#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:34:13 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178657 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/68/4076835.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_4076835
loop_
_publ_author_name
'Kautz, Jason A.'
'Kissounko, Denis A.'
'Kissounko, Natalia S.'
'Stone, F. Gordon A.'
_publ_section_title
;
 Molybdenum Complexes of an Eight-Electron-Donor Monocarbollide Ligand,
 Geometrically Constrained by Intramolecular Five-Membered-Ring Formation
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2547
_journal_paper_doi               10.1021/om020103l
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C10 H21 B10 Mo N O5'
_chemical_formula_weight         439.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.100(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3159(7)
_cell_length_b                   9.8420(12)
_cell_length_c                   15.0004(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      20.0
_cell_volume                     1964.6(3)
_computing_cell_refinement       'Enraf-Nonius CAD4 (1989)'
_computing_data_collection       'Enraf-Nonius CAD4 (1989)'
_computing_data_reduction        'XCAD4 Siemens Software (Harms, 1993)'
_computing_molecular_graphics    'XP in SHELXTL-PC (Bruker, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       ω-2θ
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4728
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        6.08
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular blocks'
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0337P)²+0.7423P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                3427
_reflns_number_total             4501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020103l.cif
_cod_data_source_block           2
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.7423P] 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^)+(0.0337P)^2^+0.7423P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4076835
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_calc_flag
_atom_site_refinement_flags
Mo Mo 0.795447(18) 0.10859(3) 0.111334(16) 0.02840(8) Uani 1 d .
C1 C 0.8817(2) 0.2837(3) 0.03663(19) 0.0310(6) Uani 1 d .
B2 B 0.7849(2) 0.3494(3) 0.0940(2) 0.0313(7) Uani 1 d .
H2 H 0.7914 0.3933 0.1614 0.038 Uiso 1 calc R
B3 B 0.6766(2) 0.2606(4) 0.0516(2) 0.0318(7) Uani 1 d .
B4 B 0.7144(2) 0.1340(4) -0.0289(2) 0.0347(8) Uani 1 d .
H4 H 0.6734 0.0392 -0.0436 0.042 Uiso 1 calc R
B5 B 0.8504(2) 0.1527(4) -0.0337(2) 0.0335(8) Uani 1 d .
H5 H 0.9009 0.0684 -0.0499 0.040 Uiso 1 calc R
B6 B 0.8372(3) 0.4378(4) 0.0038(2) 0.0387(8) Uani 1 d .
H6 H 0.8774 0.5344 0.0148 0.046 Uiso 1 calc R
B7 B 0.7059(3) 0.4255(4) 0.0094(2) 0.0397(9) Uani 1 d .
H7 H 0.6591 0.5146 0.0232 0.048 Uiso 1 calc R
B8 B 0.6643(3) 0.2959(4) -0.0649(2) 0.0385(8) Uani 1 d .
H8 H 0.5901 0.3012 -0.0996 0.046 Uiso 1 calc R
B9 B 0.7701(3) 0.2291(4) -0.1165(2) 0.0401(9) Uani 1 d .
H9 H 0.7654 0.1901 -0.1852 0.048 Uiso 1 calc R
B10 B 0.8768(3) 0.3169(4) -0.0749(2) 0.0372(8) Uani 1 d .
H10 H 0.9425 0.3348 -0.1156 0.045 Uiso 1 calc R
B11 B 0.7635(3) 0.4061(4) -0.0941(3) 0.0446(9) Uani 1 d .
H11 H 0.7546 0.4821 -0.1476 0.053 Uiso 1 calc R
C2 C 0.7782(3) 0.1494(3) 0.2426(2) 0.0437(8) Uani 1 d .
O2 O 0.7703(3) 0.1771(3) 0.31509(18) 0.0767(9) Uani 1 d .
C3 C 0.6725(2) 0.0039(3) 0.1354(2) 0.0444(8) Uani 1 d .
O3 O 0.59988(19) -0.0552(3) 0.1479(2) 0.0725(9) Uani 1 d .
C4 C 0.8324(3) -0.0831(3) 0.0770(2) 0.0435(8) Uani 1 d .
O4 O 0.8489(2) -0.1875(3) 0.0511(2) 0.0784(10) Uani 1 d .
N N 0.98229(18) 0.2860(3) 0.07791(18) 0.0371(6) Uani 1 d .
H H 1.022(3) 0.340(4) 0.058(2) 0.045 Uiso 1 d .
C5 C 1.0114(2) 0.1961(3) 0.1380(2) 0.0374(7) Uani 1 d .
O5 O 0.95152(15) 0.1075(2) 0.16447(14) 0.0432(5) Uani 1 d .
C6 C 1.1171(2) 0.1999(4) 0.1753(2) 0.0584(11) Uani 1 d .
H6A H 1.1527 0.2730 0.1483 0.088 Uiso 0.50 calc PR
H6B H 1.1498 0.1154 0.1629 0.088 Uiso 0.50 calc PR
H6C H 1.1165 0.2136 0.2386 0.088 Uiso 0.50 calc PR
H6D H 1.1266 0.1283 0.2182 0.088 Uiso 0.50 calc PR
H6E H 1.1296 0.2859 0.2037 0.088 Uiso 0.50 calc PR
H6F H 1.1628 0.1878 0.1279 0.088 Uiso 0.50 calc PR
O6 O 0.57686(15) 0.2625(2) 0.09953(15) 0.0413(5) Uani 1 d .
C7 C 0.4796(2) 0.2306(5) 0.0574(3) 0.0616(11) Uani 1 d .
H7A H 0.4782 0.1385 0.0344 0.074 Uiso 1 calc R
H7B H 0.4631 0.2932 0.0091 0.074 Uiso 1 calc R
C8 C 0.4088(3) 0.2468(5) 0.1324(3) 0.0721(13) Uani 1 d .
H8A H 0.3428 0.2752 0.1100 0.087 Uiso 1 calc R
H8B H 0.4022 0.1623 0.1649 0.087 Uiso 1 calc R
C9 C 0.4559(3) 0.3537(5) 0.1905(3) 0.0664(12) Uani 1 d .
H9A H 0.4361 0.4435 0.1697 0.080 Uiso 1 calc R
H9B H 0.4359 0.3431 0.2516 0.080 Uiso 1 calc R
C10 C 0.5643(3) 0.3348(5) 0.1842(3) 0.0705(13) Uani 1 d .
H10A H 0.5909 0.2816 0.2340 0.085 Uiso 1 calc R
H10B H 0.5985 0.4218 0.1838 0.085 Uiso 1 calc R
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'
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'
Mo Mo -1.6832 0.6857 '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_publ_flag
C3 Mo C4 76.77(13) y
C3 Mo C2 78.60(14) y
C4 Mo C2 117.95(13) y
C3 Mo O5 135.13(12) y
C4 Mo O5 81.49(12) y
C2 Mo O5 77.78(11) y
C3 Mo B3 81.38(13) y
C4 Mo B3 131.99(14) y
C2 Mo B3 98.43(13) y
O5 Mo B3 139.58(10) y
C3 Mo B4 82.11(13) y
C4 Mo B4 88.83(13) y
C2 Mo B4 141.72(13) y
O5 Mo B4 136.42(10) y
B3 Mo B4 45.79(12) ?
C3 Mo B5 123.41(13) y
C4 Mo B5 81.40(13) y
C2 Mo B5 155.08(12) y
O5 Mo B5 90.80(10) y
B3 Mo B5 75.94(12) ?
B4 Mo B5 45.65(11) ?
C3 Mo C1 151.85(12) y
C4 Mo C1 115.51(12) y
C2 Mo C1 112.82(12) y
O5 Mo C1 72.99(9) y
B3 Mo C1 71.72(11) ?
B4 Mo C1 73.35(11) ?
B5 Mo C1 42.27(11) ?
C3 Mo B2 119.42(12) y
C4 Mo B2 155.88(12) y
C2 Mo B2 84.32(12) y
O5 Mo B2 95.45(10) y
B3 Mo B2 44.39(11) ?
B4 Mo B2 76.88(12) ?
B5 Mo B2 74.70(12) ?
C1 Mo B2 41.91(10) ?
N C1 B6 114.6(2) ?
N C1 B2 118.7(2) y
B6 C1 B2 62.87(19) ?
N C1 B10 114.6(2) ?
B6 C1 B10 62.8(2) ?
B2 C1 B10 114.9(2) ?
N C1 B5 118.3(2) y
B6 C1 B5 114.9(2) ?
B2 C1 B5 115.3(2) ?
B10 C1 B5 62.5(2) ?
N C1 Mo 105.32(18) y
B6 C1 Mo 128.08(19) ?
B2 C1 Mo 69.48(15) ?
B10 C1 Mo 126.9(2) ?
B5 C1 Mo 68.44(15) ?
C1 B2 B6 58.33(19) ?
C1 B2 B7 103.7(2) ?
B6 B2 B7 59.2(2) ?
C1 B2 B3 104.5(2) ?
B6 B2 B3 107.6(2) ?
B7 B2 B3 60.2(2) ?
C1 B2 Mo 68.61(15) ?
B6 B2 Mo 123.2(2) ?
B7 B2 Mo 121.7(2) ?
B3 B2 Mo 66.18(16) ?
O6 B3 B8 114.0(2) ?
O6 B3 B2 122.0(2) ?
B8 B3 B2 107.4(2) ?
O6 B3 B7 111.1(2) ?
B8 B3 B7 59.4(2) ?
B2 B3 B7 59.84(19) ?
O6 B3 B4 125.8(3) ?
B8 B3 B4 60.05(19) ?
B2 B3 B4 109.4(2) ?
B7 B3 B4 108.5(2) ?
O6 B3 Mo 114.5(2) y
B8 B3 Mo 122.6(2) ?
B2 B3 Mo 69.43(15) ?
B7 B3 Mo 124.3(2) ?
B4 B3 Mo 67.37(15) ?
B9 B4 B8 58.6(2) ?
B9 B4 B3 105.1(3) ?
B8 B4 B3 58.98(19) ?
B9 B4 B5 58.76(19) ?
B8 B4 B5 104.9(2) ?
B3 B4 B5 104.9(2) ?
B9 B4 Mo 121.6(2) ?
B8 B4 Mo 121.1(2) ?
B3 B4 Mo 66.84(15) ?
B5 B4 Mo 67.70(15) ?
C1 B5 B10 58.64(19) ?
C1 B5 B9 103.8(3) ?
B10 B5 B9 59.4(2) ?
C1 B5 B4 105.8(2) ?
B10 B5 B4 108.4(2) ?
B9 B5 B4 59.79(19) ?
C1 B5 Mo 69.30(15) ?
B10 B5 Mo 124.2(2) ?
B9 B5 Mo 121.5(2) ?
B4 B5 Mo 66.64(15) ?
C1 B6 B7 105.2(3) ?
C1 B6 B11 105.1(3) ?
B7 B6 B11 60.2(2) ?
C1 B6 B10 58.86(19) ?
B7 B6 B10 107.9(3) ?
B11 B6 B10 59.7(2) ?
C1 B6 B2 58.80(18) ?
B7 B6 B2 60.7(2) ?
B11 B6 B2 109.1(3) ?
B10 B6 B2 108.3(3) ?
B6 B7 B11 60.1(2) ?
B6 B7 B8 108.0(3) ?
B11 B7 B8 60.3(2) ?
B6 B7 B2 60.1(2) ?
B11 B7 B2 108.4(2) ?
B8 B7 B2 108.0(3) ?
B6 B7 B3 108.0(2) ?
B11 B7 B3 108.6(3) ?
B8 B7 B3 60.1(2) ?
B2 B7 B3 59.92(19) ?
B9 B8 B7 108.0(3) ?
B9 B8 B11 60.3(2) ?
B7 B8 B11 59.8(2) ?
B9 B8 B3 108.2(2) ?
B7 B8 B3 60.5(2) ?
B11 B8 B3 108.6(3) ?
B9 B8 B4 60.5(2) ?
B7 B8 B4 110.1(2) ?
B11 B8 B4 110.0(2) ?
B3 B8 B4 60.97(19) ?
B10 B9 B8 108.1(3) ?
B10 B9 B11 59.7(2) ?
B8 B9 B11 60.3(2) ?
B10 B9 B5 60.1(2) ?
B8 B9 B5 108.8(2) ?
B11 B9 B5 108.4(3) ?
B10 B9 B4 110.3(2) ?
B8 B9 B4 60.9(2) ?
B11 B9 B4 110.4(3) ?
B5 B9 B4 61.44(19) ?
C1 B10 B9 104.8(2) ?
C1 B10 B11 105.0(2) ?
B9 B10 B11 60.7(2) ?
C1 B10 B6 58.38(19) ?
B9 B10 B6 108.1(3) ?
B11 B10 B6 60.0(2) ?
C1 B10 B5 58.83(19) ?
B9 B10 B5 60.5(2) ?
B11 B10 B5 109.5(3) ?
B6 B10 B5 108.2(2) ?
B10 B11 B6 60.3(2) ?
B10 B11 B7 107.9(3) ?
B6 B11 B7 59.7(2) ?
B10 B11 B9 59.6(2) ?
B6 B11 B9 107.5(3) ?
B7 B11 B9 107.4(3) ?
B10 B11 B8 107.2(3) ?
B6 B11 B8 107.4(3) ?
B7 B11 B8 59.9(2) ?
B9 B11 B8 59.4(2) ?
O2 C2 Mo 177.2(3) y
O3 C3 Mo 178.4(3) y
O4 C4 Mo 174.0(3) y
H N C5 121(2) y
H N C1 117(2) y
C5 N C1 121.7(3) y
O5 C5 N 120.7(3) y
O5 C5 C6 119.9(3) y
N C5 C6 119.4(3) ?
C5 O5 Mo 119.00(19) y
C7 O6 C10 110.6(2) ?
C7 O6 B3 124.5(2) ?
C10 O6 B3 122.6(2) ?
O6 C7 C8 103.0(3) ?
C9 C8 C7 104.5(3) ?
C10 C9 C8 105.6(3) ?
C9 C10 O6 105.1(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Mo C3 1.979(3) y
Mo C4 2.022(3) y
Mo C2 2.031(3) y
Mo O5 2.198(2) y
Mo B3 2.333(3) y
Mo B4 2.342(3) y
Mo B5 2.361(3) y
Mo C1 2.374(3) y
Mo B2 2.388(3) y
C1 N 1.455(3) y
C1 B6 1.695(5) ?
C1 B2 1.703(4) ?
C1 B10 1.704(4) ?
C1 B5 1.707(4) ?
B2 B6 1.772(5) ?
B2 B7 1.783(5) ?
B2 B3 1.784(5) ?
B3 O6 1.533(4) y
B3 B8 1.783(5) ?
B3 B7 1.790(5) ?
B3 B4 1.819(5) ?
B4 B9 1.795(5) ?
B4 B8 1.803(5) ?
B4 B5 1.825(5) ?
B5 B10 1.770(5) ?
B5 B9 1.776(5) ?
B6 B7 1.757(5) ?
B6 B11 1.764(5) ?
B6 B10 1.770(5) ?
B7 B11 1.767(5) ?
B7 B8 1.770(5) ?
B8 B9 1.760(5) ?
B8 B11 1.777(5) ?
B9 B10 1.757(5) ?
B9 B11 1.776(6) ?
B10 B11 1.759(5) ?
C2 O2 1.130(4) y
C3 O3 1.149(4) y
C4 O4 1.123(4) y
N H 0.81(3) y
N C5 1.311(4) y
C5 O5 1.256(4) y
C5 C6 1.495(4) ?
O6 C7 1.455(4) ?
O6 C10 1.471(4) ?
C7 C8 1.503(5) ?
C8 C9 1.490(6) ?
C9 C10 1.462(5) ?
