#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:40:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178719 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/30/4083045.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_4083045
loop_
_publ_author_name
'Friedberger, Tobias'
'Ziller, Joseph W.'
'Guan, Zhibin'
_publ_section_title
;
 Ruthenium(IV) Complexes for Ethylene Insertion Polymerization
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1913
_journal_paper_doi               10.1021/om5001343
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C22 H24 F3 Li2 O9 P S2'
_chemical_formula_weight         598.38
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                104.7052(8)
_cell_angle_beta                 91.9422(9)
_cell_angle_gamma                109.1931(8)
_cell_formula_units_Z            2
_cell_length_a                   10.1347(8)
_cell_length_b                   10.8117(8)
_cell_length_c                   13.1228(10)
_cell_measurement_reflns_used    8875
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      26.84
_cell_measurement_theta_min      2.25
_cell_volume                     1302.62(17)
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_collection       'Bruker APEX2 2011.4-1, 2011'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14701
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.860
_diffrn_reflns_theta_min         1.618
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.9189
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.156
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5564
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0415P)²+0.8146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4961
_reflns_number_total             5564
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om5001343_si_002.cif
_cod_data_source_block           zg65
_cod_depositor_comments
;Adding full bibliography for 4083043--4083045.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4083045
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.909
_shelx_estimated_absorpt_t_max   0.949
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
S1 S -0.88074(4) -0.77646(4) 0.62149(3) 0.01617(10) Uani 1 1 d . .
S2 S -0.35011(4) -0.59612(4) 0.56162(3) 0.01406(9) Uani 1 1 d . .
P1 P -0.57652(4) -0.51296(4) 0.71956(3) 0.01329(9) Uani 1 1 d . .
F1 F -0.26595(13) 0.14309(11) 1.01540(10) 0.0399(3) Uani 1 1 d . .
F2 F -0.09788(12) 0.07090(12) 1.03699(12) 0.0466(4) Uani 1 1 d . .
F3 F -0.26323(16) 0.04126(12) 1.13400(9) 0.0473(3) Uani 1 1 d . .
O1 O -0.95629(14) -0.71171(14) 0.56979(10) 0.0299(3) Uani 1 1 d . .
O2 O -0.96203(14) -0.91478(12) 0.62009(10) 0.0291(3) Uani 1 1 d . .
O3 O -0.74535(12) -0.76605(12) 0.58334(9) 0.0220(3) Uani 1 1 d . .
O4 O -0.47350(12) -0.67532(12) 0.48458(9) 0.0199(2) Uani 1 1 d . .
O5 O -0.32493(13) -0.45050(11) 0.59589(9) 0.0208(3) Uani 1 1 d . .
O6 O -0.22425(12) -0.62257(13) 0.52775(10) 0.0218(3) Uani 1 1 d . .
O7 O -1.00606(14) -0.63539(14) 0.37280(11) 0.0274(3) Uani 1 1 d D .
H7 H -0.932(2) -0.583(3) 0.397(2) 0.067(10) Uiso 1 1 d D .
O8 O -1.21097(15) -0.91201(15) 0.42226(15) 0.0434(4) Uani 1 1 d . .
H8 H -1.174(3) -0.963(3) 0.415(2) 0.041(7) Uiso 1 1 d . .
C1 C -0.72324(16) -0.56333(15) 0.79934(12) 0.0140(3) Uani 1 1 d . .
C2 C -0.84517(16) -0.67838(15) 0.75728(12) 0.0149(3) Uani 1 1 d . .
C3 C -0.95258(17) -0.71766(17) 0.81829(13) 0.0190(3) Uani 1 1 d . .
H3A H -1.0327 -0.7974 0.7884 0.023 Uiso 1 1 calc R U
C4 C -0.94398(17) -0.64159(17) 0.92239(14) 0.0205(3) Uani 1 1 d . .
H4A H -1.0172 -0.6691 0.9640 0.025 Uiso 1 1 calc R U
C5 C -0.82723(17) -0.52507(17) 0.96473(13) 0.0189(3) Uani 1 1 d . .
H5A H -0.8213 -0.4705 1.0352 0.023 Uiso 1 1 calc R U
C6 C -0.71854(17) -0.48771(16) 0.90430(13) 0.0172(3) Uani 1 1 d . .
H6A H -0.6385 -0.4083 0.9352 0.021 Uiso 1 1 calc R U
C7 C -0.46598(16) -0.35031(15) 0.81433(12) 0.0149(3) Uani 1 1 d . .
C8 C -0.49182(17) -0.23380(16) 0.80650(14) 0.0194(3) Uani 1 1 d . .
H8A H -0.5598 -0.2410 0.7516 0.023 Uiso 1 1 calc R U
C9 C -0.41918(17) -0.10712(16) 0.87811(14) 0.0207(3) Uani 1 1 d . .
H9A H -0.4393 -0.0289 0.8731 0.025 Uiso 1 1 calc R U
C10 C -0.31747(17) -0.09556(16) 0.95662(13) 0.0175(3) Uani 1 1 d . .
C11 C -0.28749(17) -0.21001(17) 0.96401(13) 0.0186(3) Uani 1 1 d . .
H11A H -0.2166 -0.2017 1.0172 0.022 Uiso 1 1 calc R U
C12 C -0.36164(17) -0.33604(16) 0.89337(13) 0.0181(3) Uani 1 1 d . .
H12A H -0.3413 -0.4140 0.8987 0.022 Uiso 1 1 calc R U
C13 C -0.23650(18) 0.03895(17) 1.03480(14) 0.0215(3) Uani 1 1 d . .
C14 C -0.48047(15) -0.62507(15) 0.74266(12) 0.0136(3) Uani 1 1 d . .
C15 C -0.50355(16) -0.68302(16) 0.82734(12) 0.0161(3) Uani 1 1 d . .
H15A H -0.5696 -0.6646 0.8731 0.019 Uiso 1 1 calc R U
C16 C -0.43251(17) -0.76677(16) 0.84630(13) 0.0174(3) Uani 1 1 d . .
H16A H -0.4505 -0.8050 0.9043 0.021 Uiso 1 1 calc R U
C17 C -0.33558(17) -0.79450(17) 0.78072(14) 0.0197(3) Uani 1 1 d . .
H17A H -0.2868 -0.8517 0.7935 0.024 Uiso 1 1 calc R U
C18 C -0.30998(17) -0.73827(16) 0.69615(13) 0.0185(3) Uani 1 1 d . .
H18A H -0.2430 -0.7566 0.6513 0.022 Uiso 1 1 calc R U
C19 C -0.38201(16) -0.65517(15) 0.67687(12) 0.0145(3) Uani 1 1 d . .
C20 C -1.0498(3) -0.6094(2) 0.27990(18) 0.0451(6) Uani 1 1 d . .
H20A H -0.9945 -0.6350 0.2237 0.068 Uiso 1 1 calc R U
H20B H -1.0353 -0.5120 0.2944 0.068 Uiso 1 1 calc R U
H20C H -1.1499 -0.6630 0.2569 0.068 Uiso 1 1 calc R U
C21 C -1.3555(2) -0.9798(2) 0.4004(2) 0.0460(6) Uani 1 1 d . .
H21A H -1.3794 -1.0369 0.3266 0.069 Uiso 1 1 calc R U
H21B H -1.4034 -0.9130 0.4110 0.069 Uiso 1 1 calc R U
H21C H -1.3859 -1.0374 0.4482 0.069 Uiso 1 1 calc R U
O9 O -0.79852(14) -0.87201(14) 0.35302(10) 0.0278(3) Uani 1 1 d . .
H9 H -0.846(3) -0.929(3) 0.373(2) 0.044(7) Uiso 1 1 d . .
C22 C -0.87768(19) -0.87547(19) 0.26003(14) 0.0257(4) Uani 1 1 d . .
H22C H -0.8863 -0.9579 0.2036 0.036(6) Uiso 1 1 calc R .
H22B H -0.8295 -0.7947 0.2367 0.039(6) Uiso 1 1 calc R .
H22A H -0.9717 -0.8762 0.2758 0.041(6) Uiso 1 1 calc R .
Li1 Li -0.6731(3) -0.7039(3) 0.4590(2) 0.0189(5) Uani 1 1 d . .
Li2 Li -1.1048(3) -0.7236(3) 0.4699(2) 0.0205(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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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
O2 S1 O1 114.39(8) . .
O2 S1 O3 111.96(8) . .
O1 S1 O3 112.10(8) . .
O2 S1 C2 106.21(7) . .
O1 S1 C2 104.33(7) . .
O3 S1 C2 107.09(7) . .
O4 S2 O5 114.55(7) . .
O4 S2 O6 112.47(7) . .
O5 S2 O6 111.21(7) . .
O4 S2 C19 106.05(7) . .
O5 S2 C19 106.25(7) . .
O6 S2 C19 105.55(7) . .
C7 P1 C14 99.85(7) . .
C7 P1 C1 98.95(7) . .
C14 P1 C1 99.04(7) . .
S1 O1 Li2 150.50(13) . .
S1 O3 Li1 128.04(11) . .
S2 O4 Li1 141.46(11) . .
S2 O5 Li1 141.98(11) . 2_446
S2 O6 Li2 159.44(12) . 1_655
C20 O7 Li2 133.28(16) . .
C21 O8 Li2 130.54(16) . .
C6 C1 C2 116.41(14) . .
C6 C1 P1 121.79(12) . .
C2 C1 P1 121.80(12) . .
C3 C2 C1 121.49(14) . .
C3 C2 S1 114.97(12) . .
C1 C2 S1 123.37(12) . .
C4 C3 C2 120.67(15) . .
C5 C4 C3 119.07(15) . .
C4 C5 C6 120.12(15) . .
C5 C6 C1 122.18(15) . .
C8 C7 C12 118.42(14) . .
C8 C7 P1 116.44(12) . .
C12 C7 P1 125.13(12) . .
C9 C8 C7 120.83(15) . .
C10 C9 C8 119.77(15) . .
C9 C10 C11 120.27(15) . .
C9 C10 C13 121.42(15) . .
C11 C10 C13 118.31(15) . .
C12 C11 C10 119.59(15) . .
C11 C12 C7 121.08(15) . .
F2 C13 F3 106.09(15) . .
F2 C13 F1 106.27(14) . .
F3 C13 F1 105.60(14) . .
F2 C13 C10 112.75(14) . .
F3 C13 C10 112.32(14) . .
F1 C13 C10 113.22(14) . .
C15 C14 C19 117.18(14) . .
C15 C14 P1 120.83(12) . .
C19 C14 P1 121.99(11) . .
C16 C15 C14 121.78(15) . .
C17 C16 C15 120.01(15) . .
C16 C17 C18 119.63(15) . .
C17 C18 C19 120.26(15) . .
C18 C19 C14 121.14(14) . .
C18 C19 S2 117.02(12) . .
C14 C19 S2 121.77(12) . .
C22 O9 Li1 125.10(14) . .
O4 Li1 O9 119.26(15) . .
O4 Li1 O5 103.64(13) . 2_446
O9 Li1 O5 106.21(13) . 2_446
O4 Li1 O3 101.79(13) . .
O9 Li1 O3 94.12(12) . .
O5 Li1 O3 133.46(16) 2_446 .
O8 Li2 O7 119.14(17) . .
O8 Li2 O1 103.94(15) . .
O7 Li2 O1 102.90(14) . .
O8 Li2 O6 110.06(15) . 1_455
O7 Li2 O6 106.19(14) . 1_455
O1 Li2 O6 114.77(15) . 1_455
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 O2 1.4459(13) .
S1 O1 1.4474(13) .
S1 O3 1.4559(12) .
S1 C2 1.7821(16) .
S2 O4 1.4456(12) .
S2 O5 1.4542(12) .
S2 O6 1.4561(12) .
S2 C19 1.7853(16) .
P1 C7 1.8423(16) .
P1 C14 1.8577(15) .
P1 C1 1.8617(16) .
F1 C13 1.335(2) .
F2 C13 1.329(2) .
F3 C13 1.334(2) .
O1 Li2 1.911(3) .
O3 Li1 1.991(3) .
O4 Li1 1.947(3) .
O5 Li1 1.984(3) 2_446
O6 Li2 1.935(3) 1_655
O7 C20 1.407(2) .
O7 Li2 1.900(3) .
O8 C21 1.387(2) .
O8 Li2 1.888(3) .
C1 C6 1.402(2) .
C1 C2 1.405(2) .
C2 C3 1.391(2) .
C3 C4 1.387(2) .
C4 C5 1.384(2) .
C5 C6 1.391(2) .
C7 C8 1.395(2) .
C7 C12 1.398(2) .
C8 C9 1.392(2) .
C9 C10 1.385(2) .
C10 C11 1.392(2) .
C10 C13 1.497(2) .
C11 C12 1.385(2) .
C14 C15 1.399(2) .
C14 C19 1.406(2) .
C15 C16 1.390(2) .
C16 C17 1.384(2) .
C17 C18 1.388(2) .
C18 C19 1.392(2) .
O9 C22 1.423(2) .
O9 Li1 1.983(3) .
Li1 O5 1.984(3) 2_446
Li2 O6 1.935(3) 1_455
