Synthesis of Ir(iii) complexes with Tp(Me2) and acac ligands and their reactivity with electrophiles.
Morales-Cerón, Judith P; Salazar-Pereda, Verónica; Mendoza-Espinosa, Daniel; Alvarado-Rodríguez, José G; Cruz-Borbolla, Julián; Andrade-López, Noemí; Vásquez-Pérez, José M; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13881–13889; doi:10.1039/c5dt01937k

data_7035496
_publ_section_title
;
 Synthesis of Ir(iii) complexes with Tp(Me2) and acac ligands and their
 reactivity with electrophiles.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13881
_journal_page_last               13889
_journal_paper_doi               10.1039/c5dt01937k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C24 H36 B Ir N6 O2'
_chemical_formula_sum            'C24 H36 B Ir N6 O2'
_chemical_formula_weight         643.60
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-08
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-12 deposited with the CCDC.
2015-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.2716(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9841(2)
_cell_length_b                   14.2878(2)
_cell_length_c                   14.0320(3)
_cell_measurement_reflns_used    37312
_cell_measurement_temperature    294
_cell_measurement_theta_max      28.7470
_cell_measurement_theta_min      3.2450
_cell_volume                     2582.20(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      294
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3659
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -87.00  -38.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  156.0000 -175.7382 49

  2 omega  -30.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672   19.0000 -150.0000 121

  3 omega  -17.00   85.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672   57.0000 -120.0000 102

  4 omega  -17.00   85.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672   57.0000   60.0000 102

  5 omega  -17.00   85.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672   57.0000  -60.0000 102

  6 omega  -25.00   52.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672  -99.0000 -120.0000 77

  7 omega  -62.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672  -57.0000  120.0000 102

  8 omega   14.00   87.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672 -153.0000   81.0876 73

  9 omega  -79.00  -31.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  145.0000  -22.4957 48

 10 omega  -85.00  -36.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  153.0000  131.8626 49

 11 omega  -84.00  -35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  152.0000 -147.9658 49

 12 omega  -85.00  -36.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  153.0000   76.7678 49

 13 omega  -33.00   50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672  -92.0000  107.6209 83

 14 omega  -20.00   56.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672 -105.0000  -23.6169 76

 15 omega  -17.00   85.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672   57.0000  120.0000 102

 16 omega  -67.00  -19.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  126.0000  162.4878 48

 17 omega  -80.00  -32.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  147.0000  101.2151 48

 18 omega  -77.00  100.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672    0.0000 -180.0000 177

 19 omega  -77.00  100.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672    0.0000 -120.0000 177

 20 omega  -77.00  -43.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672    0.0000  -90.0000 34

 21 omega  -77.00  100.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3672    0.0000 -150.0000 177
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0319712000
_diffrn_orient_matrix_UB_12      0.0398745000
_diffrn_orient_matrix_UB_13      -0.0029028000
_diffrn_orient_matrix_UB_21      -0.0048663000
_diffrn_orient_matrix_UB_22      0.0110508000
_diffrn_orient_matrix_UB_23      0.0485038000
_diffrn_orient_matrix_UB_31      0.0445890000
_diffrn_orient_matrix_UB_32      -0.0274161000
_diffrn_orient_matrix_UB_33      0.0153484000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1067
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            123703
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.163
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.203
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.318
_refine_diff_density_min         -2.175
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0840P)^2^+4.3492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4560
_reflns_number_total             5261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01937k2.cif
_cod_data_source_block           vero_01
_cod_depositor_comments
'Adding full bibliography for 7035495--7035497.cif.'
_cod_original_cell_volume        2582.21(8)
_cod_database_code               7035496
_chemical_oxdiff_formula         'C22 H30 B1 O2 Ir1 N6'
_chemical_oxdiff_usercomment     'Cristales rojos carbeno Acac'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C12(H12)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              14044
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'