#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/16/7011631.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_7011631
loop_
_publ_author_name
'Bruce, Michael I.'
'Zaitseva, Natasha N.'
'Skelton, Brian W.'
'White, Allan H.'
_publ_section_title
;
 Synthesis of carbido and related derivatives from calcium carbide and
 ruthenium carbonyl clusters
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3879
_journal_paper_doi               10.1039/b202364b
_journal_year                    2002
_chemical_formula_sum            'C15 H4 O11 Ru4'
_chemical_formula_weight         764.47
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_audit_creation_date             02-02-14
_audit_creation_method           Xtal3.6
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   11.337(2)
_cell_length_b                   13.456(2)
_cell_length_c                   12.805(2)
_cell_measurement_reflns_used    5900
_cell_measurement_temperature    150
_cell_measurement_theta_max      20.4
_cell_measurement_theta_min      2.3
_cell_volume                     1953.4(5)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .051
_diffrn_reflns_av_sigmaI/netI    .024
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14802
_diffrn_reflns_theta_max         31.25
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.09
_exptl_absorpt_correction_T_max  .86
_exptl_absorpt_correction_T_min  .69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick, 1996
;
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    2.599
_exptl_crystal_description       needle
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .08
_refine_diff_density_max         1.384
_refine_diff_density_min         -2.038
_refine_ls_abs_structure_details 'Flack xabs refined'
_refine_ls_abs_structure_Flack   .07(18)
_refine_ls_goodness_of_fit_all   2.04
_refine_ls_goodness_of_fit_ref   1.61
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1592
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .058
_refine_ls_R_factor_gt           .05
_refine_ls_shift/su_max          .01
_refine_ls_shift/su_mean         .002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .139
_refine_ls_wR_factor_ref         .107
_reflns_d_resolution_high        .685
_reflns_d_resolution_low         8.655
_reflns_Friedel_coverage         .922
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                1631
_reflns_number_total             1733
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            b202364b.txt
_cod_data_source_block           br820a
_cod_original_sg_symbol_Hall     c_2c_-2
_cod_original_sg_symbol_H-M      C_m_c_21
_cod_database_code               7011631
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,1/2+z
-x,+y,+z
+x,-y,1/2+z
1/2+x,1/2+y,+z
1/2-x,1/2-y,1/2+z
1/2-x,1/2+y,+z
1/2+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_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 1.16927(7) .26033(7) .50000 .0200(4) Uani ? ? 1.00000 ? ?
Ru2 1.00000 .34390(10) .36288(13) .0185(5) Uani ? ? 1.00000 ? ?
Ru3 1.00000 .11847(10) .54715(14) .0240(7) Uani ? ? 1.00000 ? ?
C11 1.2598(11) .3380(10) .5986(10) .021(5) Uani ? ? 1.00000 ? ?
O11 1.3070(11) .3808(8) .6607(8) .027(5) Uani ? ? 1.00000 ? ?
C12 1.2959(17) .2523(12) .4025(16) .034(8) Uani ? ? 1.00000 ? ?
O12 1.3686(18) .2499(14) .3421(16) .062(11) Uani ? ? 1.00000 ? ?
C13 1.209(3) .1321(13) .5665(17) .052(12) Uani ? ? 1.00000 ? ?
O13 1.2759(14) .0790(11) .6020(15) .054(9) Uani ? ? 1.00000 ? ?
C21 1.00000 .315(2) .2091(18) .031(9) Uani ? ? 1.00000 ? ?
O21 1.00000 .2943(14) .1293(13) .031(7) Uani ? ? 1.00000 ? ?
C22 1.1209(17) .4399(16) .3536(13) .044(9) Uani ? ? 1.00000 ? ?
O22 1.1882(18) .5018(14) .3468(13) .062(9) Uani ? ? 1.00000 ? ?
C31 1.00000 .0736(15) .6840(16) .023(7) Uani ? ? 1.00000 ? ?
O31 1.00000 .041(2) .7627(18) .053(12) Uani ? ? 1.00000 ? ?
C32 1.00000 -.0105(16) .500(2) .037(10) Uani ? ? 1.00000 ? ?
O32 1.00000 -.0974(12) .4810(15) .043(10) Uani ? ? 1.00000 ? ?
C1 1.00000 .3526(16) .5274(15) .025(8) Uani ? ? 1.00000 ? ?
C2 1.00000 .2709(12) .5943(14) .018(7) Uani ? ? 1.00000 ? ?
C3 1.0603(11) .1821(11) .3907(9) .022(5) Uani ? ? 1.00000 ? ?
H1 1.00000 .41533 .55759 .02900 Uiso ? ? 1.00000 ? ?
H2 1.00000 .28730 .66943 .02300 Uiso ? ? 1.00000 ? ?
H3 1.10160 .14569 .33793 .03700 Uiso ? ? 1.00000 ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 60 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 16 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 44 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Ru ? 0 16 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
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
Ru2 Ru1 Ru3 . . . 86.53(4) ?
Ru2 Ru1 C11 . . . 123.4(4) ?
Ru2 Ru1 C12 . . . 97.3(6) ?
Ru2 Ru1 C13 . . . 140.1(8) ?
Ru2 Ru1 C1 . . . 47.1(5) ?
Ru2 Ru1 C2 . . . 74.5(4) ?
Ru2 Ru1 C3 . . . 53.1(4) ?
Ru3 Ru1 C11 . . . 126.6(4) ?
Ru3 Ru1 C12 . . . 128.7(5) ?
Ru3 Ru1 C13 . . . 57.4(9) ?
Ru3 Ru1 C1 . . . 76.3(4) ?
Ru3 Ru1 C2 . . . 48.9(4) ?
Ru3 Ru1 C3 . . . 53.5(3) ?
C11 Ru1 C12 . . . 93.4(7) ?
C11 Ru1 C13 . . . 94.0(8) ?
C11 Ru1 C1 . . . 92.9(6) ?
C11 Ru1 C2 . . . 93.9(5) ?
C11 Ru1 C3 . . . 176.2(5) ?
C12 Ru1 C13 . . . 93.6(10) ?
C12 Ru1 C1 . . . 139.0(7) ?
C12 Ru1 C2 . . . 171.2(7) ?
C12 Ru1 C3 . . . 88.8(6) ?
C13 Ru1 C1 . . . 126.3(10) ?
C13 Ru1 C2 . . . 91.0(9) ?
C13 Ru1 C3 . . . 89.0(8) ?
C1 Ru1 C2 . . . 35.4(6) ?
C1 Ru1 C3 . . . 83.4(6) ?
C2 Ru1 C3 . . . 83.7(5) ?
Ru1 Ru2 C21 . . . 122.0(4) ?
Ru1 Ru2 C22 . . . 79.6(6) ?
Ru1 Ru2 C1 . . . 53.4(3) ?
Ru1 Ru2 C3 . . . 47.9(3) ?
Ru1 Ru2 Ru1 . . 3 85.25(5) ?
Ru1 Ru2 C22 . . 3 143.4(5) ?
Ru1 Ru2 C3 . . 3 74.4(3) ?
C21 Ru2 C22 . . . 94.1(7) ?
C21 Ru2 C1 . . . 171.9(9) ?
C21 Ru2 C3 . . . 88.2(8) ?
C21 Ru2 Ru1 . . 3 122.0(4) ?
C21 Ru2 C22 . . 3 94.1(7) ?
C21 Ru2 C3 . . 3 88.2(8) ?
C22 Ru2 C1 . . . 91.4(6) ?
C22 Ru2 C3 . . . 116.1(7) ?
C22 Ru2 Ru1 . . 3 143.4(5) ?
C22 Ru2 C22 . . 3 93.1(9) ?
C22 Ru2 C3 . . 3 150.5(7) ?
C1 Ru2 C3 . . . 84.2(6) ?
C1 Ru2 Ru1 . . 3 53.4(3) ?
C1 Ru2 C22 . . 3 91.4(6) ?
C1 Ru2 C3 . . 3 84.2(6) ?
C3 Ru2 Ru1 . . 3 74.4(3) ?
C3 Ru2 C22 . . 3 150.5(7) ?
C3 Ru2 C3 . . 3 34.4(4) ?
Ru1 Ru2 C22 3 . 3 79.6(6) ?
Ru1 Ru2 C3 3 . 3 47.9(3) ?
C22 Ru2 C3 3 . 3 116.1(7) ?
Ru1 Ru3 C13 . . . 44.2(4) ?
Ru1 Ru3 C31 . . . 115.5(4) ?
Ru1 Ru3 C32 . . . 125.5(4) ?
Ru1 Ru3 C2 . . . 53.2(2) ?
Ru1 Ru3 C3 . . . 49.0(3) ?
Ru1 Ru3 Ru1 . . 3 87.57(5) ?
Ru1 Ru3 C13 . . 3 131.0(4) ?
Ru1 Ru3 C3 . . 3 76.0(3) ?
C13 Ru3 C31 . . . 85.8(5) ?
C13 Ru3 C32 . . . 96.1(4) ?
C13 Ru3 C2 . . . 84.1(4) ?
C13 Ru3 C3 . . . 76.4(6) ?
C13 Ru3 Ru1 . . 3 131.0(4) ?
C13 Ru3 C13 . . 3 165.2(7) ?
C13 Ru3 C3 . . 3 111.0(6) ?
C31 Ru3 C32 . . . 90.0(10) ?
C31 Ru3 C2 . . . 92.6(8) ?
C31 Ru3 C3 . . . 162.1(3) ?
C31 Ru3 Ru1 . . 3 115.5(4) ?
C31 Ru3 C13 . . 3 85.8(5) ?
C31 Ru3 C3 . . 3 162.1(3) ?
C32 Ru3 C2 . . . 177.4(10) ?
C32 Ru3 C3 . . . 94.0(9) ?
C32 Ru3 Ru1 . . 3 125.5(4) ?
C32 Ru3 C13 . . 3 96.1(4) ?
C32 Ru3 C3 . . 3 94.0(9) ?
C2 Ru3 C3 . . . 83.6(6) ?
C2 Ru3 Ru1 . . 3 53.2(2) ?
C2 Ru3 C13 . . 3 84.1(4) ?
C2 Ru3 C3 . . 3 83.6(6) ?
C3 Ru3 Ru1 . . 3 76.0(3) ?
C3 Ru3 C13 . . 3 111.0(6) ?
C3 Ru3 C3 . . 3 34.8(4) ?
Ru1 Ru3 C13 3 . 3 44.2(4) ?
Ru1 Ru3 C3 3 . 3 49.0(3) ?
C13 Ru3 C3 3 . 3 76.4(6) ?
Ru1 C11 O11 . . . 175.3(12) ?
Ru1 C12 O12 . . . 177.4(18) ?
Ru1 C13 Ru3 . . . 78.3(10) ?
Ru1 C13 O13 . . . 151(2) ?
Ru3 C13 O13 . . . 131.0(18) ?
Ru2 C21 O21 . . . 176(2) ?
Ru2 C22 O22 . . . 176(2) ?
Ru3 C31 O31 . . . 175(2) ?
Ru3 C32 O32 . . . 173(2) ?
Ru1 C1 Ru2 . . . 79.6(5) ?
Ru1 C1 C2 . . . 70.7(7) ?
Ru1 C1 H1 . . . 123.5 ?
Ru1 C1 Ru1 . . 3 112.2(9) ?
Ru2 C1 C2 . . . 124.8(14) ?
Ru2 C1 H1 . . . 117.8 ?
Ru2 C1 Ru1 . . 3 79.6(5) ?
C2 C1 H1 . . . 117.4 ?
C2 C1 Ru1 . . 3 70.7(7) ?
H1 C1 Ru1 . . 3 123.5(4) ?
Ru1 C2 Ru3 . . . 77.9(5) ?
Ru1 C2 C1 . . . 73.9(7) ?
Ru1 C2 H2 . . . 122.2 ?
Ru1 C2 Ru1 . . 3 115.3(8) ?
Ru3 C2 C1 . . . 125.6(14) ?
Ru3 C2 H2 . . . 119.4 ?
Ru3 C2 Ru1 . . 3 77.9(5) ?
C1 C2 H2 . . . 115.0 ?
C1 C2 Ru1 . . 3 73.9(7) ?
H2 C2 Ru1 . . 3 122.2 ?
Ru1 C3 Ru2 . . . 79.0(5) ?
Ru1 C3 Ru3 . . . 77.5(4) ?
Ru1 C3 H3 . . . 115.5 ?
Ru1 C3 C3 . . 3 125.2(9) ?
Ru2 C3 Ru3 . . . 113.6(5) ?
Ru2 C3 H3 . . . 121.2 ?
Ru2 C3 C3 . . 3 72.8(8) ?
Ru3 C3 H3 . . . 125.0 ?
Ru3 C3 C3 . . 3 72.6 ?
H3 C3 C3 . . 3 119.3 ?
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
Ru1 Ru2 . . 2.8338(14) ?
Ru1 Ru3 . . 2.7732(14) ?
Ru1 C11 . . 1.934(13) ?
Ru1 C12 . . 1.91(2) ?
Ru1 C13 . . 1.98(2) ?
Ru1 C1 . . 2.312(12) ?
Ru1 C2 . . 2.272(10) ?
Ru1 C3 . . 2.143(12) ?
Ru2 C21 . . 2.01(2) ?
Ru2 C22 . . 1.89(2) ?
Ru2 C1 . . 2.11(2) ?
Ru2 C3 . . 2.310(15) ?
Ru2 C22 . 3 1.89(2) ?
Ru2 C3 . 3 2.310(15) ?
Ru3 C13 . . 2.39(3) ?
Ru3 C31 . . 1.85(2) ?
Ru3 C32 . . 1.84(2) ?
Ru3 C2 . . 2.138(16) ?
Ru3 C3 . . 2.283(12) ?
Ru3 C13 . 3 2.39(3) ?
Ru3 C3 . 3 2.283(12) ?
C11 O11 . . 1.118(17) ?
C12 O12 . . 1.13(3) ?
C13 O13 . . 1.14(3) ?
C21 O21 . . 1.06(3) ?
C22 O22 . . 1.13(3) ?
C31 O31 . . 1.10(3) ?
C32 O32 . . 1.19(3) ?
C1 C2 . . 1.39(3) ?
C1 H1 . . .93 ?
C2 H2 . . .986 ?
C3 H3 . . .957 ?
C3 C3 . 3 1.366(17) ?
