#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/09/4310912.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_4310912
loop_
_publ_author_name
'Christopher M. Kepert'
'Glen B. Deacon'
'Norma Sahely'
'Leone Spiccia'
'Gary D. Fallon'
'Brian W. Skelton'
'Allan H. White'
_publ_contact_author_address
;
   Department of Chemistry
   University of Western Australia
   Crawley  
   Western Australia 6009
   Australia
;
_publ_contact_author_email       bws@crystal.uwa.edu.au
_publ_contact_author_fax         (+61)_08_9380_1118
_publ_contact_author_name        'Skelton, B. W.'
_publ_contact_author_phone       (+61)_08-9380_3481
_publ_section_title
;
 Synthesis of Heteroleptic Bis(diimine)carbonylchlororuthenium(II)
 Complexes from Photodecarbonylated Precursors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2818
_journal_page_last               2827
_journal_paper_doi               10.1021/ic0351895
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C22 H18 Cl F6 N4 O3 P Ru'
_chemical_formula_weight         667.90
_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'
_cell_angle_alpha                90.00000
_cell_angle_beta                 94.48(4)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   8.612(5)
_cell_length_b                   13.314(8)
_cell_length_c                   22.727(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      12.1
_cell_volume                     2598(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXan
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  teXan
_computing_structure_solution    teXan
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device_type
;
   NICOLET diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_detector       'single counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .7107
_diffrn_reflns_av_R_equivalents  .035
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8062
_diffrn_reflns_theta_max         30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .838
_exptl_absorpt_correction_T_max  .747
_exptl_absorpt_correction_T_min  .698
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 Tompa analytical           
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          .46
_exptl_crystal_size_mid          .43
_exptl_crystal_size_min          .4
_refine_diff_density_max         .89
_refine_diff_density_min         -.74
_refine_ls_goodness_of_fit_ref   2.159
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     342
_refine_ls_number_reflns         4743
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           .0571
_refine_ls_shift/su_max          .0055
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         .0420
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                4743
_reflns_number_observed          4743
_reflns_number_total             7886
_reflns_threshold_expression     'I    > 2.00 sig(I   )'
_cod_data_source_file            ic0351895si20040210_044127_8.cif
_cod_data_source_block           bpydpk
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_formula_sum        'C22 H18 Cl1 F6 N4 O3 P1 Ru1'
_cod_database_code               4310912
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru .04888(5) .74312(3) .76131(2) .0292(2) Uani ? ? 1.00000 ? ?
Cl -.1917(2) .82440(10) .78002(6) .0455(8) Uani ? ? 1.00000 ? ?
C0 .1041(6) .8532(4) .7155(2) .040(3) Uani ? ? 1.00000 ? ?
O0 .1369(5) .9170(3) .6869(2) .063(3) Uani ? ? 1.00000 ? ?
O2 .0826(4) .4296(3) .7155(2) .049(2) Uani ? ? 1.00000 ? ?
N11 .1718(5) .7956(3) .8370(2) .032(2) Uani ? ? 1.00000 ? ?
C12 .3142(5) .7553(4) .8482(2) .034(3) Uani ? ? 1.00000 ? ?
C13 .4046(7) .7804(4) .9001(3) .053(4) Uani ? ? 1.00000 ? ?
C14 .3506(8) .8493(5) .9384(3) .060(4) Uani ? ? 1.00000 ? ?
C15 .2088(8) .8904(5) .9259(3) .056(4) Uani ? ? 1.00000 ? ?
C16 .1195(6) .8624(4) .8753(2) .044(4) Uani ? ? 1.00000 ? ?
N11' .2641(5) .6787(3) .7537(2) .032(2) Uani ? ? 1.00000 ? ?
C12' .3682(6) .6899(4) .8011(2) .035(3) Uani ? ? 1.00000 ? ?
C13' .5146(7) .6502(5) .8021(3) .052(4) Uani ? ? 1.00000 ? ?
C14' .5613(7) .5993(5) .7525(3) .063(4) Uani ? ? 1.00000 ? ?
C15' .4600(7) .5930(5) .7034(3) .055(4) Uani ? ? 1.00000 ? ?
C16' .3136(6) .6319(4) .7056(2) .041(3) Uani ? ? 1.00000 ? ?
N21 -.0185(4) .6179(3) .8139(2) .030(2) Uani ? ? 1.00000 ? ?
C22 -.0046(6) .5224(4) .7945(2) .031(3) Uani ? ? 1.00000 ? ?
C23 -.0204(7) .4399(4) .8305(2) .044(4) Uani ? ? 1.00000 ? ?
C24 -.0521(7) .4546(4) .8876(3) .052(4) Uani ? ? 1.00000 ? ?
C25 -.0712(7) .5521(5) .9074(2) .052(4) Uani ? ? 1.00000 ? ?
C26 -.0534(6) .6309(4) .8699(2) .039(3) Uani ? ? 1.00000 ? ?
C2 .0166(6) .5042(4) .7302(2) .033(3) Uani ? ? 1.00000 ? ?
N21' -.0680(5) .6703(3) .6894(2) .034(2) Uani ? ? 1.00000 ? ?
C22' -.0639(5) .5694(4) .6831(2) .031(3) Uani ? ? 1.00000 ? ?
C23' -.1389(6) .5210(4) .6351(2) .040(3) Uani ? ? 1.00000 ? ?
C24' -.2218(7) .5749(5) .5926(2) .051(4) Uani ? ? 1.00000 ? ?
C25' -.2287(7) .6767(5) .5984(2) .053(4) Uani ? ? 1.00000 ? ?
C26' -.1497(6) .7235(4) .6466(2) .045(3) Uani ? ? 1.00000 ? ?
O3 .4160(10) .5183(9) .9600(5) .154(4) Uiso ? ? 0.60000 ? ?
O4 .417(2) .5410(10) 1.0323(9) .165(7) Uiso ? ? 0.40000 ? ?
P1 .3093(2) .70330(10) .52098(8) .0591(10) Uani ? ? 1.00000 ? ?
F1 .3332(7) .7546(5) .5825(2) .158(5) Uani ? ? 1.00000 ? ?
F2 .4584(5) .7652(3) .5034(2) .100(3) Uani ? ? 1.00000 ? ?
F3 .2893(7) .6585(5) .4584(2) .169(5) Uani ? ? 1.00000 ? ?
F4 .1678(5) .6400(4) .5387(3) .148(4) Uani ? ? 1.00000 ? ?
F5 .4188(5) .6167(4) .5425(3) .161(5) Uani ? ? 1.00000 ? ?
F6 .2025(6) .7894(3) .4986(3) .144(4) Uani ? ? 1.00000 ? ?
H13 .50330 .74960 .90870 .06370 Uiso ? ? 1.00000 ? ?
H14 .41220 .86780 .97330 .07250 Uiso ? ? 1.00000 ? ?
H15 .17010 .93860 .95180 .06740 Uiso ? ? 1.00000 ? ?
H16 .01900 .89100 .86740 .05260 Uiso ? ? 1.00000 ? ?
H13' .58460 .65700 .83630 .06240 Uiso ? ? 1.00000 ? ?
H14' .66180 .56970 .75300 .07580 Uiso ? ? 1.00000 ? ?
H15' .49060 .56230 .66840 .06660 Uiso ? ? 1.00000 ? ?
H16' .24270 .62570 .67160 .04930 Uiso ? ? 1.00000 ? ?
H23 -.00930 .37380 .81550 .05250 Uiso ? ? 1.00000 ? ?
H24 -.06100 .39910 .91350 .06160 Uiso ? ? 1.00000 ? ?
H25 -.09650 .56400 .94670 .06200 Uiso ? ? 1.00000 ? ?
H26 -.06610 .69730 .88400 .04650 Uiso ? ? 1.00000 ? ?
H23' -.13260 .45000 .63180 .04720 Uiso ? ? 1.00000 ? ?
H24' -.27370 .54220 .55950 .06110 Uiso ? ? 1.00000 ? ?
H25' -.28740 .71560 .56950 .06410 Uiso ? ? 1.00000 ? ?
H26' -.15320 .79460 .64960 .05440 Uiso ? ? 1.00000 ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ru ? 0 4 -1.259 .835999 'Int Tables Vol IV Tables 2.2B and 2.3.1'
C ? 0 88 .002991 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 72 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N ? 0 16 .005981 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 12 .010986 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Cl ? 0 4 .14801 .158997 'Int Tables Vol IV Tables 2.2B and 2.3.1'
P ? 0 4 .10199 .093994 'Int Tables Vol IV Tables 2.2B and 2.3.1'
F ? 0 24 .017029 .01001 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl Ru C0 . . . 90.33(17) ?
Cl Ru N11 . . . 95.33(13) ?
Cl Ru N11' . . . 174.08(13) ?
Cl Ru N21 . . . 88.69(11) ?
Cl Ru N21' . . . 88.74(13) ?
C0 Ru N11 . . . 93.55(19) ?
C0 Ru N11' . . . 90.6(2) ?
C0 Ru N21 . . . 179.00(18) ?
C0 Ru N21' . . . 93.20(19) ?
N11 Ru N11' . . . 78.78(17) ?
N11 Ru N21 . . . 86.71(16) ?
N11 Ru N21' . . . 172.09(16) ?
N11' Ru N21 . . . 90.43(16) ?
N11' Ru N21' . . . 97.04(17) ?
N21 Ru N21' . . . 86.60(17) ?
Ru C0 O0 . . . 178.1(5) ?
Ru N11 C12 . . . 115.0(3) ?
Ru N11 C16 . . . 125.8(3) ?
C12 N11 C16 . . . 119.2(4) ?
N11 C12 C13 . . . 120.2(5) ?
N11 C12 C12' . . . 115.5(4) ?
C13 C12 C12' . . . 124.2(4) ?
C12 C13 C14 . . . 120.0(5) ?
C12 C13 H13 . . . 119.9 ?
C14 C13 H13 . . . 120.0 ?
C13 C14 C15 . . . 119.0(6) ?
C13 C14 H14 . . . 120.5 ?
C15 C14 H14 . . . 120.5 ?
C14 C15 C16 . . . 120.1(6) ?
C14 C15 H15 . . . 120.0 ?
C16 C15 H15 . . . 119.9 ?
N11 C16 C15 . . . 121.5(5) ?
N11 C16 H16 . . . 119.2 ?
C15 C16 H16 . . . 119.2 ?
Ru N11' C12' . . . 115.5(3) ?
Ru N11' C16' . . . 126.9(3) ?
C12' N11' C16' . . . 117.5(4) ?
C12 C12' N11' . . . 114.4(4) ?
C12 C12' C13' . . . 123.8(5) ?
N11' C12' C13' . . . 121.6(5) ?
C12' C13' C14' . . . 119.8(5) ?
C12' C13' H13' . . . 120.2 ?
C14' C13' H13' . . . 120.0 ?
C13' C14' C15' . . . 118.8(6) ?
C13' C14' H14' . . . 120.6 ?
C15' C14' H14' . . . 120.5 ?
C14' C15' C16' . . . 118.6(6) ?
C14' C15' H15' . . . 120.7 ?
C16' C15' H15' . . . 120.7 ?
N11' C16' C15' . . . 123.5(5) ?
N11' C16' H16' . . . 118.2 ?
C15' C16' H16' . . . 118.2 ?
Ru N21 C22 . . . 120.7(3) ?
Ru N21 C26 . . . 121.1(3) ?
C22 N21 C26 . . . 117.5(4) ?
N21 C22 C23 . . . 122.5(4) ?
N21 C22 C2 . . . 119.2(4) ?
C23 C22 C2 . . . 118.1(5) ?
C22 C23 C24 . . . 119.1(5) ?
C22 C23 H23 . . . 120.4 ?
C24 C23 H23 . . . 120.5 ?
C23 C24 C25 . . . 118.8(5) ?
C23 C24 H24 . . . 120.7 ?
C25 C24 H24 . . . 120.6 ?
C24 C25 C26 . . . 119.6(5) ?
C24 C25 H25 . . . 120.2 ?
C26 C25 H25 . . . 120.2 ?
N21 C26 C25 . . . 122.4(5) ?
N21 C26 H26 . . . 118.7 ?
C25 C26 H26 . . . 118.8 ?
O2 C2 C22 . . . 119.8(5) ?
O2 C2 C22' . . . 118.7(4) ?
C22 C2 C22' . . . 120.9(4) ?
Ru N21' C22' . . . 121.9(3) ?
Ru N21' C26' . . . 120.7(3) ?
C22' N21' C26' . . . 117.4(4) ?
C2 C22' N21' . . . 120.8(4) ?
C2 C22' C23' . . . 116.9(5) ?
N21' C22' C23' . . . 122.2(4) ?
C22' C23' C24' . . . 120.1(5) ?
C22' C23' H23' . . . 120.0 ?
C24' C23' H23' . . . 119.9 ?
C23' C24' C25' . . . 118.7(5) ?
C23' C24' H24' . . . 120.6 ?
C25' C24' H24' . . . 120.7 ?
C24' C25' C26' . . . 119.9(5) ?
C24' C25' H25' . . . 120.0 ?
C26' C25' H25' . . . 120.1 ?
N21' C26' C25' . . . 121.7(5) ?
N21' C26' H26' . . . 119.2 ?
C25' C26' H26' . . . 119.1 ?
F1 P1 F2 . . . 86.9(3) ?
F1 P1 F3 . . . 176.5(3) ?
F1 P1 F4 . . . 93.2(3) ?
F1 P1 F5 . . . 90.5(3) ?
F1 P1 F6 . . . 90.2(3) ?
F2 P1 F3 . . . 90.2(3) ?
F2 P1 F4 . . . 178.1(3) ?
F2 P1 F5 . . . 88.9(3) ?
F2 P1 F6 . . . 90.3(3) ?
F3 P1 F4 . . . 89.8(3) ?
F3 P1 F5 . . . 91.4(3) ?
F3 P1 F6 . . . 87.8(3) ?
F4 P1 F5 . . . 89.1(3) ?
F4 P1 F6 . . . 91.7(3) ?
F5 P1 F6 . . . 178.9(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ru Cl . . 2.405(2) ?
Ru C0 . . 1.880(5) ?
Ru N11 . . 2.070(4) ?
Ru N11' . . 2.062(4) ?
Ru N21 . . 2.157(4) ?
Ru N21' . . 2.090(4) ?
C0 O0 . . 1.119(7) ?
O2 C2 . . 1.205(7) ?
N11 C12 . . 1.345(6) ?
N11 C16 . . 1.346(7) ?
C12 C13 . . 1.402(8) ?
C12 C12' . . 1.483(7) ?
C13 C14 . . 1.371(9) ?
C13 H13 . . .950 ?
C14 C15 . . 1.348(10) ?
C14 H14 . . .952 ?
C15 C16 . . 1.384(8) ?
C15 H15 . . .949 ?
C16 H16 . . .950 ?
N11' C12' . . 1.355(6) ?
N11' C16' . . 1.356(7) ?
C12' C13' . . 1.366(8) ?
C13' C14' . . 1.401(10) ?
C13' H13' . . .950 ?
C14' C15' . . 1.364(9) ?
C14' H14' . . .950 ?
C15' C16' . . 1.368(8) ?
C15' H15' . . .950 ?
C16' H16' . . .950 ?
N21 C22 . . 1.354(7) ?
N21 C26 . . 1.342(7) ?
C22 C23 . . 1.383(7) ?
C22 C2 . . 1.506(7) ?
C23 C24 . . 1.361(8) ?
C23 H23 . . .951 ?
C24 C25 . . 1.388(9) ?
C24 H24 . . .952 ?
C25 C26 . . 1.368(8) ?
C25 H25 . . .949 ?
C26 H26 . . .950 ?
C2 C22' . . 1.505(7) ?
N21' C22' . . 1.352(7) ?
N21' C26' . . 1.355(6) ?
C22' C23' . . 1.383(7) ?
C23' C24' . . 1.360(7) ?
C23' H23' . . .950 ?
C24' C25' . . 1.364(9) ?
C24' H24' . . .950 ?
C25' C26' . . 1.391(7) ?
C25' H25' . . .950 ?
C26' H26' . . .950 ?
P1 F1 . . 1.555(5) ?
P1 F2 . . 1.602(5) ?
P1 F3 . . 1.539(5) ?
P1 F4 . . 1.560(5) ?
P1 F5 . . 1.545(5) ?
P1 F6 . . 1.532(5) ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
