Synthesis and Structures of Dinuclear 3,5-Bis(trifluoromethyl)pyrazolate Complexes of Ruthenium
Waheed, Abdul; Jones, Richard A.; Agapiou, Kyriacos; Yang, Xiaoping; Moore, Jennifer A.; Ekerdt, John G.; Organometallics 26 (2007) 6778–6783; doi:10.1021/om700521y

data_4073673
_publ_section_title
;
 Synthesis and Structures of Dinuclear 3,5-Bis(trifluoromethyl)pyrazolate
 Complexes of Ruthenium
;
_journal_issue                   27
_journal_name_full               Organometallics
_journal_page_first              6778
_journal_page_last               6783
_journal_paper_doi               10.1021/om700521y
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C52 H67 F12 N4 O2.5 Ru4'
_chemical_formula_weight         1420.38
_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                90.60(2)
_cell_angle_beta                 97.65(3)
_cell_angle_gamma                92.151(13)
_cell_formula_units_Z            1
_cell_length_a                   9.4914(19)
_cell_length_b                   11.171(2)
_cell_length_c                   13.850(3)
_cell_measurement_reflns_used    CCD
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.9
_cell_volume                     1454.2(5)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_computing_molecular_graphics    'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       \w-scans
_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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0383
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9621
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_T_max  0.8021
_exptl_absorpt_correction_T_min  0.7290
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Absorption correction given as Gaussian
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             711
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.808
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.253
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(8)
_refine_ls_extinction_coef       0.0035(3)
_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   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5120
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+1.5600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                4122
_reflns_number_total             5120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700521y_si.cif
_cod_data_source_block           complex-4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C52 H67 F12 N4 O2.50 Ru4'
_cod_database_code               4073673