Synthesis and characterization of rhodium-aluminum heterobimetallic complexes tethered by a 1,3-bis(diphenylphosphino)-2-propanoxy group.
Li, Zhongjing; Yokley, Timothy W.; Tran, Sheila L.; Zong, Jie; Schley, Nathan D.; Brewster, Timothy P.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8782–8790; doi:10.1039/c9dt00938h

data_7700086
_publ_section_title
;
 Synthesis and characterization of rhodium-aluminum heterobimetallic
 complexes tethered by a 1,3-bis(diphenylphosphino)-2-propanoxy group.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8782
_journal_page_last               8790
_journal_paper_doi               10.1039/c9dt00938h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C54 H52 O2 P4 Rh, 3(C H Cl3), C32 H12 B F24'
_chemical_formula_sum            'C89 H67 B Cl9 F24 O2 P4 Rh'
_chemical_formula_weight         2181.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-22 deposited with the CCDC.    2019-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                82.035(4)
_cell_angle_beta                 76.317(4)
_cell_angle_gamma                79.953(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4257(6)
_cell_length_b                   19.1875(10)
_cell_length_c                   22.2983(10)
_cell_measurement_reflns_used    7687
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.3620
_cell_measurement_theta_min      3.2520
_cell_volume                     4652.6(4)
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.939
_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    -63.00  31.00   1.00    3.00    --  -36.45  77.00-120.00   94
  2  \w    -55.00  33.00   1.00    3.00    --  -36.45  38.00-150.00   88
  3  \w   -104.00 -20.00   1.00    3.00    --  -36.45 -57.00-150.00   84
  4  \w      9.00  47.00   1.00    3.00    --   36.45  79.00 149.76   38
  5  \w     10.00 104.00   1.00    3.00    --   36.45  77.00 -60.00   94
  6  \w     10.00 104.00   1.00    3.00    --   36.45  77.00 -30.00   94
  7  \w     10.00 104.00   1.00    3.00    --   36.45  77.00  90.00   94
  8  \w     18.00 106.00   1.00    3.00    --   36.45  38.00  60.00   88
  9  \w      8.00  46.00   1.00    3.00    --   36.45  80.00  19.52   38
 10  \w    -24.00  65.00   1.00    3.00    --   36.45 -80.00 169.15   89
 11  \w     91.00 176.00   1.00   12.00    --  108.65  61.00 -30.00   85
 12  \w     41.00 137.00   1.00   12.00    --  108.65 -80.00 -37.28   96
 13  \w     41.00 137.00   1.00   12.00    --  108.65 -80.00-119.72   96
 14  \w     91.00 176.00   1.00   12.00    --  108.65  61.00 -60.00   85
 15  \w     39.00 178.00   1.00   12.00    --  108.65   0.00 120.00  139
 16  \w     41.00 137.00   1.00   12.00    --  108.65 -80.00 144.38   96
 17  \w     41.00 137.00   1.00   12.00    --  108.65 -80.00 108.11   96
 18  \w     40.00 126.00   1.00   12.00    --  108.65 -45.00 -60.00   86
 19  \w     41.00 137.00   1.00   12.00    --  108.65 -80.00 -94.71   96
 20  \w     40.00 126.00   1.00   12.00    --  108.65 -45.00-150.00   86
 21  \w     82.00 176.00   1.00   12.00    --  108.65  77.00   0.00   94
 22  \w     41.00  55.00   1.00   12.00    --  108.65 -79.00  56.08   14
;
_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      0.1099429000
_diffrn_orient_matrix_UB_12      -0.0560010000
_diffrn_orient_matrix_UB_13      0.0097495000
_diffrn_orient_matrix_UB_21      -0.0653225000
_diffrn_orient_matrix_UB_22      -0.0588886000
_diffrn_orient_matrix_UB_23      -0.0118290000
_diffrn_orient_matrix_UB_31      0.0577037000
_diffrn_orient_matrix_UB_32      0.0106916000
_diffrn_orient_matrix_UB_33      -0.0698142000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40515
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.304
_diffrn_reflns_theta_min         2.351
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.357
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.449
_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    1.557
_exptl_crystal_description       plate
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.746
_refine_diff_density_min         -1.504
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1320
_refine_ls_number_reflns         17273
_refine_ls_number_restraints     406
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0929
_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^)+(0.0941P)^2^+27.4405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2224
_refine_ls_wR_factor_ref         0.2448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12397
_reflns_number_total             17273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00938h2.cif
_cod_data_source_block           zl-0051
_cod_depositor_comments
'Adding full bibliography for 7700084--7700086.cif.'
_cod_original_cell_volume        4652.7(4)
_cod_database_code               7700086
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C90H67BCl9F24O2P4Rh1
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.439
_reflns_odcompleteness_completeness 96.62
_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. Restrained distances
 Cl7-C89 \\sim Cl9B-C89B
 with sigma of 0.02
 Cl9-C89 \\sim Cl8B-C89B
 with sigma of 0.02
 Cl8-C89 \\sim Cl7B-C89B
 with sigma of 0.02
 Cl7-Cl9 \\sim Cl9B-Cl8B
 with sigma of 0.04
 Cl7-Cl8 \\sim Cl9B-Cl7B
 with sigma of 0.04
 Cl9-Cl8 \\sim Cl8B-Cl7B
 with sigma of 0.04
 Cl2-Cl3 \\sim Cl2B-Cl3B
 with sigma of 0.04
 Cl1-C87 \\sim Cl1B-C87B
 with sigma of 0.02
 Cl2-C87 \\sim Cl2B-C87B
 with sigma of 0.02
 Cl3-C87 \\sim Cl3B-C87B
 with sigma of 0.02
 Cl1-Cl2 \\sim Cl1B-Cl2B
 with sigma of 0.04
 Cl1-Cl3 \\sim Cl1B-Cl3B
 with sigma of 0.04
 Cl5-C88 \\sim Cl6B-C88B
 with sigma of 0.02
 Cl6-C88 \\sim Cl4B-C88B
 with sigma of 0.02
 Cl4-C88 \\sim Cl5B-C88B
 with sigma of 0.02
 Cl5-Cl6 \\sim Cl6B-Cl4B
 with sigma of 0.04
 Cl5-Cl4 \\sim Cl6B-Cl5B
 with sigma of 0.04
 Cl6-Cl4 \\sim Cl4B-Cl5B
 with sigma of 0.04
 F24B-C0AA \\sim F24-C86
 with sigma of 0.02
 C83-C0AA \\sim C83-C86
 with sigma of 0.02
 F22B-C0AA \\sim F22-C86
 with sigma of 0.02
 F23B-C0AA \\sim F23-C86
 with sigma of 0.02
 F24B-C83 \\sim F24-C83
 with sigma of 0.04
 F24B-F22B \\sim F24-F22
 with sigma of 0.04
 F24B-F23B \\sim F24-F23
 with sigma of 0.04
 C83-F22B \\sim C83-F22
 with sigma of 0.04
 C83-F23B \\sim C83-F23
 with sigma of 0.04
 F22B-F23B \\sim F22-F23
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim Cl3 \\sim C87: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Cl7 \\sim Cl7B \\sim Cl8 \\sim Cl8B \\sim Cl9 \\sim Cl9B \\sim C89 \\sim C89B
\\sim Cl1 \\sim Cl1B \\sim Cl2 \\sim Cl2B \\sim Cl3 \\sim Cl3B \\sim C87 \\sim
C87B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Cl4 \\sim Cl5 \\sim Cl6: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Cl4 \\sim Cl4B \\sim Cl5 \\sim Cl5B \\sim Cl6 \\sim Cl6B \\sim C88 \\sim C88B:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
F22 \\sim F22B \\sim F23 \\sim F23B \\sim F24 \\sim F24B \\sim C0AA \\sim C86:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Cl7B)=Sof(Cl8B)=Sof(Cl9B)=Sof(C89B)=Sof(H89B)=1-FVAR(1)
 Sof(Cl7)=Sof(Cl8)=Sof(Cl9)=Sof(C89)=Sof(H89)=FVAR(1)
 Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=Sof(C87B)=Sof(H87B)=1-FVAR(2)
 Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(C87)=Sof(H87)=FVAR(2)
 Sof(Cl4B)=Sof(Cl5B)=Sof(Cl6B)=Sof(C88B)=Sof(H88B)=1-FVAR(3)
 Sof(Cl4)=Sof(Cl5)=Sof(Cl6)=Sof(C88)=Sof(H88)=FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F24)=Sof(C86)=1-FVAR(4)
 Sof(F22B)=Sof(F23B)=Sof(F24B)=Sof(C0AA)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C14(H14), C41(H41), C89(H89), C89B(H89B), C87(H87), C87B(H87B), C88(H88),
 C88B(H88B)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C40(H40A,H40B), C42(H42A,H42B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53),
 C54(H54), C56(H56), C58(H58), C60(H60), C64(H64), C66(H66), C68(H68), C72(H72),
  C74(H74), C76(H76), C80(H80), C82(H82), C84(H84)
5.d Tetrahedral OH refined with riding coordinates:
 O1(H1)
5.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              15917
_shelx_hkl_checksum              37076
_olex2_date_sample_data_collection 2018-10-30
_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 1.183
_oxdiff_exptl_absorpt_empirical_full_min 0.891