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_7705407
_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, C H2 Cl2'
_chemical_formula_sum            'C44 H39 Cl2 Ir N2 O5 P2'
_chemical_formula_weight         1000.81
_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             2019-04-13
_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                 97.1411(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.37212(18)
_cell_length_b                   22.4932(4)
_cell_length_c                   17.6765(3)
_cell_measurement_reflns_used    21918
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.6990
_cell_measurement_theta_min      2.9460
_cell_volume                     4091.98(12)
_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 0.898
_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     -1.00  87.00   1.00   12.00    --   17.49  38.00 -90.00   88
  2  \w     -9.00  85.00   1.00   12.00    --   17.49  77.00  90.00   94
  3  \w      1.00  85.00   1.00   12.00    --   17.49  57.00 -60.00   84
  4  \w    -50.00  34.00   1.00   12.00    --   17.49 -57.00-180.00   84
  5  \w    -50.00  34.00   1.00   12.00    --   17.49 -57.00 120.00   84
  6  \w    -74.00 -27.00   1.00   12.00    --  -17.73 129.00-111.00   47
  7  \w    -50.00 -10.00   1.00   12.00    --   17.49 -77.00 -30.00   40
;
_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      0.0302806000
_diffrn_orient_matrix_UB_12      -0.0267635000
_diffrn_orient_matrix_UB_13      -0.0096185000
_diffrn_orient_matrix_UB_21      -0.0452617000
_diffrn_orient_matrix_UB_22      -0.0166132000
_diffrn_orient_matrix_UB_23      0.0183480000
_diffrn_orient_matrix_UB_31      -0.0422577000
_diffrn_orient_matrix_UB_32      -0.0013703000
_diffrn_orient_matrix_UB_33      -0.0347286000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48889
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.010
_diffrn_reflns_theta_min         2.322
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.520
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.250
_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    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.104
_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     537
_refine_ls_number_reflns         10737
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0142P)^2^+5.0683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9603
_reflns_number_total             10737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02472d2.cif
_cod_data_source_block           tj-11
_cod_depositor_comments
'Adding full bibliography for 7705406--7705412.cif.'
_cod_original_cell_volume        4092.00(12)
_cod_database_code               7705407
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C44H39Cl2IrN2O5P2
_reflns_odcompleteness_completeness 99.91
_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. Restrained distances
 O4-N2 \\sim O3A-N2A \\sim O4A-N2A \\sim O3-N2 \\sim O5A-N2A \\sim O5-N2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O3 \\sim O3A \\sim O4 \\sim O4A \\sim O5 \\sim O5A \\sim N2 \\sim N2A: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N2) = Uanis(N2A)
4. Others
 Sof(O3)=Sof(O4)=Sof(O5)=Sof(N2)=1-FVAR(1)
 Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(N2A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C44(H44A,H44B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C5(H5), 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)
5.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              82530
_olex2_date_sample_data_collection 2019-03-29
_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 1.958
_oxdiff_exptl_absorpt_empirical_full_min 0.636