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_7703881
_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         'C62 H87 N7 O2 Rh2, 1.5(C6 H14)'
_chemical_formula_sum            'C71 H108 N7 O2 Rh2'
_chemical_formula_weight         1297.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-14
_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                85.510(4)
_cell_angle_beta                 76.563(4)
_cell_angle_gamma                84.116(4)
_cell_formula_units_Z            2
_cell_length_a                   13.5047(12)
_cell_length_b                   14.7204(12)
_cell_length_c                   18.3174(17)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.912
_cell_measurement_theta_min      2.177
_cell_volume                     3517.5(5)
_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 0.993
_diffrn_measured_fraction_theta_max 0.976
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48305
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.212
_diffrn_reflns_theta_min         2.507
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1321 before and 0.0558 after correction. The Ratio of minimum to maximum transmission is 0.9226. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       plate
_exptl_crystal_F_000             1378
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         15295
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0422P)^2^+0.3934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10217
_reflns_number_total             15295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00285b2.cif
_cod_data_source_block           24
_cod_depositor_comments
'Adding full bibliography for 7703878--7703902.cif.'
_cod_database_code               7703881
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.927
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C69-C70 \\sim C70-C71 \\sim C71-C72 \\sim C72-C73 \\sim C73-C74
 with sigma of 0.02
 C69-C71 \\sim C71-C73 \\sim C70-C72 \\sim C72-C74
 with sigma of 0.04
 C63-C64 \\sim C64-C65 \\sim C65-C66 \\sim C66-C67 \\sim C67-C68
 with sigma of 0.02
 C63-C65 \\sim C65-C67 \\sim C64-C66 \\sim C66-C68
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C69, C70, C71, C72, C73, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C63, C64, C65, C66, C67, C68
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5) C70(0.5) H70A(0.5)
 H70B(0.5) C71(0.5) H71A(0.5) H71B(0.5) C72(0.5) H72A(0.5) H72B(0.5) C73(0.5)
 H73A(0.5) H73B(0.5) C74(0.5) H74A(0.5) H74B(0.5) H74C(0.5)
6.a Ternary CH refined with riding coordinates:
 C32(H32), C45(H45), C24(H24), C57(H57), C21(H21), C48(H48), C12(H12),
 C36(H36), C60(H60), C9(H9)
6.b Secondary CH2 refined with riding coordinates:
 N7(H7A,H7B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B),
 C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B)
6.c Me refined with riding coordinates:
 C69(H69A,H69B,H69C), C74(H74A,H74B,H74C), C63(H63A,H63B,H63C), C68(H68A,H68B,
 H68C)
6.d Aromatic/amide H refined with riding coordinates:
 C33(H33), C30(H30), C29(H29), C41(H41), C17(H17), C18(H18), C42(H42),
 C19(H19), C54(H54), C7(H7), C53(H53), C43(H43), C55(H55), C5(H5), C6(H6)
6.e Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C35(H35A,H35B,H35C), C58(H58A,H58B,H58C), C22(H22A,H22B,
 H22C), C46(H46A,H46B,H46C), C34(H34A,H34B,H34C), C23(H23A,H23B,H23C), C26(H26A,
 H26B,H26C), C25(H25A,H25B,H25C), C50(H50A,H50B,H50C), C49(H49A,H49B,H49C),
 C59(H59A,H59B,H59C), C37(H37A,H37B,H37C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C61(H61A,H61B,H61C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C38(H38A,
 H38B,H38C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              24060
_olex2_submission_special_instructions 'No special instructions were received'