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_7706525
_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         'C41 H61 Ir N P2, C32 H12 B F24'
_chemical_formula_sum            'C73 H73 B F24 Ir N P2'
_chemical_formula_weight         1685.27
_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             2019-05-10
_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                 95.272(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6582(2)
_cell_length_b                   13.3891(2)
_cell_length_c                   39.2775(10)
_cell_measurement_reflns_used    12406
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.3440
_cell_measurement_theta_min      3.3280
_cell_volume                     7152.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  32.00   1.00   15.00    --  -42.07  37.00  60.00   98
  2  \w   -117.00 -18.00   1.00   15.00    --  -42.07 -37.00  60.00   99
  3  \w     23.00  98.00   1.00   15.00    --   42.07-125.00-180.00   75
  4  \w     34.00 133.00   1.00   60.00    --  107.00 -45.00-180.00   99
  5  \w     81.00 178.00   1.00   60.00    --  107.00  45.00   0.00   97
  6  \w     24.00 110.00   1.00   60.00    --  107.00 -94.00  60.00   86
  7  \w     34.00 118.00   1.00   60.00    --  107.00-125.00-150.00   84
  8  \w     24.00 110.00   1.00   60.00    --  107.00 -94.00 -30.00   86
  9  \w     34.00 133.00   1.00   60.00    --  107.00 -45.00  30.00   99
 10  \w     81.00 178.00   1.00   60.00    --  107.00  45.00 120.00   97
 11  \w     34.00 118.00   1.00   60.00    --  107.00-125.00 -90.00   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      -0.1097051000
_diffrn_orient_matrix_UB_12      -0.0011852000
_diffrn_orient_matrix_UB_13      0.0062468000
_diffrn_orient_matrix_UB_21      0.0273148000
_diffrn_orient_matrix_UB_22      0.0247075000
_diffrn_orient_matrix_UB_23      0.0380031000
_diffrn_orient_matrix_UB_31      -0.0071174000
_diffrn_orient_matrix_UB_32      0.1123525000
_diffrn_orient_matrix_UB_33      -0.0082882000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            42570
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        70.067
_diffrn_reflns_theta_max         70.067
_diffrn_reflns_theta_min         6.509
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.974
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (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            'pale pink'
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3384
_exptl_crystal_recrystallization_method
'Crystals grown from C6H5F-hexane at 243 K'
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.007
_refine_diff_density_max         1.959
_refine_diff_density_min         -1.823
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     981
_refine_ls_number_reflns         13504
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+17.6757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10269
_reflns_number_total             13504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04303f2.cif
_cod_data_source_block           0500abc19s
_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               7706525
_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
 C216-F10 \\sim C216-F11 \\sim C216-F12 \\sim C216-F10A \\sim C216-F11A \\sim
C216-F12A
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F10A-F11A \\sim F11A-F12A \\sim
F12A-F10A
 with sigma of 0.01
 C213-F10 \\sim C213-F11 \\sim C213-F12 \\sim C213-F10A \\sim C213-F11A \\sim
C213-F12A
 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 F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9
\\sim F10 \\sim F10A \\sim F11 \\sim F11A \\sim F12 \\sim F12A \\sim F13 \\sim
F14 \\sim F15 \\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F20 \\sim F21 \\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(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F10A) \\sim Ueq,
Uanis(F11) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F12A)
\\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq,
Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19)
\\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\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 0.007 and sigma for terminal
atoms of 0.014
4. Others
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(1)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(1)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C107(H10C,H10D), C108(H10A,H10B), C117(H11A,H11B), C118(H11W,H11X), C119(H11I,
 H11J), C120(H12K,H12L), C121(H12C,H12D), C122(H12M,H12N), C123(H12G,H12H),
 C124(H12O,H12P), C125(H12A,H12B), C126(H12Q,H12R), C127(H12I,H12J), C128(H12S,
 H12T), C129(H12E,H12F), C130(H13A,H13B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14),
 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:
 C110(H11K,H11L,H11M), C111(H11C,H11D,H11E), C112(H11N,H11O,H11P), C114(H11Q,
 H11R,H11S), C115(H11F,H11G,H11H), C116(H11T,H11U,H11V)
;
_shelx_res_checksum              99783
_shelx_hkl_checksum              24025
_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 4.009
_oxdiff_exptl_absorpt_empirical_full_min 0.532