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_7126996
_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
'Cl4.69 Sb, 0.69(Cl), C29 H25 Cl N5 Ru, 2(C3 H6 O)'
_chemical_formula_sum            'C35 H37 Cl6.39 N5 O2 Ru Sb'
_chemical_formula_weight         1009.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-12
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.348(7)
_cell_length_b                   13.355(4)
_cell_length_c                   12.292(4)
_cell_measurement_reflns_used    9754
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.148
_cell_measurement_theta_min      2.252
_cell_volume                     3833(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            70231
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.150
_diffrn_reflns_theta_min         1.744
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.584
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2007
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.289
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4428
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0221P)^2^+20.1460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3943
_reflns_number_total             4428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04426a2.cif
_cod_data_source_block           berry750
_cod_depositor_comments
'Adding full bibliography for 7126994--7126998.cif.'
_cod_database_code               7126996
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.877
_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. Uiso/Uaniso restraints and constraints
C20 \\sim C21: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C20A \\sim C21A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O2) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C19A)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uiso(Cl3A) = Uiso(Cl3B) = Uiso(Cl4A) = Uiso(Cl4B)
3. Same fragment restrains
{O1, C16, C17, C18} sigma for 1-2: 0.01, 1-3: 0.02
as
{O2, C19, C20, C21}
{O1, C16, C17, C18} sigma for 1-2: 0.01, 1-3: 0.02
as
{O2A, C19A, C20A, C21A}
4. Others
 1*[Sof(Cl3)+Sof(Cl4)+Sof(Cl5)+Sof(Cl6)]+1.333333*[Sof(Cl3A)+Sof(Cl4A)+
 Sof(Cl3B)+Sof(Cl4B)]=1 with esd of 0
 Sof(Cl3)=Sof(Cl5)=Sof(Cl6)=0.5*FVAR(2)
 Sof(Cl4)=FVAR(1)
 Sof(Cl3A)=Sof(Cl4A)=Sof(Cl3B)=Sof(Cl4B)=0.5*FVAR(3)
 Sof(O2A)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20A)=Sof(C21A)=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=0.5*(1-FVAR(4))
 Sof(O2)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=0.5*FVAR(4)
 Fixed Sof: O1(0.5) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C17(0.5) C18(0.5)
 H18A(0.5) H18B(0.5) H18C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C19A(H19D,H19E,H19F), C21A(H21D,H21E,H21F)
;
_shelx_res_checksum              91649
_shelx_hkl_checksum              13752
_olex2_submission_special_instructions 'No special instructions were received'