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_1567322
_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         'C28 H29 N2 Rh'
_chemical_formula_sum            'C28 H29 N2 Rh'
_chemical_formula_weight         496.44
_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             2022-06-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-07 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.469(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.0964(18)
_cell_length_b                   10.3051(9)
_cell_length_c                   23.860(2)
_cell_measurement_reflns_used    7405
_cell_measurement_temperature    145.00
_cell_measurement_theta_max      28.293
_cell_measurement_theta_min      1.573
_cell_volume                     4546.5(7)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      145.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0632
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40214
_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         28.293
_diffrn_reflns_theta_min         1.573
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_T_max  0.9315
_exptl_absorpt_correction_T_min  0.5614
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       plate
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.431
_exptl_crystal_size_min          0.104
_refine_diff_density_max         1.991
_refine_diff_density_min         -1.372
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         11261
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0535P)^2^+28.1825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7405
_reflns_number_total             11261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03227a2.cif
_cod_data_source_block           sar320
_cod_database_code               1567322
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.673
_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 0.001 and
sigma for terminal atoms of 0.002
Uanis(C30) = Uanis(C40) = Uanis(C014) = Uanis(C38) = Uanis(C31)
Uanis(C47) = Uanis(C48) = Uanis(C54) = Uanis(C49) = Uanis(C46)
3.a Aromatic/amide H refined with riding coordinates:
 C41(H41), C38(H38), C45(H45), C6(H6), C33(H33), C12(H12), C42(H42), C40(H40),
 C18(H18), C4(H4), C16(H16), C8(H8), C9(H9), C3(H3), C37(H37), C014(H014),
 C39(H39), C14(H14), C36(H36), C17(H17), C15(H15), C5(H5), C34(H34), C43(H43),
 C13(H13), C35(H35), C44(H44), C7(H7)
3.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C53(H53A,H53B,H53C), C24(H24A,H24B,H24C), C50(H50A,H50B,
 H50C), C55(H55A,H55B,H55C), C27(H27A,H27B,H27C), C51(H51A,H51B,H51C), C25(H25A,
 H25B,H25C), C28(H28A,H28B,H28C), C52(H52A,H52B,H52C)
;
_smtbx_masks_void_probe_radius   0.2
_smtbx_masks_void_truncation_radius 0.2
_shelx_res_checksum              31858
_shelx_hkl_checksum              25892
_shelx_fab_checksum              98822
_olex2_submission_special_instructions 'No special instructions were received'