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_7048747
_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         'C40 H35 Ir O P2'
_chemical_formula_sum            'C40 H35 Ir O P2'
_chemical_formula_weight         785.82
_chemical_name_common
'Iridium allyl carbonyl bis(triphenylphosphine)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5318)
;
_audit_update_record
;
2018-10-03 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.633(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2878(7)
_cell_length_b                   18.4100(12)
_cell_length_c                   17.6432(11)
_cell_measurement_reflns_used    8117
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      2.32
_cell_volume                     3340.2(4)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      115.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26828
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         1.60
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.124
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.505
_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    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.741
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         9645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                7834
_reflns_number_total             9645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt04723e2.cif
_cod_data_source_block           sbd0303m
_cod_depositor_comments
'Adding full bibliography for 7048745--7048747.cif.'
_cod_database_code               7048747
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C30(H30), C22(H22), C24(H24), C29(H29), C28(H28), C6(H6), C27(H27),
 C18(H18), C12(H12), C21(H21), C14(H14), C15(H15), C20(H20), C10(H10), C8(H8),
 C23(H23), C3(H3), C9(H9), C4(H4), C2(H2), C17(H17), C26(H26), C5(H5), C11(H11),
  C36(H36), C39(H39), C32(H32), C35(H35), C33(H33), C34(H34)
2.b X=CH2 refined with riding coordinates:
 C38(H38a,H38b), C40(H40a,H40b)
;
_olex2_submission_special_instructions 'No special instructions were received'