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_7124492
_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         'C23 H29 N2 Rh, F6 P, 0.33(C)'
_chemical_formula_sum            'C23.33 H29 F6 N2 P Rh'
_chemical_formula_weight         585.32
_chemical_properties_physical    Air-sensitive
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-09-08
_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                117.2535(17)
_cell_angle_beta                 108.4380(17)
_cell_angle_gamma                97.3701(17)
_cell_formula_units_Z            2
_cell_length_a                   10.6800(2)
_cell_length_b                   11.8136(3)
_cell_length_c                   11.8896(3)
_cell_measurement_reflns_used    4926
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      69.904
_cell_measurement_theta_min      4.450
_cell_volume                     1196.94(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_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    'XS (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 0.964
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19004
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         70.292
_diffrn_reflns_theta_min         4.401
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    6.956
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1467 before and 0.0756 after correction.
The Ratio of minimum to maximum transmission is 0.7293.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       Plate
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.015
_refine_diff_density_max         2.604
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         4268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0898P)^2^+2.3136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3638
_reflns_number_total             4268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09164h3.cif
_cod_data_source_block           4
_cod_original_cell_volume        1196.94(5)
_cod_database_code               7124492
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.642
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'