#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/13/2001380.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2001380
loop_
_publ_author_name
'Reibenspies, J. H.'
'Fontal, B.'
'Darensbourg, D. J.'
_publ_contact_author
;
Dr. Joseph H. Reibenspies
Department of Chemistry
Texas A \& M University
College Station, Texas 77843
U.S.A.
;
_publ_section_title
;
 Structure of Ru₄(CO)₈(O₂CCH₂CH=CH₂)₄(NMe₃)₂
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1619
_journal_page_last               1621
_journal_paper_doi               10.1107/S0108270193002483
_journal_volume                  49
_journal_year                    1993
_chemical_formula_sum            'C30 H38 N2 O16 Ru4'
_chemical_formula_weight         1086.91
_chemical_name_systematic
;
bis(μ³-butenato)-bis(μ²-butenato)-octacarbonylbis(
trimethylammine)tetraruthenium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.000000
_cell_angle_beta                 97.45(2)
_cell_angle_gamma                90.000000
_cell_formula_units_Z            2.0
_cell_length_a                   7.628(2)
_cell_length_b                   19.526(4)
_cell_length_c                   13.120(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    197
_cell_measurement_theta_max      34.23
_cell_measurement_theta_min      19.89
_cell_volume                     1937.7(8)
_computing_data_collection       'Siemens P3VAX (Siemens, 1990)'
_computing_data_reduction        'REFRED (Reibenspies, 1992)'
_computing_publication_material  SHELXTL-PLUS
_computing_structure_refinement  SHELXTL-PLUS
_computing_structure_solution    'SHELXTL-PLUS. (Sheldrick, 1990)'
_diffrn_ambient_temperature      296
_diffrn_measurement_device       'Siemens R3m diffractometer'
_diffrn_measurement_method       'ω (Wyckoff)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray Tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_av_sigmaI/netI    0.04
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3637
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.568
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072.0
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.7310
_refine_diff_density_min         -0.7900
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.5814
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     248
_refine_ls_number_reflns         2823
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_obs          0.0634
_refine_ls_shift/esd_max         0.0580
_refine_ls_shift/esd_mean        0.0042
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F)+0.00001F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0784
_refine_ls_wR_factor_obs         0.0622
_reflns_number_observed          2823
_reflns_number_total             3637
_reflns_observed_criterion       F>2.0\s(F)
_cod_data_source_file            st1057.cif
_cod_data_source_block           st1057_structure_1_of_1
_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_enum 1527 2010-12-29 10:47:43Z saulius 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(F)+0.00001F^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(F)+0.00001F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 2 1/ c'
_cod_original_formula_sum        'C30 H38 N2 O16 Ru4 '
_cod_database_code               2001380
loop_
_symmetry_equiv_pos_as_xyz
'+x,+y,+z '
'-x,-y,-z '
'-x,1/2+y,1/2-z '
'+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_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_refinement_flags
Ru(1) 0.29180(10) 0.38000(10) 0.77920(10) 0.03540(10) Uani ? ? .
Ru(2) 0.51620(10) 0.41890(10) 0.94060(10) 0.03520(10) Uani ? ? .
C(1) 0.2005(13) 0.3064(6) 0.8445(8) 0.0523(4) Uani ? ? .
O(1) 0.1499(11) 0.2603(4) 0.8839(7) 0.0784(4) Uani ? ? .
C(2) 0.4437(13) 0.3210(5) 0.7288(8) 0.0491(4) Uani ? ? .
O(2) 0.5418(10) 0.2830(4) 0.6972(6) 0.0680(3) Uani ? ? .
C(3) 0.4079(13) 0.3700(6) 1.0336(8) 0.0510(4) Uani ? ? .
O(3) 0.3352(11) 0.3393(4) 1.0907(6) 0.0678(3) Uani ? ? .
C(4) 0.6663(12) 0.3449(5) 0.9317(8) 0.0432(3) Uani ? ? .
O(4) 0.7501(10) 0.2973(4) 0.9255(6) 0.0709(3) Uani ? ? .
O(5) 0.3384(7) 0.5044(3) 0.9442(5) 0.0382(2) Uani ? ? .
O(6) 0.1254(8) 0.4551(3) 0.8355(5) 0.0435(2) Uani ? ? .
C(5) 0.1809(11) 0.5025(5) 0.8963(7) 0.0340(3) Uani ? ? .
C(6) 0.0554(13) 0.5607(5) 0.9079(8) 0.0508(4) Uani ? ? .
C(7) 0.0728(18) 0.6201(7) 0.8400(10) 0.0707(5) Uani ? ? .
C(8) 0.149(2) 0.6266(8) 0.7697(11) 0.0905(7) Uani ? ? .
O(7) 0.6296(7) 0.4805(3) 0.8330(5) 0.0430(2) Uani ? ? .
O(8) 0.4033(8) 0.4647(3) 0.7069(5) 0.0443(2) Uani ? ? .
C(9) 0.5483(12) 0.4929(5) 0.7471(8) 0.0398(3) Uani ? ? .
C(10) 0.6238(14) 0.5460(6) 0.6823(9) 0.0610(4) Uani ? ? .
C(11) 0.5068(19) 0.5822(9) 0.6065(12) 0.1015(7) Uani ? ? .
C(12) 0.4797(19) 0.6406(9) 0.5802(15) 0.1335(9) Uani ? ? .
N(1) 0.0751(10) 0.3780(4) 0.6432(6) 0.0470(3) Uani ? ? .
C(13) 0.060(2) 0.4441(8) 0.5888(10) 0.0559(6) Uani ? ? .
C(14) 0.100(2) 0.3232(9) 0.5716(12) 0.0668(6) Uani ? ? .
C(15) -0.0992(17) 0.3641(10) 0.6830(12) 0.0689(7) Uani ? ? .
C(13') 0.157(7) 0.386(3) 0.535(4) 0.0887(19) Uiso ? ? .
C(14') -0.025(5) 0.313(2) 0.624(3) 0.0455(12) Uiso ? ? .
C(15') -0.051(7) 0.436(3) 0.631(4) 0.0705(16) Uiso ? ? .
H(6A) 0.0746 0.5762 0.9779 0.0800 Uiso calc C(6) RT
H(6B) -0.0633 0.5436 0.8950 0.0800 Uiso calc C(6) RT
H(7A) 0.0091 0.6602 0.8563 0.0800 Uiso calc C(7) RT
H(8A) 0.2164 0.5889 0.7483 0.0800 Uiso calc C(8) RT
H(8B) 0.1461 0.6693 0.7332 0.0800 Uiso calc C(8) RT
H(10A) 0.7117 0.5240 0.6476 0.0800 Uiso calc C(10) RT
H(10B) 0.6839 0.5795 0.7277 0.0800 Uiso calc C(10) RT
H(11A) 0.4291 0.5513 0.5654 0.0800 Uiso calc C(11) RT
H(12A) 0.5486 0.6767 0.6152 0.0800 Uiso calc C(12) RT
H(12B) 0.3892 0.6512 0.5246 0.0800 Uiso calc C(12) RT
H(13A) -0.0321 0.4422 0.5316 0.0800 Uiso calc C(13) RT
H(13B) 0.0336 0.4794 0.6354 0.0800 Uiso calc C(13) RT
H(13C) 0.1706 0.4541 0.5644 0.0800 Uiso calc C(13) RT
H(14A) 0.0065 0.3239 0.5152 0.0800 Uiso calc C(14) RT
H(14B) 0.2115 0.3295 0.5461 0.0800 Uiso calc C(14) RT
H(14C) 0.1001 0.2800 0.6066 0.0800 Uiso calc C(14) RT
H(15A) -0.1932 0.3630 0.6268 0.0800 Uiso calc C(15) RT
H(15B) -0.0917 0.3206 0.7174 0.0800 Uiso calc C(15) RT
H(15C) -0.1226 0.3993 0.7306 0.0800 Uiso calc C(15) RT
H(13D) 0.0650 0.3850 0.4775 0.0800 Uiso calc C(13) RT
H(13E) 0.2209 0.4283 0.5344 0.0800 Uiso calc C(13) RT
H(13F) 0.2369 0.3484 0.5291 0.0800 Uiso calc C(13) RT
H(14D) -0.1128 0.3178 0.5652 0.0800 Uiso calc C(14) RT
H(14E) 0.0564 0.2772 0.6112 0.0800 Uiso calc C(14) RT
H(14F) -0.0817 0.3005 0.6829 0.0800 Uiso calc C(14) RT
H(15D) -0.1384 0.4311 0.5715 0.0800 Uiso calc C(15) RT
H(15E) -0.1091 0.4390 0.6914 0.0800 Uiso calc C(15) RT
H(15F) 0.0160 0.4771 0.6242 0.0800 Uiso calc C(15) RT
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.002 0.002 International_Tables_Vol_IV_Table_2.2B
H 0.000 0.000 International_Tables_Vol_IV_Table_2.2B
N 0.004 0.003 International_Tables_Vol_IV_Table_2.2B
O 0.008 0.006 International_Tables_Vol_IV_Table_2.2B
RU -1.420 0.836 International_Tables_Vol_IV_Table_2.2B
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 0 0
1 0 4
0 2 0
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
Ru(2) Ru(1) C(1) . . . 95.5(3) yes
Ru(2) Ru(1) C(2) . . . 95.5(3) yes
C(1) Ru(1) C(2) . . . 88.4(5) yes
Ru(2) Ru(1) O(6) . . . 83.0(2) yes
C(1) Ru(1) O(6) . . . 95.5(4) yes
C(2) Ru(1) O(6) . . . 175.9(4) yes
Ru(2) Ru(1) O(8) . . . 83.1(2) yes
C(1) Ru(1) O(8) . . . 178.5(3) yes
C(2) Ru(1) O(8) . . . 91.1(4) yes
O(6) Ru(1) O(8) . . . 84.9(3) yes
Ru(2) Ru(1) N(1) . . . 163.8(2) yes
C(1) Ru(1) N(1) . . . 94.1(4) yes
C(2) Ru(1) N(1) . . . 97.9(4) yes
O(6) Ru(1) N(1) . . . 83.0(3) yes
O(8) Ru(1) N(1) . . . 87.4(3) yes
Ru(1) Ru(2) C(3) . . . 94.7(3) yes
Ru(1) Ru(2) C(4) . . . 93.8(3) yes
C(3) Ru(2) C(4) . . . 88.3(5) yes
Ru(1) Ru(2) O(5) . . . 84.10(10) yes
C(3) Ru(2) O(5) . . . 92.9(4) yes
C(4) Ru(2) O(5) . . . 177.6(3) yes
Ru(1) Ru(2) O(7) . . . 84.7(2) yes
C(3) Ru(2) O(7) . . . 176.4(4) yes
C(4) Ru(2) O(7) . . . 95.2(4) yes
O(5) Ru(2) O(7) . . . 83.6(2) yes
Ru(1) Ru(2) O(5) . . 2_667 156.00(10) yes
C(3) Ru(2) O(5) . . 2_667 97.0(4) yes
C(4) Ru(2) O(5) . . 2_667 107.4(3) yes
O(5) Ru(2) O(5) . . 2_667 74.5(2) yes
O(7) Ru(2) O(5) . . 2_667 82.3(2) yes
Ru(1) C(1) O(1) . . . 177.6(10) yes
Ru(1) C(2) O(2) . . . 179.5(10) yes
Ru(2) C(3) O(3) . . . 178.2(9) yes
Ru(2) C(4) O(4) . . . 176.2(9) yes
Ru(2) O(5) C(5) . . . 121.2(6) yes
Ru(2) O(5) Ru(2) . . 2_667 105.5(2) yes
C(5) O(5) Ru(2) . . 2_667 132.9(6) yes
Ru(1) O(6) C(5) . . . 123.9(5) yes
O(5) C(5) O(6) . . . 123.3(8) yes
O(5) C(5) C(6) . . . 119.7(8) yes
O(6) C(5) C(6) . . . 116.9(7) yes
C(5) C(6) C(7) . . . 115.1(9) yes
C(6) C(7) C(8) . . . 131.1(14) yes
Ru(2) O(7) C(9) . . . 121.2(6) yes
Ru(1) O(8) C(9) . . . 121.4(6) yes
O(7) C(9) O(8) . . . 126.3(9) yes
O(7) C(9) C(10) . . . 117.8(8) yes
O(8) C(9) C(10) . . . 115.9(8) yes
C(9) C(10) C(11) . . . 118.8(10) yes
C(10) C(11) C(12) . . . 137.3(15) yes
Ru(1) N(1) C(13) . . . 111.7(7) yes
Ru(1) N(1) C(14) . . . 112.2(7) yes
C(13) N(1) C(14) . . . 109.9(10) yes
Ru(1) N(1) C(15) . . . 108.3(7) yes
C(13) N(1) C(15) . . . 107.9(10) yes
C(14) N(1) C(15) . . . 106.6(11) yes
Ru(1) N(1) C(13') . . . 111.1(19) yes
C(13) N(1) C(13') . . . 61.(2) yes
C(14) N(1) C(13') . . . 54.(2) yes
C(15) N(1) C(13') . . . 140.(2) yes
Ru(1) N(1) C(14') . . . 116.8(15) yes
C(13) N(1) C(14') . . . 131.5(16) yes
C(14) N(1) C(14') . . . 50.9(17) yes
C(15) N(1) C(14') . . . 56.7(18) yes
C(13') N(1) C(14') . . . 100.(3) yes
Ru(1) N(1) C(15') . . . 118.0(19) yes
C(13) N(1) C(15') . . . 43.(2) yes
C(14) N(1) C(15') . . . 129.(2) yes
C(15) N(1) C(15') . . . 66.(2) yes
C(13') N(1) C(15') . . . 99.(3) yes
C(14') N(1) C(15') . . . 109.(3) yes
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(1) Ru(2) . . 2.6550(10) yes
Ru(1) C(1) . . 1.854(12) yes
Ru(1) C(2) . . 1.819(11) yes
Ru(1) O(6) . . 2.133(7) yes
Ru(1) O(8) . . 2.136(7) yes
Ru(1) N(1) . . 2.270(7) yes
Ru(2) C(3) . . 1.829(11) yes
Ru(2) C(4) . . 1.858(10) yes
Ru(2) O(5) . . 2.155(6) yes
Ru(2) O(7) . . 2.122(7) yes
Ru(2) O(5) . 2_667 2.306(6) yes
C(1) O(1) . . 1.131(15) yes
C(2) O(2) . . 1.166(13) yes
C(3) O(3) . . 1.156(14) yes
C(4) O(4) . . 1.137(13) yes
O(5) C(5) . . 1.282(9) yes
O(5) Ru(2) . 2_667 2.306(6) yes
O(6) C(5) . . 1.259(11) yes
C(5) C(6) . . 1.507(13) yes
C(6) C(7) . . 1.479(17) yes
C(7) C(8) . . 1.16(2) yes
O(7) C(9) . . 1.238(11) yes
O(8) C(9) . . 1.286(11) yes
C(9) C(10) . . 1.502(15) yes
C(10) C(11) . . 1.433(18) yes
C(11) C(12) . . 1.20(3) yes
N(1) C(13) . . 1.472(17) yes
N(1) C(14) . . 1.453(18) yes
N(1) C(15) . . 1.515(16) yes
N(1) C(13') . . 1.64(6) yes
N(1) C(14') . . 1.49(4) yes
N(1) C(15') . . 1.48(5) yes
