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_7047746
_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         '2(C21 H35 Ir O P2)'
_chemical_formula_sum            'C42 H70 Ir2 O2 P4'
_chemical_formula_weight         1115.26
_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
_audit_creation_date             2017-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-07-12 deposited with the CCDC.
2018-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.215(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2062(7)
_cell_length_b                   14.0106(8)
_cell_length_c                   28.6995(18)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.311
_cell_measurement_theta_min      2.525
_cell_volume                     4459.7(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 0.996
_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  0.0818
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            79985
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.356
_diffrn_reflns_theta_min         1.434
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.138
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.739
_refine_diff_density_min         -1.972
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         11064
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8585
_reflns_number_total             11064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02861c2.cif
_cod_data_source_block           iprpcpirco_0m
_cod_depositor_comments
'Adding full bibliography for 7047742--7047746.cif.'
_cod_database_code               7047746
_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.a Ternary CH refined with riding coordinates:
 C40(H40), C37(H37), C33(H33), C30(H30), C13(H13), C16(H16), C10(H10), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C35(H35A,H35B), C8(H8A,H8B), C8BA(H8BA,H8BB)
2.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C23(H23), C25(H25), C3(H3), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C32(H32A,H32B,
 H32C), C31(H31A,H31B,H31C), C18(H18A,H18B,H18C), C11(H11A,H11B,H11C), C17(H17A,
 H17B,H17C), C34(H34A,H34B,H34C), C20(H20A,H20B,H20C), C41(H41A,H41B,H41C),
 C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C29(H29A,H29B,H29C),
  C14(H14A,H14B,H14C)
;
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'