Synthesis and reactivity of iridium complexes of a macrocyclic PNP pincer ligand.
Hood, Thomas M.; Chaplin, Adrian B.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2472–2482; doi:10.1039/d0dt04303f

data_7706526
_publ_section_title
;
 Synthesis and reactivity of iridium complexes of a macrocyclic PNP pincer
 ligand.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2472
_journal_page_last               2482
_journal_paper_doi               10.1039/d0dt04303f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C47 H83 Ir0.96 N P1.91, 0.04(Ir P2), C32 H12 B F24'
_chemical_formula_sum            'C79 H95 B F24 Ir N P2'
_chemical_formula_weight         1779.50
_chemical_melting_point          ?
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-18 deposited with the CCDC.	2021-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                72.0620(8)
_cell_angle_beta                 88.7669(7)
_cell_angle_gamma                88.6010(8)
_cell_formula_units_Z            2
_cell_length_a                   14.33551(13)
_cell_length_b                   17.06824(16)
_cell_length_c                   17.35886(15)
_cell_measurement_reflns_used    61561
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.5490
_cell_measurement_theta_min      3.0260
_cell_volume                     4039.29(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -66.00  33.00   1.00    1.00    --  -41.82  37.00  60.00   99
  2  \w   -116.00 -17.00   1.00    1.00    --  -41.82 -37.00-120.00   99
  3  \w    -87.00  -6.00   1.00    1.00    --  -41.82 125.00 120.00   81
  4  \w    -66.00  33.00   1.00    1.00    --  -41.82  37.00-180.00   99
  5  \w      7.00  33.00   1.00    1.00    --   41.82  84.00  60.67   26
  6  \w      8.00  34.00   1.00    1.00    --   41.82  83.00 -25.30   26
  7  \w     10.00  36.00   1.00    1.00    --   41.82  75.00 124.50   26
  8  \w      8.00  34.00   1.00    1.00    --   41.82  83.00 -92.53   26
  9  \w     97.00 178.00   1.00    4.00    --  107.00 125.00   0.00   81
 10  \w     78.00 178.00   1.00    4.00    --  107.00  61.00 -30.00  100
 11  \w     34.00 112.00   1.00    4.00    --  107.00-125.00 -60.00   78
 12  \w     24.00 107.00   1.00    4.00    --  107.00 -94.00  90.00   83
 13  \w     35.00 136.00   1.00    4.00    --  107.00 -61.00 120.00  101
 14  \w     34.00 133.00   1.00    4.00    --  107.00 -45.00  60.00   99
 15  \w    103.00 178.00   1.00    4.00    --  107.00  77.00   0.00   75
 16  \w     97.00 178.00   1.00    4.00    --  107.00 125.00-120.00   81
 17  \w     78.00 178.00   1.00    4.00    --  107.00  61.00  60.00  100
 18  \w     81.00 178.00   1.00    4.00    --  107.00  45.00  90.00   97
 19  \w     34.00 112.00   1.00    4.00    --  107.00-125.00 -30.00   78
 20  \w     97.00 178.00   1.00    4.00    --  107.00 125.00  90.00   81
 21  \w     24.00 107.00   1.00    4.00    --  107.00 -94.00-180.00   83
 22  \w    103.00 178.00   1.00    4.00    --  107.00  77.00 120.00   75
 23  \w     24.00 107.00   1.00    4.00    --  107.00 -94.00  60.00   83
 24  \w     34.00 112.00   1.00    4.00    --  107.00-125.00  60.00   78
 25  \w     24.00 107.00   1.00    4.00    --  107.00 -94.00 -90.00   83
 26  \w     24.00 107.00   1.00    4.00    --  107.00 -94.00   0.00   83
 27  \w     81.00 178.00   1.00    4.00    --  107.00  45.00 -30.00   97
 28  \w     24.00 107.00   1.00    4.00    --  107.00 -94.00 150.00   83
 29  \w    103.00 178.00   1.00    4.00    --  107.00  77.00-180.00   75
 30  \w    103.00 178.00   1.00    4.00    --  107.00  77.00-120.00   75
 31  \w     78.00 178.00   1.00    4.00    --  107.00  61.00   0.00  100
 32  \w     24.00 107.00   1.00    4.00    --  107.00 -94.00 -60.00   83
 33  \w     34.00 112.00   1.00    4.00    --  107.00-125.00 120.00   78
 34  \w   -114.00 -14.00   1.00    1.00    --  -41.82 -57.00   0.00  100
 35  \w    -87.00  -6.00   1.00    1.00    --  -41.82 125.00-150.00   81
 36  \w   -114.00 -14.00   1.00    1.00    --  -41.82 -57.00  60.00  100
 37  \w   -116.00 -17.00   1.00    1.00    --  -41.82 -37.00 120.00   99
 38  \w      7.00  33.00   1.00    1.00    --   41.82  84.00-129.58   26
 39  \w      8.00  34.00   1.00    1.00    --   41.82  83.00  27.49   26
 40  \w      8.00  42.00   1.00    1.00    --   41.82  82.00 173.79   34
 41  \w     81.00 176.00   1.00    4.00    --  107.00  45.00-150.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0879328000
_diffrn_orient_matrix_UB_12      -0.0309836000
_diffrn_orient_matrix_UB_13      -0.0301218000
_diffrn_orient_matrix_UB_21      -0.0482095000
_diffrn_orient_matrix_UB_22      0.0845397000
_diffrn_orient_matrix_UB_23      -0.0122812000
_diffrn_orient_matrix_UB_31      0.0387522000
_diffrn_orient_matrix_UB_32      0.0299437000
_diffrn_orient_matrix_UB_33      -0.0874375000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78361
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        70.075
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         6.363
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.431
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
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    1.463
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_recrystallization_method
'Crystals grown from Et2O-SiMe4 at 293 K'
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.097
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1110
_refine_ls_number_reflns         15312
_refine_ls_number_restraints     540
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0220
_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^)+(0.0235P)^2^+3.1414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14980
_reflns_number_total             15312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04303f2.cif
_cod_data_source_block           0564abc19s
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7706524--7706528.cif.
;
_cod_database_code               7706526
_shelx_shelxl_version_number     2014/7
_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
 C208-F4 \\sim C208-F5 \\sim C208-F6 \\sim C208-F4A \\sim C208-F5A \\sim
C208-F6A
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4A-F5A \\sim F5A-F6A \\sim F6A-F4A
 with sigma of 0.01
 C205-F4 \\sim C205-F5 \\sim C205-F6 \\sim C205-F4A \\sim C205-F5A \\sim
C205-F6A
 with sigma of 0.01
 C223-F13 \\sim C223-F14 \\sim C223-F15 \\sim C223-F13A \\sim C223-F14A \\sim
C223-F15A
 with sigma of 0.01
 F13-F14 \\sim F14-F15 \\sim F15-F13 \\sim F13A-F14A \\sim F14A-F15A \\sim
F15A-F13A
 with sigma of 0.01
 C219-F13 \\sim C219-F14 \\sim C219-F15 \\sim C219-F13A \\sim C219-F14A \\sim
C219-F15A
 with sigma of 0.01
 C231-F19 \\sim C231-F20 \\sim C231-F21 \\sim C231-F19A \\sim C231-F20A \\sim
C231-F21A
 with sigma of 0.01
 F19-F20 \\sim F20-F21 \\sim F21-F19 \\sim F19A-F20A \\sim F20A-F21A \\sim
F21A-F19A
 with sigma of 0.01
 C227-F19 \\sim C227-F20 \\sim C227-F21 \\sim C227-F19A \\sim C227-F20A \\sim
C227-F21A
 with sigma of 0.01
 C232-F22 \\sim C232-F23 \\sim C232-F24 \\sim C232-F22A \\sim C232-F23A \\sim
C232-F24A
 with sigma of 0.01
 F22-F23 \\sim F23-F24 \\sim F24-F22 \\sim F22A-F23A \\sim F23A-F24A \\sim
F24A-F22A
 with sigma of 0.01
 C229-F22 \\sim C229-F23 \\sim C229-F24 \\sim C229-F22A \\sim C229-F23A \\sim
C229-F24A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6 \\sim F6A
\\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12 \\sim F13 \\sim F13A
\\sim F14 \\sim F14A \\sim F15 \\sim F15A \\sim F16 \\sim F17 \\sim F18 \\sim
F19 \\sim F19A \\sim F20 \\sim F20A \\sim F21 \\sim F21A \\sim F22 \\sim F22A
\\sim F23 \\sim F23A \\sim F24 \\sim F24A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6)
\\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq,
Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F14) \\sim Ueq,
Uanis(F14A) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F15A) \\sim Ueq, Uanis(F16)
\\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq,
Uanis(F19A) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F20A) \\sim Ueq, Uanis(F21)
\\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F22A) \\sim Ueq,
Uanis(F23) \\sim Ueq, Uanis(F23A) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F24A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(Ir1A)=Sof(P2A)=Sof(P3A)=1-FVAR(1)
 Sof(Ir1)=Sof(P2)=Sof(P3)=FVAR(1)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(2)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(2)
 Fixed Sof: F4(0.5) F4A(0.5) F5(0.5) F5A(0.5) F6(0.5) F6A(0.5) F13(0.5)
 F13A(0.5) F14(0.5) F14A(0.5) F15(0.5) F15A(0.5) F22(0.5) F22A(0.5) F23(0.5)
 F23A(0.5) F24(0.5) F24A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C107(H10A,H10B), C108(H10C,H10D), C117(H11V,H11W), C118(H11X,H11Y), C119(H11Z,
 H), C120(H12D,H12E), C121(H12F,H12G), C122(H12H,H12I), C123(H12J,H12K),
 C124(H12L,H12M), C125(H12N,H12O), C126(H12P,H12Q), C127(H12R,H12S), C128(H12T,
 H12U), C129(H12V,H12W), C130(H13D,H13E)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C103(H103), C104(H104), C105(H105), C202(H202),
 C204(H204), C206(H206), C210(H210), C212(H212), C214(H214), C218(H218),
 C220(H220), C222(H222), C226(H226), C228(H228), C230(H230)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C), C110(H11D,H11E,H11F), C111(H11G,H11H,H11I),
 C112(H11J,H11K,H11L), C114(H11M,H11N,H11O), C115(H11P,H11Q,H11R), C116(H11S,
 H11T,H11U)
;
_shelx_res_checksum              79061
_shelx_hkl_checksum              80745
_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 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.826