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_7011838
_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         'C36 H45 Cl2 P Ru, C6 H6'
_chemical_formula_sum            'C42 H51 Cl2 P Ru'
_chemical_formula_weight         758.81
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             2002-02-26
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
Refinement by David Hockless
Report by David Hockless April 1999
Cif edited by Tony Willis (hence e-mail address) for Martin Bennett Mar 2002
2002-03-20  passes checkcif with minor warnings.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.358(2)
_cell_length_b                   19.226(1)
_cell_length_c                   20.478(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      46.2
_cell_measurement_theta_min      30.0
_cell_volume                     3684.3(9)
_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_details
;      
Rigaku AFC6R diffractometer with extended arm and 
evacuated collimator and beam tunnel.
Data cannot be collected beyond \y 60 deg in this configuration.
;
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.00018
_diffrn_orient_matrix_UB_12      0.01328
_diffrn_orient_matrix_UB_13      0.04721
_diffrn_orient_matrix_UB_21      -0.01859
_diffrn_orient_matrix_UB_22      -0.04953
_diffrn_orient_matrix_UB_23      0.01226
_diffrn_orient_matrix_UB_31      0.10523
_diffrn_orient_matrix_UB_32      -0.00873
_diffrn_orient_matrix_UB_33      0.00225
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.00000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3131
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        60.
_diffrn_reflns_theta_max         60.06
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        -2.53
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.397
_exptl_absorpt_correction_T_max  .723
_exptl_absorpt_correction_T_min  .572
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584.00
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.23
_refine_ls_abs_structure_details
;
Absolute structure determined by comparative refinement.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.448
_refine_ls_goodness_of_fit_ref   1.473
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     415
_refine_ls_number_reflns         2857
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.0130
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0282
_refine_ls_wR_factor_ref         0.0274
_reflns_number_gt                2857
_reflns_number_total             3131
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            b204875m.txt
_cod_data_source_block           rxb4
_cod_original_cell_volume        3684.2(6)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C42 H51 Cl2 P Ru '
_cod_database_code               7011838