#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/92/7029204.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_7029204
loop_
_publ_author_name
'Metherell, Alexander J.'
'Cullen, William'
'Stephenson, Andrew'
'Hunter, Christopher A.'
'Ward, Michael D.'
_publ_section_title
;
 Fac and mer isomers of Ru(II) tris(pyrazolyl-pyridine) complexes as
 models for the vertices of coordination cages: structural
 characterisation and hydrogen-bonding characteristics.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              71
_journal_page_last               84
_journal_paper_doi               10.1039/c3dt52479e
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C27 H27 N9 Ru, 2(F6 P)'
_chemical_formula_sum            'C27 H27 F12 N9 P2 Ru'
_chemical_formula_weight         868.59
_space_group_IT_number           158
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2"c'
_symmetry_space_group_name_H-M   'P 3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.3032(3)
_cell_length_b                   10.3032(3)
_cell_length_c                   17.0022(5)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.28
_cell_volume                     1563.08(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0117
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26517
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.8822
_exptl_absorpt_correction_T_min  0.8416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.962
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2421
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0965P)²+1.6743P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                2305
_reflns_number_total             2421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52479e.txt
_cod_data_source_block           imw1774p3c1try2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P3c1 '
_cod_database_code               7029204
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, 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 0.6667 0.3333 0.41845(4) 0.01714(16) Uani 1 3 d S
N11 N 0.8624(5) 0.4305(4) 0.4854(3) 0.0196(9) Uani 1 1 d .
C12 C 0.4243(4) 0.3878(5) 0.4672(2) 0.0215(7) Uani 1 1 d .
C13 C 0.3411(4) 0.4296(4) 0.5141(2) 0.0246(7) Uani 1 1 d .
H13 H 0.2396 0.3983 0.5020 0.030 Uiso 1 1 calc R
C14 C 0.4106(5) 0.5181(5) 0.5790(2) 0.0281(7) Uani 1 1 d .
H14 H 0.3540 0.5425 0.6140 0.034 Uiso 1 1 calc R
C15 C 1.0110(4) 0.4392(5) 0.5942(2) 0.0271(8) Uani 1 1 d .
H15 H 1.0285 0.3904 0.6369 0.033 Uiso 1 1 calc R
C16 C 0.8892(4) 0.3625(4) 0.5458(2) 0.0245(7) Uani 1 1 d .
H16 H 0.8223 0.2590 0.5551 0.029 Uiso 1 1 calc R
N21 N 0.4627(5) 0.2574(5) 0.3624(2) 0.0207(6) Uani 1 1 d .
N22 N 0.3865(5) 0.1763(4) 0.2988(3) 0.0281(8) Uani 1 1 d .
C23 C 0.2441(5) 0.1590(5) 0.2942(2) 0.0290(8) Uani 1 1 d .
H23 H 0.1697 0.1055 0.2555 0.035 Uiso 1 1 calc R
C24 C 0.2336(4) 0.2356(5) 0.3575(2) 0.0259(7) Uani 1 1 d .
H24 H 0.1501 0.2464 0.3711 0.031 Uiso 1 1 calc R
C25 C 0.3685(4) 0.2943(4) 0.3979(2) 0.0216(7) Uani 1 1 d .
C31 C 0.4488(5) 0.1079(5) 0.2478(2) 0.0299(8) Uani 1 1 d .
H31A H 0.5402 0.1865 0.2227 0.045 Uiso 1 1 calc R
H31B H 0.3754 0.0485 0.2072 0.045 Uiso 1 1 calc R
H31C H 0.4728 0.0427 0.2790 0.045 Uiso 1 1 calc R
P1 P 1.0000 0.0000 0.57284(17) 0.0300(5) Uani 1 3 d S
F1 F 0.8635(4) -0.0233(5) 0.62888(18) 0.0534(8) Uani 1 1 d .
F2 F 0.9790(4) 0.1153(3) 0.51959(16) 0.0421(7) Uani 1 1 d .
P2 P 0.3333 0.6667 0.80402(14) 0.0251(5) Uani 1 3 d S
F3 F 0.4676(3) 0.6830(4) 0.74874(15) 0.0372(6) Uani 1 1 d .
F4 F 0.4519(3) 0.8006(3) 0.85791(14) 0.0348(6) 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'
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'
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
N21 Ru1 N21 100.54(13) 2_655 3_665
N21 Ru1 N21 100.54(13) 2_655 .
N21 Ru1 N21 100.54(13) 3_665 .
N21 Ru1 N11 88.51(13) 2_655 .
N21 Ru1 N11 77.97(15) 3_665 .
N21 Ru1 N11 170.94(14) . .
N21 Ru1 N11 77.97(15) 2_655 3_665
N21 Ru1 N11 170.94(14) 3_665 3_665
N21 Ru1 N11 88.51(13) . 3_665
N11 Ru1 N11 93.03(16) . 3_665
N21 Ru1 N11 170.94(14) 2_655 2_655
N21 Ru1 N11 88.50(13) 3_665 2_655
N21 Ru1 N11 77.97(15) . 2_655
N11 Ru1 N11 93.03(16) . 2_655
N11 Ru1 N11 93.03(16) 3_665 2_655
C16 N11 C12 120.0(4) . 3_665
C16 N11 Ru1 124.6(3) . .
C12 N11 Ru1 115.3(3) 3_665 .
N11 C12 C13 120.7(4) 2_655 .
N11 C12 C25 114.3(4) 2_655 .
C13 C12 C25 125.0(3) . .
C14 C13 C12 117.9(4) . .
C14 C13 H13 121.1 . .
C12 C13 H13 121.1 . .
C13 C14 C15 121.3(4) . 2_655
C13 C14 H14 119.3 . .
C15 C14 H14 119.3 2_655 .
C16 C15 C14 118.1(4) . 3_665
C16 C15 H15 120.9 . .
C14 C15 H15 120.9 3_665 .
N11 C16 C15 121.6(4) . .
N11 C16 H16 119.2 . .
C15 C16 H16 119.2 . .
C25 N21 N22 104.7(4) . .
C25 N21 Ru1 115.2(3) . .
N22 N21 Ru1 140.1(3) . .
N21 N22 C23 111.9(4) . .
N21 N22 C31 121.1(4) . .
C23 N22 C31 126.8(4) . .
C24 C23 N22 105.4(4) . .
C24 C23 H23 127.3 . .
N22 C23 H23 127.3 . .
C23 C24 C25 106.9(4) . .
C23 C24 H24 126.6 . .
C25 C24 H24 126.6 . .
N21 C25 C24 111.1(3) . .
N21 C25 C12 116.7(3) . .
C24 C25 C12 132.2(4) . .
N22 C31 H31A 109.5 . .
N22 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
N22 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
F2 P1 F2 90.85(18) 2_645 3_765
F2 P1 F2 90.85(18) 2_645 .
F2 P1 F2 90.86(19) 3_765 .
F2 P1 F1 178.3(2) 2_645 3_765
F2 P1 F1 90.77(18) 3_765 3_765
F2 P1 F1 89.67(16) . 3_765
F2 P1 F1 90.77(18) 2_645 2_645
F2 P1 F1 89.67(16) 3_765 2_645
F2 P1 F1 178.3(2) . 2_645
F1 P1 F1 88.7(2) 3_765 2_645
F2 P1 F1 89.66(16) 2_645 .
F2 P1 F1 178.3(2) 3_765 .
F2 P1 F1 90.77(18) . .
F1 P1 F1 88.7(2) 3_765 .
F1 P1 F1 88.7(2) 2_645 .
F4 P2 F4 90.36(16) 2_665 .
F4 P2 F4 90.36(16) 2_665 3_565
F4 P2 F4 90.36(16) . 3_565
F4 P2 F3 89.91(14) 2_665 2_665
F4 P2 F3 90.36(14) . 2_665
F4 P2 F3 179.2(2) 3_565 2_665
F4 P2 F3 179.2(2) 2_665 .
F4 P2 F3 89.90(14) . .
F4 P2 F3 90.35(14) 3_565 .
F3 P2 F3 89.37(16) 2_665 .
F4 P2 F3 90.36(14) 2_665 3_565
F4 P2 F3 179.2(2) . 3_565
F4 P2 F3 89.90(14) 3_565 3_565
F3 P2 F3 89.38(16) 2_665 3_565
F3 P2 F3 89.37(16) . 3_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N21 2.071(4) 2_655
Ru1 N21 2.071(4) 3_665
Ru1 N21 2.071(4) .
Ru1 N11 2.085(4) .
Ru1 N11 2.085(4) 3_665
Ru1 N11 2.085(4) 2_655
N11 C16 1.347(5) .
N11 C12 1.364(5) 3_665
C12 N11 1.364(5) 2_655
C12 C13 1.388(5) .
C12 C25 1.446(5) .
C13 C14 1.382(6) .
C13 H13 0.9500 .
C14 C15 1.382(6) 2_655
C14 H14 0.9500 .
C15 C16 1.373(5) .
C15 C14 1.382(6) 3_665
C15 H15 0.9500 .
C16 H16 0.9500 .
N21 C25 1.349(6) .
N21 N22 1.353(5) .
N22 C23 1.389(6) .
N22 C31 1.453(5) .
C23 C24 1.370(6) .
C23 H23 0.9500 .
C24 C25 1.388(5) .
C24 H24 0.9500 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
P1 F2 1.592(3) 2_645
P1 F2 1.592(3) 3_765
P1 F2 1.592(3) .
P1 F1 1.614(4) 3_765
P1 F1 1.614(4) 2_645
P1 F1 1.614(4) .
P2 F4 1.597(3) 2_665
P2 F4 1.597(3) .
P2 F4 1.597(3) 3_565
P2 F3 1.611(3) 2_665
P2 F3 1.611(3) .
P2 F3 1.611(3) 3_565
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N21 Ru1 N11 C16 -75.5(3) 2_655 .
N21 Ru1 N11 C16 -176.6(3) 3_665 .
N21 Ru1 N11 C16 102.0(10) . .
N11 Ru1 N11 C16 2.4(4) 3_665 .
N11 Ru1 N11 C16 95.6(3) 2_655 .
N21 Ru1 N11 C12 108.1(3) 2_655 3_665
N21 Ru1 N11 C12 7.0(3) 3_665 3_665
N21 Ru1 N11 C12 -74.5(13) . 3_665
N11 Ru1 N11 C12 -174.0(3) 3_665 3_665
N11 Ru1 N11 C12 -80.8(4) 2_655 3_665
N11 C12 C13 C14 0.6(6) 2_655 .
C25 C12 C13 C14 179.2(4) . .
C12 C13 C14 C15 4.2(6) . 2_655
C12 N11 C16 C15 5.3(6) 3_665 .
Ru1 N11 C16 C15 -171.0(3) . .
C14 C15 C16 N11 -0.5(6) 3_665 .
N21 Ru1 N21 C25 165.5(3) 2_655 .
N21 Ru1 N21 C25 -91.6(4) 3_665 .
N11 Ru1 N21 C25 -11.9(13) . .
N11 Ru1 N21 C25 88.0(3) 3_665 .
N11 Ru1 N21 C25 -5.4(3) 2_655 .
N21 Ru1 N21 N22 -13.2(5) 2_655 .
N21 Ru1 N21 N22 89.7(4) 3_665 .
N11 Ru1 N21 N22 169.4(8) . .
N11 Ru1 N21 N22 -90.7(5) 3_665 .
N11 Ru1 N21 N22 175.9(5) 2_655 .
C25 N21 N22 C23 -1.1(5) . .
Ru1 N21 N22 C23 177.7(4) . .
C25 N21 N22 C31 -176.1(4) . .
Ru1 N21 N22 C31 2.6(7) . .
N21 N22 C23 C24 1.1(5) . .
C31 N22 C23 C24 175.8(4) . .
N22 C23 C24 C25 -0.6(5) . .
N22 N21 C25 C24 0.7(5) . .
Ru1 N21 C25 C24 -178.4(3) . .
N22 N21 C25 C12 -177.6(3) . .
Ru1 N21 C25 C12 3.2(4) . .
C23 C24 C25 N21 -0.1(5) . .
C23 C24 C25 C12 177.9(4) . .
N11 C12 C25 N21 2.7(4) 2_655 .
C13 C12 C25 N21 -175.9(4) . .
N11 C12 C25 C24 -175.1(4) 2_655 .
C13 C12 C25 C24 6.3(6) . .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139163547
