H<sub>2</sub> addition to (<sup>Me4</sup>PCP)Ir(CO): studies of the isomerization mechanism.
Lekich, Travis T.; Gary, J. Brannon; Bellows, Sarina M.; Cundari, Thomas R.; Guard, Louise M.; Heinekey, D. Michael; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16119–16125; doi:10.1039/c8dt02861c

data_7047745
_publ_section_title
;
 H<sub>2</sub> addition to (<sup>Me4</sup>PCP)Ir(CO): studies of the
 isomerization mechanism.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16119
_journal_page_last               16125
_journal_paper_doi               10.1039/c8dt02861c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C25 H45 Ir O P2, C2.5 H6'
_chemical_formula_sum            'C27.5 H51 Ir O P2'
_chemical_formula_weight         651.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-12 deposited with the CCDC.
2018-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.108(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3793(6)
_cell_length_b                   14.3928(8)
_cell_length_c                   32.473(2)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.49
_cell_volume                     5784.7(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            24968
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.417
_diffrn_reflns_theta_min         1.548
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.744
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1158 before and 0.0444 after correction. The Ratio of minimum to maximum transmission is 0.6197. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         7236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+12.9473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0376
_refine_ls_wR_factor_ref         0.0420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5596
_reflns_number_total             7236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02861c2.cif
_cod_data_source_block           shelx_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7047742--7047746.cif.'
_cod_original_formula_sum        'C27.50 H51 Ir O P2'
_cod_database_code               7047745
_shelxl_version_number           2013-4
_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. Others
 Fixed Sof: H28A(0.5) H28B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C28(H28A,H28B), C29(H29A,H29B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C5(H5)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C17(H17A,H17B,
 H17C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C12(H12A,
 H12B,H12C), C19(H19A,H19B,H19C), C25(H25A,H25B,H25C), C15(H15A,H15B,H15C),
 C20(H20A,H20B,H20C), C30(H30A,H30B,H30C)
;
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'