Heteroleptic "open ruthenocene" for deposition of Ru films from the gas phase.
Kultyshev, Roman; Harkness, Ian; Berry, Daniel B. G.; Jobson, Hoi; Marchbank, Huw; Eralp Erden, Tugce; Ashfield, Laura; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2261–2264; doi:10.1039/d4dt02466d

data_7717846
_publ_section_title
;
 Heteroleptic "open ruthenocene" for deposition of Ru films from the gas
 phase.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2261
_journal_page_last               2264
_journal_paper_doi               10.1039/d4dt02466d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C13 H20 O Ru'
_chemical_formula_sum            'C13 H20 O Ru'
_chemical_formula_weight         293.36
_chemical_melting_point          346
_chemical_name_systematic
'(\h5-2,4-dimethylpentadienyl)(\h5-2,4-dimethyl-1-oxapentadienyl) ruthenium'
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-07-22 deposited with the CCDC.	2024-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.493(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3396(2)
_cell_length_b                   16.8660(4)
_cell_length_c                   10.2918(3)
_cell_measurement_reflns_used    44045
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.7160
_cell_measurement_theta_min      2.3320
_cell_volume                     1238.85(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -54.00  30.00   0.50    3.00    --   18.20 -56.00 125.00  168
  2  \w      7.00  61.00   0.50    3.00    --   18.20  56.00 -92.00  108
  3  \w     21.00  64.00   0.50    3.00    --  -14.92  19.00-150.00   86
  4  \w    -56.00  -2.00   0.50    3.00    --  -14.92 -57.00 -60.00  108
  5  \w    -27.00  59.00   0.50    3.00    --  -14.92  56.00 -92.00  172
  6  \w     21.00  64.00   0.50    3.00    --  -14.92  19.00 -30.00   86
  7  \w    -60.00 -17.00   0.50    3.00    --   18.20 -19.00-180.00   86
  8  \w    -60.00 -17.00   0.50    3.00    --   18.20 -19.00  30.00   86
  9  \w    -60.00 -27.00   0.50    3.00    --   18.20 -19.00 150.00   66
 10  \w    -60.00 -35.00   0.50    3.00    --   18.20 -19.00   0.00   50
 11  \w    -55.00  -9.00   0.50    3.00    --  -14.92 -56.00 125.00   92
 12  \w    -48.00 -23.00   0.50    3.00    --  -14.92 103.00 101.05   50
 13  \w    -42.00  13.00   0.50    3.00    --  -14.92  90.00-143.99  110
 14  \w    -68.00 -43.00   0.50    3.00    --  -14.92 137.00 135.56   50
 15  \w    -49.00  -1.00   0.50    3.00    --  -14.92 105.00 171.34   96
 16  \w    -83.00 -17.00   0.50    3.00    --  -14.92 -19.00 150.00  132
 17  \w    -68.00 -43.00   0.50    3.00    --  -14.92 137.00  53.25   50
 18  \w    -44.00  -3.00   0.50    3.00    --  -14.92  94.00  15.93   82
 19  \w    -68.00 -33.00   0.50    3.00    --  -14.92 137.00 -76.90   70
 20  \w      6.00  62.00   0.50    3.00    --   18.20  57.00  90.00  112
 21  \w      1.00  41.00   0.50    3.00    --   18.20  68.00 117.63   80
 22  \w     21.00  94.00   0.50    3.00    --   18.20  19.00-180.00  146
 23  \w     21.00  96.00   0.50    3.00    --   18.20  19.00 -30.00  150
 24  \w     23.00  49.00   0.50    3.00    --   18.20 -99.00  30.00   52
 25  \w      4.00  51.00   0.50    3.00    --   18.20  64.00 -46.96   94
 26  \w    -63.00 -14.00   0.50    3.00    --  -14.92 130.00 -97.30   98
 27  \w    -48.00   4.00   0.50    3.00    --  -14.92 103.00 101.05  104
 28  \w    -46.00 -17.00   0.50    3.00    --  -14.92  99.00 163.84   58
 29  \w     21.00  64.00   0.50    3.00    --  -14.92  19.00 120.00   86
 30  \w    -36.00  24.00   0.50    3.00    --  -14.92  77.00  30.00  120
 31  \w    -56.00  -2.00   0.50    3.00    --  -14.92 -57.00-180.00  108
 32  \w    -56.00  -2.00   0.50    3.00    --  -14.92 -57.00  90.00  108
 33  \w    -68.00 -19.00   0.50    3.00    --  -14.92 137.00 -76.90   98
 34  \w    -56.00  -2.00   0.50    3.00    --  -14.92 -57.00-120.00  108
 35  \w      6.00  62.00   0.50    3.00    --   18.20  57.00-180.00  112
 36  \w     -1.00  31.00   0.50    3.00    --   18.20  73.00  94.99   64
 37  \w     10.00  94.00   0.50    3.00    --   18.20  38.00  90.00  168
 38  \w    -60.00 -17.00   0.50    3.00    --   18.20 -19.00 -30.00   86
 39  \w      0.00  49.00   0.50    3.00    --   18.20 -99.00 -90.00   98
 40  \w    -60.00 -17.00   0.50    3.00    --   18.20 -19.00  60.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ diffractometer with Arc)Sec VHF Varimax confocal mirrors, a UG2 goniometer and HyPix 6000HE detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0305753000
_diffrn_orient_matrix_UB_12      -0.0270428000
_diffrn_orient_matrix_UB_13      -0.0533975000
_diffrn_orient_matrix_UB_21      0.0945596000
_diffrn_orient_matrix_UB_22      -0.0082230000
_diffrn_orient_matrix_UB_23      -0.0006249000
_diffrn_orient_matrix_UB_31      0.0015226000
_diffrn_orient_matrix_UB_32      -0.0311605000
_diffrn_orient_matrix_UB_33      0.0465563000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, Arc)Sec VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24849
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.573
_diffrn_reflns_theta_min         2.366
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.238
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.61a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_recrystallization_method
'The material was recrystallised from hexane'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0200
_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^)+(0.0254P)^2^+0.5783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3152
_reflns_number_total             3462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02466d2.cif
_cod_data_source_block           2023ncsc0203r1e
_cod_depositor_comments          'Adding full bibliography for 7717846.cif.'
_cod_database_code               7717846
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C13 H20 O Ru'
_chemical_oxdiff_usercomment     AJ4218_003
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.764
_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.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              43456
_shelx_hkl_checksum              77056
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in oil'
_olex2_submission_original_sample_id AJ4218_003
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 6.263
_oxdiff_exptl_absorpt_empirical_full_min 0.369