#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:22:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179324 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/21/4322131.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4322131
loop_
_publ_author_name
'Tiziana Funaioli'
'Claudia Cavazza'
'Fabio Marchetti'
'Giuseppe Fachinetti'
_publ_contact_author
;
        Fabio Marchetti
        Dipartimento di Chimica e Chimica Industriale
        Universita' di Pisa
        Via Risorgimento, 35
        56126 Pisa
        Italy
;
_publ_contact_author_email       fama@dcci.unipi.it
_publ_contact_author_fax         '050 20237'
_publ_contact_author_phone       '050 918233'
_publ_section_title
;
 Aqueous Organometallic Chemistry of Ruthenium(II). Aquo Carbonyl
 Derivatives and Related Ethene Hydrocarboxylation in Fully Aqueous
 Solvent
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3361
_journal_page_last               3368
_journal_paper_doi               10.1021/ic981429i
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         '[Ru(CO)3(H2O)3](BF4)2'
_chemical_formula_sum            'C3 H6 B2 F8 O6 Ru'
_chemical_formula_weight         412.77
_chemical_name_systematic
; 
 Tris-aquo-tricarbonyl-ruthenium(II) di-tetrafluoborate 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   7.5675(11)
_cell_length_b                   7.5675(11)
_cell_length_c                   34.703(5)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      11.83
_cell_measurement_theta_min      5.15
_cell_volume                     1721.1(4)
_computing_cell_refinement       'XSCANS 2.1'
_computing_data_collection       'XSCANS 2.1'
_computing_data_reduction        'SHELXTL-Plus 5.03'
_computing_molecular_graphics    'SHELXTL-Plus 5.03'
_computing_publication_material  'SHELXTL-Plus 5.03'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.269
_diffrn_measured_fraction_theta_max 0.269
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       ω/2θ
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1182
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.499
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   XABS2
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Fragment of hexagonal plate'
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         946
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.437
_refine_ls_shift/su_mean         0.085
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0332P)²+0.5055P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0483
_refine_ls_wR_factor_ref         0.0491
_reflns_number_gt                916
_reflns_number_total             946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic981429i_2.cif
_cod_data_source_block           r3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.5055P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.5055P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4322131
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.6667 0.3333 0.143134(12) 0.0120(2) Uani 1 d SD . .
OW1 O 0.5671(12) 0.0933(10) 0.1033(2) 0.023(2) Uani 1 d D . .
H1 H 0.4621 0.0611 0.0931 0.030 Uiso 1 d . . .
H2 H 0.5438 0.0002 0.1163 0.030 Uiso 1 d . . .
C1 C 0.4329(12) 0.1947(13) 0.1761(2) 0.020(2) Uiso 1 d D . .
O1 O 0.2886(11) 0.1050(13) 0.1931(3) 0.0244(18) Uani 1 d D . .
Ru2 Ru 0.3333 0.6667 0.315192(10) 0.0130(3) Uani 1 d SD . .
OW2 O 0.4741(11) 0.5611(12) 0.35486(14) 0.0136(15) Uani 1 d D . .
H3 H 0.5509 0.5388 0.3424 0.018 Uiso 1 d . . .
H4 H 0.4060 0.4527 0.3637 0.018 Uiso 1 d . . .
C2 C 0.2261(17) 0.4249(11) 0.2838(2) 0.018(2) Uiso 1 d D . .
O2 O 0.1696(16) 0.2943(13) 0.2636(3) 0.033(2) Uani 1 d D . .
B1 B 0.0000 0.0000 0.0857(4) 0.029(6) Uani 1 d SD . .
F11 F 0.0000 0.0000 0.0459(3) 0.035(4) Uani 1 d SD . .
F12 F 0.1685(11) -0.0038(16) 0.0996(3) 0.055(3) Uani 1 d D . .
B2 B 0.3333 -0.3333 0.17342(15) 0.0019(18) Uani 1 d SD . .
F21 F 0.3333 -0.3333 0.2132(2) 0.036(3) Uani 1 d SD . .
F22 F 0.5213(8) -0.1859(12) 0.1596(2) 0.034(2) Uani 1 d D . .
B3 B 0.6667 0.3333 0.2863(4) 0.057(7) Uani 1 d SD . .
F31 F 0.6667 0.3333 0.2465(2) 0.061(5) Uani 1 d SD . .
F32 F 0.7016(15) 0.5210(10) 0.29954(18) 0.036(2) Uani 1 d D . .
B4 B 0.0000 0.0000 0.37244(18) 0.008(3) Uani 1 d SD . .
F41 F 0.0000 0.0000 0.4125(2) 0.018(3) Uani 1 d SD . .
F42 F 0.1869(9) 0.1569(11) 0.3595(2) 0.0298(14) Uani 1 d D . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ru1 C1 88.1(4) 2_655 . ?
C1 Ru1 C1 88.1(4) 2_655 3_665 ?
C1 Ru1 C1 88.1(4) . 3_665 ?
C1 Ru1 OW1 95.5(4) 2_655 . ?
C1 Ru1 OW1 94.9(3) . . ?
C1 Ru1 OW1 175.4(4) 3_665 . ?
C1 Ru1 OW1 94.9(3) 2_655 2_655 ?
C1 Ru1 OW1 175.4(4) . 2_655 ?
C1 Ru1 OW1 95.5(4) 3_665 2_655 ?
OW1 Ru1 OW1 81.4(3) . 2_655 ?
C1 Ru1 OW1 175.4(4) 2_655 3_665 ?
C1 Ru1 OW1 95.5(4) . 3_665 ?
C1 Ru1 OW1 94.9(3) 3_665 3_665 ?
OW1 Ru1 OW1 81.4(3) . 3_665 ?
OW1 Ru1 OW1 81.4(3) 2_655 3_665 ?
O1 C1 Ru1 174.7(9) . . ?
C2 Ru2 C2 91.1(4) 3_565 2_665 ?
C2 Ru2 C2 91.1(4) 3_565 . ?
C2 Ru2 C2 91.1(4) 2_665 . ?
C2 Ru2 OW2 92.4(4) 3_565 2_665 ?
C2 Ru2 OW2 93.5(3) 2_665 2_665 ?
C2 Ru2 OW2 174.0(4) . 2_665 ?
C2 Ru2 OW2 93.5(3) 3_565 3_565 ?
C2 Ru2 OW2 174.0(4) 2_665 3_565 ?
C2 Ru2 OW2 92.4(4) . 3_565 ?
OW2 Ru2 OW2 82.6(3) 2_665 3_565 ?
C2 Ru2 OW2 174.0(4) 3_565 . ?
C2 Ru2 OW2 92.4(4) 2_665 . ?
C2 Ru2 OW2 93.5(3) . . ?
OW2 Ru2 OW2 82.6(3) 2_665 . ?
OW2 Ru2 OW2 82.6(3) 3_565 . ?
O2 C2 Ru2 175.2(10) . . ?
F11 B1 F12 110.6(5) . 3 ?
F11 B1 F12 110.6(5) . . ?
F12 B1 F12 108.3(5) 3 . ?
F11 B1 F12 110.6(5) . 2 ?
F12 B1 F12 108.3(5) 3 2 ?
F12 B1 F12 108.3(5) . 2 ?
F22 B2 F22 108.7(4) 2_545 . ?
F22 B2 F22 108.7(4) 2_545 3_655 ?
F22 B2 F22 108.7(4) . 3_655 ?
F22 B2 F21 110.3(4) 2_545 . ?
F22 B2 F21 110.3(4) . . ?
F22 B2 F21 110.3(4) 3_655 . ?
F31 B3 F32 109.3(5) . 3_665 ?
F31 B3 F32 109.3(5) . 2_655 ?
F32 B3 F32 109.6(5) 3_665 2_655 ?
F31 B3 F32 109.3(5) . . ?
F32 B3 F32 109.6(5) 3_665 . ?
F32 B3 F32 109.6(5) 2_655 . ?
F42 B4 F42 110.1(3) 3 . ?
F42 B4 F42 110.1(3) 3 2 ?
F42 B4 F42 110.1(3) . 2 ?
F42 B4 F41 108.8(3) 3 . ?
F42 B4 F41 108.8(3) . . ?
F42 B4 F41 108.8(3) 2 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C1 1.920(5) 2_655 ?
Ru1 C1 1.920(5) . ?
Ru1 C1 1.920(5) 3_665 ?
Ru1 OW1 2.100(5) . ?
Ru1 OW1 2.100(5) 2_655 ?
Ru1 OW1 2.100(5) 3_665 ?
C1 O1 1.121(5) . ?
Ru2 C2 1.926(4) 3_565 ?
Ru2 C2 1.925(4) 2_665 ?
Ru2 C2 1.925(4) . ?
Ru2 OW2 2.126(4) 2_665 ?
Ru2 OW2 2.126(4) 3_565 ?
Ru2 OW2 2.126(4) . ?
C2 O2 1.107(5) . ?
B1 F11 1.382(8) . ?
B1 F12 1.378(5) 3 ?
B1 F12 1.378(5) . ?
B1 F12 1.378(5) 2 ?
B2 F22 1.382(4) 2_545 ?
B2 F22 1.382(4) . ?
B2 F22 1.382(4) 3_655 ?
B2 F21 1.380(6) . ?
B3 F31 1.381(8) . ?
B3 F32 1.386(5) 3_665 ?
B3 F32 1.386(5) 2_655 ?
B3 F32 1.386(5) . ?
B4 F42 1.390(5) 3 ?
B4 F42 1.390(5) . ?
B4 F42 1.390(5) 2 ?
B4 F41 1.392(6) . ?
