Rhodium and iridium NNO-Scorpionate complexes: synthesis, structure, and reactivity with aluminum alkyls
Yokley, Timothy W.; Schley, Nathan D.; Brewster, Timothy P.; Inorganica Chimica Acta 506 (2020) 119529–; doi:10.1016/j.ica.2020.119529

data_1565204
_publ_section_title
;
 Rhodium and iridium NNO-Scorpionate complexes: synthesis, structure, and
 reactivity with aluminum alkyls
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119529
_journal_paper_doi               10.1016/j.ica.2020.119529
_journal_volume                  506
_journal_year                    2020
_chemical_formula_moiety
'C20 H28 Ir N4 O2, 2.5(C H2 Cl2), C32 H12 B F24'
_chemical_formula_sum            'C54.5 H45 B Cl5 F24 Ir N4 O2'
_chemical_formula_weight         1624.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                108.581(3)
_cell_angle_beta                 92.978(2)
_cell_angle_gamma                103.244(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7123(3)
_cell_length_b                   12.9256(4)
_cell_length_c                   20.2507(5)
_cell_measurement_reflns_used    23662
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5110
_cell_measurement_theta_min      3.1870
_cell_volume                     3041.86(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.891
_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    -50.00  44.00   1.00   10.00    --   17.65 -77.00 150.00   94
  2  \w     -9.00  85.00   1.00   10.00    --   17.65  77.00-150.00   94
  3  \w      1.00  85.00   1.00   10.00    --   17.65  57.00  90.00   84
  4  \w    -50.00  34.00   1.00   10.00    --   17.65 -57.00 -90.00   84
  5  \w     -9.00  85.00   1.00   10.00    --   17.65  77.00   0.00   94
  6  \w    -85.00 -35.00   1.00   10.00    --  -17.73 148.00  15.00   50
  7  \w    -71.00 -22.00   1.00   10.00    --  -17.73 124.00-148.00   49
  8  \w     -1.00  87.00   1.00   10.00    --   17.65  38.00 -60.00   88
  9  \w      1.00  85.00   1.00   10.00    --   17.65  57.00-180.00   84
 10  \w     35.00  78.00   1.00   10.00    --   17.65 178.00 -30.00   43
 11  \w     35.00  90.00   1.00   10.00    --   17.65 178.00 120.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0130383000
_diffrn_orient_matrix_UB_12      -0.0287752000
_diffrn_orient_matrix_UB_13      -0.0367862000
_diffrn_orient_matrix_UB_21      -0.0503861000
_diffrn_orient_matrix_UB_22      -0.0315235000
_diffrn_orient_matrix_UB_23      0.0052877000
_diffrn_orient_matrix_UB_31      -0.0252649000
_diffrn_orient_matrix_UB_32      0.0420941000
_diffrn_orient_matrix_UB_33      -0.0031267000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            57450
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.005
_diffrn_reflns_theta_min         2.246
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.533
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.173
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       block
_exptl_crystal_F_000             1598
_exptl_crystal_size_max          0.535
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.122
_refine_diff_density_max         1.631
_refine_diff_density_min         -1.896
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         15839
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0404P)^2^+3.9113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14141
_reflns_number_total             15839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tj08.cif
_cod_data_source_block           tj08
_cod_original_cell_volume        3041.86(15)
_cod_original_formula_sum        'C54.50 H45 B Cl5 F24 Ir N4 O2'
_cod_database_code               1565204
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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. Rigid body (RIGU) restrains
 F4, F4A, F5, F5A, F6, F6A, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F19, F19A, F20, F20A, F21, F21A, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(2)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(2)
 Fixed Sof: C55(0.5) H55A(0.5) H55B(0.5)
4.a Ternary CH refined with riding coordinates:
 C2(H2), C13(H13), C14(H14), C17(H17), C18(H18)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C15(H15A,H15B), C16(H16A,H16B), C19(H19A,H19B), C20(H20A,H20B),
 C54(H54A,H54B), C55(H55A,H55B), C53(H53A,H53B)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C22(H22), C24(H24), C26(H26), C30(H30), C32(H32), C34(H34), C38(H38),
 C40(H40), C42(H42), C46(H46), C48(H48), C50(H50)
4.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              78314
_shelx_hkl_checksum              56589
_olex2_date_sample_data_collection 2019-02-09
_olex2_exptl_crystal_mounting_method 'mounted in a polyimide loop'
_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 2.061
_oxdiff_exptl_absorpt_empirical_full_min 0.356