#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:08:49 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178618 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/29/4072997.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_4072997
loop_
_publ_author_name
'Caskey, Stephen R.'
'Stewart, Michael H.'
'Ahn, Yi Joon'
'Johnson, Marc J. A.'
'Rowsell, Jesse L. C.'
'Kampf, Jeff W.'
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Four-, Five-, and Six-Coordinate
 Ruthenium Carbyne Complexes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1912
_journal_paper_doi               10.1021/om061192v
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C44 H72 F3 P2 Ru, C H2 Cl2'
_chemical_formula_sum            'C45 H74 Cl2 F3 P2 Ru'
_chemical_formula_weight         905.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_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                 113.372(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5265(18)
_cell_length_b                   23.609(5)
_cell_length_c                   11.124(2)
_cell_measurement_reflns_used    3923
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      22.18
_cell_measurement_theta_min      2.17
_cell_volume                     2296.6(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART 1K CCD'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1525
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            28679
_diffrn_reflns_theta_full        22.64
_diffrn_reflns_theta_max         22.64
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.9667
_exptl_absorpt_correction_T_min  0.9453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2.10) Bruker/Siemens area
  detector absorption and other corrections, University of
  Gottingen, Germany 2003.
;
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3141
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0305P)²+6.1243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                2171
_reflns_number_total             3141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061192vsi20061231_072132.cif
_cod_data_source_block           sc1527
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/m
_cod_database_code               4072997
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ru1 Ru 0.64172(8) 0.2500 0.83394(8) 0.0231(2) Uani 1 2 d S
P1 P 0.63066(18) 0.14661(6) 0.82229(16) 0.0237(4) Uani 1 1 d .
F1 F 0.4112(5) 0.2500 0.7064(5) 0.0354(13) Uani 1 2 d S
F2 F 0.5646(5) 0.2500 0.9755(5) 0.0334(12) Uani 1 2 d S
F3 F 0.6687(5) 0.2500 0.6656(4) 0.0274(11) Uani 1 2 d S
C1 C 0.8298(10) 0.2500 0.9374(8) 0.024(2) Uani 1 2 d S
C2 C 0.9875(9) 0.2500 1.0239(9) 0.026(2) Uani 1 2 d S
C3 C 1.0323(9) 0.2500 1.1601(9) 0.029(2) Uani 1 2 d S
H3A H 0.9568 0.2500 1.1959 0.034 Uiso 1 2 calc SR
C4 C 1.1825(10) 0.2500 1.2413(9) 0.035(2) Uani 1 2 d S
H4A H 1.2110 0.2500 1.3334 0.042 Uiso 1 2 calc SR
C5 C 1.2979(9) 0.2500 1.1906(10) 0.033(2) Uani 1 2 d S
C6 C 1.2546(10) 0.2500 1.0563(10) 0.035(2) Uani 1 2 d S
H6A H 1.3304 0.2500 1.0209 0.042 Uiso 1 2 calc SR
C7 C 1.1022(9) 0.2500 0.9738(9) 0.031(2) Uani 1 2 d S
H7A H 1.0738 0.2500 0.8817 0.037 Uiso 1 2 calc SR
C8 C 1.4660(10) 0.2500 1.2839(9) 0.042(3) Uani 1 2 d S
H8A H 1.5299 0.2500 1.2333 0.063 Uiso 1 2 calc SR
H8B H 1.4881 0.2161 1.3393 0.063 Uiso 0.00 1 calc PR
H8C H 1.4881 0.2839 1.3393 0.063 Uiso 0.50 1 calc PR
C9 C 0.4653(6) 0.1223(2) 0.6766(5) 0.0247(14) Uani 1 1 d .
H9A H 0.3754 0.1432 0.6794 0.030 Uiso 1 1 calc R
C10 C 0.4730(7) 0.1395(3) 0.5462(6) 0.0347(16) Uani 1 1 d .
H10A H 0.4971 0.1804 0.5483 0.042 Uiso 1 1 calc R
H10B H 0.5558 0.1182 0.5340 0.042 Uiso 1 1 calc R
C11 C 0.3212(8) 0.1276(3) 0.4319(7) 0.0438(18) Uani 1 1 d .
H11A H 0.2404 0.1515 0.4405 0.053 Uiso 1 1 calc R
H11B H 0.3300 0.1378 0.3488 0.053 Uiso 1 1 calc R
C12 C 0.2753(8) 0.0656(3) 0.4270(6) 0.0411(17) Uani 1 1 d .
H12A H 0.1736 0.0600 0.3553 0.049 Uiso 1 1 calc R
H12B H 0.3499 0.0418 0.4084 0.049 Uiso 1 1 calc R
C13 C 0.2699(7) 0.0477(3) 0.5546(6) 0.0404(17) Uani 1 1 d .
H13A H 0.2458 0.0068 0.5507 0.048 Uiso 1 1 calc R
H13B H 0.1870 0.0686 0.5677 0.048 Uiso 1 1 calc R
C14 C 0.4220(7) 0.0589(2) 0.6717(6) 0.0344(16) Uani 1 1 d .
H14A H 0.5037 0.0354 0.6633 0.041 Uiso 1 1 calc R
H14B H 0.4120 0.0482 0.7540 0.041 Uiso 1 1 calc R
C15 C 0.8136(6) 0.1167(2) 0.8293(6) 0.0242(14) Uani 1 1 d .
H39A H 0.8918 0.1285 0.9165 0.029 Uiso 1 1 calc R
C16 C 0.8240(6) 0.0521(2) 0.8274(6) 0.0308(15) Uani 1 1 d .
H16A H 0.7551 0.0377 0.7403 0.037 Uiso 1 1 calc R
H16B H 0.7900 0.0359 0.8935 0.037 Uiso 1 1 calc R
C17 C 0.9896(7) 0.0328(2) 0.8573(6) 0.0354(16) Uani 1 1 d .
H17A H 1.0574 0.0445 0.9471 0.042 Uiso 1 1 calc R
H17B H 0.9931 -0.0090 0.8525 0.042 Uiso 1 1 calc R
C18 C 1.0454(7) 0.0585(2) 0.7605(7) 0.0345(17) Uani 1 1 d .
H18A H 0.9844 0.0433 0.6721 0.041 Uiso 1 1 calc R
H18B H 1.1534 0.0476 0.7841 0.041 Uiso 1 1 calc R
C19 C 1.0328(7) 0.1230(3) 0.7575(7) 0.0360(16) Uani 1 1 d .
H19A H 1.1023 0.1385 0.8431 0.043 Uiso 1 1 calc R
H19B H 1.0649 0.1382 0.6894 0.043 Uiso 1 1 calc R
C20 C 0.8693(6) 0.1416(2) 0.7285(6) 0.0318(16) Uani 1 1 d .
H20A H 0.8011 0.1289 0.6396 0.038 Uiso 1 1 calc R
H20B H 0.8648 0.1835 0.7307 0.038 Uiso 1 1 calc R
C21 C 0.6044(6) 0.1101(2) 0.9577(6) 0.0265(15) Uani 1 1 d .
H21A H 0.6008 0.0687 0.9385 0.032 Uiso 1 1 calc R
C22 C 0.4525(6) 0.1251(3) 0.9670(6) 0.0324(16) Uani 1 1 d .
H22A H 0.3675 0.1189 0.8808 0.039 Uiso 1 1 calc R
H22B H 0.4529 0.1656 0.9898 0.039 Uiso 1 1 calc R
C23 C 0.4265(7) 0.0889(3) 1.0706(6) 0.0356(16) Uani 1 1 d .
H23A H 0.3306 0.1009 1.0779 0.043 Uiso 1 1 calc R
H23B H 0.4151 0.0487 1.0430 0.043 Uiso 1 1 calc R
C24 C 0.5585(7) 0.0945(3) 1.2031(6) 0.0400(18) Uani 1 1 d .
H24A H 0.5429 0.0680 1.2658 0.048 Uiso 1 1 calc R
H24B H 0.5604 0.1335 1.2366 0.048 Uiso 1 1 calc R
C25 C 0.7132(7) 0.0815(3) 1.1947(6) 0.0365(16) Uani 1 1 d .
H25A H 0.7973 0.0880 1.2812 0.044 Uiso 1 1 calc R
H25B H 0.7160 0.0413 1.1708 0.044 Uiso 1 1 calc R
C26 C 0.7355(6) 0.1190(3) 1.0934(6) 0.0322(16) Uani 1 1 d .
H26A H 0.8345 0.1100 1.0883 0.039 Uiso 1 1 calc R
H26B H 0.7382 0.1592 1.1197 0.039 Uiso 1 1 calc R
Cl1 Cl 0.8816(2) 0.18870(8) 0.41634(19) 0.0634(6) Uani 1 1 d .
C45 C 0.8829(11) 0.2500 0.5051(9) 0.045(3) Uani 1 2 d S
H45A H 0.9752 0.2500 0.5880 0.054 Uiso 1 2 calc SR
H45B H 0.7921 0.2500 0.5274 0.04(3) Uiso 1 2 calc SR
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'
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'
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_3
C1 Ru1 F2 94.9(3) .
C1 Ru1 F3 98.2(3) .
F2 Ru1 F3 166.95(19) .
C1 Ru1 F1 179.8(3) .
F2 Ru1 F1 85.32(19) .
F3 Ru1 F1 81.62(18) .
C1 Ru1 P1 92.72(4) .
F2 Ru1 P1 91.16(4) .
F3 Ru1 P1 88.23(5) .
F1 Ru1 P1 87.27(4) .
C1 Ru1 P1 92.72(4) 4_565
F2 Ru1 P1 91.16(4) 4_565
F3 Ru1 P1 88.23(5) 4_565
F1 Ru1 P1 87.27(4) 4_565
P1 Ru1 P1 173.88(9) 4_565
C21 P1 C9 103.1(3) .
C21 P1 C15 102.7(3) .
C9 P1 C15 112.3(3) .
C21 P1 Ru1 116.21(19) .
C9 P1 Ru1 111.17(19) .
C15 P1 Ru1 110.97(18) .
C2 C1 Ru1 179.9(7) .
C3 C2 C7 118.4(8) .
C3 C2 C1 121.1(7) .
C7 C2 C1 120.4(8) .
C4 C3 C2 120.5(8) .
C3 C4 C5 121.0(9) .
C6 C5 C4 118.8(8) .
C6 C5 C8 121.2(8) .
C4 C5 C8 120.0(9) .
C7 C6 C5 120.3(8) .
C6 C7 C2 120.9(9) .
C10 C9 C14 109.6(5) .
C10 C9 P1 113.7(4) .
C14 C9 P1 117.1(4) .
C11 C10 C9 110.7(5) .
C12 C11 C10 111.8(5) .
C13 C12 C11 110.7(5) .
C12 C13 C14 112.2(5) .
C13 C14 C9 110.1(5) .
C16 C15 C20 109.2(5) .
C16 C15 P1 116.4(4) .
C20 C15 P1 114.6(4) .
C15 C16 C17 110.9(5) .
C18 C17 C16 110.3(5) .
C17 C18 C19 111.8(5) .
C20 C19 C18 111.0(5) .
C19 C20 C15 110.8(5) .
C22 C21 C26 108.8(5) .
C22 C21 P1 112.8(4) .
C26 C21 P1 114.6(4) .
C21 C22 C23 111.1(5) .
C24 C23 C22 111.3(5) .
C23 C24 C25 111.5(5) .
C26 C25 C24 110.4(5) .
C25 C26 C21 110.5(5) .
Cl1 C45 Cl1 111.7(5) 4_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 C1 1.703(9) .
Ru1 F2 1.985(4) .
Ru1 F3 1.989(4) .
Ru1 F1 2.089(4) .
Ru1 P1 2.4443(14) .
Ru1 P1 2.4444(14) 4_565
P1 C21 1.837(6) .
P1 C9 1.848(6) .
P1 C15 1.853(5) .
C1 C2 1.426(11) .
C2 C3 1.402(11) .
C2 C7 1.411(11) .
C3 C4 1.356(11) .
C4 C5 1.420(12) .
C5 C6 1.384(12) .
C5 C8 1.524(11) .
C6 C7 1.376(11) .
C9 C10 1.536(8) .
C9 C14 1.546(7) .
C10 C11 1.526(8) .
C11 C12 1.521(8) .
C12 C13 1.501(9) .
C13 C14 1.538(8) .
C15 C16 1.530(7) .
C15 C20 1.535(7) .
C16 C17 1.547(7) .
C17 C18 1.504(8) .
C18 C19 1.526(8) .
C19 C20 1.525(7) .
C21 C22 1.532(7) .
C21 C26 1.545(8) .
C22 C23 1.532(8) .
C23 C24 1.517(9) .
C24 C25 1.544(8) .
C25 C26 1.513(8) .
Cl1 C45 1.749(5) .
C45 Cl1 1.749(5) 4_565
