Synthesis, structures and dynamic NMR spectra of ??6-hexaethylbenzene complexes of ruthenium(0) and ruthenium(ii)
Baldwin, Richard; Bennett, Martin A.; Hockless, David C. R.; Pertici, Paolo; Verrazzani, Alessandra; Uccello Barretta, Gloria; Marchetti, Fabio; Salvadori, Piero; Journal of the Chemical Society, Dalton Transactions  (2002) 4488–; doi:10.1039/b204875m

data_7011837
_publ_section_title
;
 Synthesis, structures and dynamic NMR spectra of ??6-hexaethylbenzene
 complexes of ruthenium(0) and ruthenium(ii)
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4488
_journal_paper_doi               10.1039/b204875m
_journal_year                    2002
_chemical_formula_moiety         'C21 H39 Cl2 P Ru, H2 O'
_chemical_formula_sum            'C21 H41 Cl2 O P Ru'
_chemical_formula_weight         512.50
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_audit_creation_date             2002-02-26
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
Refinement by David Hockless
Report by David Hockless Sept 1994
Cif editted by Tony Willis (hence e-mail address) for Martin Bennett Mar
2002
2002-03-19  passes checkcif with some warnings.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.01(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.698(2)
_cell_length_b                   14.618(4)
_cell_length_c                   9.613(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      19.5
_cell_measurement_theta_min      13.5
_cell_volume                     1207.2(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      296.2
_diffrn_measured_fraction_theta_full 1.
_diffrn_measured_fraction_theta_max 1.
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.01685
_diffrn_orient_matrix_UB_12      -0.01616
_diffrn_orient_matrix_UB_13      0.10234
_diffrn_orient_matrix_UB_21      0.00908
_diffrn_orient_matrix_UB_22      0.06641
_diffrn_orient_matrix_UB_23      0.02489
_diffrn_orient_matrix_UB_31      -0.11483
_diffrn_orient_matrix_UB_32      0.00288
_diffrn_orient_matrix_UB_33      0.00028
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.02880
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2399
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        -0.35
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  .768
_exptl_absorpt_correction_T_min  .739
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             536.00
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.44
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.370
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2008
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.0000|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.0240
_reflns_number_gt                2008
_reflns_number_total             2246
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            b204875m.txt
_cod_data_source_block           rxb3
_cod_original_cell_volume        1207.1(4)
_cod_original_sg_symbol_H-M      'P 21/m     '
_cod_original_formula_sum        'C21 H41 Cl2 O P Ru '
_cod_database_code               7011837