#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:18:08 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178644 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/55/4075572.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_4075572
loop_
_publ_author_name
'Braunschweig, Holger'
'Radacki, Krzysztof'
'Seeler, Fabian'
'Whittell, George R.'
_publ_section_title
;
 Synthesis and Reactivity of Dihaloboryl Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4605
_journal_paper_doi               10.1021/om060377z
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C10 B2 Br2 Mn2 O11'
_chemical_formula_weight         587.42
_chemical_name_common
;            
Bis[Bromo(pentacarbonylmanganese)boryl]oxide 
;
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 120.051(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.022(3)
_cell_length_b                   6.3286(8)
_cell_length_c                   13.1563(16)
_cell_measurement_reflns_used    8917
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      3.10
_cell_volume                     1803.3(4)
_computing_cell_refinement       'Saint-NT v. 6.45'
_computing_data_collection       'Smart-NT v. 5.63'
_computing_data_reduction        'Saint-NT v. 6.45'
_computing_molecular_graphics    'XP in ShelxTL-97'
_computing_publication_material  'XP in ShelxTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14341
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    5.884
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_correction_T_min  0.281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs2.0 (Sheldrick 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0187
_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)+(0.0302P)²+1.7536P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0503
_reflns_number_gt                1699
_reflns_number_total             1784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060377zsi20060714_091644.cif
_cod_data_source_block           kr006
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               4075572
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Br1 Br 0.417742(9) 0.18552(3) 0.053762(18) 0.03641(9) Uani 1 1 d .
Mn1 Mn 0.371678(11) 0.50699(4) 0.21875(2) 0.02190(9) Uani 1 1 d .
O1 O 0.31980(8) 0.6817(2) -0.02295(13) 0.0430(4) Uani 1 1 d .
O3 O 0.44435(8) 0.3030(3) 0.45368(14) 0.0443(4) Uani 1 1 d .
O4 O 0.45225(8) 0.8870(3) 0.30828(14) 0.0471(4) Uani 1 1 d .
O5 O 0.27758(8) 0.6974(3) 0.26882(16) 0.0454(4) Uani 1 1 d .
O6 O 0.5000 0.4167(4) 0.2500 0.0379(5) Uani 1 2 d S
C5 C 0.31285(9) 0.6240(3) 0.24935(17) 0.0300(4) Uani 1 1 d .
C4 C 0.42202(9) 0.7427(3) 0.27520(16) 0.0289(4) Uani 1 1 d .
B1 B 0.43913(9) 0.3785(3) 0.18731(18) 0.0242(4) Uani 1 1 d .
O2 O 0.30174(8) 0.1055(3) 0.12197(17) 0.0491(4) Uani 1 1 d .
C2 C 0.32766(9) 0.2586(3) 0.15864(19) 0.0320(4) Uani 1 1 d .
C3 C 0.41642(9) 0.3803(3) 0.36476(18) 0.0298(4) Uani 1 1 d .
C1 C 0.33864(8) 0.6160(3) 0.06865(17) 0.0285(4) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.03924(13) 0.04082(14) 0.03412(13) -0.00193(8) 0.02207(10) 0.00607(8)
Mn1 0.01950(14) 0.02336(15) 0.02396(15) 0.00193(10) 0.01171(11) 0.00032(9)
O1 0.0441(9) 0.0479(10) 0.0270(8) 0.0078(7) 0.0104(7) 0.0019(7)
O3 0.0493(9) 0.0497(10) 0.0376(9) 0.0183(7) 0.0246(8) 0.0162(7)
O4 0.0504(9) 0.0406(9) 0.0395(9) -0.0006(7) 0.0144(7) -0.0174(8)
O5 0.0397(8) 0.0584(11) 0.0467(9) 0.0081(8) 0.0280(8) 0.0179(7)
O6 0.0221(9) 0.0469(12) 0.0449(12) 0.000 0.0169(9) 0.000
C5 0.0277(9) 0.0333(10) 0.0289(9) 0.0044(8) 0.0142(8) 0.0038(8)
C4 0.0293(9) 0.0314(10) 0.0236(9) 0.0037(8) 0.0113(7) -0.0004(8)
B1 0.0233(9) 0.0262(10) 0.0245(10) 0.0058(8) 0.0130(8) 0.0020(8)
O2 0.0446(9) 0.0382(9) 0.0729(12) -0.0143(8) 0.0357(9) -0.0165(8)
C2 0.0264(9) 0.0339(10) 0.0403(11) -0.0003(9) 0.0202(8) -0.0016(8)
C3 0.0310(9) 0.0302(10) 0.0354(10) 0.0044(8) 0.0220(9) 0.0036(8)
C1 0.0234(8) 0.0295(10) 0.0294(10) -0.0017(8) 0.0107(8) 0.0005(7)
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'
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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_3
C1 Mn1 C4 88.75(8) .
C1 Mn1 C3 169.40(8) .
C4 Mn1 C3 89.79(9) .
C1 Mn1 C2 90.48(9) .
C4 Mn1 C2 173.70(8) .
C3 Mn1 C2 89.82(9) .
C1 Mn1 C5 95.93(8) .
C4 Mn1 C5 92.60(9) .
C3 Mn1 C5 94.62(8) .
C2 Mn1 C5 93.69(9) .
C1 Mn1 B1 84.69(8) .
C4 Mn1 B1 86.46(9) .
C3 Mn1 B1 84.75(8) .
C2 Mn1 B1 87.24(8) .
C5 Mn1 B1 178.87(9) .
B1 O6 B1 159.3(3) 2_655
O5 C5 Mn1 179.1(2) .
O4 C4 Mn1 179.2(2) .
O6 B1 Br1 112.05(14) .
O6 B1 Mn1 126.03(15) .
Br1 B1 Mn1 121.91(10) .
O2 C2 Mn1 178.72(18) .
O3 C3 Mn1 179.15(17) .
O1 C1 Mn1 178.30(18) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 B1 1.981(2) .
Mn1 C1 1.850(2) .
Mn1 C4 1.851(2) .
Mn1 C3 1.853(2) .
Mn1 C2 1.854(2) .
Mn1 C5 1.863(2) .
Mn1 B1 2.093(2) .
O1 C1 1.131(3) .
O3 C3 1.130(3) .
O4 C4 1.125(3) .
O5 C5 1.134(2) .
O6 B1 1.342(2) .
O6 B1 1.342(2) 2_655
O2 C2 1.131(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
B1 O6 B1 Mn1 128.41(15) 2_655
C1 Mn1 B1 O6 120.31(19) .
C4 Mn1 B1 O6 31.23(18) .
C3 Mn1 B1 O6 -58.88(18) .
C2 Mn1 B1 O6 -148.95(19) .
C1 Mn1 B1 Br1 -58.18(12) .
C4 Mn1 B1 Br1 -147.26(12) .
C3 Mn1 B1 Br1 122.63(12) .
C2 Mn1 B1 Br1 32.56(12) .
