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_7700085
_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 P4 Rh, 2(C H Cl3), Cl'
_chemical_formula_sum            'C56 H54 Cl7 P4 Rh'
_chemical_formula_weight         1201.93
_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             2019-02-09
_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                88.981(3)
_cell_angle_beta                 77.421(3)
_cell_angle_gamma                69.857(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0851(4)
_cell_length_b                   12.1298(4)
_cell_length_c                   21.8397(7)
_cell_measurement_reflns_used    18893
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.3420
_cell_measurement_theta_min      3.0740
_cell_volume                     2685.53(17)
_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 0.884
_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  85.00   1.00    2.00    --   17.65  57.00-180.00   84
  2  \w     -9.00  85.00   1.00    2.00    --   17.65  77.00  30.00   94
  3  \w     -9.00  85.00   1.00    2.00    --   17.65  77.00 -90.00   94
  4  \w     -1.00  87.00   1.00    2.00    --   17.65  38.00-150.00   88
  5  \w    -20.00  57.00   1.00    2.00    --   17.65 -99.00 120.00   77
  6  \w     35.00  90.00   1.00    2.00    --   17.65 178.00 120.00   55
  7  \w      1.00  85.00   1.00    2.00    --   17.65  57.00   0.00   84
  8  \w    -51.00  37.00   1.00    2.00    --   17.65 -38.00  30.00   88
  9  \w    -20.00  57.00   1.00    2.00    --   17.65 -99.00 -90.00   77
 10  \w    -37.00  35.00   1.00    2.00    --  -17.73  38.00 -60.00   72
;
_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      0.0018706000
_diffrn_orient_matrix_UB_12      -0.0195841000
_diffrn_orient_matrix_UB_13      -0.0307165000
_diffrn_orient_matrix_UB_21      0.0318363000
_diffrn_orient_matrix_UB_22      0.0395678000
_diffrn_orient_matrix_UB_23      -0.0129349000
_diffrn_orient_matrix_UB_31      0.0622654000
_diffrn_orient_matrix_UB_32      -0.0441084000
_diffrn_orient_matrix_UB_33      -0.0009105000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            50653
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.967
_diffrn_reflns_theta_min         2.412
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.206
_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    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.209
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         13809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0282P)^2^+3.0572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11595
_reflns_number_total             13809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00938h2.cif
_cod_data_source_block           z1dppe
_cod_depositor_comments
'Adding full bibliography for 7700084--7700086.cif.'
_cod_original_cell_volume        2685.52(16)
_cod_database_code               7700085
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C56H54Cl7P4Rh
_reflns_odcompleteness_completeness 99.92
_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
2.a Ternary CH refined with riding coordinates:
 C29(H29), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C13B(H13C,H13D), C14(H14A,H14B), C14B(H14C,H14D), C15(H15A,
 H15B), C15B(H15C,H15D)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C2B(H2B), C3(H3), C3B(H3B), C4(H4), C4B(H4B), C5(H5), C5B(H5B),
 C6(H6), C6B(H6B), C8(H8), C8B(H8B), C9(H9), C9B(H9B), C10(H10), C10B(H10B),
 C11(H11), C11B(H11B), C12(H12), C12B(H12B), C17(H17), C17B(H17B), C18(H18),
 C18B(H18B), C19(H19), C19B(H19B), C20(H20), C20B(H20B), C21(H21), C21B(H21B),
 C23(H23), C23B(H23B), C24(H24), C24B(H24B), C25(H25), C25B(H25B), C26(H26),
 C26B(H26B), C27(H27), C27B(H27B)
;
_shelx_res_checksum              76017
_shelx_hkl_checksum              96368
_olex2_date_sample_data_collection 2019-02-09
_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 1.571
_oxdiff_exptl_absorpt_empirical_full_min 0.695