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_7129986
_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         'C18 H22 N2 O2 P2'
_chemical_formula_sum            'C18 H22 N2 O2 P2'
_chemical_formula_weight         360.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-26
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.9909(4)
_cell_length_b                   6.10090(10)
_cell_length_c                   5.10270(10)
_cell_measurement_reflns_used    29551
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9230
_cell_measurement_theta_min      2.2830
_cell_volume                     840.26(2)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.999
_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  59.00   0.50    0.50    --    5.00 -42.00 117.00  286
  2  \w   -104.00  40.00   0.50    0.50    --  -14.40 -42.00 117.00  288
  3  \w    -68.00  75.00   0.50    0.50    --  -14.40  42.00 -90.00  286
  4  \w    -48.00  94.00   0.50    0.50    --    5.00  42.00 -90.00  284
  5  \w   -104.00  23.00   0.50    0.50    --  -14.40 -60.00 -60.00  254
  6  \w    -52.00  75.00   0.50    0.50    --  -14.40  57.00 120.00  254
  7  \w    -52.00  75.00   0.50    0.50    --  -14.40  60.00 150.00  254
  8  \w    -52.00  75.00   0.50    0.50    --  -14.40  60.00   0.00  254
  9  \w   -104.00  23.00   0.50    0.50    --  -14.40 -60.00  60.00  254
 10  \w   -104.00  23.00   0.50    0.50    --  -14.40 -60.00-180.00  254
 11  \w    -52.00  75.00   0.50    0.50    --  -14.40  60.00 -60.00  254
 12  \w    -52.00  75.00   0.50    0.50    --  -14.40  60.00-120.00  254
 13  \w    -52.00  75.00   0.50    0.50    --  -14.40  60.00  30.00  254
 14  \w   -104.00 -72.00   0.50    0.50    --  -14.40  19.00-180.00   64
 15  \w    -75.00  75.00   0.50    0.50    --  -14.40  38.00-180.00  300
;
_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      -0.0135564000
_diffrn_orient_matrix_UB_12      -0.0899818000
_diffrn_orient_matrix_UB_13      0.0512149000
_diffrn_orient_matrix_UB_21      -0.0034063000
_diffrn_orient_matrix_UB_22      0.0575918000
_diffrn_orient_matrix_UB_23      0.1194240000
_diffrn_orient_matrix_UB_31      -0.0222403000
_diffrn_orient_matrix_UB_32      0.0459607000
_diffrn_orient_matrix_UB_33      -0.0494034000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0088
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            38376
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64937
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.141
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 754 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0203
_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^)+(0.0256P)^2^+0.2683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0545
_reflns_Friedel_coverage         0.646
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1919
_reflns_number_total             1936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00706a2.cif
_cod_data_source_block           P-P(OMe)
_cod_database_code               7129986
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C18 H22 N2 O2 P2'
_chemical_oxdiff_usercomment     PL68
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.945
_reflns_odcompleteness_completeness 99.83
_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)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              38721
_shelx_hkl_checksum              61545
_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 PL68
_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 2.131
_oxdiff_exptl_absorpt_empirical_full_min 0.543