable iridium catalyst designs with bidentate N-heterocyclic carbene ligands for SABRE hyperpolarization of sterically hindered substrates.
Pham, Pierce; Hilty, Christian; Chemical communications (Cambridge, England) 56 (2020) 15466–15469; doi:10.1039/d0cc06840c

data_7127434
_publ_section_title
;
 Tunable iridium catalyst designs with bidentate N-heterocyclic carbene
 ligands for SABRE hyperpolarization of sterically hindered substrates.
;
_journal_issue                   98
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              15466
_journal_page_last               15469
_journal_paper_doi               10.1039/d0cc06840c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C24 H30 Ir N4, C24 H20 B, C4 H5 O'
_chemical_formula_sum            'C53 H47 B Ir N3 O0.25'
_chemical_formula_weight         932.94
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-14 deposited with the CCDC.	2020-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.043(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.2922(15)
_cell_length_b                   13.8681(9)
_cell_length_c                   14.6786(9)
_cell_measurement_reflns_used    9446
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      29.82
_cell_measurement_theta_min      2.45
_cell_volume                     4338.6(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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_temperature      110.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8-Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            245032
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.062
_diffrn_reflns_theta_min         2.089
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.117
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0722 before and 0.0642 after correction. The Ratio of minimum to maximum transmission is 0.9164. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       prism
_exptl_crystal_F_000             1880
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/pentane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.899
_refine_diff_density_min         -1.700
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         12719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0187P)^2^+8.6173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10958
_reflns_number_total             12719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06840c2.cif
_cod_data_source_block           precatalyst1_0ma
_cod_depositor_comments          'Adding full bibliography for 7127434.cif.'
_cod_database_code               7127434
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.574
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H005(0.026) H006(0.028) H008(0.027) H00A(0.026) H00B(0.026)
 H00J(0.023) H00K(0.023) H00L(0.026) H00F(0.026) H00H(0.026) H00O(0.027)
 H00M(0.024) H00N(0.027) H00C(0.038) H00D(0.038) H00E(0.038) H00G(0.03)
 H00I(0.03) H00Q(0.027) H00R(0.027) H00S(0.031) H00T(0.04) H00U(0.026)
 H00V(0.026) H00X(0.029) H00Y(0.027) H00Z(0.03) H010(0.041) H011(0.031)
 H012(0.042) H013(0.029) H01A(0.084) H01B(0.084) H01C(0.084) H016(0.04)
 H01D(0.054) H01E(0.054) H01F(0.054) H018(0.036) H01G(0.033) H01H(0.033)
 H01N(0.039) H01I(0.031) H01J(0.031) H01O(0.035) H01P(0.031) H01K(0.033)
 H01L(0.033) H01M(0.033) H01Q(0.042) H01R(0.094) H01S(0.166) H01T(0.166)
 H01U(0.124) H01V(0.167)
 Fixed X: H005(0.629442) H006(0.940394) H008(0.804146) H00A(0.826584)
 H00B(0.863853) H00J(0.945652) H00K(0.913792) H00L(0.838786) H00F(0.792907)
 H00H(0.991388) H00O(0.958656) H00M(0.893388) H00N(0.661767) H00C(0.744993)
 H00D(0.715323) H00E(0.736753) H00G(0.611468) H00I(0.637917) H00Q(1.011736)
 H00R(0.694361) H00S(0.98927) H00T(0.492972) H00U(0.833367) H00V(0.963843)
 H00X(0.825672) H00Y(0.876023) H00Z(0.932492) H010(0.869291) H011(0.899798)
 H012(0.59276) H013(0.76391) H01A(0.470131) H01B(0.496669) H01C(0.451071)
 H016(0.63802) H01D(0.602008) H01E(0.531823) H01F(0.588514) H018(0.656777)
 H01G(0.761318) H01H(0.708347) H01N(0.945458) H01I(0.704826) H01J(0.704329)
 H01O(0.768037) H01P(0.744471) H01K(0.606008) H01L(0.657628) H01M(0.7201)
 H01Q(0.781349) H01R(0.528042) H01S(0.499409) H01T(0.559777) H01U(0.677854)
 H01V(0.574551)
 Fixed Y: H005(0.496013) H006(0.845595) H008(0.634324) H00A(0.408854)
 H00B(0.309269) H00J(0.500876) H00K(0.648928) H00L(0.305221) H00F(0.166934)
 H00H(0.463391) H00O(0.791711) H00M(0.558145) H00N(0.512954) H00C(0.300334)
 H00D(0.347922) H00E(0.414839) H00G(0.62113) H00I(0.694328) H00Q(0.37814)
 H00R(0.150596) H00S(0.217108) H00T(0.333403) H00U(0.609057) H00V(0.343608)
 H00X(0.678062) H00Y(0.753255) H00Z(0.421761) H010(0.474616) H011(0.181643)
 H012(0.489617) H013(0.362585) H01A(0.449375) H01B(0.381063) H01C(0.337793)
 H016(0.628227) H01D(0.334464) H01E(0.299744) H01F(0.224273) H018(0.356573)
 H01G(0.765879) H01H(0.762218) H01N(0.411622) H01I(0.721659) H01J(0.611376)
 H01O(0.559268) H01P(0.633534) H01K(0.379677) H01L(0.690087) H01M(0.641563)
 H01Q(0.549902) H01R(0.457231) H01S(0.613756) H01T(0.644034) H01U(0.559682)
 H01V(0.64522)
 Fixed Z: H005(0.535204) H006(0.384569) H008(0.717909) H00A(0.441439)
 H00B(0.471013) H00J(0.392571) H00K(0.172612) H00L(0.213485) H00F(0.485023)
 H00H(0.74707) H00O(0.243855) H00M(0.734016) H00N(0.406659) H00C(0.731221)
 H00D(0.807507) H00E(0.733854) H00G(0.622353) H00I(0.558942) H00Q(0.471983)
 H00R(0.529726) H00S(0.426437) H00T(0.500534) H00U(0.382495) H00V(0.613122)
 H00X(0.586221) H00Y(0.452452) H00Z(0.153806) H010(-0.129236) H011(0.299368)
 H012(0.196596) H013(0.276029) H01A(0.65094) H01B(0.741722) H01C(0.64506)
 H016(0.154985) H01D(0.38301) H01E(0.372392) H01F(0.402776) H018(0.258026)
 H01G(0.468941) H01H(0.52265) H01N(0.002451) H01I(0.705382) H01J(0.737129)
 H01O(0.044031) H01P(0.171514) H01K(0.766285) H01L(0.384289) H01M(0.372824)
 H01Q(-0.106663) H01R(0.965224) H01S(0.873584) H01T(0.960135) H01U(0.890417)
 H01V(0.779047)
;
_shelx_res_checksum              83427
_olex2_submission_special_instructions 'No special instructions were received'