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_7126998
_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 Cl N5 Ru, F6 P, 0.5(C6 H12 O2)'
_chemical_formula_sum            'C32 H31 Cl F6 N5 O P Ru'
_chemical_formula_weight         783.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           26
_space_group_name_Hall           'P 2c -2'
_space_group_name_H-M_alt        'P m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-15
_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            2
_cell_length_a                   10.366(3)
_cell_length_b                   8.964(3)
_cell_length_c                   17.126(6)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.951
_cell_measurement_theta_min      2.272
_cell_volume                     1591.4(9)
_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      99.99
_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 1.000
_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  0.0451
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29870
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.130
_diffrn_reflns_theta_min         1.965
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7099
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 1682 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3704
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0237
_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^)+(0.0324P)^2^+0.8499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0584
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                3599
_reflns_number_total             3704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04426a2.cif
_cod_data_source_block           berry751
_cod_depositor_comments
'Adding full bibliography for 7126994--7126998.cif.'
_cod_original_cell_volume        1591.3(9)
_cod_database_code               7126998
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.944
_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
 C20-C21 = C20-C21A
 1.49563 with sigma of 0.005
 O1-C21 = O1-C21A
 2.36038 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C21A \\sim C21 \\sim C20: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C21) \\sim Ueq, Uanis(C21A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Fixed Sof: H7A(0.5) H7B(0.5) H7C(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C21(0.5)
 H21A(0.5) H21B(0.5) H21C(0.5) C21A(0.5) H21D(0.5) H21E(0.5) H21F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C16(H16),
 C17(H17), C18(H18), C19(H19)
5.b Idealised Me refined with riding coordinates:
 C7(H7A,H7B,H7C)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F)
;
_shelx_res_checksum              87868
_shelx_hkl_checksum              65332
_olex2_submission_special_instructions 'No special instructions were received'