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_7703878
_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         '2(C26 H34 N3 O2 Rh)'
_chemical_formula_sum            'C52 H68 N6 O4 Rh2'
_chemical_formula_weight         1046.94
_chemical_name_systematic        '[{Rh(CO)2(N3Dipp2)}2]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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                81.307(2)
_cell_angle_beta                 74.676(2)
_cell_angle_gamma                77.317(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2722(5)
_cell_length_b                   13.4363(5)
_cell_length_c                   15.3662(7)
_cell_measurement_reflns_used    2611
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.36
_cell_measurement_theta_min      2.45
_cell_volume                     2565.68(18)
_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 0.989
_diffrn_measured_fraction_theta_max 0.981
_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  0.0623
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39793
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.177
_diffrn_reflns_theta_min         1.620
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1342 before and 0.0579 after correction. The Ratio of minimum to maximum transmission is 0.8940. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         11201
_refine_ls_number_restraints     467
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7895
_reflns_number_total             11201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00285b2.cif
_cod_data_source_block           p_1
_cod_depositor_comments
'Adding full bibliography for 7703878--7703902.cif.'
_cod_database_code               7703878
_shelx_shelxl_version_number     2018/3
_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
 Rh2-C28 \\sim Rh2_$1-C28
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Rh2 \\sim C28 \\sim O4: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. 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
5.a Ternary CH refined with riding coordinates:
 C35(H35), C47(H47), C9(H9), C38(H38), C24(H24), C50(H50), C12(H12), C21(H21)
5.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C19(H19), C17(H17), C32(H32), C33(H33), C18(H18), C43(H43),
 C45(H45), C44(H44), C7(H7), C6(H6), C5(H5)
5.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C48(H48A,H48B,H48C), C25(H25A,H25B,H25C), C49(H49A,H49B,
 H49C), C37(H37A,H37B,H37C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C51(H51A,
 H51B,H51C), C11(H11A,H11B,H11C), C52(H52A,H52B,H52C), C26(H26A,H26B,H26C),
 C10(H10A,H10B,H10C), C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              37046
_olex2_submission_special_instructions 'No special instructions were received'