Cationic Protic Imidazolylidene NHC Complexes of Cp*IrCl+ and Cp*RhCl+ with a Pyridyl Tether Formed at Ambient Temperature
Grotjahn, D.B.; Martin, J.K.; Tom, T.N.; Rheingold, A.L.; Inorganics 6 (2018) 27–; doi:10.3390/inorganics6010027

data_1556591
_publ_section_title
;
 Cationic Protic Imidazolylidene NHC Complexes of Cp*IrCl+ and Cp*RhCl+
 with a Pyridyl Tether Formed at Ambient Temperature
;
_journal_name_full               Inorganics
_journal_page_first              27
_journal_paper_doi               10.3390/inorganics6010027
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety
'2(C23 H32 Cl Ir N3), C4 H8 F18 K O P3, C4 H8 O'
_chemical_formula_sum            'C54 H84 Cl2 F18 Ir2 K N6 O2 P3'
_chemical_formula_weight         1778.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.6979(12)
_cell_length_b                   20.6402(10)
_cell_length_c                   28.5118(13)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.00
_cell_measurement_theta_min      10.49
_cell_volume                     13357.5(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            73349
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        65.104
_diffrn_reflns_theta_max         65.104
_diffrn_reflns_theta_min         3.283
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.412
_exptl_absorpt_correction_T_max  0.4542
_exptl_absorpt_correction_T_min  0.1407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7040
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.058
_refine_diff_density_min         -1.662
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         11166
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      2.980
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+49.7045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8943
_reflns_number_total             11166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            9bIr_plus_KPF6_Fig1_Grot292.cif
_cod_data_source_block           grot292
_cod_database_code               1556591
_shelx_estimated_absorpt_t_max   0.454
_shelx_estimated_absorpt_t_min   0.141
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H4SB-C4S
 0.9 with sigma of 0.001
 H4SA-C4S
 0.9 with sigma of 0.001
 H3SB-C3S
 0.9 with sigma of 0.001
 H3SA-C3S
 0.9 with sigma of 0.001
 H2SA-C2S
 0.9 with sigma of 0.001
 H2SB-C2S
 0.9 with sigma of 0.001
 H2SC-C2SB
 0.9 with sigma of 0.001
 H2SD-C2SB
 0.9 with sigma of 0.001
 H1SA-C1S
 0.9 with sigma of 0.001
 H1SB-C1S
 0.9 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C2S) \\sim Ueq, Uanis(C2SB) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: C2S(0.5) H2SA(0.5) H2SB(0.5) C2SB(0.5) H2SC(0.5) H2SD(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C4'(H4'A,H4'B), C1S(H1SA,H1SB), C2S(H2SA,H2SB), C2SB(H2SC,H2SD),
 C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB), C6S(H6SA,H6SB), C7S(H7SA,H7SB),
  C8S(H8SA,H8SB)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C3'(H3'), C6'(H6'), C7'(H7'),
 C8'(H8'), C9'(H9'), N2(H2), N2'(H2')
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C11'(H11D,H11E,H11F), C12'(H12D,H12E,H12F), C13'(H13D,H13E,H13F),
 C19'(H19D,H19E,H19F), C20'(H20D,H20E,H20F), C21'(H21D,H21E,H21F), C22'(H22D,
 H22E,H22F), C23'(H23D,H23E,H23F)
;