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_7712715
_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         'C12 H18 N2 Rh, C10 F15'
_chemical_formula_sum            'C22 H18 F15 N2 Rh'
_chemical_formula_weight         698.29
_chemical_properties_physical    Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-09 deposited with the CCDC.	2023-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.1520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7638(4)
_cell_length_b                   21.5907(8)
_cell_length_c                   10.9819(4)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    104.0
_cell_measurement_theta_max      27.832
_cell_measurement_theta_min      2.646
_cell_volume                     2552.16(16)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      104.0
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.931
_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  0.0262
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23894
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.909
_diffrn_reflns_theta_min         2.114
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.9679
_exptl_absorpt_correction_T_min  0.8428
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0529 before and 0.0291 after correction.
The Ratio of minimum to maximum transmission is 0.8340.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.730
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0025(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         5683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0168P)^2^+9.3040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4348
_reflns_number_total             5683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00425b2.cif
_cod_data_source_block           p21n_hr_num
_cod_database_code               7712715
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.683
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: F8(0.5) F10(0.5) F12(0.5) F14(0.5) F16(0.5) F18(0.5) F20(0.5)
 F22(0.5) F24(0.5) C8(0.5) C10(0.5) C12(0.5) F26(0.5) H16(0.5) H16A(0.5)
 F27(0.5) H18A(0.5) H18(0.5) F7(0.5) F15(0.5) F2(0.5) H22(0.5) H22A(0.5)
 C24(0.5) H24A(0.5) H24B(0.5) C26(0.5) H30C(0.5) H30D(0.5) H30A(0.5) H30B(0.5)
 C32(0.5) C34(0.5) C17(0.5) C9(0.5) C19(0.5) C5(0.5) C21(0.5) C11(0.5) C23(0.5)
 C3(0.5) C25(0.5) F17(0.5) F9(0.5) F19(0.5) F5(0.5) F21(0.5) F11(0.5) F23(0.5)
 F3(0.5) F25(0.5) F13(0.5) C13(0.5) C27(0.5) C7(0.5) C29(0.5) H29A(0.5)
 H29B(0.5) C15(0.5) H15A(0.5) H15B(0.5) C31(0.5) H31A(0.5) H31B(0.5) C2(0.5)
 H2A(0.5) H2B(0.5) C33(0.5) H33A(0.5) H33B(0.5)
3.a Ternary CH refined with riding coordinates:
 C16(H16), C16(H16A), C18(H18A), C18(H18), C22(H22), C22(H22A), C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C30(H30C,H30D), C30(H30A,H30B), C29(H29A,H29B), C15(H15A,
 H15B), C31(H31A,H31B), C2(H2A,H2B), C33(H33A,H33B)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C20(H20A,H20B,H20C)
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_shelx_res_checksum              34961
_olex2_submission_special_instructions 'No special instructions were received'