A metastable Ru<sup>III</sup> azido complex with metallo-Staudinger reactivity.
Park, Sungho V.; Fry, Charles G.; Bill, Eckhard; Berry, John F.; Chemical communications (Cambridge, England) 56 (2020) 10738–10741; doi:10.1039/d0cc04426a

data_7126994
_publ_section_title
;
 A metastable Ru<sup>III</sup> azido complex with metallo-Staudinger
 reactivity.
;
_journal_issue                   73
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10738
_journal_page_last               10741
_journal_paper_doi               10.1039/d0cc04426a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C29 H25 N8 Ru, 2(F6 P), C3 H6 O'
_chemical_formula_sum            'C32 H31 F12 N8 O P2 Ru'
_chemical_formula_weight         934.66
_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             2018-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-17 deposited with the CCDC.	2020-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                99.814(10)
_cell_angle_beta                 116.882(13)
_cell_angle_gamma                96.323(13)
_cell_formula_units_Z            4
_cell_length_a                   15.546(4)
_cell_length_b                   15.7344(18)
_cell_length_c                   16.911(2)
_cell_measurement_reflns_used    1772
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.073
_cell_measurement_theta_min      2.217
_cell_volume                     3552.1(12)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1386
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14615
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.485
_diffrn_reflns_theta_min         1.344
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 62510 reflections, Rint = 0.1296
 (8276 with I > 3sig(I), Rint = 0.0660)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.017
_exptl_transmission_factor_max   0.745371
_exptl_transmission_factor_min   0.387534
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1032
_refine_ls_number_reflns         14615
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+14.0683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9030
_reflns_number_total             14615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04426a2.cif
_cod_data_source_block           berry747
_cod_depositor_comments
'Adding full bibliography for 7126994--7126998.cif.'
_cod_original_cell_volume        3552.2(12)
_cod_database_code               7126994
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.876
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7966(15)
 0.2034(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C59-C60 = C59A-C60 = C60-C61 = C60-C61A
 1.47902 with sigma of 0.01
 O1-C59 = O1-C59A = O1-C61 = O1-C61A
 2.33997 with sigma of 0.015
 C59-C61 = C59A-C61A
 2.52706 with sigma of 0.015
4. Uiso/Uaniso restraints and constraints
C63 \\sim C64: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C64) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Others
 Sof(C59A)=Sof(H59D)=Sof(H59E)=Sof(H59F)=Sof(C61A)=Sof(H61D)=Sof(H61E)=
 Sof(H61F)=1-FVAR(1)
 Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=
 FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C38(H38),
 C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C50(H50),
  C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58)
6.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C19(H19A,H19B,H19C), C36(H36A,H36B,H36C), C48(H48A,H48B,
 H48C), C59(H59A,H59B,H59C), C59A(H59D,H59E,H59F), C61(H61A,H61B,H61C),
 C61A(H61D,H61E,H61F), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C)
;
_shelx_res_checksum              45745
_shelx_hkl_checksum              87793
_olex2_submission_special_instructions 'No special instructions were received'