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_7048745
_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         'C55 H46 Ir O P3, C7 H8'
_chemical_formula_sum            'C62 H54 Ir O P3'
_chemical_formula_weight         1100.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-15 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.22571(13)
_cell_length_b                   18.46616(17)
_cell_length_c                   20.7044(2)
_cell_measurement_reflns_used    39274
_cell_measurement_temperature    115
_cell_measurement_theta_max      31.5440
_cell_measurement_theta_min      2.1270
_cell_volume                     5056.60(8)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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      2.19 182.15   0.30    4.99    --   28.00  73.91 -25.81  600
  2  \w      2.19 132.66   0.30    4.99    --   28.00  73.91  64.19  435
  3  \w      2.19  71.18   0.30    4.99    --   28.00  73.91 154.19  230
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      -0.0106150000
_diffrn_orient_matrix_UB_12      0.0374710000
_diffrn_orient_matrix_UB_13      -0.0032894000
_diffrn_orient_matrix_UB_21      0.0156598000
_diffrn_orient_matrix_UB_22      -0.0013399000
_diffrn_orient_matrix_UB_23      -0.0327325000
_diffrn_orient_matrix_UB_31      -0.0501920000
_diffrn_orient_matrix_UB_32      -0.0083586000
_diffrn_orient_matrix_UB_33      -0.0095269000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0124
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40071
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         1.827
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.777
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_correction_T_min  0.381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Sheldrick)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_recrystallization_method 'Evaporation of toluene'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 6488 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0196(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         14716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0155
_refine_ls_R_factor_gt           0.0152
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+2.0539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0367
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                14579
_reflns_number_total             14716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04723e2.cif
_cod_data_source_block           sbd0306
_cod_depositor_comments
'Adding full bibliography for 7048745--7048747.cif.'
_cod_original_cell_volume        5056.61(8)
_cod_database_code               7048745
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C64 H54 Ir1 O1 P3'
_shelx_estimated_absorpt_t_max   0.532
_shelx_estimated_absorpt_t_min   0.452
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C61B) = Uanis(C58B)
Uanis(C60A) = Uanis(C57A)
Uanis(C58A) = Uanis(C61A)
Uanis(C57B) = Uanis(C60B)
Uanis(C59A) = Uanis(C56A)
Uanis(C56B) = Uanis(C59B)
Uanis(C62B) = Uanis(C62A)
3. Others
 Sof(C56B)=Sof(C57B)=Sof(H57B)=Sof(C58B)=Sof(H58B)=Sof(C59B)=Sof(H59B)=
 Sof(C60B)=Sof(H60B)=Sof(C61B)=Sof(H61B)=Sof(C62B)=Sof(H62A)=Sof(H62B)=
 Sof(H62C)=1-FVAR(1)
 Sof(C58A)=Sof(H58A)=Sof(C59A)=Sof(H59A)=Sof(C60A)=Sof(H60A)=Sof(C61A)=
 Sof(H61A)=Sof(C56A)=Sof(C57A)=Sof(H57A)=Sof(C62A)=Sof(H62D)=Sof(H62E)=
 Sof(H62F)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40),
  C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C57B(H57B),
 C58B(H58B), C59B(H59B), C60B(H60B), C61B(H61B), C58A(H58A), C59A(H59A),
 C60A(H60A), C61A(H61A), C57A(H57A)
4.b Fitted hexagon refined as free rotating group:
 C56B(C57B,C58B,C59B,C60B,C61B), C58A(C59A,C60A,C61A,C56A,C57A)
4.c Idealised Me refined as rotating group:
 C62A(H62D,H62E,H62F), C62B(H62A,H62B,H62C)
;
_shelx_res_checksum              52322
_olex2_exptl_crystal_mounting_method 'oil on glass fibre'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 'SADABS v2.03 (Sheldrick)'