On the mechanism of intermolecular nitrogen-atom transfer from a lattice-isolated diruthenium nitride intermediate.
Cosio, Mario N.; Alharbi, Waad S.; Sur, Aishanee; Wang, Chen-Hao; Najafian, Ahmad; Cundari, Thomas R.; Powers, David C.; Faraday discussions 244 (2023) 154–168; doi:10.1039/d2fd00167e

data_1568975
_publ_section_title
;
 On the mechanism of intermolecular nitrogen-atom transfer from a
 lattice-isolated diruthenium nitride intermediate.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              154
_journal_page_last               168
_journal_paper_doi               10.1039/d2fd00167e
_journal_volume                  244
_journal_year                    2023
_chemical_formula_moiety         'C64 H80 N6 O16 Ru4'
_chemical_formula_sum            'C64 H80 N6 O16 Ru4'
_chemical_formula_weight         1593.62
_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             2022-11-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-23 deposited with the CCDC.	2022-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                64.903(2)
_cell_angle_beta                 89.935(2)
_cell_angle_gamma                74.563(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2116(9)
_cell_length_b                   17.2969(13)
_cell_length_c                   19.8432(15)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      26.27
_cell_measurement_theta_min      2.34
_cell_volume                     3331.4(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.999
_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  0.1158
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            157822
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.444
_diffrn_reflns_theta_min         1.900
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6622
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1207 before and 0.0825 after correction.
The Ratio of minimum to maximum transmission is 0.8884.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       plate
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.810
_refine_diff_density_min         -2.093
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         13694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0842
_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^)+(0.0226P)^2^+60.0740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.1850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11184
_reflns_number_total             13694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2fd00167e2.cif
_cod_data_source_block           mnc3117_dmf_04212022_0m
_cod_depositor_comments          'Adding full bibliography for 1568975.cif.'
_cod_original_cell_volume        3331.4(4)
_cod_database_code               1568975
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.963
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C29) = Uanis(C60)
3.a Secondary CH2 refined with riding coordinates:
 C01K(H01A,H01B), C01R(H01C,H01D), C01S(H01E,H01F), C5(H5A,H5B), C12(H12A,
 H12B), C27(H27A,H27B), C35(H35A,H35B), C49(H49A,H49B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C11(H11), C22(H22), C23(H23), C24(H24), C26(H26),
 C37(H37), C39(H39), C40(H40), C41(H41), C51(H51), C52(H52), C53(H53), C55(H55)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C),
 C60(H60A,H60B,H60C)
;
_shelx_res_checksum              29864
_olex2_submission_special_instructions 'No special instructions were received'