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_7129987
_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_formula_moiety         'C28 H37 Cl2 Ir N2 O2 P2'
_chemical_formula_sum            'C28 H37 Cl2 Ir N2 O2 P2'
_chemical_formula_weight         758.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-04 deposited with the CCDC.	2022-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.2803(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2647(3)
_cell_length_b                   24.6280(4)
_cell_length_c                   8.18186(15)
_cell_measurement_reflns_used    25189
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.9680
_cell_measurement_theta_min      2.8270
_cell_volume                     2844.41(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.998
_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  61.00   0.50    1.00    --    5.00 -19.00-180.00  290
  2  \w    -95.00  25.00   0.50    1.00    --   -5.80 -57.00  30.00  240
  3  \w    -95.00  25.00   0.50    1.00    --   -5.80 -57.00-180.00  240
  4  \w    -95.00  26.00   0.50    1.00    --   -5.80 -60.00 -60.00  242
  5  \w    -84.00 -49.00   0.50    1.00    --    5.00 -38.00 -60.00   70
  6  \w    -84.00  37.00   0.50    1.00    --    5.00 -38.00  60.00  242
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type  ROSHyPix
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0502343000
_diffrn_orient_matrix_UB_12      0.0006586000
_diffrn_orient_matrix_UB_13      0.0126289000
_diffrn_orient_matrix_UB_21      -0.0011230000
_diffrn_orient_matrix_UB_22      0.0277808000
_diffrn_orient_matrix_UB_23      0.0226265000
_diffrn_orient_matrix_UB_31      0.0002965000
_diffrn_orient_matrix_UB_32      -0.0075807000
_diffrn_orient_matrix_UB_33      0.0836739000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            31747
_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         27.485
_diffrn_reflns_theta_min         2.870
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    5.024
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.772
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.333
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.011(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6469
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0437P)^2^+0.3213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.986
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                6328
_reflns_number_total             6469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00706a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2844.42(9)
_cod_database_code               7129987
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C28 H37 N2 O2 P2 Cl Ir'
_chemical_oxdiff_usercomment     MS2723
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.152
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C13(H13), C14(H14), C16(H16), C17(H17)
2.c 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              23520
_shelx_hkl_checksum              81567
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id ms2723
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.879
_oxdiff_exptl_absorpt_empirical_full_min 0.556