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_7706524
_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         'C37 H65 Ir N P2, C32 H12 B F24'
_chemical_formula_sum            'C69 H77 B F24 Ir N P2'
_chemical_formula_weight         1641.26
_chemical_melting_point          ?
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-10-16
_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                90
_cell_angle_beta                 100.3117(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5578(3)
_cell_length_b                   19.4887(3)
_cell_length_c                   19.6039(3)
_cell_measurement_reflns_used    35385
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.6400
_cell_measurement_theta_min      2.8230
_cell_volume                     6975.58(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_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 0.999
_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    -97.00   2.00   1.00    6.00    --  -22.18 -37.00  60.00   99
  2  \w    -51.00  48.00   1.00    6.00    --   23.58 -37.00 150.00   99
  3  \w     -9.00 100.00   1.00    6.00    --   23.58  77.00 -60.00  109
  4  \w     35.00 112.00   1.00    6.00    --   23.58 178.00 120.00   77
  5  \w   -111.00 -57.00   1.00    6.00    --  -22.18-178.00-180.00   54
  6  \w     35.00  71.00   1.00    6.00    --   23.58 178.00-150.00   36
  7  \w     -1.00  83.00   1.00    6.00    --   23.58  37.00-120.00   84
;
_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      0.0104995000
_diffrn_orient_matrix_UB_12      -0.0101055000
_diffrn_orient_matrix_UB_13      0.0351299000
_diffrn_orient_matrix_UB_21      0.0367926000
_diffrn_orient_matrix_UB_22      -0.0034897000
_diffrn_orient_matrix_UB_23      -0.0048586000
_diffrn_orient_matrix_UB_31      0.0067308000
_diffrn_orient_matrix_UB_32      0.0347903000
_diffrn_orient_matrix_UB_33      0.0097269000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            87992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.102
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.972
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.066
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
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    1.563
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3304
_exptl_crystal_recrystallization_method
'Crystals grown from CH2Cl2-hexane at 293 K'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         2.042
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1004
_refine_ls_number_reflns         15378
_refine_ls_number_restraints     631
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+9.4442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13274
_reflns_number_total             15378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04303f2.cif
_cod_data_source_block           0465abc19s
_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_original_cell_volume        6975.6(2)
_cod_database_code               7706524
_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
 C423-F13 \\sim C423-F14 \\sim C423-F15 \\sim C423-F13A \\sim C423-F14A \\sim
C423-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
 C419-F13 \\sim C419-F14 \\sim C419-F15 \\sim C419-F13A \\sim C419-F14A \\sim
C419-F15A
 with sigma of 0.01
 C407-F1 \\sim C407-F2 \\sim C407-F3 \\sim C507-F1A \\sim C507-F2A \\sim
C507-F3A
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.01
 C403-F1 \\sim C403-F2 \\sim C403-F3 \\sim C403-F1A \\sim C403-F2A \\sim
C403-F3A
 with sigma of 0.01
 C403-C407 \\sim C403-C507
 with sigma of 0.01
 C415-F7 \\sim C415-F8 \\sim C415-F9 \\sim C415-F7A \\sim C415-F8A \\sim
C415-F9A
 with sigma of 0.01
 F7-F8 \\sim F8-F9 \\sim F9-F7 \\sim F7A-F8A \\sim F8A-F9A \\sim F9A-F7A
 with sigma of 0.01
 C411-F7 \\sim C411-F8 \\sim C411-F9 \\sim C411-F7A \\sim C411-F8A \\sim
C411-F9A
 with sigma of 0.01
 C424-F16 \\sim C424-F17 \\sim C424-F18 \\sim C424-F16A \\sim C424-F17A \\sim
C424-F18A
 with sigma of 0.01
 F16-F17 \\sim F17-F18 \\sim F18-F16 \\sim F16A-F17A \\sim F17A-F18A \\sim
F18A-F16A
 with sigma of 0.01
 C421-F16 \\sim C421-F17 \\sim C421-F18 \\sim C421-F16A \\sim C421-F17A \\sim
C421-F18A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F4 \\sim F5 \\sim F6
\\sim F7 \\sim F7A \\sim F8 \\sim F8A \\sim F9 \\sim F9A \\sim F10 \\sim F11
\\sim F12 \\sim F13 \\sim F13A \\sim F14 \\sim F14A \\sim F15 \\sim F15A \\sim
F16 \\sim F16A \\sim F17 \\sim F17A \\sim F18 \\sim F18A \\sim F19 \\sim F20
\\sim F21 \\sim F22 \\sim F23 \\sim F24 \\sim C407 \\sim C507: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F1) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F2A)
\\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F4) \\sim Ueq,
Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F7A) \\sim
Ueq, Uanis(F8) \\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F9A)
\\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(F16A) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F17A) \\sim Ueq, Uanis(F18)
\\sim Ueq, Uanis(F18A) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq,
Uanis(F21) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24)
\\sim Ueq, Uanis(C407) \\sim Ueq, Uanis(C507) \\sim Ueq: with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(C407) = Uanis(C507)
4. Others
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(C507)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C407)=FVAR(2)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(3)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(3)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(4)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C9(H9)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C11(H11A,H11B), C107(H10C,H10D),
 C108(H10E,H10F), C117(H11U,H11V), C118(H11W,H11X), C119(H,H11Y), C120(H12A,
 H12B), C121(H12C,H12D), C122(H12E,H12F), C123(H12G,H12H), C124(H12I,H12J),
 C125(H12K,H12L), C126(H12M,H12N), C127(H12O,H12P), C128(H12Q,H12R), C129(H12S,
 H12T), C130(H13A,H13B)
5.c Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105), C402(H402), C404(H404), C406(H406),
 C410(H410), C412(H412), C414(H414), C418(H418), C420(H420), C422(H422),
 C426(H426), C428(H428), C430(H430)
5.d Idealised Me refined as rotating group:
 C110(H11C,H11D,H11E), C111(H11F,H11G,H11H), C112(H11I,H11J,H11K), C114(H11L,
 H11M,H11N), C115(H11O,H11P,H11Q), C116(H11R,H11S,H11T)
;
_shelx_res_checksum              34104
_shelx_hkl_checksum              79937
_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 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.695