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_7035497
_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         'C20 H25 B Br5 Ir N6 O2, C6 H14'
_chemical_formula_sum            'C26 H39 B Br5 Ir N6 O2'
_chemical_formula_weight         1070.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-13
_audit_creation_method
;
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                 103.2370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8577(5)
_cell_length_b                   16.3125(7)
_cell_length_c                   18.7394(8)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.369
_cell_measurement_theta_min      2.239
_cell_volume                     3528.4(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1536
_diffrn_reflns_av_unetI/netI     0.1026
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18079
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.283
_diffrn_reflns_theta_max         23.283
_diffrn_reflns_theta_min         1.675
_exptl_absorpt_coefficient_mu    9.479
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.3197
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1593 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.4292.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_description       plate
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.353
_refine_diff_density_min         -1.453
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         5076
_refine_ls_number_restraints     393
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1029P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3750
_reflns_number_total             5076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01937k2.cif
_cod_data_source_block           mm014m
_cod_depositor_comments
'Adding full bibliography for 7035495--7035497.cif.'
_cod_database_code               7035497
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22-C23 = C23-C24 = C24-C25 = C25-C26 = C26-C27
 1.54 with sigma of 0.01
 C22-C24 = C23-C25 = C24-C26 = C25-C27
 2.5 with sigma of 0.01
 N1-C1 \\sim N2-C3 \\sim N1-C1A \\sim N2-C3A
 with sigma of 0.01
3. Restrained planarity
 N1, N2, C1, C2, C3, C4, C5, Br1
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C22A \\sim C23A
\\sim C24A \\sim C25A \\sim C26A \\sim C27A: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim Br1 \\sim C1A \\sim C2A \\sim C3A
\\sim C12A \\sim C5A \\sim Br1A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C22, C23, C24, C25, C26, C27, C22A, C23A, C24A, C25A, C26A, C27A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C1, C2, C3, C4, C5, Br1, C1A, C2A, C3A, C12A, C5A, Br1A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
6. Same fragment restrains
{C1, C2, C3, C4, C5, Br1} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1A, C2A, C3A, C12A, C5A, Br1A}
{C22, C23, C24, C25, C26, C27} sigma for 1-2: 0.02, 1-3: 0.04
as
{C22A, C23A, C24A, C25A, C26A, C27A}
7. Others
 Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23A)=Sof(H23C)=Sof(H23D)=
 Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26A)=
 Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=
 Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
 Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C5A)=
 Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(Br1A)=1-FVAR(2)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=
 Sof(H5B)=Sof(H5C)=Sof(Br1)=FVAR(2)
8.a Ternary CH refined with riding coordinates:
 B1(H1)
8.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C23A(H23C,
 H23D), C24A(H24C,H24D), C25A(H25C,H25D), C26A(H26C,H26D)
8.c Me refined with riding coordinates:
 C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C22A(H22D,H22E,H22F), C27A(H27D,
 H27E,H27F)
8.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C), C10(H10A,H10B,
 H10C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C12A(H12A,H12B,H12C), C5A(H5AA,H5AB,
 H5AC), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              56497
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'