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_7126997
_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 F2 N5 O2 P Ru, 0.84(F2 O2 P), 0.25(F3.91 P0.65), 0.5(C3 H6 O)'
_chemical_formula_sum            'C30.5 H28 F4.65 N5 O4.18 P2 Ru'
_chemical_formula_weight         782.78
_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             2020-06-16
_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                99.440(12)
_cell_angle_beta                 94.919(12)
_cell_angle_gamma                109.589(19)
_cell_formula_units_Z            4
_cell_length_a                   11.390(4)
_cell_length_b                   16.353(5)
_cell_length_c                   20.162(6)
_cell_measurement_reflns_used    4575
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.569
_cell_measurement_theta_min      2.171
_cell_volume                     3450(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  '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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.1337
_diffrn_reflns_av_unetI/netI     0.1126
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            74964
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.417
_diffrn_reflns_theta_min         1.036
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6816
_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    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1581
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.813
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.196
_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     1084
_refine_ls_number_reflns         14156
_refine_ls_number_restraints     366
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1633
_refine_ls_R_factor_gt           0.0882
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1610P)^2^+12.0100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2513
_refine_ls_wR_factor_ref         0.3014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7676
_reflns_number_total             14156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04426a2.cif
_cod_data_source_block           berry933
_cod_depositor_comments
'Adding full bibliography for 7126994--7126998.cif.'
_cod_original_cell_volume        3450.0(19)
_cod_original_formula_sum        'C30.50 H28 F4.65 N5 O4.18 P2 Ru'
_cod_database_code               7126997
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.947
_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
 P1-O2 = P1-O2A = P2-O4 = P2-O4A
 1.41602 with sigma of 0.01
 P1-F1A = P1-F2 = P2-F3 = P2-F4A
 1.67967 with sigma of 0.01
 P1-F1 = P1-F2A = P2-F3A = P2-F4
 1.54943 with sigma of 0.01
 P4-F7 = P4-F8 = P4-F8A = P4-F9 = P4-F9A
 1.56588 with sigma of 0.01
 F7-F8 = F7-F8A = F7-F9 = F7-F9A = F8-F9 = F8A-F9A
 2.17952 with sigma of 0.015
 P3-O5 = P3-O6
 1.465 with sigma of 0.005
 P3-F5 = P3-F6
 1.527 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
P1 \\sim F1 \\sim F2 \\sim O2 \\sim F1A \\sim F2A \\sim O2A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
P2 \\sim F3 \\sim F4 \\sim O4 \\sim F3A \\sim F4A \\sim O4A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
P3A \\sim F5A \\sim F6A \\sim O5A \\sim O6A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O7 \\sim C64 \\sim C65 \\sim C66: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O7A \\sim C64A \\sim C65A \\sim C66A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
O7B \\sim C64B \\sim C65B \\sim C66B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
P3 \\sim F5 \\sim F6 \\sim O5 \\sim O6: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
P3B \\sim F5B \\sim F6B \\sim O5B \\sim O6B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(P4) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F9) \\sim
Ueq, Uanis(F9A) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C66A) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(O7C) = Uiso(C64C) = Uiso(C65C) = Uiso(C66C)
4. Same fragment restrains
{P3, F5, F6, O5, O6} sigma for 1-2: 0.005, 1-3: 0.01
as
{P3A, F5A, F6A, O5A, O6A}
{P3, F5, F6, O5, O6} sigma for 1-2: 0.005, 1-3: 0.01
as
{P3B, F5B, F6B, O5B, O6B}
5. Others
 1*[Sof(P3)+Sof(F5)+Sof(F6)+Sof(O5)+Sof(O6)]+1*[Sof(P3A)+Sof(F5A)+Sof(F6A)+
 Sof(O5A)+Sof(O6A)]+1*[Sof(P3B)+Sof(F5B)+Sof(F6B)+Sof(O5B)+Sof(O6B)]+0.5*
 [Sof(P4)+Sof(F7)]=2 with esd of 0
 1*[Sof(P4)+Sof(F7)]-1*[Sof(F8)+Sof(F9)]-1*[Sof(F8A)+Sof(F9A)]=0 with esd of 0
 1*[Sof(O7)+Sof(C64)+Sof(H64A)+Sof(H64B)+Sof(H64C)+Sof(C65)+Sof(C66)+Sof(H66A)+
 Sof(H66B)+Sof(H66C)]+1*[Sof(O7A)+Sof(C64A)+Sof(H64D)+Sof(H64E)+Sof(H64F)+
 Sof(C65A)+Sof(C66A)+Sof(H66D)+Sof(H66E)+Sof(H66F)]+1*[Sof(O7B)+Sof(C64B)+
 Sof(H64G)+Sof(H64H)+Sof(H64I)+Sof(C65B)+Sof(C66B)+Sof(H66G)+Sof(H66H)+
 Sof(H66I)]+1*[Sof(O7C)+Sof(C64C)+Sof(H64J)+Sof(H64K)+Sof(H64L)+Sof(C65C)+
 Sof(C66C)+Sof(H66J)+Sof(H66K)+Sof(H66L)]=1 with esd of 0
 Sof(F1A)=Sof(F2A)=Sof(O2A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(O2)=FVAR(1)
 Sof(F3A)=Sof(F4A)=Sof(O4A)=1-FVAR(2)
 Sof(F3)=Sof(F4)=Sof(O4)=FVAR(2)
 Sof(P3)=Sof(F5)=Sof(F6)=Sof(O5)=Sof(O6)=FVAR(3)
 Sof(P3A)=Sof(F5A)=Sof(F6A)=Sof(O5A)=Sof(O6A)=FVAR(4)
 Sof(P3B)=Sof(F5B)=Sof(F6B)=Sof(O5B)=Sof(O6B)=FVAR(5)
 Sof(P4)=0.5*FVAR(7)
 Sof(F7)=FVAR(6)
 Sof(F8)=Sof(F9)=FVAR(7)
 Sof(F8A)=Sof(F9A)=FVAR(8)
 Sof(O7)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C65)=Sof(C66)=Sof(H66A)=
 Sof(H66B)=Sof(H66C)=FVAR(9)
 Sof(O7A)=Sof(C64A)=Sof(H64D)=Sof(H64E)=Sof(H64F)=Sof(C65A)=Sof(C66A)=
 Sof(H66D)=Sof(H66E)=Sof(H66F)=FVAR(10)
 Sof(O7B)=Sof(C64B)=Sof(H64G)=Sof(H64H)=Sof(H64I)=Sof(C65B)=Sof(C66B)=
 Sof(H66G)=Sof(H66H)=Sof(H66I)=FVAR(11)
 Sof(O7C)=Sof(C64C)=Sof(H64J)=Sof(H64K)=Sof(H64L)=Sof(C65C)=Sof(C66C)=
 Sof(H66J)=Sof(H66K)=Sof(H66L)=FVAR(12)
6.a Free rotating group:
 O7(C64,C65,C66), O7A(C64A,C65A,C66A), O7B(C64B,C65B,C66B), O7C(C64C,C65C,C66C)
6.b 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.c Idealised Me refined with riding coordinates:
 C64A(H64D,H64E,H64F), C66B(H66G,H66H,H66I), C64C(H64J,H64K,H64L)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C19(H19A,H19B,H19C), C36(H36A,H36B,H36C), C48(H48A,H48B,
 H48C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C66A(H66D,H66E,H66F),
 C64B(H64G,H64H,H64I), C66C(H66J,H66K,H66L)
;
_shelx_res_checksum              64514
_shelx_hkl_checksum              49325
_olex2_submission_special_instructions 'No special instructions were received'