Using para hydrogen induced polarization to study steps in the hydroformylation reaction.
Guan, Dexin; Godard, Cyril; Polas, Stacey M.; Tooze, Robert P.; Whitwood, Adrian C.; Duckett, Simon B.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2664–2675; doi:10.1039/c8dt04723e

data_7048746
_publ_section_title
;
 Using para hydrogen induced polarization to study steps in the
 hydroformylation reaction.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2664
_journal_page_last               2675
_journal_paper_doi               10.1039/c8dt04723e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C46 H47 Ir O P2'
_chemical_formula_sum            'C46 H47 Ir O P2'
_chemical_formula_weight         869.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-26 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                67.732(2)
_cell_angle_beta                 88.193(2)
_cell_angle_gamma                63.247(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2491(12)
_cell_length_b                   12.2632(12)
_cell_length_c                   16.0048(15)
_cell_measurement_reflns_used    8527
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.53
_cell_volume                     1958.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker Smart Apex'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14091
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.380
_diffrn_reflns_theta_min         1.943
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    3.524
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03; (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.11
_refine_diff_density_max         4.065
_refine_diff_density_min         -2.427
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+4.2994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8745
_reflns_number_total             9580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04723e2.cif
_cod_data_source_block           sbd0409m
_cod_depositor_comments
'Adding full bibliography for 7048745--7048747.cif.'
_cod_database_code               7048746
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.698
_shelx_estimated_absorpt_t_min   0.363
_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
2.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C41(H41), C45(H45), C44(H44), C31(H31), C20(H20), C42(H42),
 C24(H24), C21(H21), C16(H16), C23(H23), C30(H30), C38(H38), C10(H10), C13(H13),
  C27(H27), C28(H28), C37(H37), C14(H14), C6(H6), C7(H7), C35(H35), C34(H34),
 C9(H9), C3(H3)
2.b X=CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C25(H25A,H25B,H25C), C46(H46A,H46B,H46C), C32(H32A,H32B,
 H32C), C18(H18A,H18B,H18C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              55521
_olex2_exptl_crystal_mounting_method 'oil on glass fibre'
_olex2_submission_special_instructions 'No special instructions were received'