#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:08:53 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178637 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/48/4074836.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_4074836
loop_
_publ_author_name
'Bernechea, María'
'Lugan, Noël'
'Gil, Belén'
'Lalinde, Elena'
'Lavigne, Guy'
_publ_section_title
;
 Six-Coordinate Alkynyldiphenylphosphine Ruthenium(II) Complexes: 
 Synthesis, Structure, and Catalytic Activity as ROMP Initiators
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              684
_journal_paper_doi               10.1021/om050935u
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C80 H60 Cl2 O4 P4 Ru'
_chemical_formula_weight         1381.13
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.4930(8)
_cell_length_b                   25.4930(8)
_cell_length_c                   12.0850(3)
_cell_measurement_reflns_used    13878
_cell_measurement_temperature    293(2)
_cell_volume                     7854.0(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0347714
_diffrn_orient_matrix_UB_12      -0.0045139
_diffrn_orient_matrix_UB_13      0.0370984
_diffrn_orient_matrix_UB_21      -0.017736
_diffrn_orient_matrix_UB_22      0.000314
_diffrn_orient_matrix_UB_23      -0.0738029
_diffrn_orient_matrix_UB_31      0.0038852
_diffrn_orient_matrix_UB_32      -0.0389646
_diffrn_orient_matrix_UB_33      -0.0048924
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            21045
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         4666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.153
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0670P)²+8.3674P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.124
_refine_ls_wR_factor_ref         0.1441
_reflns_number_gt                3081
_reflns_number_total             4666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050935usi20051129_063723.cif
_cod_data_source_block           complex1.4H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_sg_symbol_H-M      'I 4 1/a'
_cod_database_code               4074836
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'
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 0.25 0.625 0.03403(15) Uani 1 4 d S
Cl1 Cl 0 0.25 0.42367(8) 0.0439(3) Uani 1 2 d S
P1 P 0.09139(3) 0.27381(3) 0.62741(6) 0.0403(2) Uani 1 1 d .
C1 C 0.11788(13) 0.28077(15) 0.4940(3) 0.0505(8) Uani 1 1 d .
C2 C 0.13102(15) 0.28337(16) 0.3993(3) 0.0566(9) Uani 1 1 d .
C3 C 0.14286(17) 0.28575(17) 0.2828(3) 0.0634(10) Uani 1 1 d .
C4 C 0.1925(2) 0.2935(3) 0.2461(4) 0.1053(19) Uani 1 1 d .
H4 H 0.22 0.297 0.296 0.126 Uiso 1 1 calc R
C5 C 0.2020(3) 0.2962(3) 0.1307(5) 0.126(2) Uani 1 1 d .
H5 H 0.2358 0.3026 0.105 0.152 Uiso 1 1 calc R
C6 C 0.1623(3) 0.2895(3) 0.0575(5) 0.123(2) Uani 1 1 d .
H6 H 0.169 0.2893 -0.0181 0.148 Uiso 1 1 calc R
C7 C 0.1133(3) 0.2833(4) 0.0951(5) 0.161(4) Uani 1 1 d .
H7 H 0.0856 0.2806 0.0453 0.193 Uiso 1 1 calc R
C8 C 0.1038(2) 0.2808(3) 0.2066(4) 0.122(2) Uani 1 1 d .
H8 H 0.0696 0.2756 0.231 0.146 Uiso 1 1 calc R
C9 C 0.14028(13) 0.23118(13) 0.6938(3) 0.0465(8) Uani 1 1 d .
C10 C 0.18810(14) 0.22000(15) 0.6448(3) 0.0609(10) Uani 1 1 d .
H10 H 0.1954 0.2321 0.5739 0.073 Uiso 1 1 calc R
C11 C 0.22502(16) 0.19072(19) 0.7017(4) 0.0798(13) Uani 1 1 d .
H11 H 0.2572 0.1834 0.6687 0.096 Uiso 1 1 calc R
C12 C 0.21472(18) 0.17251(19) 0.8056(5) 0.0830(14) Uani 1 1 d .
H12 H 0.2397 0.1526 0.8429 0.1 Uiso 1 1 calc R
C13 C 0.16814(18) 0.18337(19) 0.8544(4) 0.0761(12) Uani 1 1 d .
H13 H 0.1613 0.1711 0.9255 0.091 Uiso 1 1 calc R
C14 C 0.13064(15) 0.21263(15) 0.7992(3) 0.0597(9) Uani 1 1 d .
H14 H 0.0987 0.2198 0.8333 0.072 Uiso 1 1 calc R
C15 C 0.11184(13) 0.33574(13) 0.6929(3) 0.0475(8) Uani 1 1 d .
C16 C 0.14445(14) 0.37094(15) 0.6397(3) 0.0621(10) Uani 1 1 d .
H16 H 0.1552 0.3647 0.5673 0.075 Uiso 1 1 calc R
C17 C 0.16135(18) 0.41624(17) 0.6955(5) 0.0837(14) Uani 1 1 d .
H17 H 0.1836 0.4398 0.6601 0.1 Uiso 1 1 calc R
C18 C 0.1455(2) 0.4258(2) 0.8005(5) 0.0909(16) Uani 1 1 d .
H18 H 0.1565 0.4561 0.8366 0.109 Uiso 1 1 calc R
C19 C 0.1135(2) 0.39107(19) 0.8536(4) 0.0836(14) Uani 1 1 d .
H19 H 0.1031 0.3976 0.9261 0.1 Uiso 1 1 calc R
C20 C 0.09634(16) 0.34624(16) 0.8003(3) 0.0628(10) Uani 1 1 d .
H20 H 0.0742 0.323 0.8369 0.075 Uiso 1 1 calc R
O1 O 0.2098(13) 0.0394(19) 0.002(5) 1.04(5) 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 0 '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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.006 '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
P1 Ru1 P1 178.62(4) 2 .
P1 Ru1 P1 90.0090(10) 2 16_556
P1 Ru1 P1 90.0080(10) . 16_556
P1 Ru1 P1 90.0080(10) 2 15_556
P1 Ru1 P1 90.0080(10) . 15_556
P1 Ru1 P1 178.61(4) 16_556 15_556
P1 Ru1 Cl1 89.311(18) 2 15_556
P1 Ru1 Cl1 89.311(18) . 15_556
P1 Ru1 Cl1 90.695(18) 16_556 15_556
P1 Ru1 Cl1 90.695(18) 15_556 15_556
P1 Ru1 Cl1 90.689(18) 2 .
P1 Ru1 Cl1 90.689(18) . .
P1 Ru1 Cl1 89.305(18) 16_556 .
P1 Ru1 Cl1 89.305(18) 15_556 .
Cl1 Ru1 Cl1 180 15_556 .
C1 P1 C9 101.50(16) . .
C1 P1 C15 101.49(16) . .
C9 P1 C15 97.31(14) . .
C1 P1 Ru1 112.74(12) . .
C9 P1 Ru1 120.82(11) . .
C15 P1 Ru1 119.69(11) . .
C2 C1 P1 173.1(3) . .
C1 C2 C3 175.7(4) . .
C4 C3 C8 118.3(4) . .
C4 C3 C2 121.4(4) . .
C8 C3 C2 120.3(4) . .
C3 C4 C5 119.3(6) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C6 C5 C4 120.6(6) . .
C6 C5 H5 119.7 . .
C4 C5 H5 119.7 . .
C7 C6 C5 119.4(5) . .
C7 C6 H6 120.3 . .
C5 C6 H6 120.3 . .
C6 C7 C8 120.3(6) . .
C6 C7 H7 119.9 . .
C8 C7 H7 119.9 . .
C3 C8 C7 122.1(5) . .
C3 C8 H8 118.9 . .
C7 C8 H8 118.9 . .
C10 C9 C14 118.7(3) . .
C10 C9 P1 122.2(3) . .
C14 C9 P1 119.0(3) . .
C9 C10 C11 119.8(4) . .
C9 C10 H10 120.1 . .
C11 C10 H10 120.1 . .
C12 C11 C10 120.7(4) . .
C12 C11 H11 119.7 . .
C10 C11 H11 119.7 . .
C13 C12 C11 120.0(4) . .
C13 C12 H12 120 . .
C11 C12 H12 120 . .
C12 C13 C14 120.4(4) . .
C12 C13 H13 119.8 . .
C14 C13 H13 119.8 . .
C9 C14 C13 120.4(4) . .
C9 C14 H14 119.8 . .
C13 C14 H14 119.8 . .
C16 C15 C20 118.9(3) . .
C16 C15 P1 121.8(3) . .
C20 C15 P1 119.2(3) . .
C15 C16 C17 119.7(4) . .
C15 C16 H16 120.2 . .
C17 C16 H16 120.2 . .
C18 C17 C16 120.4(4) . .
C18 C17 H17 119.8 . .
C16 C17 H17 119.8 . .
C17 C18 C19 120.2(4) . .
C17 C18 H18 119.9 . .
C19 C18 H18 119.9 . .
C18 C19 C20 120.4(4) . .
C18 C19 H19 119.8 . .
C20 C19 H19 119.8 . .
C19 C20 C15 120.5(4) . .
C19 C20 H20 119.8 . .
C15 C20 H20 119.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 P1 2.4077(8) 2
Ru1 P1 2.4077(8) .
Ru1 P1 2.4077(8) 16_556
Ru1 P1 2.4077(8) 15_556
Ru1 Cl1 2.4330(10) 15_556
Ru1 Cl1 2.4332(10) .
P1 C1 1.757(3) .
P1 C9 1.838(3) .
P1 C15 1.842(3) .
C1 C2 1.194(5) .
C2 C3 1.442(5) .
C3 C4 1.355(6) .
C3 C8 1.362(7) .
C4 C5 1.417(7) .
C4 H4 0.93 .
C5 C6 1.355(9) .
C5 H5 0.93 .
C6 C7 1.338(9) .
C6 H6 0.93 .
C7 C8 1.371(7) .
C7 H7 0.93 .
C8 H8 0.93 .
C9 C10 1.385(5) .
C9 C14 1.381(5) .
C10 C11 1.384(6) .
C10 H10 0.93 .
C11 C12 1.365(7) .
C11 H11 0.93 .
C12 C13 1.355(6) .
C12 H12 0.93 .
C13 C14 1.384(5) .
C13 H13 0.93 .
C14 H14 0.93 .
C15 C16 1.382(5) .
C15 C20 1.382(5) .
C16 C17 1.405(6) .
C16 H16 0.93 .
C17 C18 1.354(7) .
C17 H17 0.93 .
C18 C19 1.365(7) .
C18 H18 0.93 .
C19 C20 1.383(5) .
C19 H19 0.93 .
C20 H20 0.93 .
