#------------------------------------------------------------------------------
#$Date: 2025-08-20 15:37:07 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301831 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/40/4084082.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_4084082
loop_
_publ_author_name
'Barlow, Stephen'
'Cowley, Andrew'
'Green, Jennifer C.'
'Brunker, Tim J.'
'Hascall, Tony'
_publ_section_title
;
 The Ruthenocenylmethylium Cation:  Isolation and Structures
 of\h5-Cyclopentadienyl-\h6-fulvene-ruthenium(II) Salts
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5351
_journal_paper_doi               10.1021/om010667+
_journal_volume                  20
_journal_year                    2001
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C29 H26 B1 F4 P1 Ru1'
_chemical_formula_structural     'C29 H26 P1 RU B F4'
_chemical_formula_sum            'C29.5 H27 B Cl F4 P Ru'
_chemical_formula_weight         635.81
_chemical_name_systematic
;
(ruthenocenylmethyl)triphenylphosphonium tetrafluoroborate 
dichloromethane solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-07-04T16:41:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.5910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.0591(7)
_cell_length_b                   12.5182(3)
_cell_length_c                   13.7757(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     5584.7(2)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines  (Farrugia, 1999)''
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0995
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10107
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.759
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.689
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.00073(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         6308
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0986P)²+7.1400P] where  P=(Fo²+2Fc²)/3''
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.1854
_reflns_number_gt                4083
_reflns_number_total             6308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010667%2B.cif
_cod_data_source_block           RcCH2PPh3BF4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C29.50 H27 B Cl F4 P Ru'
_cod_database_code               4084082
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Ru Ru 0.259724(13) 0.59577(3) 0.14793(3) 0.02032(18) Uani 1 1 d .
P P 0.39089(4) 0.70752(12) 0.34884(10) 0.0231(3) Uani 1 1 d .
C1 C 0.21117(18) 0.5062(5) 0.0544(4) 0.0321(14) Uani 1 1 d .
H1 H 0.1867 0.4841 0.0751 0.038 Uiso 1 1 calc R
C2 C 0.24838(19) 0.4462(5) 0.0667(4) 0.0296(13) Uani 1 1 d .
H2 H 0.2532 0.3777 0.0964 0.036 Uiso 1 1 calc R
C3 C 0.27720(18) 0.5086(4) 0.0260(4) 0.0274(13) Uani 1 1 d .
H3 H 0.3048 0.4889 0.0244 0.033 Uiso 1 1 calc R
C4 C 0.25754(19) 0.6045(4) -0.0113(4) 0.0292(13) Uani 1 1 d .
H4 H 0.2695 0.6601 -0.043 0.035 Uiso 1 1 calc R
C5 C 0.21623(19) 0.6032(5) 0.0068(4) 0.0307(13) Uani 1 1 d .
H5 H 0.1961 0.6577 -0.0102 0.037 Uiso 1 1 calc R
C6 C 0.28756(17) 0.7357(5) 0.2268(4) 0.0263(12) Uani 1 1 d .
H6 H 0.2964 0.7967 0.1957 0.032 Uiso 1 1 calc R
C7 C 0.24743(18) 0.7197(5) 0.2486(4) 0.0297(13) Uani 1 1 d .
H7 H 0.2248 0.7679 0.2342 0.036 Uiso 1 1 calc R
C8 C 0.24753(19) 0.6186(5) 0.2958(4) 0.0332(15) Uani 1 1 d .
H8 H 0.2248 0.5875 0.3179 0.04 Uiso 1 1 calc R
C9 C 0.28759(18) 0.5714(5) 0.3045(4) 0.0283(13) Uani 1 1 d .
H9 H 0.2963 0.5046 0.3342 0.034 Uiso 1 1 calc R
C10 C 0.31194(16) 0.6442(5) 0.2599(4) 0.0237(12) Uani 1 1 d .
C11 C 0.35702(17) 0.6263(5) 0.2577(4) 0.0333(14) Uani 1 1 d .
H11A H 0.3618 0.6437 0.1908 0.04 Uiso 1 1 calc R
H11B H 0.3638 0.5499 0.2707 0.04 Uiso 1 1 calc R
C12 C 0.44325(16) 0.6625(5) 0.3600(4) 0.0258(12) Uani 1 1 d .
C13 C 0.45145(18) 0.5531(5) 0.3618(4) 0.0311(13) Uani 1 1 d .
H13 H 0.4296 0.5026 0.3547 0.037 Uiso 1 1 calc R
C14 C 0.4923(2) 0.5192(6) 0.3742(5) 0.0418(16) Uani 1 1 d .
H14 H 0.4983 0.4449 0.3751 0.05 Uiso 1 1 calc R
C15 C 0.52423(19) 0.5922(6) 0.3852(5) 0.0411(17) Uani 1 1 d .
H15 H 0.5519 0.5679 0.3933 0.049 Uiso 1 1 calc R
C16 C 0.51605(19) 0.6997(7) 0.3843(5) 0.0465(18) Uani 1 1 d .
H16 H 0.5382 0.7493 0.393 0.056 Uiso 1 1 calc R
C17 C 0.47512(18) 0.7374(6) 0.3707(5) 0.0380(15) Uani 1 1 d .
H17 H 0.4694 0.8118 0.3689 0.046 Uiso 1 1 calc R
C18 C 0.37653(16) 0.6989(4) 0.4681(4) 0.0228(12) Uani 1 1 d .
C19 C 0.40222(19) 0.6524(5) 0.5470(4) 0.0349(15) Uani 1 1 d .
H19 H 0.4279 0.6234 0.5392 0.042 Uiso 1 1 calc R
C20 C 0.3908(2) 0.6476(5) 0.6384(5) 0.0396(15) Uani 1 1 d .
H20 H 0.4088 0.6153 0.693 0.048 Uiso 1 1 calc R
C21 C 0.3537(2) 0.6891(5) 0.6504(4) 0.0384(16) Uani 1 1 d .
H21 H 0.3457 0.6838 0.7127 0.046 Uiso 1 1 calc R
C22 C 0.32803(19) 0.7389(5) 0.5714(4) 0.0316(14) Uani 1 1 d .
H22 H 0.3028 0.77 0.5803 0.038 Uiso 1 1 calc R
C23 C 0.33895(18) 0.7433(5) 0.4800(4) 0.0272(12) Uani 1 1 d .
H23 H 0.3211 0.7763 0.4255 0.033 Uiso 1 1 calc R
C24 C 0.38760(18) 0.8451(5) 0.3117(5) 0.0372(16) Uani 1 1 d .
C25 C 0.3814(3) 0.8716(9) 0.2135(6) 0.081(3) Uani 1 1 d .
H25 H 0.3786 0.8187 0.1632 0.097 Uiso 1 1 calc R
C26 C 0.3793(3) 0.9880(12) 0.1897(9) 0.109(5) Uani 1 1 d .
H26 H 0.3736 1.0125 0.123 0.131 Uiso 1 1 calc R
C27 C 0.3859(4) 1.0575(12) 0.2667(15) 0.129(6) Uani 1 1 d .
H27 H 0.3854 1.1317 0.252 0.155 Uiso 1 1 calc R
C28 C 0.3927(3) 1.0293(8) 0.3586(12) 0.103(4) Uani 1 1 d .
H28 H 0.3974 1.0823 0.409 0.124 Uiso 1 1 calc R
C29 C 0.3931(3) 0.9252(6) 0.3835(7) 0.061(2) Uani 1 1 d .
H29 H 0.3973 0.9059 0.4515 0.074 Uiso 1 1 calc R
B B 0.3756(2) 0.3297(6) 0.4415(5) 0.0309(15) Uani 1 1 d .
F1 F 0.33945(16) 0.3042(6) 0.3873(4) 0.110(2) Uani 1 1 d .
F2 F 0.38107(18) 0.2953(10) 0.5309(4) 0.183(5) Uani 1 1 d .
F3 F 0.3751(2) 0.4369(6) 0.4543(9) 0.179(5) Uani 1 1 d .
F4 F 0.40904(14) 0.3102(4) 0.3995(3) 0.0754(15) Uani 1 1 d .
C101 C 0.498(2) 0.822(2) 0.642(2) 0.35(5) Uani 0.5 1 d PD
H10A H 0.5245 0.8005 0.6243 0.417 Uiso 0.5 1 calc PR
H10B H 0.4764 0.7806 0.598 0.417 Uiso 0.5 1 calc PR
Cl1 Cl 0.4910(4) 0.9424(13) 0.6038(12) 0.257(7) Uani 0.5 1 d PD
Cl2 Cl 0.5 0.7711(9) 0.75 0.298(6) Uani 1 2 d SD
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 0 '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'
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'
Ru Ru -1.2594 0.8363 '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'
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
C10 Ru C1 164.6(2) .
C10 Ru C6 38.4(2) .
C1 Ru C6 155.4(2) .
C10 Ru C7 64.4(2) .
C1 Ru C7 122.7(2) .
C6 Ru C7 38.5(2) .
C10 Ru C8 64.2(2) .
C1 Ru C8 111.8(2) .
C6 Ru C8 64.1(2) .
C7 Ru C8 38.2(2) .
C10 Ru C2 129.8(2) .
C1 Ru C2 38.3(2) .
C6 Ru C2 165.0(2) .
C7 Ru C2 155.2(2) .
C8 Ru C2 123.4(2) .
C10 Ru C5 156.5(2) .
C1 Ru C5 37.8(2) .
C6 Ru C5 123.5(2) .
C7 Ru C5 111.4(2) .
C8 Ru C5 128.2(2) .
C2 Ru C5 64.0(2) .
C10 Ru C3 113.2(2) .
C1 Ru C3 63.9(2) .
C6 Ru C3 129.8(2) .
C7 Ru C3 164.4(2) .
C8 Ru C3 156.5(2) .
C2 Ru C3 38.4(2) .
C5 Ru C3 64.0(2) .
C10 Ru C4 124.4(2) .
C1 Ru C4 63.6(2) .
C6 Ru C4 112.9(2) .
C7 Ru C4 129.3(2) .
C8 Ru C4 163.8(2) .
C2 Ru C4 63.8(2) .
C5 Ru C4 38.5(2) .
C3 Ru C4 37.8(2) .
C10 Ru C9 38.5(2) .
C1 Ru C9 129.1(2) .
C6 Ru C9 64.3(2) .
C7 Ru C9 64.3(2) .
C8 Ru C9 38.4(2) .
C2 Ru C9 112.5(2) .
C5 Ru C9 163.3(2) .
C3 Ru C9 124.5(2) .
C4 Ru C9 156.8(2) .
C24 P C12 109.1(3) .
C24 P C18 107.8(3) .
C12 P C18 109.2(3) .
C24 P C11 110.3(3) .
C12 P C11 109.4(3) .
C18 P C11 111.0(3) .
C5 C1 C2 109.3(5) .
C5 C1 Ru 71.7(3) .
C2 C1 Ru 71.4(3) .
C1 C2 C3 107.1(5) .
C1 C2 Ru 70.3(3) .
C3 C2 Ru 70.9(3) .
C4 C3 C2 108.2(5) .
C4 C3 Ru 71.4(3) .
C2 C3 Ru 70.7(3) .
C3 C4 C5 108.1(5) .
C3 C4 Ru 70.8(3) .
C5 C4 Ru 70.5(3) .
C1 C5 C4 107.3(5) .
C1 C5 Ru 70.5(3) .
C4 C5 Ru 71.1(3) .
C10 C6 C7 108.0(5) .
C10 C6 Ru 70.5(3) .
C7 C6 Ru 71.0(3) .
C8 C7 C6 107.6(5) .
C8 C7 Ru 70.9(3) .
C6 C7 Ru 70.5(3) .
C7 C8 C9 108.8(5) .
C7 C8 Ru 70.9(3) .
C9 C8 Ru 71.4(3) .
C10 C9 C8 107.0(5) .
C10 C9 Ru 69.6(3) .
C8 C9 Ru 70.2(3) .
C6 C10 C9 108.6(5) .
C6 C10 C11 127.6(5) .
C9 C10 C11 123.7(5) .
C6 C10 Ru 71.1(3) .
C9 C10 Ru 72.0(3) .
C11 C10 Ru 126.4(3) .
C10 C11 P 112.1(4) .
C13 C12 C17 121.2(5) .
C13 C12 P 119.3(4) .
C17 C12 P 119.5(5) .
C14 C13 C12 118.7(6) .
C15 C14 C13 120.9(7) .
C16 C15 C14 120.2(6) .
C15 C16 C17 120.8(6) .
C12 C17 C16 118.2(6) .
C19 C18 C23 120.0(5) .
C19 C18 P 121.0(4) .
C23 C18 P 119.0(4) .
C18 C19 C20 120.1(6) .
C21 C20 C19 120.4(6) .
C20 C21 C22 119.8(5) .
C23 C22 C21 120.2(6) .
C22 C23 C18 119.5(5) .
C25 C24 C29 120.0(8) .
C25 C24 P 120.3(7) .
C29 C24 P 119.7(5) .
C24 C25 C26 116.5(10) .
C27 C26 C25 117.5(10) .
C28 C27 C26 124.1(13) .
C27 C28 C29 120.4(14) .
C28 C29 C24 121.4(10) .
F2 B F1 113.5(7) .
F2 B F3 102.2(9) .
F1 B F3 106.3(7) .
F2 B F4 112.1(7) .
F1 B F4 115.9(6) .
F3 B F4 105.3(6) .
Cl1 C101 Cl2 131(2) .
C101 Cl2 C101 133(3) 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru C10 2.158(5) .
Ru C1 2.160(6) .
Ru C6 2.166(5) .
Ru C7 2.173(5) .
Ru C8 2.173(5) .
Ru C2 2.174(6) .
Ru C5 2.175(6) .
Ru C3 2.176(5) .
Ru C4 2.183(5) .
Ru C9 2.190(5) .
P C24 1.794(7) .
P C12 1.798(5) .
P C18 1.802(5) .
P C11 1.817(6) .
C1 C5 1.406(8) .
C1 C2 1.421(8) .
C2 C3 1.430(8) .
C3 C4 1.412(8) .
C4 C5 1.437(8) .
C6 C10 1.422(8) .
C6 C7 1.432(8) .
C7 C8 1.422(9) .
C8 C9 1.433(8) .
C9 C10 1.433(8) .
C10 C11 1.514(7) .
C12 C13 1.396(9) .
C12 C17 1.396(8) .
C13 C14 1.393(8) .
C14 C15 1.381(10) .
C15 C16 1.372(10) .
C16 C17 1.410(8) .
C18 C19 1.368(8) .
C18 C23 1.400(7) .
C19 C20 1.385(8) .
C20 C21 1.372(9) .
C21 C22 1.387(9) .
C22 C23 1.379(7) .
C24 C25 1.367(10) .
C24 C29 1.395(11) .
C25 C26 1.492(16) .
C26 C27 1.355(19) .
C27 C28 1.290(18) .
C28 C29 1.348(11) .
B F2 1.283(8) .
B F1 1.315(8) .
B F3 1.353(10) .
B F4 1.368(8) .
C101 Cl1 1.599(19) .
C101 Cl2 1.605(19) .
Cl2 C101 1.605(19) 2_656
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139111262
