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#$Date: 2016-03-21 16:45:23 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178753 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/07/4100780.cif $
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#
# 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_4100780
loop_
_publ_author_name
'Chun-Yuen Wong'
'Chi-Ming Che'
'Michael C. W. Chan'
'King-Hung Leung'
'David Lee Phillips'
'Nianyong Zhu'
_publ_section_title
;
Probing the Ruthenium-Cumulene Bonding Interaction: Synthesis and
Spectroscopic Studies of Vinylidene- and Allenylidene-Ruthenium
Complexes Supported by Tetradentate Macrocyclic Tertiary Amine and
Comparisons with Diphosphine Analogues of Ruthenium and Osmium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2501
_journal_page_last               2514
_journal_paper_doi               10.1021/ja0380648
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C33 H50 Cl F6 N4 P Ru'
_chemical_formula_sum            'C33 H50 Cl F6 N4 P Ru'
_chemical_formula_weight         784.26
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 133.14(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.517(3)
_cell_length_b                   31.896(6)
_cell_length_c                   10.380(2)
_cell_measurement_temperature    301(2)
_cell_volume                     3507.1(12)
_diffrn_ambient_temperature      301(2)
_exptl_crystal_density_diffrn    1.485
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4100780
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.0000 0.339790(15) 0.2500 0.0326(2) Uani 1 2 d S . .
Cl1 Cl 0.0000 0.26301(5) 0.2500 0.0466(5) Uani 1 2 d S . .
N1 N 0.1084(4) 0.33774(12) 0.5406(5) 0.0504(11) Uani 1 1 d D . .
N2 N 0.1825(4) 0.33872(12) 0.3111(6) 0.0503(11) Uani 1 1 d D . .
C1 C 0.0000 0.3982(2) 0.2500 0.0441(17) Uani 1 2 d S . .
C2 C 0.0000 0.4370(2) 0.2500 0.0533(19) Uani 1 2 d S . .
C3 C 0.0000 0.4802(2) 0.2500 0.0524(19) Uani 1 2 d S . .
C4 C 0.1094(5) 0.50418(15) 0.3034(7) 0.0519(14) Uani 1 1 d . . .
C5 C 0.1524(6) 0.54055(16) 0.4019(7) 0.0623(16) Uani 1 1 d . . .
H5 H 0.1070 0.5520 0.4267 0.075 Uiso 1 1 calc R . .
C6 C 0.2603(6) 0.56014(19) 0.4641(8) 0.0718(18) Uani 1 1 d . . .
H6 H 0.2882 0.5840 0.5335 0.086 Uiso 1 1 calc R . .
C7 C 0.3280(5) 0.54505(19) 0.4257(9) 0.0717(18) Uani 1 1 d . . .
C8 C 0.2813(6) 0.5102(2) 0.3184(10) 0.086(2) Uani 1 1 d . . .
H8 H 0.3217 0.5005 0.2835 0.104 Uiso 1 1 calc R . .
C9 C 0.1747(6) 0.48945(18) 0.2615(9) 0.0762(18) Uani 1 1 d . . .
H9 H 0.1474 0.4652 0.1941 0.091 Uiso 1 1 calc R . .
C10 C 0.4477(6) 0.5671(2) 0.4956(11) 0.109(3) Uani 1 1 d . . .
H10A H 0.4832 0.5522 0.4579 0.164 Uiso 1 1 calc R . .
H10B H 0.5076 0.5677 0.6223 0.164 Uiso 1 1 calc R . .
H10C H 0.4278 0.5952 0.4509 0.164 Uiso 1 1 calc R . .
C11 C 0.0384(10) 0.3611(4) 0.5780(15) 0.067(3) Uani 0.50 1 d PD . 1
H11A H 0.0133 0.3885 0.5225 0.080 Uiso 0.50 1 calc PR . 1
H11B H 0.0933 0.3651 0.7043 0.080 Uiso 0.50 1 calc PR . 1
C12 C 0.2302(8) 0.3622(4) 0.6450(15) 0.067(3) Uani 0.50 1 d PD . 1
H12A H 0.2681 0.3654 0.7657 0.080 Uiso 0.50 1 calc PR . 1
H12B H 0.2124 0.3899 0.5941 0.080 Uiso 0.50 1 calc PR . 1
C13 C 0.3257(6) 0.3388(2) 0.6439(8) 0.093(2) Uani 1 1 d D . .
H13C H 0.3875 0.3181 0.6759 0.112 Uiso 0.50 1 calc PR . 2
H13D H 0.3707 0.3589 0.7400 0.112 Uiso 0.50 1 calc PR . 2
H13A H 0.3876 0.3594 0.6760 0.112 Uiso 0.50 1 d PR . 1
H13B H 0.3704 0.3184 0.7390 0.112 Uiso 0.50 1 d PR . 1
C14 C 0.2821(7) 0.3156(2) 0.4795(10) 0.069(2) Uani 0.75 1 d PD . 1
H14A H 0.3544 0.3112 0.4928 0.083 Uiso 0.75 1 calc PR . 1
H14B H 0.2496 0.2882 0.4725 0.083 Uiso 0.75 1 calc PR . 1
C15 C 0.1670(8) 0.3122(3) 0.1768(11) 0.076(3) Uani 0.75 1 d PD . 1
H15A H 0.1282 0.2857 0.1624 0.091 Uiso 0.75 1 calc PR . 1
H15B H 0.2493 0.3064 0.2185 0.091 Uiso 0.75 1 calc PR . 1
C16 C 0.0838(7) 0.3352(3) -0.0035(10) 0.113(3) Uani 1 1 d D . .
H16C H 0.0613 0.3532 -0.0967 0.136 Uiso 0.50 1 calc PR . 2
H16D H 0.1383 0.3135 0.0141 0.136 Uiso 0.50 1 calc PR . 2
H16A H 0.0560 0.3142 -0.0917 0.136 Uiso 0.50 1 d PR . 1
H16B H 0.1384 0.3544 0.0024 0.136 Uiso 0.50 1 d PR . 1
C17 C 0.1431(13) 0.2963(3) 0.6276(16) 0.078(4) Uani 0.50 1 d PD . 1
H17A H 0.0688 0.2793 0.5648 0.116 Uiso 0.50 1 calc PR . 1
H17B H 0.1812 0.3000 0.7472 0.116 Uiso 0.50 1 calc PR . 1
H17C H 0.2020 0.2827 0.6273 0.116 Uiso 0.50 1 calc PR . 1
C18 C 0.2325(7) 0.3792(2) 0.3235(13) 0.082(3) Uani 0.75 1 d PD . 1
H18A H 0.2408 0.3963 0.4071 0.123 Uiso 0.75 1 calc PR . 1
H18B H 0.1761 0.3926 0.2099 0.123 Uiso 0.75 1 calc PR . 1
H18C H 0.3137 0.3758 0.3617 0.123 Uiso 0.75 1 calc PR . 1
C11' C 0.0396(12) 0.3130(4) 0.5782(17) 0.082(4) Uani 0.50 1 d PD . 2
H11C H 0.0947 0.3095 0.7048 0.098 Uiso 0.50 1 calc PR . 2
H11D H 0.0194 0.2854 0.5260 0.098 Uiso 0.50 1 calc PR . 2
C12' C 0.2316(9) 0.3152(4) 0.6464(15) 0.080(4) Uani 0.50 1 d PD . 2
H12C H 0.2166 0.2872 0.5992 0.096 Uiso 0.50 1 calc PR . 2
H12D H 0.2698 0.3126 0.7675 0.096 Uiso 0.50 1 calc PR . 2
C14' C 0.2845(15) 0.3634(5) 0.4777(14) 0.058(6) Uani 0.25 1 d PD . 2
H14C H 0.2528 0.3909 0.4702 0.070 Uiso 0.25 1 calc PR . 2
H14D H 0.3568 0.3670 0.4905 0.070 Uiso 0.25 1 calc PR . 2
C15' C 0.1680(17) 0.3625(5) 0.1711(16) 0.047(5) Uani 0.25 1 d PD . 2
H15C H 0.2502 0.3675 0.2115 0.057 Uiso 0.25 1 calc PR . 2
H15D H 0.1281 0.3894 0.1484 0.057 Uiso 0.25 1 calc PR . 2
C17' C 0.1333(10) 0.3794(3) 0.6155(15) 0.064(3) Uani 0.50 1 d PD . 2
H17D H 0.0556 0.3948 0.5469 0.096 Uiso 0.50 1 calc PR . 2
H17E H 0.1905 0.3939 0.6140 0.096 Uiso 0.50 1 calc PR . 2
H17F H 0.1702 0.3771 0.7350 0.096 Uiso 0.50 1 calc PR . 2
C18' C 0.2389(15) 0.2982(5) 0.3346(16) 0.049(5) Uani 0.25 1 d PD . 2
H18D H 0.1776 0.2809 0.2337 0.073 Uiso 0.25 1 calc PR . 2
H18E H 0.2662 0.2849 0.4388 0.073 Uiso 0.25 1 calc PR . 2
H18F H 0.3101 0.3023 0.3468 0.073 Uiso 0.25 1 calc PR . 2
P1 P 0.5000 0.30984(7) 0.2500 0.0603(6) Uani 1 2 d S . .
F1 F 0.6078(5) 0.34217(17) 0.3473(10) 0.167(3) Uani 1 1 d . . .
F2 F 0.5051(5) 0.3098(2) 0.4026(7) 0.168(3) Uani 1 1 d . . .
F3 F 0.3962(5) 0.27594(19) 0.1618(8) 0.165(2) Uani 1 1 d . . .
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 1.862(7) . ?
Ru1 N1 2.256(4) 2 ?
Ru1 N1 2.256(4) . ?
Ru1 N2 2.264(4) . ?
Ru1 N2 2.264(4) 2 ?
Ru1 Cl1 2.4490(17) . ?
N1 C17' 1.456(9) . ?
N1 C17 1.483(10) . ?
N1 C12' 1.496(10) . ?
N1 C11 1.509(9) . ?
N1 C12 1.513(9) . ?
N1 C11' 1.518(10) . ?
N2 C18 1.444(7) . ?
N2 C18' 1.457(13) . ?
N2 C14 1.495(7) . ?
N2 C15 1.511(8) . ?
N2 C14' 1.516(12) . ?
N2 C15' 1.521(12) . ?
C1 C2 1.239(10) . ?
C2 C3 1.378(10) . ?
C3 C4 1.486(6) . ?
C3 C4 1.486(6) 2 ?
C4 C9 1.369(8) . ?
C4 C5 1.381(7) . ?
C5 C6 1.370(8) . ?
C6 C7 1.376(9) . ?
C7 C8 1.378(9) . ?
C7 C10 1.521(8) . ?
C8 C9 1.390(8) . ?
C11 C16 1.596(13) 2 ?
C12 C13 1.582(10) . ?
C13 C14 1.544(9) . ?
C13 C12' 1.576(11) . ?
C13 C14' 1.593(12) . ?
C15 C16 1.551(9) . ?
C16 C11' 1.552(15) 2 ?
C16 C15' 1.585(12) . ?
C16 C11 1.596(13) 2 ?
C11' C16 1.552(15) 2 ?
P1 F2 1.534(5) 2_655 ?
P1 F2 1.534(5) . ?
P1 F1 1.540(4) . ?
P1 F1 1.540(4) 2_655 ?
P1 F3 1.546(5) . ?
P1 F3 1.546(5) 2_655 ?
