#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:17:09 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180070 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/16/7051682.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_7051682
loop_
_publ_author_name
'Kizas, Ol'ga A.'
'Erdyakov, Sergey Yu.'
'Antonov, Dmitrii Yu.'
'Godovikov, Ivan A.'
'Vorontsov, Evgenii V.'
'Dolgushin, Fedor M.'
'Ezernitskaya, Mariam G.'
'Barakovskaya, Irina G.'
_publ_section_title
;
 Reactions of H2Os3(CO)10 with triallylboranes: formation of novel
 triosmium boron-containing olefin clusters
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1760
_journal_paper_doi               10.1039/b822277k
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety         'C19 H17 B O10 Os3'
_chemical_formula_sum            'C19 H17 B O10 Os3'
_chemical_formula_weight         986.74
_chemical_name_systematic
;
?
;
_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'
_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                 114.8310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5816(7)
_cell_length_b                   28.057(2)
_cell_length_c                   9.7448(7)
_cell_measurement_reflns_used    6191
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.3
_cell_volume                     2377.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18626
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    16.044
_exptl_absorpt_correction_T_max  0.265
_exptl_absorpt_correction_T_min  0.127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.195
_refine_diff_density_min         -3.315
_refine_diff_density_rms         0.360
_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     301
_refine_ls_number_reflns         6820
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0360P)²+27.3000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                5033
_reflns_number_total             6820
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b822277k.txt
_cod_data_source_block           osrem
_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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7051682
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.53554(4) 0.094282(11) 0.79937(4) 0.01737(9) Uani 1 1 d . . .
Os2 Os 0.70469(4) 0.134971(11) 0.63560(4) 0.01645(9) Uani 1 1 d . . .
Os3 Os 0.86280(4) 0.109118(12) 0.94922(4) 0.02125(9) Uani 1 1 d . . .
O1 O 0.5698(8) -0.0050(2) 0.6853(8) 0.0288(15) Uani 1 1 d . . .
O2 O 0.4905(8) 0.1940(2) 0.9069(8) 0.0289(16) Uani 1 1 d . . .
O3 O 0.5199(11) 0.0486(3) 1.0741(9) 0.042(2) Uani 1 1 d . . .
O4 O 0.7536(8) 0.0370(2) 0.5205(8) 0.0291(16) Uani 1 1 d . . .
O5 O 0.6699(8) 0.2364(2) 0.7369(8) 0.0270(15) Uani 1 1 d . . .
O6 O 0.9856(9) 0.1679(3) 0.5978(10) 0.042(2) Uani 1 1 d . . .
O7 O 0.9015(9) 0.0091(3) 0.8410(9) 0.0389(19) Uani 1 1 d . . .
O8 O 0.8254(9) 0.2098(3) 1.0542(9) 0.0370(18) Uani 1 1 d . . .
O9 O 1.1942(10) 0.1305(3) 1.0069(12) 0.052(2) Uani 1 1 d . . .
O10 O 0.9206(11) 0.0710(3) 1.2617(10) 0.050(2) Uani 1 1 d . . .
C1 C 0.5620(11) 0.0316(3) 0.7275(11) 0.0198(18) Uani 1 1 d . . .
C2 C 0.5112(10) 0.1576(3) 0.8654(10) 0.0189(18) Uani 1 1 d . . .
C3 C 0.5263(12) 0.0662(3) 0.9726(12) 0.029(2) Uani 1 1 d . . .
C4 C 0.7321(10) 0.0726(3) 0.5661(10) 0.0225(19) Uani 1 1 d . . .
C5 C 0.6805(11) 0.1979(3) 0.7032(11) 0.024(2) Uani 1 1 d . . .
C6 C 0.8822(11) 0.1550(3) 0.6147(11) 0.0219(19) Uani 1 1 d . . .
C7 C 0.8817(11) 0.0456(4) 0.8736(11) 0.026(2) Uani 1 1 d . . .
C8 C 0.8351(11) 0.1725(3) 1.0120(11) 0.024(2) Uani 1 1 d . . .
C9 C 1.0726(14) 0.1235(4) 0.9868(12) 0.032(2) Uani 1 1 d . . .
C10 C 0.8981(13) 0.0849(4) 1.1454(12) 0.033(2) Uani 1 1 d . . .
C11 C 0.3288(10) 0.0950(3) 0.5776(10) 0.0211(19) Uani 1 1 d U . .
H11A H 0.3135 0.0657 0.5144 0.025 Uiso 1 1 calc R . .
C12 C 0.2698(11) 0.0927(4) 0.6875(12) 0.027(2) Uani 1 1 d . . .
H12A H 0.2226 0.1233 0.6991 0.032 Uiso 1 1 calc R . .
C13 C 0.1919(13) 0.0493(4) 0.7158(15) 0.039(3) Uani 1 1 d . . .
H13A H 0.0822 0.0499 0.6479 0.059 Uiso 1 1 calc R . .
H13B H 0.2046 0.0494 0.8210 0.059 Uiso 1 1 calc R . .
H13C H 0.2386 0.0204 0.6970 0.059 Uiso 1 1 calc R . .
C14 C 0.4800(11) 0.1310(3) 0.4305(10) 0.0231(19) Uani 1 1 d . . .
H14A H 0.4584 0.1003 0.3729 0.028 Uiso 1 1 calc R . .
C15 C 0.5671(12) 0.1641(3) 0.3945(11) 0.027(2) Uani 1 1 d . . .
H15A H 0.5315 0.1977 0.3921 0.032 Uiso 1 1 calc R . .
C16 C 0.6284(15) 0.1538(4) 0.2789(12) 0.037(3) Uani 1 1 d . . .
H16A H 0.5538 0.1645 0.1792 0.055 Uiso 1 1 calc R . .
H16B H 0.6454 0.1194 0.2760 0.055 Uiso 1 1 calc R . .
H16C H 0.7258 0.1707 0.3059 0.055 Uiso 1 1 calc R . .
C17 C 0.3185(11) 0.1913(4) 0.5319(12) 0.030(2) Uani 1 1 d . . .
H17A H 0.2928 0.1923 0.6203 0.036 Uiso 1 1 calc R . .
H17B H 0.3960 0.2163 0.5450 0.036 Uiso 1 1 calc R . .
C18 C 0.1738(13) 0.2003(4) 0.3867(13) 0.032(2) Uani 1 1 d . . .
H18A H 0.2009 0.1995 0.2992 0.039 Uiso 1 1 calc R . .
H18B H 0.0985 0.1746 0.3731 0.039 Uiso 1 1 calc R . .
C19 C 0.1007(14) 0.2482(4) 0.3903(14) 0.044(3) Uani 1 1 d . . .
H19A H -0.0029 0.2495 0.3080 0.066 Uiso 1 1 calc R . .
H19B H 0.1635 0.2739 0.3776 0.066 Uiso 1 1 calc R . .
H19C H 0.0943 0.2519 0.4874 0.066 Uiso 1 1 calc R . .
B1 B 0.3864(11) 0.1401(4) 0.5210(12) 0.022(2) Uani 1 1 d U . .
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'
B B 0.0013 0.0007 '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'
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 C2 91.6(4) . . ?
C3 Os1 C1 90.4(4) . . ?
C2 Os1 C1 177.9(4) . . ?
C3 Os1 C11 120.7(4) . . ?
C2 Os1 C11 97.5(3) . . ?
C1 Os1 C11 81.8(4) . . ?
C3 Os1 C12 87.6(4) . . ?
C2 Os1 C12 85.0(4) . . ?
C1 Os1 C12 95.6(4) . . ?
C11 Os1 C12 36.0(3) . . ?
C3 Os1 Os3 93.2(3) . . ?
C2 Os1 Os3 87.5(3) . . ?
C1 Os1 Os3 92.0(3) . . ?
C11 Os1 Os3 145.4(3) . . ?
C12 Os1 Os3 172.4(3) . . ?
C3 Os1 Os2 152.3(3) . . ?
C2 Os1 Os2 89.7(3) . . ?
C1 Os1 Os2 88.3(3) . . ?
C11 Os1 Os2 86.5(3) . . ?
C12 Os1 Os2 120.0(2) . . ?
Os3 Os1 Os2 59.216(13) . . ?
C6 Os2 C5 90.4(4) . . ?
C6 Os2 C4 88.3(4) . . ?
C5 Os2 C4 178.7(4) . . ?
C6 Os2 C14 119.5(4) . . ?
C5 Os2 C14 98.1(4) . . ?
C4 Os2 C14 82.2(4) . . ?
C6 Os2 C15 86.6(4) . . ?
C5 Os2 C15 85.7(4) . . ?
C4 Os2 C15 93.9(4) . . ?
C14 Os2 C15 35.5(3) . . ?
C6 Os2 Os3 95.4(3) . . ?
C5 Os2 Os3 87.3(3) . . ?
C4 Os2 Os3 93.2(3) . . ?
C14 Os2 Os3 144.5(2) . . ?
C15 Os2 Os3 172.8(2) . . ?
C6 Os2 Os1 154.6(3) . . ?
C5 Os2 Os1 89.9(3) . . ?
C4 Os2 Os1 91.5(3) . . ?
C14 Os2 Os1 85.6(3) . . ?
C15 Os2 Os1 118.7(3) . . ?
Os3 Os2 Os1 59.329(13) . . ?
C10 Os3 C9 98.7(5) . . ?
C10 Os3 C8 90.1(4) . . ?
C9 Os3 C8 91.0(4) . . ?
C10 Os3 C7 92.7(4) . . ?
C9 Os3 C7 90.5(4) . . ?
C8 Os3 C7 176.7(4) . . ?
C10 Os3 Os2 160.2(4) . . ?
C9 Os3 Os2 101.0(3) . . ?
C8 Os3 Os2 91.3(3) . . ?
C7 Os3 Os2 85.5(3) . . ?
C10 Os3 Os1 98.8(4) . . ?
C9 Os3 Os1 162.3(3) . . ?
C8 Os3 Os1 91.6(3) . . ?
C7 Os3 Os1 86.0(3) . . ?
Os2 Os3 Os1 61.455(12) . . ?
O1 C1 Os1 176.4(8) . . ?
O2 C2 Os1 176.0(8) . . ?
O3 C3 Os1 178.5(9) . . ?
O4 C4 Os2 175.6(8) . . ?
O5 C5 Os2 175.5(8) . . ?
O6 C6 Os2 177.5(9) . . ?
O7 C7 Os3 174.7(9) . . ?
O8 C8 Os3 176.8(9) . . ?
O9 C9 Os3 177.9(10) . . ?
O10 C10 Os3 179.0(12) . . ?
C12 C11 B1 128.2(9) . . ?
C12 C11 Os1 74.9(6) . . ?
B1 C11 Os1 92.7(5) . . ?
C12 C11 H11A 115.4 . . ?
B1 C11 H11A 115.4 . . ?
Os1 C11 H11A 115.4 . . ?
C11 C12 C13 124.3(9) . . ?
C11 C12 Os1 69.1(5) . . ?
C13 C12 Os1 117.4(8) . . ?
C11 C12 H12A 113.0 . . ?
C13 C12 H12A 113.0 . . ?
Os1 C12 H12A 113.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 B1 126.7(9) . . ?
C15 C14 Os2 74.8(6) . . ?
B1 C14 Os2 93.1(6) . . ?
C15 C14 H14A 115.9 . . ?
B1 C14 H14A 115.9 . . ?
Os2 C14 H14A 115.9 . . ?
C14 C15 C16 121.8(9) . . ?
C14 C15 Os2 69.7(5) . . ?
C16 C15 Os2 117.4(7) . . ?
C14 C15 H15A 113.7 . . ?
C16 C15 H15A 113.7 . . ?
Os2 C15 H15A 113.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 B1 108.9(8) . . ?
C18 C17 H17A 109.9 . . ?
B1 C17 H17A 109.9 . . ?
C18 C17 H17B 109.9 . . ?
B1 C17 H17B 109.9 . . ?
H17A C17 H17B 108.3 . . ?
C19 C18 C17 111.9(9) . . ?
C19 C18 H18A 109.2 . . ?
C17 C18 H18A 109.2 . . ?
C19 C18 H18B 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C14 B1 C11 116.6(8) . . ?
C14 B1 C17 123.1(9) . . ?
C11 B1 C17 119.2(8) . . ?
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 1.898(10) . ?
Os1 C2 1.937(9) . ?
Os1 C1 1.948(9) . ?
Os1 C11 2.236(9) . ?
Os1 C12 2.311(10) . ?
Os1 Os3 2.8797(5) . ?
Os1 Os2 2.9410(5) . ?
Os2 C6 1.881(9) . ?
Os2 C5 1.933(10) . ?
Os2 C4 1.934(10) . ?
Os2 C14 2.242(9) . ?
Os2 C15 2.308(10) . ?
Os2 Os3 2.8763(5) . ?
Os3 C10 1.921(11) . ?
Os3 C9 1.929(12) . ?
Os3 C8 1.935(10) . ?
Os3 C7 1.965(10) . ?
O1 C1 1.120(10) . ?
O2 C2 1.145(11) . ?
O3 C3 1.131(12) . ?
O4 C4 1.146(11) . ?
O5 C5 1.145(11) . ?
O6 C6 1.131(11) . ?
O7 C7 1.113(11) . ?
O8 C8 1.142(11) . ?
O9 C9 1.115(13) . ?
O10 C10 1.130(13) . ?
C11 C12 1.407(14) . ?
C11 B1 1.571(14) . ?
C11 H11A 1.0000 . ?
C12 C13 1.513(13) . ?
C12 H12A 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.390(13) . ?
C14 B1 1.520(14) . ?
C14 H14A 1.0000 . ?
C15 C16 1.500(14) . ?
C15 H15A 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.530(14) . ?
C17 B1 1.598(14) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.522(14) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
