#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:18:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178621 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/32/4073255.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_4073255
loop_
_publ_author_name
'Zhang, Hong'
'Feng, Li'
'Gong, Lei'
'Wu, Liqiong'
'He, Guomei'
'Wen, Tingbin'
'Yang, Fangzu'
'Xia, Haiping'
_publ_section_title
;
 Synthesis and Characterization of Stable Ruthenabenzenes Starting from
 HC⋮CCH(OH)C⋮CH
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2705
_journal_paper_doi               10.1021/om070195k
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C57 H59 N2 P4 Ru,  Cl3'
_chemical_formula_sum            'C57 H59 Cl3 N2 P4 Ru'
_chemical_formula_weight         1103.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                90.00
_cell_formula_units_Z            16
_cell_length_a                   24.495(4)
_cell_length_b                   25.713(4)
_cell_length_c                   43.627(10)
_cell_measurement_reflns_used    5495
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.70
_cell_measurement_theta_min      2.48
_cell_volume                     27478(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            49116
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.858035
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9120
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6461
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1153P)²+83.0477P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.1970
_reflns_number_gt                5151
_reflns_number_total             6461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070195ksi20070302_044625.cif
_cod_data_source_block           complex8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        27479(9)
_cod_original_sg_symbol_H-M      Fddd
_cod_database_code               4073255
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
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 0.3750 0.3750 0.545142(9) 0.03026(18) Uani 1 2 d S
P1 P 0.37228(6) 0.28341(5) 0.54276(3) 0.0487(3) Uani 1 1 d .
P2 P 0.26488(4) 0.36594(4) 0.63095(2) 0.0359(3) Uani 1 1 d .
N1 N 0.42918(15) 0.37434(14) 0.50530(8) 0.0382(8) Uani 1 1 d .
C1 C 0.32064(17) 0.37241(17) 0.57667(9) 0.0359(9) Uani 1 1 d .
H1A H 0.2848 0.3726 0.5696 0.043 Uiso 1 1 calc R
C2 C 0.32562(16) 0.37026(15) 0.60829(9) 0.0321(8) Uani 1 1 d .
C3 C 0.3750 0.3750 0.62329(13) 0.0368(13) Uani 1 2 d S
H3A H 0.3750 0.3750 0.6446 0.044 Uiso 1 2 calc SR
C11 C 0.4048(2) 0.37374(17) 0.47761(9) 0.0403(10) Uani 1 1 d .
C12 C 0.4351(2) 0.3710(2) 0.45079(11) 0.0561(13) Uani 1 1 d .
H12A H 0.4176 0.3703 0.4319 0.067 Uiso 1 1 calc R
C13 C 0.4913(2) 0.3693(2) 0.45236(12) 0.0605(14) Uani 1 1 d .
H13A H 0.5121 0.3679 0.4345 0.073 Uiso 1 1 calc R
C14 C 0.5162(2) 0.3697(2) 0.48059(12) 0.0577(13) Uani 1 1 d .
H14A H 0.5540 0.3689 0.4823 0.069 Uiso 1 1 calc R
C15 C 0.4836(2) 0.3713(2) 0.50637(11) 0.0483(11) Uani 1 1 d .
H15A H 0.5004 0.3703 0.5255 0.058 Uiso 1 1 calc R
C111 C 0.3996(5) 0.2524(3) 0.57593(16) 0.107(3) Uani 1 1 d .
H11A H 0.3973 0.2154 0.5735 0.160 Uiso 1 1 calc R
H11B H 0.3791 0.2628 0.5937 0.160 Uiso 1 1 calc R
H11C H 0.4371 0.2624 0.5784 0.160 Uiso 1 1 calc R
C121 C 0.4075(4) 0.2541(3) 0.51161(15) 0.095(3) Uani 1 1 d .
H12B H 0.4037 0.2170 0.5128 0.142 Uiso 1 1 calc R
H12C H 0.4455 0.2632 0.5126 0.142 Uiso 1 1 calc R
H12D H 0.3924 0.2663 0.4926 0.142 Uiso 1 1 calc R
C131 C 0.3052(4) 0.2571(3) 0.5420(3) 0.124(4) Uani 1 1 d .
H13B H 0.3073 0.2198 0.5411 0.186 Uiso 1 1 calc R
H13C H 0.2862 0.2699 0.5243 0.186 Uiso 1 1 calc R
H13D H 0.2860 0.2674 0.5602 0.186 Uiso 1 1 calc R
C211 C 0.21260(18) 0.3350(2) 0.60876(10) 0.0464(11) Uani 1 1 d .
C212 C 0.2021(2) 0.2831(2) 0.61231(13) 0.0636(15) Uani 1 1 d .
H21A H 0.2205 0.2637 0.6270 0.076 Uiso 1 1 calc R
C213 C 0.1632(3) 0.2599(3) 0.59328(17) 0.080(2) Uani 1 1 d .
H21B H 0.1547 0.2249 0.5960 0.097 Uiso 1 1 calc R
C214 C 0.1382(3) 0.2865(4) 0.57167(17) 0.089(3) Uani 1 1 d .
H21C H 0.1131 0.2699 0.5590 0.107 Uiso 1 1 calc R
C215 C 0.1487(2) 0.3378(4) 0.56776(14) 0.077(2) Uani 1 1 d .
H21D H 0.1308 0.3563 0.5525 0.092 Uiso 1 1 calc R
C216 C 0.1854(2) 0.3621(3) 0.58605(11) 0.0577(14) Uani 1 1 d .
H21E H 0.1923 0.3974 0.5833 0.069 Uiso 1 1 calc R
C221 C 0.2779(2) 0.3284(2) 0.66463(10) 0.0469(12) Uani 1 1 d .
C222 C 0.2547(2) 0.3435(3) 0.69249(11) 0.0618(15) Uani 1 1 d .
H22A H 0.2336 0.3734 0.6938 0.074 Uiso 1 1 calc R
C223 C 0.2636(4) 0.3136(3) 0.71735(14) 0.088(2) Uani 1 1 d .
H22B H 0.2501 0.3241 0.7363 0.106 Uiso 1 1 calc R
C224 C 0.2921(4) 0.2681(4) 0.71519(16) 0.096(3) Uani 1 1 d .
H22C H 0.2947 0.2465 0.7322 0.115 Uiso 1 1 calc R
C225 C 0.3167(3) 0.2541(3) 0.68861(17) 0.083(2) Uani 1 1 d .
H22D H 0.3390 0.2249 0.6879 0.100 Uiso 1 1 calc R
C226 C 0.3084(2) 0.2835(2) 0.66267(12) 0.0616(14) Uani 1 1 d .
H22E H 0.3232 0.2731 0.6440 0.074 Uiso 1 1 calc R
C231 C 0.2430(2) 0.42931(19) 0.64281(11) 0.0478(11) Uani 1 1 d .
C232 C 0.1888(2) 0.4400(3) 0.64746(16) 0.0723(17) Uani 1 1 d .
H23A H 0.1627 0.4152 0.6422 0.087 Uiso 1 1 calc R
C233 C 0.1724(3) 0.4861(3) 0.6596(2) 0.091(2) Uani 1 1 d .
H23B H 0.1356 0.4928 0.6629 0.109 Uiso 1 1 calc R
C234 C 0.2120(4) 0.5230(3) 0.6670(2) 0.108(3) Uani 1 1 d .
H23C H 0.2016 0.5552 0.6748 0.130 Uiso 1 1 calc R
C235 C 0.2646(4) 0.5121(3) 0.6627(2) 0.098(3) Uani 1 1 d .
H23D H 0.2908 0.5365 0.6683 0.118 Uiso 1 1 calc R
C236 C 0.2813(3) 0.4655(2) 0.65012(17) 0.0724(17) Uani 1 1 d .
H23E H 0.3181 0.4589 0.6467 0.087 Uiso 1 1 calc R
Cl1 Cl 1.1250 0.1250 0.6250 0.0826(11) Uani 1 4 d S
Cl2 Cl 0.54890(17) 0.27648(15) 0.54486(8) 0.0890(11) Uani 0.50 1 d PD
Cl3 Cl 0.6554(2) 0.36965(13) 0.45457(13) 0.1137(18) Uani 0.50 1 d PD
Cl4 Cl 0.6635(8) 0.3160(8) 0.5193(3) 0.129(8) Uani 0.12 1 d PD
Cl5 Cl 0.5155(7) 0.1616(5) 0.5591(4) 0.111(6) Uani 0.13 1 d PD
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'
P P 0.1023 0.0942 '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'
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
C1 Ru1 C1 88.2(2) 2 .
C1 Ru1 N1 172.87(15) 2 2
C1 Ru1 N1 98.58(16) . 2
C1 Ru1 N1 98.58(16) 2 .
C1 Ru1 N1 172.87(15) . .
N1 Ru1 N1 74.73(19) 2 .
C1 Ru1 P1 94.94(13) 2 .
C1 Ru1 P1 88.70(13) . .
N1 Ru1 P1 87.45(10) 2 .
N1 Ru1 P1 88.53(10) . .
C1 Ru1 P1 88.70(13) 2 2
C1 Ru1 P1 94.94(13) . 2
N1 Ru1 P1 88.53(10) 2 2
N1 Ru1 P1 87.45(10) . 2
P1 Ru1 P1 174.95(6) . 2
C131 P1 C121 105.9(5) . .
C131 P1 C111 101.0(6) . .
C121 P1 C111 104.4(4) . .
C131 P1 Ru1 114.0(3) . .
C121 P1 Ru1 116.3(2) . .
C111 P1 Ru1 113.6(3) . .
C221 P2 C2 109.8(2) . .
C221 P2 C211 109.4(2) . .
C2 P2 C211 108.87(19) . .
C221 P2 C231 107.9(2) . .
C2 P2 C231 110.6(2) . .
C211 P2 C231 110.2(2) . .
C15 N1 C11 118.3(4) . .
C15 N1 Ru1 125.3(3) . .
C11 N1 Ru1 116.3(3) . .
C2 C1 Ru1 130.9(3) . .
C3 C2 C1 123.0(4) . .
C3 C2 P2 118.2(3) . .
C1 C2 P2 118.6(3) . .
C2 C3 C2 123.4(5) . 2
N1 C11 C12 121.2(4) . .
N1 C11 C11 116.3(2) . 2
C12 C11 C11 122.5(3) . 2
C13 C12 C11 119.6(5) . .
C14 C13 C12 119.1(5) . .
C13 C14 C15 118.3(5) . .
N1 C15 C14 123.4(5) . .
C212 C211 C216 118.9(5) . .
C212 C211 P2 120.4(4) . .
C216 C211 P2 120.5(4) . .
C211 C212 C213 118.5(6) . .
C214 C213 C212 121.4(7) . .
C213 C214 C215 120.5(6) . .
C214 C215 C216 120.2(7) . .
C215 C216 C211 120.5(6) . .
C226 C221 C222 120.5(5) . .
C226 C221 P2 119.9(4) . .
C222 C221 P2 119.5(5) . .
C223 C222 C221 118.5(7) . .
C222 C223 C224 121.1(7) . .
C225 C224 C223 120.9(6) . .
C224 C225 C226 119.5(7) . .
C225 C226 C221 119.3(6) . .
C236 C231 C232 119.8(5) . .
C236 C231 P2 118.8(4) . .
C232 C231 P2 121.0(4) . .
C233 C232 C231 121.2(6) . .
C232 C233 C234 118.7(7) . .
C235 C234 C233 119.7(7) . .
C234 C235 C236 121.7(7) . .
C231 C236 C235 118.8(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 C1 1.916(4) 2
Ru1 C1 1.916(4) .
Ru1 N1 2.187(3) 2
Ru1 N1 2.187(3) .
Ru1 P1 2.3583(14) .
Ru1 P1 2.3583(14) 2
P1 C131 1.776(9) .
P1 C121 1.777(6) .
P1 C111 1.782(7) .
P2 C221 1.787(5) .
P2 C2 1.790(4) .
P2 C211 1.791(4) .
P2 C231 1.792(5) .
N1 C15 1.336(6) .
N1 C11 1.348(5) .
C1 C2 1.386(5) .
C2 C3 1.381(5) .
C3 C2 1.381(5) 2
C11 C12 1.388(6) .
C11 C11 1.460(10) 2
C12 C13 1.380(9) .
C13 C14 1.374(8) .
C14 C15 1.380(7) .
C211 C212 1.368(8) .
C211 C216 1.383(7) .
C212 C213 1.399(9) .
C213 C214 1.315(12) .
C214 C215 1.355(12) .
C215 C216 1.355(8) .
C221 C226 1.378(8) .
C221 C222 1.396(7) .
C222 C223 1.347(9) .
C223 C224 1.365(12) .
C224 C225 1.355(11) .
C225 C226 1.375(8) .
C231 C236 1.359(8) .
C231 C232 1.370(8) .
C232 C233 1.359(9) .
C233 C234 1.393(12) .
C234 C235 1.333(12) .
C235 C236 1.380(9) .
