#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/21/7012168.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_7012168
loop_
_publ_author_name
'Li, Yat'
'Wong, Wing-Tak'
_publ_section_title
;
 Tetraosmium carbonyl clusters containing µ-NH2 amido ligands:
 syntheses, crystal structures and reactivities
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              398
_journal_paper_doi               10.1039/b208321c
_journal_year                    2003
_chemical_formula_moiety         'C11 H6 Br N O11 Os4 '
_chemical_formula_sum            'C11 H6 Br N O11 Os4'
_chemical_formula_weight         1168.87
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Sun Oct 13 16:22:22 2002'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                91.88(1)
_cell_angle_beta                 102.76(1)
_cell_angle_gamma                113.96(1)
_cell_formula_units_Z            2
_cell_length_a                   8.5990(8)
_cell_length_b                   9.6870(8)
_cell_length_c                   14.047(1)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     1032.96(18)
_computing_cell_refinement       'SMART (Bruker, 1996)'
_computing_data_collection       'SMART (Bruker, 1996)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_publication_material  'teXsan (MSC, 1992)'
_computing_structure_refinement  'teXsan (MSC, 1992)'
_computing_structure_solution    'SIR88 (Burla, 1989)'
_diffrn_ambient_temperature      298.2
_diffrn_measured_fraction_theta_full 27
_diffrn_measured_fraction_theta_max 27
_diffrn_measurement_device       'Bruker SMART 1K CCD Detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       'Bruker SMART 1K CCD Detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6315
_diffrn_reflns_reduction_process 'SAINT+ (Bruker, 1999)'
_diffrn_reflns_theta_full        27
_diffrn_reflns_theta_max         27
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    26.499
_exptl_absorpt_correction_T_max  0.160
_exptl_absorpt_correction_T_min  0.073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1012.00
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_refine_diff_density_max         4.74
_refine_diff_density_min         -4.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.577
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3673
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.0261
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                3673
_reflns_number_total             4444
_reflns_threshold_expression     I>\1.5σ(I)
_cod_data_source_file            b208321c.txt
_cod_data_source_block           wt0390w_Yat080_compound_4b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 34 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1033.0(2)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C11 H6 Br N O11 Os4 '
_cod_database_code               7012168
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -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
Os(1) -0.07738(8) 0.23342(7) 0.64229(4) 0.0290(2) Uani ? ?
Os(2) 0.14433(7) 0.13929(6) 0.77746(4) 0.0271(2) Uani ? ?
Os(3) -0.09530(7) 0.23640(7) 0.85666(4) 0.0279(2) Uani ? ?
Os(4) 0.26976(7) 0.47980(6) 0.77113(4) 0.0269(2) Uani ? ?
Br(1) -0.2909(2) 0.3723(2) 0.8666(2) 0.0517(6) Uani ? ?
O(1) -0.271(2) 0.391(2) 0.520(1) 0.087(5) Uani ? ?
O(2) 0.081(2) 0.184(2) 0.479(1) 0.069(4) Uani ? ?
O(3) -0.394(2) -0.079(2) 0.585(1) 0.067(4) Uani ? ?
O(4) 0.338(2) 0.090(2) 0.632(1) 0.064(4) Uani ? ?
O(5) -0.135(2) -0.193(1) 0.725(1) 0.057(3) Uani ? ?
O(6) 0.375(2) 0.063(2) 0.9455(10) 0.060(4) Uani ? ?
O(7) -0.028(2) 0.229(2) 1.0720(3) 0.071(5) Uani ? ?
O(8) -0.393(2) -0.082(1) 0.823(1) 0.076(4) Uani ? ?
O(9) 0.597(1) 0.646(2) 0.938(1) 0.058(3) Uani ? ?
O(10) 0.238(2) 0.768(2) 0.710(1) 0.064(4) Uani ? ?
O(11) 0.484(2) 0.470(2) 0.625(1) 0.066(5) Uani ? ?
N(1) 0.112(1) 0.462(1) 0.8722(9) 0.030(3) Uani ? ?
C(1) -0.199(2) 0.329(2) 0.566(1) 0.042(4) Uani ? ?
C(2) 0.023(2) 0.197(2) 0.541(1) 0.046(5) Uani ? ?
C(3) -0.269(2) 0.038(2) 0.607(1) 0.038(4) Uani ? ?
C(4) 0.267(2) 0.115(3) 0.687(1) 0.057(6) Uani ? ?
C(5) -0.036(2) -0.068(2) 0.740(1) 0.035(3) Uani ? ?
C(6) 0.291(2) 0.092(2) 0.884(1) 0.028(3) Uani ? ?
C(7) -0.055(2) 0.230(2) 0.9984(7) 0.029(3) Uani ? ?
C(8) -0.279(2) 0.038(2) 0.835(1) 0.040(4) Uani ? ?
C(9) 0.473(2) 0.583(2) 0.873(1) 0.038(4) Uani ? ?
C(10) 0.246(2) 0.657(2) 0.734(1) 0.050(4) Uani ? ?
C(11) 0.410(2) 0.482(2) 0.678(1) 0.048(4) Uani ? ?
H(1) 0.0669 0.5244 0.8620 0.0357 Uani ? ?
H(2) 0.1770 0.4842 0.9299 0.0357 Uani ? ?
H(3) -0.2289 0.1986 0.7374 0.0608 Uani ? ?
H(4) -0.0099 0.1066 0.8702 0.0608 Uani ? ?
H(5) 0.1307 0.4378 0.6536 0.0608 Uani ? ?
H(6) 0.3497 0.3458 0.7864 0.0608 Uani ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Os 0 8 -1.216 7.603 'International Tables'
N 0 2 0.006 0.003 'International Tables'
C 0 22 0.003 0.002 'International Tables'
O 0 22 0.011 0.006 'International Tables'
H 0 12 0.000 0.000 'International Tables'
Br 0 2 -0.290 2.459 'International Tables'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Os(2) Os(1) Os(3) 60.82(3) ? ? ? yes
Os(2) Os(1) Os(4) 61.82(3) ? ? ? yes
Os(2) Os(1) C(1) 170.0(9) ? ? ? yes
Os(2) Os(1) C(2) 89.1(7) ? ? ? yes
Os(2) Os(1) C(3) 95.4(8) ? ? ? yes
Os(3) Os(1) Os(4) 71.23(3) ? ? ? yes
Os(3) Os(1) C(1) 115.3(9) ? ? ? yes
Os(3) Os(1) C(2) 149.9(7) ? ? ? yes
Os(3) Os(1) C(3) 91.1(8) ? ? ? yes
Os(4) Os(1) C(1) 108.5(9) ? ? ? yes
Os(4) Os(1) C(2) 95.1(9) ? ? ? yes
Os(4) Os(1) C(3) 155.8(8) ? ? ? yes
C(1) Os(1) C(2) 94(1) ? ? ? yes
C(1) Os(1) C(3) 93(1) ? ? ? yes
C(2) Os(1) C(3) 92(1) ? ? ? yes
Os(1) Os(2) Os(3) 63.25(3) ? ? ? yes
Os(1) Os(2) Os(4) 63.01(3) ? ? ? yes
Os(1) Os(2) C(4) 95.1(8) ? ? ? yes
Os(1) Os(2) C(5) 88.4(7) ? ? ? yes
Os(1) Os(2) C(6) 171.9(6) ? ? ? yes
Os(3) Os(2) Os(4) 72.61(3) ? ? ? yes
Os(3) Os(2) C(4) 157.8(9) ? ? ? yes
Os(3) Os(2) C(5) 91.5(8) ? ? ? yes
Os(3) Os(2) C(6) 109.3(7) ? ? ? yes
Os(4) Os(2) C(4) 93(1) ? ? ? yes
Os(4) Os(2) C(5) 151.1(7) ? ? ? yes
Os(4) Os(2) C(6) 112.7(7) ? ? ? yes
C(4) Os(2) C(5) 92(1) ? ? ? yes
C(4) Os(2) C(6) 92(1) ? ? ? yes
C(5) Os(2) C(6) 95.1(10) ? ? ? yes
Os(1) Os(3) Os(2) 55.93(3) ? ? ? yes
Os(1) Os(3) Br(1) 103.53(9) ? ? ? yes
Os(1) Os(3) N(1) 82.7(6) ? ? ? yes
Os(1) Os(3) C(7) 166.0(6) ? ? ? yes
Os(1) Os(3) C(8) 94.2(8) ? ? ? yes
Os(2) Os(3) Br(1) 157.95(9) ? ? ? yes
Os(2) Os(3) N(1) 84.2(5) ? ? ? yes
Os(2) Os(3) C(7) 110.3(6) ? ? ? yes
Os(2) Os(3) C(8) 94.5(8) ? ? ? yes
Br(1) Os(3) N(1) 85.2(5) ? ? ? yes
Br(1) Os(3) C(7) 89.7(7) ? ? ? yes
Br(1) Os(3) C(8) 95.1(8) ? ? ? yes
N(1) Os(3) C(7) 93.9(9) ? ? ? yes
N(1) Os(3) C(8) 176.8(10) ? ? ? yes
C(7) Os(3) C(8) 89(1) ? ? ? yes
Os(1) Os(4) Os(2) 55.17(3) ? ? ? yes
Os(1) Os(4) N(1) 82.5(5) ? ? ? yes
Os(1) Os(4) C(9) 162.7(9) ? ? ? yes
Os(1) Os(4) C(10) 100.2(9) ? ? ? yes
Os(1) Os(4) C(11) 95.4(9) ? ? ? yes
Os(2) Os(4) N(1) 83.1(5) ? ? ? yes
Os(2) Os(4) C(9) 108.6(8) ? ? ? yes
Os(2) Os(4) C(10) 155.0(9) ? ? ? yes
Os(2) Os(4) C(11) 93.2(9) ? ? ? yes
N(1) Os(4) C(9) 90.0(10) ? ? ? yes
N(1) Os(4) C(10) 90(1) ? ? ? yes
N(1) Os(4) C(11) 176(1) ? ? ? yes
C(9) Os(4) C(10) 95(1) ? ? ? yes
C(9) Os(4) C(11) 91(1) ? ? ? yes
C(10) Os(4) C(11) 93(1) ? ? ? yes
Os(3) N(1) Os(4) 112.3(9) ? ? ? yes
Os(1) C(1) O(1) 178(2) ? ? ? yes
Os(1) C(2) O(2) 175(2) ? ? ? yes
Os(1) C(3) O(3) 176(2) ? ? ? yes
Os(2) C(4) O(4) 175(3) ? ? ? yes
Os(2) C(5) O(5) 174(2) ? ? ? yes
Os(2) C(6) O(6) 178(2) ? ? ? yes
Os(3) C(7) O(7) 177(2) ? ? ? yes
Os(3) C(8) O(8) 178(2) ? ? ? yes
Os(4) C(9) O(9) 178(2) ? ? ? yes
Os(4) C(10) O(10) 177(2) ? ? ? yes
Os(4) C(11) O(11) 174(2) ? ? ? yes
Os(2) Os(1) H(3) 88.16 ? ? ? yes
Os(2) Os(1) H(5) 88.99 ? ? ? yes
Os(3) Os(1) H(3) 32.77 ? ? ? yes
Os(3) Os(1) H(5) 99.46 ? ? ? yes
Os(4) Os(1) H(3) 99.80 ? ? ? yes
Os(4) Os(1) H(5) 32.30 ? ? ? yes
C(1) Os(1) H(3) 91.51 ? ? ? yes
C(1) Os(1) H(5) 82.58 ? ? ? yes
C(2) Os(1) H(3) 161.45 ? ? ? yes
C(2) Os(1) H(5) 77.94 ? ? ? yes
C(3) Os(1) H(3) 69.58 ? ? ? yes
C(3) Os(1) H(5) 169.37 ? ? ? yes
H(3) Os(1) H(5) 120.34 ? ? ? yes
Os(1) Os(2) H(4) 90.53 ? ? ? yes
Os(1) Os(2) H(6) 89.71 ? ? ? yes
Os(3) Os(2) H(4) 32.76 ? ? ? yes
Os(3) Os(2) H(6) 100.16 ? ? ? yes
Os(4) Os(2) H(4) 100.93 ? ? ? yes
Os(4) Os(2) H(6) 32.01 ? ? ? yes
C(4) Os(2) H(4) 165.13 ? ? ? yes
C(4) Os(2) H(6) 73.49 ? ? ? yes
C(5) Os(2) H(4) 73.68 ? ? ? yes
C(5) Os(2) H(6) 165.84 ? ? ? yes
C(6) Os(2) H(4) 83.49 ? ? ? yes
C(6) Os(2) H(6) 88.59 ? ? ? yes
H(4) Os(2) H(6) 120.39 ? ? ? yes
Os(1) Os(3) H(3) 38.67 ? ? ? yes
Os(1) Os(3) H(4) 89.74 ? ? ? yes
Os(2) Os(3) H(3) 88.65 ? ? ? yes
Os(2) Os(3) H(4) 39.83 ? ? ? yes
Br(1) Os(3) H(3) 76.04 ? ? ? yes
Br(1) Os(3) H(4) 161.07 ? ? ? yes
N(1) Os(3) H(3) 106.92 ? ? ? yes
N(1) Os(3) H(4) 110.15 ? ? ? yes
C(7) Os(3) H(3) 153.36 ? ? ? yes
C(7) Os(3) H(4) 78.65 ? ? ? yes
C(8) Os(3) H(3) 70.16 ? ? ? yes
C(8) Os(3) H(4) 70.17 ? ? ? yes
H(3) Os(3) H(4) 108.34 ? ? ? yes
Os(1) Os(4) H(5) 38.71 ? ? ? yes
Os(1) Os(4) H(6) 88.83 ? ? ? yes
Os(2) Os(4) H(5) 88.29 ? ? ? yes
Os(2) Os(4) H(6) 39.53 ? ? ? yes
N(1) Os(4) H(5) 106.78 ? ? ? yes
N(1) Os(4) H(6) 108.72 ? ? ? yes
C(9) Os(4) H(5) 157.78 ? ? ? yes
C(9) Os(4) H(6) 78.81 ? ? ? yes
C(10) Os(4) H(5) 70.63 ? ? ? yes
C(10) Os(4) H(6) 160.09 ? ? ? yes
C(11) Os(4) H(5) 72.98 ? ? ? yes
C(11) Os(4) H(6) 68.11 ? ? ? yes
H(5) Os(4) H(6) 108.30 ? ? ? yes
Os(3) N(1) H(1) 108.75 ? ? ? yes
Os(3) N(1) H(2) 108.75 ? ? ? yes
Os(4) N(1) H(1) 108.76 ? ? ? yes
Os(4) N(1) H(2) 108.76 ? ? ? yes
H(1) N(1) H(2) 109.46 ? ? ? yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os(1) Os(2) 2.828(1) ? ? yes
Os(1) Os(3) 3.049(1) ? ? yes
Os(1) Os(4) 3.070(1) ? ? yes
Os(1) C(1) 1.86(3) ? ? yes
Os(1) C(2) 1.91(2) ? ? yes
Os(1) C(3) 1.89(3) ? ? yes
Os(2) Os(3) 2.981(1) ? ? yes
Os(2) Os(4) 3.037(1) ? ? yes
Os(2) C(4) 1.88(3) ? ? yes
Os(2) C(5) 1.94(3) ? ? yes
Os(2) C(6) 1.93(2) ? ? yes
Os(3) Br(1) 2.544(3) ? ? yes
Os(3) N(1) 2.15(2) ? ? yes
Os(3) C(7) 1.95(1) ? ? yes
Os(3) C(8) 1.89(3) ? ? yes
Os(4) N(1) 2.13(2) ? ? yes
Os(4) C(9) 1.87(3) ? ? yes
Os(4) C(10) 1.88(3) ? ? yes
Os(4) C(11) 1.96(3) ? ? yes
O(1) C(1) 1.15(4) ? ? yes
O(2) C(2) 1.12(3) ? ? yes
O(3) C(3) 1.17(3) ? ? yes
O(4) C(4) 1.16(3) ? ? yes
O(5) C(5) 1.14(3) ? ? yes
O(6) C(6) 1.13(3) ? ? yes
O(7) C(7) 1.01(1) ? ? yes
O(8) C(8) 1.15(3) ? ? yes
O(9) C(9) 1.16(3) ? ? yes
O(10) C(10) 1.16(3) ? ? yes
O(11) C(11) 1.12(3) ? ? yes
Os(1) H(3) 2.010 ? ? yes
Os(1) H(5) 2.031 ? ? yes
Os(2) H(4) 2.001 ? ? yes
Os(2) H(6) 2.038 ? ? yes
Os(3) H(3) 1.741 ? ? yes
Os(3) H(4) 1.691 ? ? yes
Os(4) H(5) 1.735 ? ? yes
Os(4) H(6) 1.697 ? ? yes
N(1) H(1) 0.840 ? ? yes
N(1) H(2) 0.840 ? ? yes
