#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:25:53 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180078 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/24/7052427.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_7052427
loop_
_publ_author_name
'Clarke, Lionel P.'
'Cole, Jacqueline M.'
'Davies, John E.'
'French, Alexandra'
'Koentjoro, Olivia F.'
'Raithby, Paul R.'
'Shields, Gregory P.'
_publ_section_title
;
 Molecular rearrangements of diynes coordinated to triosmium carbonyl
 clusters: reactions of [Os3(�-H)2(CO)10] and [Os3(CO)10(MeCN)2]
 with 1,4-dipyridylbuta-1,3-diyne
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              145
_journal_paper_doi               10.1039/b412578a
_journal_volume                  29
_journal_year                    2005
_chemical_formula_moiety         'C34 H8 N2 O20 Os6, 2(C H2 Cl2)'
_chemical_formula_sum            'C36 H12 Cl4 N2 O20 Os6'
_chemical_formula_weight         2075.48
_chemical_name_systematic        'Compound 6 . 2 dichloromethane'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                104.69(3)
_cell_angle_beta                 103.26(3)
_cell_angle_gamma                85.71(3)
_cell_formula_units_Z            1
_cell_length_a                   11.258(2)
_cell_length_b                   12.994(3)
_cell_length_c                   8.381(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     1154.2(5)
_computing_molecular_graphics    'SHELXTL-PLUS (Siemens, 1991)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-PLUS (Siemens, 1991)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Rigaku AFC5R four-circle diffractometer'
_diffrn_measurement_method       'ω/2θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0833
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7402
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        -0.3
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    16.759
_exptl_absorpt_correction_T_max  0.040
_exptl_absorpt_correction_T_min  0.026
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.986
_exptl_crystal_description       block
_exptl_crystal_F_000             926
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.918
_refine_diff_density_min         -2.198
_refine_diff_density_rms         0.358
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.549
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_obs          0.0379
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w==1/[σ²(Fo²)+(0.0407P)²+0.0000P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1484
_refine_ls_wR_factor_obs         0.0882
_reflns_number_observed          3942
_reflns_number_total             5297
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            b412578a.txt
_cod_data_source_block           pr9707
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_refine_ls_weighting_scheme' value 'calc
w==1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
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^(Fo^2^)+(0.0407P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1154.2(4)
_cod_database_code               7052427
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Os1 Os 0.28836(4) 0.17766(3) -0.15713(5) 0.01483(10) Uani 1 d . .
Os2 Os 0.28744(4) 0.36622(3) 0.09769(5) 0.01413(10) Uani 1 d . .
Os3 Os 0.21900(4) 0.37492(3) -0.23597(5) 0.01479(10) Uani 1 d . .
N1 N 0.0987(8) 0.1704(7) -0.1491(11) 0.017(2) Uani 1 d . .
C1 C 0.2694(10) 0.0909(10) -0.3823(14) 0.022(2) Uani 1 d . .
O1 O 0.2621(8) 0.0397(7) -0.5156(11) 0.034(2) Uani 1 d . .
O2 O 0.3567(8) -0.0067(7) 0.0141(11) 0.032(2) Uani 1 d . .
C2 C 0.3313(10) 0.0620(9) -0.0508(14) 0.020(2) Uani 1 d . .
O3 O 0.5536(7) 0.2138(7) -0.1495(11) 0.031(2) Uani 1 d . .
C3 C 0.4540(11) 0.2015(8) -0.1493(14) 0.022(2) Uani 1 d . .
O4 O 0.2359(8) 0.1880(7) 0.2514(10) 0.029(2) Uani 1 d . .
C4 C 0.2583(9) 0.2511(9) 0.1891(14) 0.018(2) Uani 1 d . .
O5 O 0.5604(7) 0.3673(8) 0.2681(12) 0.037(2) Uani 1 d . .
C5 C 0.4600(11) 0.3643(9) 0.2006(14) 0.023(2) Uani 1 d . .
C6 C 0.2457(11) 0.4767(9) 0.2726(13) 0.024(2) Uani 1 d . .
O6 O 0.2170(9) 0.5446(8) 0.3774(12) 0.045(3) Uani 1 d . .
C7 C 0.3219(10) 0.4849(9) -0.0156(13) 0.022(2) Uani 1 d . .
O7 O 0.3711(9) 0.5653(7) 0.0160(11) 0.037(2) Uani 1 d . .
O8 O 0.4304(7) 0.3764(7) -0.4114(11) 0.033(2) Uani 1 d . .
C8 C 0.3519(10) 0.3767(9) -0.3490(14) 0.023(2) Uani 1 d . .
C9 C 0.1366(10) 0.5007(10) -0.2904(15) 0.026(3) Uani 1 d . .
O9 O 0.0820(9) 0.5728(8) -0.3253(12) 0.042(2) Uani 1 d . .
O10 O 0.0581(7) 0.2278(7) -0.5358(11) 0.033(2) Uani 1 d . .
C10 C 0.1210(10) 0.2805(9) -0.4222(13) 0.020(2) Uani 1 d . .
C11 C 0.0431(10) 0.0785(9) -0.1818(15) 0.024(2) Uani 1 d . .
H11 H 0.0849(10) 0.0146(9) -0.2235(15) 0.029 Uiso 1 calc R .
C12 C -0.0724(10) 0.0722(9) -0.1578(14) 0.024(2) Uani 1 d . .
H12 H -0.1071(10) 0.0045(9) -0.1764(14) 0.028 Uiso 1 calc R .
C13 C -0.1394(11) 0.1646(11) -0.1061(16) 0.033(3) Uani 1 d . .
H13 H -0.2205(11) 0.1616(11) -0.0926(16) 0.040 Uiso 1 calc R .
C14 C -0.0834(10) 0.2597(9) -0.0758(15) 0.025(2) Uani 1 d . .
H14 H -0.1264(10) 0.3238(9) -0.0388(15) 0.030 Uiso 1 calc R .
C15 C 0.0366(9) 0.2655(8) -0.0978(13) 0.016(2) Uani 1 d . .
C16 C 0.1013(9) 0.3652(8) -0.0646(12) 0.014(2) Uani 1 d . .
C17 C 0.0274(9) 0.4597(8) -0.0195(13) 0.017(2) Uani 1 d . .
C18 C -0.3423(12) 0.2002(11) -0.4995(18) 0.038(3) Uani 1 d . .
H18A H -0.3123(12) 0.1736(11) -0.3964(18) 0.045 Uiso 1 calc R .
H18B H -0.3642(12) 0.2765(11) -0.4639(18) 0.045 Uiso 1 calc R .
Cl1 Cl -0.4722(3) 0.1304(3) -0.6212(5) 0.0430(8) Uani 1 d . .
Cl2 Cl -0.2246(4) 0.1863(3) -0.6126(7) 0.0631(13) Uani 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 0.0000 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 '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'
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
_geom_angle_publ_flag
C3 Os1 C1 90.9(5) . . ?
C3 Os1 C2 92.2(5) . . ?
C1 Os1 C2 95.0(5) . . ?
C3 Os1 N1 173.0(4) . . ?
C1 Os1 N1 94.6(4) . . ?
C2 Os1 N1 91.6(4) . . ?
C3 Os1 Os2 88.9(3) . . ?
C1 Os1 Os2 156.9(3) . . ?
C2 Os1 Os2 108.1(3) . . ?
N1 Os1 Os2 84.3(2) . . ?
C3 Os1 Os3 90.7(3) . . ?
C1 Os1 Os3 98.4(3) . . ?
C2 Os1 Os3 166.3(3) . . ?
N1 Os1 Os3 84.3(2) . . ?
Os2 Os1 Os3 58.56(2) . . ?
C6 Os2 C4 96.0(5) . . ?
C6 Os2 C5 95.3(5) . . ?
C4 Os2 C5 91.5(4) . . ?
C6 Os2 C7 87.6(4) . . ?
C4 Os2 C7 176.4(4) . . ?
C5 Os2 C7 88.3(4) . . ?
C6 Os2 C16 92.7(4) . . ?
C4 Os2 C16 94.6(4) . . ?
C5 Os2 C16 169.3(4) . . ?
C7 Os2 C16 85.0(4) . . ?
C6 Os2 Os3 121.6(4) . . ?
C4 Os2 Os3 126.2(3) . . ?
C5 Os2 Os3 118.4(3) . . ?
C7 Os2 Os3 51.0(3) . . ?
C16 Os2 Os3 51.1(2) . . ?
C6 Os2 Os1 163.8(3) . . ?
C4 Os2 Os1 72.9(3) . . ?
C5 Os2 Os1 96.8(3) . . ?
C7 Os2 Os1 103.5(3) . . ?
C16 Os2 Os1 76.8(2) . . ?
Os3 Os2 Os1 60.79(3) . . ?
C10 Os3 C9 94.1(5) . . ?
C10 Os3 C8 95.1(5) . . ?
C9 Os3 C8 95.9(4) . . ?
C10 Os3 C7 176.6(4) . . ?
C9 Os3 C7 84.9(5) . . ?
C8 Os3 C7 88.2(4) . . ?
C10 Os3 C16 92.9(4) . . ?
C9 Os3 C16 93.1(4) . . ?
C8 Os3 C16 167.5(4) . . ?
C7 Os3 C16 84.0(4) . . ?
C10 Os3 Os2 129.6(3) . . ?
C9 Os3 Os2 119.0(3) . . ?
C8 Os3 Os2 115.9(3) . . ?
C7 Os3 Os2 48.9(3) . . ?
C16 Os3 Os2 51.8(3) . . ?
C10 Os3 Os1 78.9(3) . . ?
C9 Os3 Os1 167.5(3) . . ?
C8 Os3 Os1 95.0(3) . . ?
C7 Os3 Os1 101.5(3) . . ?
C16 Os3 Os1 77.1(3) . . ?
Os2 Os3 Os1 60.65(3) . . ?
C11 N1 C15 119.7(9) . . ?
C11 N1 Os1 121.9(7) . . ?
C15 N1 Os1 118.3(7) . . ?
O1 C1 Os1 177.8(10) . . ?
O2 C2 Os1 179.4(9) . . ?
O3 C3 Os1 177.9(10) . . ?
O4 C4 Os2 174.7(10) . . ?
O5 C5 Os2 176.4(10) . . ?
O6 C6 Os2 178.2(11) . . ?
O7 C7 Os2 141.6(9) . . ?
O7 C7 Os3 138.3(9) . . ?
Os2 C7 Os3 80.1(4) . . ?
O8 C8 Os3 178.2(10) . . ?
O9 C9 Os3 176.5(11) . . ?
O10 C10 Os3 176.5(10) . . ?
N1 C11 C12 122.5(11) . . ?
C11 C12 C13 120.4(11) . . ?
C14 C13 C12 117.2(11) . . ?
C13 C14 C15 122.0(11) . . ?
N1 C15 C14 118.0(10) . . ?
N1 C15 C16 117.9(8) . . ?
C14 C15 C16 124.1(9) . . ?
C17 C16 C15 113.8(8) . . ?
C17 C16 Os3 114.7(7) . . ?
C15 C16 Os3 117.4(7) . . ?
C17 C16 Os2 115.2(7) . . ?
C15 C16 Os2 113.9(7) . . ?
Os3 C16 Os2 77.1(3) . . ?
C17 C17 C16 176.4(15) 2_565 . ?
Cl1 C18 Cl2 111.8(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C3 1.896(12) . ?
Os1 C1 1.911(11) . ?
Os1 C2 1.912(11) . ?
Os1 N1 2.161(8) . ?
Os1 Os2 2.8137(12) . ?
Os1 Os3 2.8176(9) . ?
Os2 C6 1.892(11) . ?
Os2 C4 1.924(11) . ?
Os2 C5 1.937(13) . ?
Os2 C7 2.105(11) . ?
Os2 C16 2.220(10) . ?
Os2 Os3 2.7541(9) . ?
Os3 C10 1.897(11) . ?
Os3 C9 1.923(11) . ?
Os3 C8 1.951(11) . ?
Os3 C7 2.173(11) . ?
Os3 C16 2.197(9) . ?
N1 C11 1.328(14) . ?
N1 C15 1.392(12) . ?
C1 O1 1.134(13) . ?
O2 C2 1.145(13) . ?
O3 C3 1.145(13) . ?
O4 C4 1.147(13) . ?
O5 C5 1.141(14) . ?
C6 O6 1.161(13) . ?
C7 O7 1.160(13) . ?
O8 C8 1.124(13) . ?
C9 O9 1.145(14) . ?
O10 C10 1.144(13) . ?
C11 C12 1.37(2) . ?
C12 C13 1.40(2) . ?
C13 C14 1.37(2) . ?
C14 C15 1.414(14) . ?
C15 C16 1.467(14) . ?
C16 C17 1.448(13) . ?
C17 C17 1.19(2) 2_565 ?
C18 Cl1 1.745(13) . ?
C18 Cl2 1.772(14) . ?
