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_7705408
_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 Ir N O2 P2, N O3'
_chemical_formula_sum            'C43 H37 Ir N2 O5 P2'
_chemical_formula_weight         915.88
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-29
_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                 110.521(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1415(5)
_cell_length_b                   11.3474(3)
_cell_length_c                   18.5807(4)
_cell_measurement_reflns_used    15705
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.9010
_cell_measurement_theta_min      2.9360
_cell_volume                     3779.74(18)
_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 0.897
_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    -20.00  56.00   1.00   20.00    --   17.49 -99.00 -90.00   76
  2  \w     35.00  90.00   1.00   20.00    --   17.49 178.00 -60.00   55
  3  \w    -52.00  36.00   1.00   20.00    --   17.49 -38.00 -60.00   88
  4  \w    -52.00  87.00   1.00   20.00    --   17.49   0.00 -60.00  139
  5  \w    -52.00  26.00   1.00   20.00    --   17.49 -38.00  90.00   78
  6  \w     -9.00  85.00   1.00   20.00    --   17.49  77.00  30.00   94
;
_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      0.0056811000
_diffrn_orient_matrix_UB_12      -0.0330478000
_diffrn_orient_matrix_UB_13      0.0340023000
_diffrn_orient_matrix_UB_21      -0.0236656000
_diffrn_orient_matrix_UB_22      -0.0449690000
_diffrn_orient_matrix_UB_23      -0.0220006000
_diffrn_orient_matrix_UB_31      0.0311947000
_diffrn_orient_matrix_UB_32      -0.0281141000
_diffrn_orient_matrix_UB_33      -0.0047448000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45522
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.914
_diffrn_reflns_theta_min         2.215
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.666
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.415
_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    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0122P)^2^+2.5915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0556
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8356
_reflns_number_total             9804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02472d2.cif
_cod_data_source_block           tj-21
_cod_depositor_comments
'Adding full bibliography for 7705406--7705412.cif.'
_cod_original_cell_volume        3779.77(16)
_cod_database_code               7705408
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C43H36IrN2O5P2
_reflns_odcompleteness_completeness 99.90
_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 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), C5(H5), 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)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              71843
_olex2_date_sample_data_collection 2019-05-28
_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 1.718
_oxdiff_exptl_absorpt_empirical_full_min 0.597