Substitution Lability of the Perfluorinated Cp* Ligand in Rh(I) Complexes
Parche, Joshua; Rupf, Susanne M.; Sievers, Robin; Malischewski, Moritz; Dalton Transactions  (2023) –; doi:10.1039/D3DT00425B

data_7712714
_publ_section_title
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 Substitution Lability of the Perfluorinated Cp* Ligand in Rh(I) Complexes
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00425B
_journal_year                    2023
_chemical_formula_moiety         '2(C18 H20 F2 N2 Rh), 2(C10 F15)'
_chemical_formula_sum            'C56 H40 F34 N4 Rh2'
_chemical_formula_weight         1620.74
_chemical_properties_physical    Moisture-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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-01
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-02-09 deposited with the CCDC.	2023-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                112.269(4)
_cell_angle_beta                 91.270(3)
_cell_angle_gamma                104.241(3)
_cell_formula_units_Z            2
_cell_length_a                   14.3033(16)
_cell_length_b                   14.7648(13)
_cell_length_c                   15.3305(13)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    112.0
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.37
_cell_volume                     2879.9(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      112.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            67365
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_min         2.050
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1569 before and 0.1021 after correction.
The Ratio of minimum to maximum transmission is 0.8391.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.153
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         13238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0406P)^2^+8.1232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10822
_reflns_number_total             13238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00425b2.cif
_cod_data_source_block           p_1_fast
_cod_database_code               7712714
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.817
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C34) = Uanis(C01S) = Uanis(C26) = Uanis(C022) = Uanis(C14) = Uanis(C02I)
= Uanis(C1) = Uanis(C027) = Uanis(C2) = Uanis(C01O)
Uanis(C02L) = Uanis(C13)
Uanis(C3) = Uanis(C21)
Uanis(F19) = Uanis(F18) = Uanis(F17)
Uanis(F7) = Uanis(F10) = Uanis(F2) = Uanis(F016) = Uanis(F6) = Uanis(F14)
3. Others
 Fixed Sof: F00L(0.7) F00N(0.75) F00O(0.66667) F00R(0.66667) F00S(0.5)
 F00X(0.66667) H00Y(0.3) F011(0.66667) F016(0.5) F01F(0.66667) F3(0.5)
 H01I(0.7) H01J(0.4) F01N(0.5) C01O(0.5) C01S(0.5) C3(0.33333) F01V(0.25)
 C022(0.5) F023(0.66667) H024(0.6) C027(0.5) F02B(0.66667) F02C(0.6) C02I(0.5)
 C02K(0.5) C02L(0.5) F02M(0.4) F02N(0.3) C02O(0.5) C02P(0.5) C4(0.5) F2(0.5)
 C7(0.5) C10(0.5) C13(0.5) C15(0.5) C16(0.5) F5(0.5) F1(0.5) F4(0.5) F6(0.5)
 F7(0.5) F14(0.5) C1(0.5) C14(0.5) C2(0.5) C26(0.5) C34(0.5) F9(0.33333)
 F12(0.33333) F15(0.33333) F13(0.33333) F16(0.33333) F17(0.33333) F19(0.33333)
 C21(0.66667) F22(0.75) F21(0.25) F10(0.5)
4.a Ternary CH refined with riding coordinates:
 C015(H015), C018(H018), C01B(H01B), C01K(H01K), C01P(H01P), C01Y(H01Y),
 C01Z(H01Z), C029(H029)
4.b Secondary CH2 refined with riding coordinates:
 C01L(H01L,H01M), C01M(H01D,H01E), C01R(H01N,H01O), C01X(H01R,H01S), C025(H02A,
 H02B), C02E(H02G,H02H), C02H(H02C,H02D), C02J(H02E,H02F)
4.c Aromatic/amide H refined with riding coordinates:
 C00Q(H00Q), C00Y(H00Y), C017(H017), C019(H019), C01A(H01A), C01C(H01C),
 C01D(H01F), C01E(H01H), C01G(H01G), C01I(H01I), C01J(H01J), C01Q(H01Q),
 C01U(H01U), C01W(H01W), C020(H020), C021(H021), C024(H024), C028(H028)
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_shelx_res_checksum              82364
_olex2_submission_special_instructions 'No special instructions were received'