Reversible P–P bond cleavage at an iridium(iii) metal centre
Coles, Simon J.; Horton, Peter N.; Kimber, Patrick; Klooster, Wim T.; Liu, Pingchuan; Plasser, Felix; Smith, Martin B.; Tizzard, Graham J.; Chemical Communications  (2022) –; doi:10.1039/D2CC00706A

data_7129988
_publ_section_title
;
 Reversible P--P bond cleavage at an iridium(iii) metal centre
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00706A
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H35 Au Cl3 Ir N2 O2 P2, C Cl3 D'
_chemical_formula_sum            'C29 H35 Au Cl6 D Ir N2 O2 P2'
_chemical_formula_weight         1109.41
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-05 deposited with the CCDC.	2022-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6870(2)
_cell_length_b                   15.3847(3)
_cell_length_c                   16.7249(3)
_cell_measurement_reflns_used    23356
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.9500
_cell_measurement_theta_min      1.9220
_cell_volume                     3521.77(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_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    -84.00  36.00   0.50    2.00    --    5.00 -54.00 142.00  240
  2  \w    -45.00  76.00   0.50    2.00    --  -13.40  54.00 -73.00  242
  3  \w    -45.00  61.00   0.50    2.00    --  -13.40  57.00  60.00  212
  4  \w    -38.00  62.00   0.50    2.00    --  -13.40  38.00   0.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
;
Rigaku FRE+ diffractometer with Arc)Sec VHF Varimax confocal mirrors, an AFC12 goniometer and HyPix 6000HE detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0435344000
_diffrn_orient_matrix_UB_12      -0.0015516000
_diffrn_orient_matrix_UB_13      0.0229760000
_diffrn_orient_matrix_UB_21      0.0143426000
_diffrn_orient_matrix_UB_22      -0.0408327000
_diffrn_orient_matrix_UB_23      0.0158251000
_diffrn_orient_matrix_UB_31      0.0241680000
_diffrn_orient_matrix_UB_32      0.0213731000
_diffrn_orient_matrix_UB_33      0.0319357000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, Arc)Sec VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            46521
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.335
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    8.513
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.013
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         3.288
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details
;
 Flack x determined using 3142 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         8067
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+9.7987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0656
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7524
_reflns_number_total             8067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00706a2.cif
_cod_data_source_block           3-CDCl3
_cod_database_code               7129988
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H35 Au Cl6 D Ir N2 O2 P2'
_chemical_oxdiff_usercomment     ms2828
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.343
_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. Restrained distances
 Cl5A-C29 \\sim Cl5B-C29
 with sigma of 0.02
 Cl6A-C29 \\sim Cl6B-C29
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl4, C29, Cl5A, Cl6A, Cl5B, Cl6B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(D29A)=Sof(Cl5B)=Sof(Cl6B)=1-FVAR(1)
 Sof(D29)=Sof(Cl5A)=Sof(Cl6A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C29(D29), C29(D29A)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C14(H14), C16(H16), C17(H17)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              69067
_shelx_hkl_checksum              82488
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.776
_oxdiff_exptl_absorpt_empirical_full_min 0.406