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_1565203
_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         '2(C20 H27 N4 O2 Rh)'
_chemical_formula_sum            'C40 H54 N8 O4 Rh2'
_chemical_formula_weight         916.73
_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                93.506(2)
_cell_angle_beta                 102.353(3)
_cell_angle_gamma                92.412(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6115(3)
_cell_length_b                   10.8579(3)
_cell_length_c                   17.2908(7)
_cell_measurement_reflns_used    8554
_cell_measurement_temperature    99.94(14)
_cell_measurement_theta_max      29.6480
_cell_measurement_theta_min      2.6560
_cell_volume                     1939.34(11)
_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      99.94(14)
_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 0.873
_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   12.00    --   17.65 -77.00   0.00   94
  2  \w     -9.00  85.00   1.00   12.00    --   17.65  77.00 120.00   94
  3  \w     -9.00  85.00   1.00   12.00    --   17.65  77.00 -60.00   94
  4  \w      1.00  85.00   1.00   12.00    --   17.65  57.00  90.00   84
  5  \w     -1.00  87.00   1.00   12.00    --   17.65  38.00 -90.00   88
  6  \w    -50.00  34.00   1.00   12.00    --   17.65 -57.00  90.00   84
  7  \w    -85.00  -1.00   1.00   12.00    --  -17.73 -57.00 120.00   84
;
_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      -0.0051296000
_diffrn_orient_matrix_UB_12      0.0147936000
_diffrn_orient_matrix_UB_13      -0.0399064000
_diffrn_orient_matrix_UB_21      0.0137852000
_diffrn_orient_matrix_UB_22      0.0633445000
_diffrn_orient_matrix_UB_23      0.0129183000
_diffrn_orient_matrix_UB_31      0.0669394000
_diffrn_orient_matrix_UB_32      -0.0081142000
_diffrn_orient_matrix_UB_33      0.0036402000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27019
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.921
_diffrn_reflns_theta_min         2.418
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.720
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         9803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0270P)^2^+0.8482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7686
_reflns_number_total             9803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tj05.cif
_cod_data_source_block           tj05
_cod_original_cell_volume        1939.35(10)
_cod_database_code               1565203
_reflns_odcompleteness_completeness 99.92
_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.a Ternary CH refined with riding coordinates:
 C2(H2), C13(H13), C16(H16), C17(H17), C20(H20), C26(H26), C33(H33), C34(H34),
 C37(H37), C38(H38)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C18(H18A,H18B), C19(H19A,H19B), C35(H35A,
 H35B), C36(H36A,H36B), C39(H39A,H39B), C40(H40A,H40B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), C22(H22), C29(H29)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              31671
_shelx_hkl_checksum              45949
_olex2_date_sample_data_collection 2018-10-17
_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 1.941
_oxdiff_exptl_absorpt_empirical_full_min 0.616