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_7700084
_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
'C55 H52 O3 P4 Rh, 2(C H2 Cl2), 2(C1 H1 Cl3), Cl'
_chemical_formula_sum            'C59 H58 Cl11 O3 P4 Rh'
_chemical_formula_weight         1431.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-30
_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                90
_cell_angle_beta                 92.8655(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.88291(13)
_cell_length_b                   20.7830(2)
_cell_length_c                   21.00080(16)
_cell_measurement_reflns_used    14038
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.9660
_cell_measurement_theta_min      3.5400
_cell_volume                     6487.67(10)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.969
_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    -55.00  33.00   1.00    4.00    --  -36.45  38.00 120.00   88
  2  \w   -104.00 -10.00   1.00    4.00    --  -36.45 -77.00 -30.00   94
  3  \w      7.00 108.00   1.00    4.00    --   36.45  19.00 -60.00  101
  4  \w      8.00  46.00   1.00    4.00    --   36.45  80.00  97.91   38
  5  \w      9.00  47.00   1.00    4.00    --   36.45  79.00  24.62   38
  6  \w    -28.00  64.00   1.00    4.00    --   36.45 -78.00  94.91   92
  7  \w    -31.00  63.00   1.00    4.00    --   36.45 -77.00  60.00   94
  8  \w      9.00  47.00   1.00    4.00    --   36.45  79.00 -45.36   38
  9  \w     41.00 136.00   1.00   20.00    --  108.65 -79.00   3.15   95
 10  \w    111.00 176.00   1.00   20.00    --  108.65  61.00  90.00   65
 11  \w     78.00 105.00   1.00   20.00    --  108.65 -80.00  29.38   27
 12  \w     41.00 125.00   1.00   20.00    --  108.65 -45.00 120.00   84
 13  \w     55.00 103.00   1.00   20.00    --  108.65 -80.00-108.44   48
 14  \w     41.00 106.00   1.00   20.00    --  108.65 -80.00 -38.37   65
 15  \w     66.00 138.00   1.00   20.00    --  108.65   0.00 -90.00   72
 16  \w     86.00 176.00   1.00   20.00    --  108.65  77.00-120.00   90
 17  \w     53.00 100.00   1.00   20.00    --  108.65 -79.00 -74.20   47
 18  \w     68.00 134.00   1.00   20.00    --  108.65 -80.00  54.32   66
;
_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      -0.0499334000
_diffrn_orient_matrix_UB_12      0.0649244000
_diffrn_orient_matrix_UB_13      0.0002635000
_diffrn_orient_matrix_UB_21      0.0903048000
_diffrn_orient_matrix_UB_22      0.0357322000
_diffrn_orient_matrix_UB_23      -0.0038158000
_diffrn_orient_matrix_UB_31      -0.0100875000
_diffrn_orient_matrix_UB_32      -0.0015807000
_diffrn_orient_matrix_UB_33      -0.0733226000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36335
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.273
_diffrn_reflns_theta_min         2.993
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.566
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.490
_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    1.466
_exptl_crystal_description       plate
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.013
_refine_diff_density_max         2.358
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         12419
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1071P)^2^+30.8979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.1965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10504
_reflns_number_total             12419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00938h2.cif
_cod_data_source_block           zl-0048
_cod_depositor_comments
'Adding full bibliography for 7700084--7700086.cif.'
_cod_database_code               7700084
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C60H58Cl10O3P4Rh1
_reflns_odcompleteness_completeness 98.97
_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
 Cl5-C59B \\sim Cl10-C59 \\sim Cl9B-C59B \\sim Cl6-C59B \\sim Cl9-C59 \\sim
Cl11-C59
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl5 \\sim Cl6 \\sim Cl9 \\sim Cl9B \\sim Cl10 \\sim Cl11 \\sim C59 \\sim C59B:
within 2.4A with sigma of 0.01 and sigma for terminal atoms of 0.02
Cl5B \\sim Cl5C \\sim Cl6B \\sim Cl6C \\sim Cl12 \\sim Cl13 \\sim C57 \\sim
C57B \\sim C57C: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Others
 1*[Sof(Cl6B)+Sof(Cl5B)+Sof(C57B)+Sof(H57A)+Sof(H57B)]+1*[Sof(Cl6C)+Sof(Cl5C)+
 Sof(C57C)+Sof(H57C)+Sof(H57D)]+1*[Sof(Cl12)+Sof(Cl13)+Sof(C57)+Sof(H57E)+
 Sof(H57F)]=1 with esd of 0.001
 Sof(Cl5)=Sof(Cl6)=Sof(Cl9B)=Sof(C59B)=Sof(H59B)=1-FVAR(1)
 Sof(Cl9)=Sof(Cl10)=Sof(Cl11)=Sof(C59)=Sof(H59)=FVAR(1)
 Sof(Cl6B)=Sof(Cl5B)=Sof(C57B)=Sof(H57A)=Sof(H57B)=FVAR(2)
 Sof(Cl6C)=Sof(Cl5C)=Sof(C57C)=Sof(H57C)=Sof(H57D)=FVAR(3)
 Sof(Cl12)=Sof(Cl13)=Sof(C57)=Sof(H57E)=Sof(H57F)=FVAR(4)
5.a Free rotating group:
 Cl6B(Cl5B,C57B), Cl6C(Cl5C,C57C), Cl12(Cl13,C57)
5.b Ternary CH refined with riding coordinates:
 C15(H15), C42(H42), C59(H59), C59B(H59B), C56(H56)
5.c Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C16(H16A,H16B), C41(H41A,H41B), C43(H43A,H43B), C58(H58A,
 H58B), C57B(H57A,H57B), C57C(H57C,H57D), C57(H57E,H57F)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
  C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C45(H45),
 C46(H46), C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54),
  C55(H55)
5.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3)
;
_shelx_res_checksum              35597
_shelx_hkl_checksum              11374
_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 1.121
_oxdiff_exptl_absorpt_empirical_full_min 0.870