A photochemical route to a square planar, ruthenium(iv)-bis(imide)
Aldrich, Kelly E.; Odom, Aaron L.; Chemical Communications  (2019) –; doi:10.1039/C9CC01019J

data_7123226
_publ_section_title
;
 A photochemical route to a square planar, ruthenium(iv)-bis(imide)
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01019J
_journal_year                    2019
_chemical_formula_moiety         'C30 H55 N4 P3 Ru, C2 H4 O0.25'
_chemical_formula_sum            'C32 H59 N4 O0.25 P3 Ru'
_chemical_formula_weight         697.81
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-01 deposited with the CCDC.    2019-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.336(6)
_cell_length_b                   16.773(5)
_cell_length_c                   24.001(7)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.24
_cell_volume                     7382(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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
'SHELXS (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0966
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            62482
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.139
_diffrn_reflns_theta_min         1.645
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_T_max  0.4712
_exptl_absorpt_correction_T_min  0.3852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0848 before and 0.0646 after correction.
The Ratio of minimum to maximum transmission is 0.8175.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.422
_exptl_crystal_size_min          0.408
_refine_diff_density_max         1.271
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         7364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0777P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1394
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4932
_reflns_number_total             7364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01019j2.cif
_cod_data_source_block           pbcn_a
_cod_database_code               7123226
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.787
_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(C24B) = Uanis(C24A) = Uanis(C22A) = Uanis(C22B) = Uanis(C23B) =
Uanis(C23A)
Uanis(C26B) = Uanis(C26A) = Uanis(C27B) = Uanis(C27A)
Uanis(C25B) = Uanis(C25A)
3. Others
 Fixed Sof: C25A(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C24B(0.5) H24A(0.5)
 H24B(0.5) H24C(0.5) C22B(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C26A(0.5)
 H26A(0.5) H26B(0.5) H26C(0.5) C23B(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 C27B(0.5) H27A(0.5) H27B(0.5) H27C(0.5) O1(0.25) C27A(0.5) H27D(0.5) H27E(0.5)
 H27F(0.5) C26B(0.5) H26D(0.5) H26E(0.5) H26F(0.5) C22A(0.5) H22D(0.5)
 H22E(0.5) H22F(0.5) C23A(0.5) H23D(0.5) H23E(0.5) H23F(0.5) C24A(0.5)
 H24D(0.5) H24E(0.5) H24F(0.5) C25B(0.5) H25D(0.5) H25E(0.5) H25F(0.5)
4.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19)
4.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C5(H5), C3(H3), C14(H14), C13(H13)
4.d Idealised Me refined as rotating group:
 C25A(H25A,H25B,H25C), C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C24B(H24A,H24B,
 H24C), C30(H30A,H30B,H30C), C9(H9A,H9B,H9C), C22B(H22A,H22B,H22C), C8(H8A,H8B,
 H8C), C28(H28A,H28B,H28C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C26A(H26A,
 H26B,H26C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23B(H23A,H23B,H23C),
 C27B(H27A,H27B,H27C), C27A(H27D,H27E,H27F), C26B(H26D,H26E,H26F), C22A(H22D,
 H22E,H22F), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F), C25B(H25D,H25E,H25F)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'