Multiple binding modes of an unconjugated bis(pyridine) ligand stabilize low-valent [Cp*Rh] complexes.
Lionetti, Davide; Day, Victor W.; Lassalle-Kaiser, Benedikt; Blakemore, James D.; Chemical communications (Cambridge, England) 54 (2018) 1694–1697; doi:10.1039/c7cc09164h

data_7124491
_publ_section_title
;
 Multiple binding modes of an unconjugated bis(pyridine) ligand stabilize
 low-valent [Cp*Rh] complexes.
;
_journal_issue                   14
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1694
_journal_page_last               1697
_journal_paper_doi               10.1039/c7cc09164h
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '2(C23 H29 Cl N2 Rh), 2(F6 P)'
_chemical_formula_sum            'C46 H58 Cl2 F12 N4 P2 Rh2'
_chemical_formula_weight         1233.62
_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     direct
_audit_creation_date             2017-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-11 deposited with the CCDC.
2018-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                95.308(4)
_cell_angle_beta                 94.332(4)
_cell_angle_gamma                93.372(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2841(10)
_cell_length_b                   11.8607(16)
_cell_length_c                   25.557(4)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      33.071
_cell_measurement_theta_min      2.409
_cell_volume                     2487.7(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      199.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            38264
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.264
_diffrn_reflns_theta_min         1.728
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0543 before and 0.0423 after correction. The Ratio of minimum to maximum transmission is 0.8788. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         17715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+2.6660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14267
_reflns_number_total             17715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09164h3.cif
_cod_data_source_block           3-Cl
_cod_original_cell_volume        2487.8(6)
_cod_database_code               7124491
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.618
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10), C11(H11), C12(H12), C13(H13),
 C1B(H1B), C2B(H2B), C3B(H3B), C4B(H4B), C10B(H10B), C11B(H11B), C12B(H12B),
 C13B(H13B)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C7B(H7BA,H7BB,
 H7BC), C8B(H8BA,H8BB,H8BC), C19B(H19D,H19E,H19F), C20B(H20D,H20E,H20F),
 C21B(H21D,H21E,H21F), C22B(H22D,H22E,H22F), C23B(H23D,H23E,H23F)
;
_olex2_submission_special_instructions 'No special instructions were received'