Bulky bis(aryl)triazenides: just aspiring amidinates? A structural and spectroscopic study.
Gyton, Matthew R.; Leverett, Anthony R.; Cole, Marcus L.; McKay, Alasdair I.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5653–5661; doi:10.1039/d0dt00285b

data_7703884
_publ_section_title
;
 Bulky bis(aryl)triazenides: just aspiring amidinates? A structural and
 spectroscopic study.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5653
_journal_page_last               5661
_journal_paper_doi               10.1039/d0dt00285b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C81 H105 Cl Li N6 O6 Rh3'
_chemical_formula_sum            'C81 H105 Cl Li N6 O6 Rh3'
_chemical_formula_weight         1609.82
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-14 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.098(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.876(3)
_cell_length_b                   26.438(3)
_cell_length_c                   22.979(2)
_cell_measurement_reflns_used    7401
_cell_measurement_temperature    150
_cell_measurement_theta_max      20.662
_cell_measurement_theta_min      2.393
_cell_volume                     19187(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1459
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            96613
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.813
_diffrn_reflns_theta_max         20.813
_diffrn_reflns_theta_min         2.393
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1354 before and 0.0808 after correction. The Ratio of minimum to maximum transmission is 0.9027. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       block
_exptl_crystal_F_000             6688
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.00032(5)
_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   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         10018
_refine_ls_number_restraints     935
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0589
_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^)+(0.1152P)^2^+25.2332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6601
_reflns_number_total             10018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00285b2.cif
_cod_data_source_block           2LiCl
_cod_depositor_comments
'Adding full bibliography for 7703878--7703902.cif.'
_cod_database_code               7703884
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.944
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C61(H61), C64(H64), C34(H34), C47(H47), C77(H77), C23(H23), C7(H7), C74(H74),
 C50(H50), C10(H10), C20(H20), C37(H37)
3.b Aromatic/amide H refined with riding coordinates:
 C59(H59), C40(H40), C57(H57), C58(H58), C18(H18), C67(H67), C45(H45),
 C44(H44), C5(H5), C71(H71), C43(H43), C70(H70), C72(H72), C4(H4), C13(H13),
 C17(H17), C30(H30), C3(H3), C16(H16), C32(H32), C31(H31)
3.c Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C62(H62A,H62B,H62C), C36(H36A,H36B,H36C), C9(H9A,H9B,
 H9C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C8(H8A,H8B,H8C), C79(H79A,H79B,
 H79C), C78(H78A,H78B,H78C), C49(H49A,H49B,H49C), C11(H11A,H11B,H11C), C35(H35A,
 H35B,H35C), C51(H51A,H51B,H51C), C75(H75A,H75B,H75C), C52(H52A,H52B,H52C),
 C48(H48A,H48B,H48C), C76(H76A,H76B,H76C), C12(H12A,H12B,H12C), C25(H25A,H25B,
 H25C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C39(H39A,
 H39B,H39C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              34671
_shelx_fab_checksum              87499
_olex2_submission_special_instructions 'No special instructions were received'