Rhodium Diamidobenzene Complexes: A Tale of Different Substituents on the Diamidobenzene Ligand
Suhr, Simon; Walter, Robert Richerd Marten; Beerhues, Julia; Albold, Uta; Sarkar, Biprajit; Chemical Science  (2022) –; doi:10.1039/D2SC03227A

data_1567318
_publ_section_title
;
 Rhodium Diamidobenzene Complexes: A Tale of Different Substituents on the
 Diamidobenzene Ligand
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC03227A
_journal_year                    2022
_chemical_formula_moiety         'C38 H44 N2 Rh2, 2(B F4)'
_chemical_formula_sum            'C38 H44 B2 F8 N2 Rh2'
_chemical_formula_weight         908.19
_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             2021-07-21
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-05-26 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.504(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9758(7)
_cell_length_b                   16.8728(9)
_cell_length_c                   18.2875(9)
_cell_measurement_reflns_used    7158
_cell_measurement_temperature    140.01
_cell_measurement_theta_max      28.402
_cell_measurement_theta_min      1.653
_cell_volume                     3948.9(4)
_computing_cell_refinement       'APEX2 (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT+ (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      140.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'omega + phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53346
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.402
_diffrn_reflns_theta_min         1.653
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.9527
_exptl_absorpt_correction_T_min  0.6845
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red-purple
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       plate
_exptl_crystal_F_000             1832
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloroethane, pentane'
_exptl_crystal_size_max          0.752
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.156
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         9848
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0346P)^2^+5.4300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7158
_reflns_number_total             9848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03227a2.cif
_cod_data_source_block           sar276
_cod_database_code               1567318
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.550
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
 Sof(F5A)=Sof(F2A)=1-FVAR(1)
 Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F00W)=Sof(F00Z)=1-FVAR(2)
 Sof(F1)=Sof(F3)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C6(H6), C3(H3), C4(H4), C5(H5)
4.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C38(H38), C32(H32), C31(H31), C29(H29), C37(H37), C34(H34),
 C30(H30), C35(H35), C36(H36)
4.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C14(H14A,H14B,
 H14C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C13(H13A,H13B,H13C), C23(H23A,
 H23B,H23C), C25(H25A,H25B,H25C), C22(H22A,H22B,H22C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67780
_shelx_hkl_checksum              56037
_shelx_fab_checksum              96888
_olex2_submission_special_instructions 'No special instructions were received'