Synthesis and Structure of a Triruthenium Complex Containing a Perpendicularly Coordinatedμ3-η2:η2(⊥)-Nitrile Ligand and Its Protonation To Yield a Perpendicularly Coordinated Iminoacyl Ligand
Takao, Toshiro; Kawashima, Takashi; Matsubara, Kouki; Suzuki, Hiroharu; Organometallics 24 (2005) 3371–; doi:10.1021/om050320x

data_4075941
_publ_section_title
;
 Synthesis and Structure of a Triruthenium Complex Containing a
 Perpendicularly Coordinated\m3-\h2:\h2(&#x22A5;)-Nitrile Ligand and Its
 Protonation To Yield a Perpendicularly Coordinated Iminoacyl Ligand
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3371
_journal_paper_doi               10.1021/om050320x
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C37 H54 B F4 N Ru3'
_chemical_formula_weight         902.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                116.505(4)
_cell_angle_beta                 102.326(4)
_cell_angle_gamma                89.202(4)
_cell_formula_units_Z            4
_cell_length_a                   10.8217(10)
_cell_length_b                   19.8704(16)
_cell_length_c                   20.0472(18)
_cell_measurement_reflns_used    39992
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      3.02
_cell_volume                     3752.4(6)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku Rotating Anode Ultrax18'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39992
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.238
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8240
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.836
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.00000(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         21102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          1.034
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+8.5762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                15265
_reflns_number_total             21178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050320xsi20050421_111633.cif
_cod_data_source_block           4a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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_sg_symbol_H-M      P-1
_cod_database_code               4075941