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_1567323
_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         'C30 H32 N3 Rh, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C32 H35 B2 F8 N4 Rh'
_chemical_formula_weight         752.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-02
_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                 92.687(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2373(6)
_cell_length_b                   12.7617(6)
_cell_length_c                   19.6601(9)
_cell_measurement_reflns_used    10757
_cell_measurement_temperature    140.0
_cell_measurement_theta_max      33.183
_cell_measurement_theta_min      1.540
_cell_volume                     3317.5(3)
_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      140.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0257
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            89550
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.183
_diffrn_reflns_theta_min         1.540
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.9300
_exptl_absorpt_correction_T_min  0.8367
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       prism
_exptl_crystal_F_000             1528
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: aceotrnile, diethyl ether'
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.198
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         12669
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+1.7530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10757
_reflns_number_total             12669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03227a2.cif
_cod_data_source_block           sar243
_cod_database_code               1567323
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.785
_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. Restrained distances
 F7A-F6A \\sim F7B-F8B
 with sigma of 0.04
 F2A-F1A \\sim F2B-F1B
 with sigma of 0.04
 F7A-B2 \\sim F7B-B2A
 with sigma of 0.04
 F7A-F5A \\sim F7B-F6B
 with sigma of 0.04
 F7A-F8A \\sim F7B-F5B
 with sigma of 0.04
 F6A-B2 \\sim F8B-B2A
 with sigma of 0.04
 F6A-F5A \\sim F8B-F6B
 with sigma of 0.04
 F6A-F8A \\sim F8B-F5B
 with sigma of 0.04
 F1A-B1 \\sim F1B-B1
 with sigma of 0.02
 B2-F5A \\sim B2A-F6B
 with sigma of 0.04
 B2-F8A \\sim B2A-F5B
 with sigma of 0.04
 F3A-B1 \\sim F3B-B1
 with sigma of 0.04
 F4A-B1 \\sim F4B-B1
 with sigma of 0.04
 F5A-F8A \\sim F6B-F5B
 with sigma of 0.04
 F2A-B1 \\sim F2B-B1
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(F8A) \\sim Ueq, Uanis(F8B) \\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F7B)
\\sim Ueq, Uanis(F5B) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6B) \\sim Ueq,
Uanis(F6A) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.03
4. Others
 Sof(F6B)=Sof(F7B)=Sof(B2A)=Sof(F8B)=Sof(F5B)=1-FVAR(1)
 Sof(F7A)=Sof(F6A)=Sof(B2)=Sof(F5A)=Sof(F8A)=FVAR(1)
 Sof(F1B)=Sof(F3B)=Sof(F2B)=Sof(F4B)=1-FVAR(2)
 Sof(F3A)=Sof(F4A)=Sof(F2A)=Sof(F1A)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H00D), C8(H00J), C6(H00L), C12(H00N), C4(H00P), C5(H00Q), C18(H00R),
 C9(H00S), C14(H00U), C11(H00W), C10(H00Z), C17(H012), C15(H013), C16(H017)
5.b Idealised Me refined as rotating group:
 C26(H00A,H00B,H00C), C25(H00E,H00F,H00G), C29(H00H,H00I,H00K), C27(H01A,H01B,
 H01C), C28(H01D,H01E,H01F), C33(H01J,H01K,H01L), C31(H01G,H01H,H01I)
;
_shelx_res_checksum              7996
_shelx_hkl_checksum              29584
_olex2_submission_original_sample_id sar243
_olex2_submission_special_instructions 'No special instructions were received'