A new binuclear ruthenium complex with an annelated C7 bridge via an unprecedented [2 + 2] coupling reaction
Rigaut, Stéphane; Le Pichon, Luc; Touchard, Daniel; Dixneuf, Pierre H.; Daran, Jean-Claude; Chemical Communications  (2001) 1206–; doi:10.1039/b103301h

data_7114666
_publ_section_title
;
 A new binuclear ruthenium complex with an annelated C7 bridge via an
 unprecedented [2 + 2] coupling reaction
;
_journal_issue                   13
_journal_name_full               'Chemical Communications'
_journal_page_first              1206
_journal_paper_doi               10.1039/b103301h
_journal_year                    2001
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C58 H48 Cl1 F3 P4 Ru1'
_chemical_formula_structural     'C58 H48 CL F3 P4.5 RU1'
_chemical_formula_sum            'C58 H48 Cl F3 P4 Ru'
_chemical_formula_weight         1077.85
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.204(13)
_cell_angle_beta                 98.910(12)
_cell_angle_gamma                101.264(13)
_cell_formula_units_Z            2
_cell_length_a                   9.7811(10)
_cell_length_b                   12.1069(14)
_cell_length_c                   20.503(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      1.89
_cell_volume                     2334.0(5)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19015
_diffrn_reflns_theta_full        24.20
_diffrn_reflns_theta_max         24.20
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.6975
_exptl_absorpt_correction_T_min  0.2367
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998)
I/sigma threshold for reflections     =   5.000
Delta(U)/lambda**2                    =   0.000
Highest even order spherical harmonic =       6
Highest odd  order spherical harmonic =       3
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flat box'
_exptl_crystal_F_000             1103
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         6976
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0766
_reflns_number_gt                5466
_reflns_number_total             6976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103301h.txt
_cod_data_source_block           (3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2334.0(4)
_cod_original_formula_sum        'C58 H48 Cl1 F3 P4 Ru1'
_cod_database_code               7114666
_exptl_absorpt_factor_mur        0.000
_exptl_absorpt_rmerge_before     0.0599
_exptl_absorpt_rmerge_after      0.0577