Systematic evaluation of the electronic effect of aluminum-containing ligands in iridium-aluminum and rhodium-aluminum bimetallic complexes.
Charles, R. Malcolm; Taylor, Natalie S.; Mercado, Angel A.; Frost, Connor E.; Yokley, Timothy W.; Eckenhoff, William T.; Schley, Nathan D.; DeYonker, Nathan J.; Brewster, Timothy P.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13029–13043; doi:10.1039/d0dt02472d

data_7705412
_publ_section_title
;
 Systematic evaluation of the electronic effect of aluminum-containing
 ligands in iridium-aluminum and rhodium-aluminum bimetallic complexes.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13029
_journal_page_last               13043
_journal_paper_doi               10.1039/d0dt02472d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C43 H37 N O2 P2 Rh, N O3, C3 H3'
_chemical_formula_sum            'C46 H40 N2 O5 P2 Rh'
_chemical_formula_weight         865.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-02 deposited with the CCDC.	2020-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.0310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.44630(10)
_cell_length_b                   16.82500(10)
_cell_length_c                   21.39890(10)
_cell_measurement_reflns_used    32049
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.8390
_cell_measurement_theta_min      3.2880
_cell_volume                     7930.87(9)
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -66.00  35.00   1.00    1.00    --  -36.45  19.00  60.00  101
  2  \w   -106.00 -18.00   1.00    1.00    --  -36.45 -38.00-120.00   88
  3  \w     23.00  90.00   1.00    1.00    --   36.45-125.00 150.00   67
  4  \w     20.00 104.00   1.00    1.00    --   36.45  57.00-150.00   84
  5  \w     23.00  90.00   1.00    1.00    --   36.45-125.00   0.00   67
  6  \w     40.00 126.00   1.00    2.83    --  108.65 -45.00-150.00   86
  7  \w     91.00 177.00   1.00    2.83    --  108.65  45.00   0.00   86
  8  \w    100.00 178.00   1.00    2.83    --  108.65 111.00   0.00   78
  9  \w     40.00 126.00   1.00    2.83    --  108.65 -45.00  60.00   86
 10  \w     39.00 109.00   1.00    2.83    --  108.65 -94.00  60.00   70
 11  \w     39.00 115.00   1.00    2.83    --  108.65-111.00  30.00   76
 12  \w     39.00 109.00   1.00    2.83    --  108.65 -94.00-120.00   70
 13  \w     70.00 178.00   1.00    2.83    --  108.65  15.00 120.00  108
 14  \w   -106.00 -18.00   1.00    1.00    --  -36.45 -38.00  90.00   88
 15  \w    -55.00  33.00   1.00    1.00    --  -36.45  38.00-150.00   88
 16  \w   -104.00 -10.00   1.00    1.00    --  -36.45 -77.00  60.00   94
 17  \w     82.00 176.00   1.00    2.83    --  108.65  77.00 150.00   94
 18  \w     87.00 178.00   1.00    2.83    --  108.65  30.00 -60.00   91
 19  \w     82.00 176.00   1.00    2.83    --  108.65  77.00-150.00   94
 20  \w     39.00 109.00   1.00    2.83    --  108.65 -94.00 150.00   70
 21  \w     91.00 177.00   1.00    2.83    --  108.65  45.00  30.00   86
 22  \w     70.00 178.00   1.00    2.83    --  108.65  15.00-120.00  108
 23  \w    -55.00  33.00   1.00    1.00    --  -36.45  38.00 120.00   88
 24  \w   -104.00 -20.00   1.00    1.00    --  -36.45 -57.00 -30.00   84
 25  \w    -53.00  31.00   1.00    1.00    --  -36.45  57.00 -90.00   84
 26  \w     82.00 176.00   1.00    2.83    --  108.65  77.00-120.00   94
 27  \w     87.00 178.00   1.00    2.83    --  108.65  30.00 150.00   91
 28  \w     82.00 120.00   1.00    2.83    --  108.65  77.00  30.00   38
 29  \w     91.00 177.00   1.00    2.83    --  108.65  45.00 -30.00   86
;
_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      -0.0475586000
_diffrn_orient_matrix_UB_12      0.0372569000
_diffrn_orient_matrix_UB_13      0.0260857000
_diffrn_orient_matrix_UB_21      -0.0489393000
_diffrn_orient_matrix_UB_22      -0.0557360000
_diffrn_orient_matrix_UB_23      -0.0452855000
_diffrn_orient_matrix_UB_31      0.0153383000
_diffrn_orient_matrix_UB_32      -0.0623716000
_diffrn_orient_matrix_UB_33      0.0560214000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46102
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.263
_diffrn_reflns_theta_min         3.305
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.649
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.321
_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    1.450
_exptl_crystal_description       prism
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0155P)^2^+24.9752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7755
_reflns_number_total             7785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02472d2.cif
_cod_data_source_block           tj-17
_cod_depositor_comments
'Adding full bibliography for 7705406--7705412.cif.'
_cod_original_cell_volume        7930.87(8)
_cod_database_code               7705412
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C46H39N2O5P2Rh
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              3423
_olex2_date_sample_data_collection 2019-05-22
_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 1.151
_oxdiff_exptl_absorpt_empirical_full_min 0.875