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#$Date: 2025-08-20 14:05:43 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301829 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/84/4068452.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_4068452
loop_
_publ_author_name
'Martín, Marta'
'Horváth, Henrietta'
'Sola, Eduardo'
'Kathó, Ágnes'
'Joó, Ferenc'
_publ_section_title
;
 Water-Soluble Triisopropylphosphine Complexes of Ruthenium(II):
 Synthesis, Equilibria, and Acetonitrile Hydration
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              561
_journal_paper_doi               10.1021/om8008553
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C14 H27 N2 P Ru0.50, B F4, C H Cl3'
_chemical_formula_sum            'C14 H28 B Cl3 F4 N2 P Ru0.5'
_chemical_formula_weight         499.05
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.9210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9787(9)
_cell_length_b                   17.9817(14)
_cell_length_c                   11.5691(9)
_cell_measurement_reflns_used    1935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.44
_cell_measurement_theta_min      2.25
_cell_volume                     2185.0(3)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.10,BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.6
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'ω rotations with narrow frames'
_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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.1165
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20201
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
  within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0116P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                3521
_reflns_number_total             5285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8008553_si_001.cif
_cod_data_source_block           marta33s
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C14 H28 B Cl3 F4 N2 P Ru0.50'
_cod_database_code               4068452
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ru1 Ru 0.5000 0.0000 0.5000 0.01487(10) Uani 1 2 d S
Cl1 Cl 0.86929(10) 0.18825(6) 0.30087(9) 0.0333(3) Uani 1 1 d .
Cl2 Cl 0.79720(10) 0.06025(6) 0.14587(9) 0.0371(3) Uani 1 1 d .
Cl3 Cl 0.84923(11) 0.20085(6) 0.04814(9) 0.0404(3) Uani 1 1 d .
P1 P 0.67813(8) 0.01576(5) 0.68289(8) 0.0165(2) Uani 1 1 d .
F1 F 0.50617(19) 0.15627(11) 0.15493(18) 0.0294(5) Uani 1 1 d .
F2 F 0.3506(2) 0.24300(12) 0.12882(19) 0.0388(6) Uani 1 1 d .
F3 F 0.3618(2) 0.17172(12) -0.02930(18) 0.0324(6) Uani 1 1 d .
F4 F 0.5123(2) 0.25969(13) 0.04582(19) 0.0444(7) Uani 1 1 d .
N1 N 0.3813(3) 0.05108(15) 0.5792(2) 0.0165(7) Uani 1 1 d .
N2 N 0.5409(3) 0.10105(16) 0.4464(2) 0.0166(7) Uani 1 1 d .
C1 C 0.3160(3) 0.08118(19) 0.6237(3) 0.0192(8) Uani 1 1 d .
C2 C 0.2316(3) 0.1184(2) 0.6817(3) 0.0267(9) Uani 1 1 d .
H2A H 0.1719 0.0822 0.6980 0.040 Uiso 1 1 calc R
H2B H 0.1839 0.1575 0.6283 0.040 Uiso 1 1 calc R
H2C H 0.2821 0.1407 0.7579 0.040 Uiso 1 1 calc R
C3 C 0.5606(3) 0.1609(2) 0.4242(3) 0.0187(8) Uani 1 1 d .
C4 C 0.5842(4) 0.23778(19) 0.3995(3) 0.0248(9) Uani 1 1 d .
H4A H 0.5133 0.2564 0.3331 0.037 Uiso 1 1 calc R
H4B H 0.6633 0.2411 0.3768 0.037 Uiso 1 1 calc R
H4C H 0.5919 0.2678 0.4720 0.037 Uiso 1 1 calc R
C5 C 0.6415(3) 0.06889(19) 0.8060(3) 0.0187(8) Uani 1 1 d .
H5 H 0.7234 0.0722 0.8725 0.022 Uiso 1 1 calc R
C6 C 0.6020(3) 0.14904(18) 0.7700(3) 0.0221(9) Uani 1 1 d .
H6A H 0.5322 0.1493 0.6945 0.033 Uiso 1 1 calc R
H6B H 0.6748 0.1764 0.7584 0.033 Uiso 1 1 calc R
H6C H 0.5737 0.1729 0.8339 0.033 Uiso 1 1 calc R
C7 C 0.5484(3) 0.02706(19) 0.8596(3) 0.0238(9) Uani 1 1 d .
H7A H 0.5142 0.0614 0.9081 0.036 Uiso 1 1 calc R
H7B H 0.5933 -0.0137 0.9109 0.036 Uiso 1 1 calc R
H7C H 0.4784 0.0068 0.7940 0.036 Uiso 1 1 calc R
C8 C 0.7366(3) -0.07357(19) 0.7580(3) 0.0186(8) Uani 1 1 d .
H8 H 0.6597 -0.0978 0.7710 0.022 Uiso 1 1 calc R
C9 C 0.8339(3) -0.0704(2) 0.8846(3) 0.0271(9) Uani 1 1 d .
H9A H 0.8408 -0.1196 0.9224 0.041 Uiso 1 1 calc R
H9B H 0.8055 -0.0342 0.9345 0.041 Uiso 1 1 calc R
H9C H 0.9172 -0.0555 0.8772 0.041 Uiso 1 1 calc R
C10 C 0.7844(4) -0.12876(19) 0.6804(3) 0.0267(9) Uani 1 1 d .
H10A H 0.8601 -0.1084 0.6632 0.040 Uiso 1 1 calc R
H10B H 0.7176 -0.1373 0.6043 0.040 Uiso 1 1 calc R
H10C H 0.8062 -0.1759 0.7239 0.040 Uiso 1 1 calc R
C11 C 0.8102(3) 0.07239(19) 0.6583(3) 0.0177(8) Uani 1 1 d .
H11 H 0.7729 0.1229 0.6356 0.021 Uiso 1 1 calc R
C12 C 0.9231(3) 0.0849(2) 0.7707(3) 0.0254(9) Uani 1 1 d .
H12A H 0.9697 0.0381 0.7935 0.038 Uiso 1 1 calc R
H12B H 0.8920 0.1020 0.8374 0.038 Uiso 1 1 calc R
H12C H 0.9800 0.1225 0.7533 0.038 Uiso 1 1 calc R
C13 C 0.8595(4) 0.0485(2) 0.5538(3) 0.0277(10) Uani 1 1 d .
H13A H 0.9214 0.0851 0.5429 0.042 Uiso 1 1 calc R
H13B H 0.7882 0.0454 0.4796 0.042 Uiso 1 1 calc R
H13C H 0.9004 -0.0003 0.5715 0.042 Uiso 1 1 calc R
C14 C 0.7876(4) 0.1576(2) 0.1554(3) 0.0273(9) Uani 1 1 d .
H14 H 0.6959 0.1718 0.1380 0.033 Uiso 1 1 calc R
B1 B 0.4321(4) 0.2075(3) 0.0746(4) 0.0251(10) Uani 1 1 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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N2 Ru1 N2 180.00(7) 3_656 .
N2 Ru1 N1 87.74(11) 3_656 3_656
N2 Ru1 N1 92.26(11) . 3_656
N2 Ru1 N1 92.26(11) 3_656 .
N2 Ru1 N1 87.74(11) . .
N1 Ru1 N1 180.0 3_656 .
N2 Ru1 P1 88.16(8) 3_656 3_656
N2 Ru1 P1 91.84(8) . 3_656
N1 Ru1 P1 90.79(8) 3_656 3_656
N1 Ru1 P1 89.21(8) . 3_656
N2 Ru1 P1 91.84(8) 3_656 .
N2 Ru1 P1 88.16(8) . .
N1 Ru1 P1 89.21(8) 3_656 .
N1 Ru1 P1 90.79(8) . .
P1 Ru1 P1 180.00(3) 3_656 .
C8 P1 C5 102.10(15) . .
C8 P1 C11 111.56(16) . .
C5 P1 C11 100.86(16) . .
C8 P1 Ru1 112.77(11) . .
C5 P1 Ru1 115.28(12) . .
C11 P1 Ru1 113.22(11) . .
C1 N1 Ru1 178.5(3) . .
C3 N2 Ru1 173.9(3) . .
N1 C1 C2 178.9(4) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N2 C3 C4 178.0(4) . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C6 C5 C7 113.8(3) . .
C6 C5 P1 112.6(2) . .
C7 C5 P1 112.1(2) . .
C6 C5 H5 105.9 . .
C7 C5 H5 105.9 . .
P1 C5 H5 105.9 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C10 C8 C9 108.7(3) . .
C10 C8 P1 114.8(2) . .
C9 C8 P1 117.6(2) . .
C10 C8 H8 104.8 . .
C9 C8 H8 104.8 . .
P1 C8 H8 104.8 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C13 C11 C12 109.3(3) . .
C13 C11 P1 116.1(2) . .
C12 C11 P1 115.2(2) . .
C13 C11 H11 105.0 . .
C12 C11 H11 105.0 . .
P1 C11 H11 105.0 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
Cl1 C14 Cl3 110.2(2) . .
Cl1 C14 Cl2 110.5(2) . .
Cl3 C14 Cl2 110.7(2) . .
Cl1 C14 H14 108.5 . .
Cl3 C14 H14 108.5 . .
Cl2 C14 H14 108.5 . .
F3 B1 F2 109.7(3) . .
F3 B1 F1 110.1(3) . .
F2 B1 F1 109.4(3) . .
F3 B1 F4 109.7(3) . .
F2 B1 F4 109.5(4) . .
F1 B1 F4 108.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N2 2.013(3) 3_656
Ru1 N2 2.013(3) .
Ru1 N1 2.019(3) 3_656
Ru1 N1 2.019(3) .
Ru1 P1 2.4440(9) 3_656
Ru1 P1 2.4440(9) .
Cl1 C14 1.750(4) .
Cl2 C14 1.759(4) .
Cl3 C14 1.758(4) .
P1 C8 1.850(3) .
P1 C5 1.854(3) .
P1 C11 1.860(3) .
F1 B1 1.390(4) .
F2 B1 1.389(5) .
F3 B1 1.384(5) .
F4 B1 1.393(5) .
N1 C1 1.134(4) .
N2 C3 1.141(4) .
C1 C2 1.456(5) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.450(5) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C6 1.528(4) .
C5 C7 1.537(4) .
C5 H5 1.0000 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C10 1.530(4) .
C8 C9 1.542(4) .
C8 H8 1.0000 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C13 1.523(4) .
C11 C12 1.529(4) .
C11 H11 1.0000 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14 1.0000 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168332079
