#------------------------------------------------------------------------------
#$Date: 2023-12-08 16:16:31 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/81/4318105.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_4318105
loop_
_publ_author_name
'Shaowu Du'
'Jason A. Kautz'
'Thomas D. McGrath'
'F. Gordon A. Stone'
_publ_contact_author_address
; Department of Chemistry
   Baylor University
   PO Box 97348
   Waco
   TX, 76798-7348
;
_publ_contact_author_email       Gordon_Stone@baylor.edu
_publ_contact_author_fax         '254 710 2403'
_publ_contact_author_name        'Prof. F. Gordon A. Stone'
_publ_contact_author_phone       '254 710 4427'
_publ_section_title
;
 Unprecedented Cage-Carbon to Cage-Boron NMe3 Transfer in a Monocarbon
 Molybdenacarborane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3202
_journal_page_last               3211
_journal_paper_doi               10.1021/ic020091w
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C12 H29 B10 Mo N O2'
_chemical_formula_weight         423.40
_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                 98.749(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9100(9)
_cell_length_b                   25.7956(16)
_cell_length_c                   9.0850(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.24
_cell_measurement_theta_min      4.69
_cell_volume                     2063.8(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      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       w-2q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0122
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3764
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        8.5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  0.731
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.00136(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0184P)²+2.9786P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                3122
_reflns_number_total             3531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020091w_3.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4318105
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo Mo 0.06559(2) 0.109932(8) 0.03720(2) 0.01727(7) Uani 1 1 d . . .
C1 C -0.0284(3) 0.10670(10) -0.2228(3) 0.0221(5) Uani 1 1 d . . .
H1 H 0.0563 0.0817 -0.2685 0.027 Uiso 1 1 calc R . .
B2 B 0.0196(3) 0.16927(10) -0.1705(3) 0.0181(5) Uani 1 1 d . . .
B3 B -0.0871(3) 0.18708(10) -0.0271(3) 0.0192(5) Uani 1 1 d . . .
H3 H -0.0488 0.2172 0.0592 0.023 Uiso 1 1 calc R . .
B4 B -0.1989(3) 0.13150(11) 0.0081(3) 0.0232(6) Uani 1 1 d . . .
H4 H -0.2369 0.1250 0.1186 0.028 Uiso 1 1 calc R . .
B5 B -0.1522(3) 0.07978(11) -0.1193(3) 0.0250(6) Uani 1 1 d . . .
H5 H -0.1567 0.0374 -0.0936 0.030 Uiso 1 1 calc R . .
B6 B -0.1067(3) 0.15562(12) -0.3368(3) 0.0241(6) Uani 1 1 d . . .
H6 H -0.0757 0.1637 -0.4495 0.029 Uiso 1 1 calc R . .
B7 B -0.1481(3) 0.20612(11) -0.2158(3) 0.0200(6) Uani 1 1 d . . .
H7 H -0.1455 0.2479 -0.2487 0.024 Uiso 1 1 calc R . .
B8 B -0.2832(3) 0.18172(11) -0.1099(3) 0.0224(6) Uani 1 1 d . . .
H8 H -0.3724 0.2073 -0.0735 0.027 Uiso 1 1 calc R . .
B9 B -0.3215(3) 0.11648(12) -0.1618(3) 0.0272(6) Uani 1 1 d . . .
H9 H -0.4348 0.0982 -0.1578 0.033 Uiso 1 1 calc R . .
B10 B -0.2146(3) 0.10084(11) -0.3049(3) 0.0266(6) Uani 1 1 d . . .
H10 H -0.2562 0.0728 -0.3962 0.032 Uiso 1 1 calc R . .
B11 B -0.2940(3) 0.16352(12) -0.2983(3) 0.0249(6) Uani 1 1 d . . .
H11 H -0.3888 0.1771 -0.3850 0.030 Uiso 1 1 calc R . .
C2 C -0.0277(3) 0.05851(10) 0.1614(3) 0.0294(6) Uani 1 1 d . . .
O2 O -0.0763(2) 0.02854(8) 0.2331(2) 0.0424(5) Uani 1 1 d . . .
C3 C 0.0966(3) 0.15217(10) 0.2233(3) 0.0244(5) Uani 1 1 d . . .
O3 O 0.1112(2) 0.17666(8) 0.3288(2) 0.0370(5) Uani 1 1 d . . .
C4 C 0.2468(3) 0.06684(10) -0.0048(3) 0.0249(5) Uani 1 1 d . . .
H4A H 0.287(3) 0.0482(12) -0.070(3) 0.040(9) Uiso 1 1 d . . .
C5 C 0.2781(3) 0.08034(9) 0.1333(3) 0.0218(5) Uani 1 1 d . . .
C6 C 0.3993(3) 0.07406(10) 0.2664(3) 0.0274(6) Uani 1 1 d . . .
C7 C 0.3288(4) 0.05714(12) 0.4028(3) 0.0423(7) Uani 1 1 d . . .
H7A H 0.4090 0.0534 0.4888 0.063 Uiso 1 1 calc R . .
H7B H 0.2768 0.0239 0.3821 0.063 Uiso 1 1 calc R . .
H7C H 0.2557 0.0834 0.4246 0.063 Uiso 1 1 calc R . .
C8 C 0.4807(3) 0.12626(11) 0.2966(3) 0.0334(6) Uani 1 1 d . . .
H8A H 0.5599 0.1231 0.3836 0.050 Uiso 1 1 calc R . .
H8B H 0.4073 0.1527 0.3159 0.050 Uiso 1 1 calc R . .
H8C H 0.5269 0.1363 0.2096 0.050 Uiso 1 1 calc R . .
C9 C 0.5129(3) 0.03296(11) 0.2308(3) 0.0365(7) Uani 1 1 d . . .
H9A H 0.5926 0.0285 0.3170 0.055 Uiso 1 1 calc R . .
H9B H 0.5587 0.0441 0.1446 0.055 Uiso 1 1 calc R . .
H9C H 0.4600 -0.0001 0.2081 0.055 Uiso 1 1 calc R . .
N N 0.1777(2) 0.19539(8) -0.1977(2) 0.0230(4) Uani 1 1 d . . .
C10 C 0.2732(3) 0.21167(11) -0.0553(3) 0.0315(6) Uani 1 1 d . . .
H10A H 0.2146 0.2350 -0.0006 0.047 Uiso 1 1 calc R . .
H10B H 0.3640 0.2297 -0.0775 0.047 Uiso 1 1 calc R . .
H10C H 0.3036 0.1810 0.0056 0.047 Uiso 1 1 calc R . .
C11 C 0.1509(3) 0.24378(12) -0.2906(4) 0.0432(8) Uani 1 1 d . . .
H11A H 0.0885 0.2354 -0.3860 0.065 Uiso 1 1 calc R . .
H11B H 0.2485 0.2579 -0.3085 0.065 Uiso 1 1 calc R . .
H11C H 0.0981 0.2695 -0.2377 0.065 Uiso 1 1 calc R . .
C12 C 0.2702(3) 0.16000(12) -0.2791(3) 0.0366(7) Uani 1 1 d . . .
H12A H 0.2090 0.1487 -0.3725 0.055 Uiso 1 1 calc R . .
H12B H 0.3016 0.1297 -0.2171 0.055 Uiso 1 1 calc R . .
H12C H 0.3603 0.1785 -0.3010 0.055 Uiso 1 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Mo C2 84.26(10) . . y
C3 Mo C4 116.35(10) . . y
C2 Mo C4 98.78(10) . . y
C3 Mo C5 81.19(10) . . y
C2 Mo C5 87.17(10) . . y
C4 Mo C5 36.22(10) . . y
C3 Mo B5 133.37(10) . . y
C2 Mo B5 75.34(10) . . y
C4 Mo B5 108.02(10) . . y
C5 Mo B5 137.49(9) . . y
C3 Mo C1 147.26(9) . . y
C2 Mo C1 114.94(10) . . y
C4 Mo C1 87.96(9) . . y
C5 Mo C1 123.81(9) . . y
B5 Mo C1 42.09(9) . . ?
C3 Mo B4 88.50(10) . . y
C2 Mo B4 74.36(10) . . y
C4 Mo B4 153.81(10) . . y
C5 Mo B4 159.69(9) . . y
B5 Mo B4 45.91(10) . . ?
C1 Mo B4 72.99(9) . . ?
C3 Mo B2 107.53(10) . . y
C2 Mo B2 145.52(10) . . y
C4 Mo B2 104.10(10) . . y
C5 Mo B2 126.06(9) . . y
B5 Mo B2 73.24(10) . . ?
C1 Mo B2 41.94(9) . . ?
B4 Mo B2 73.72(9) . . ?
C3 Mo B3 75.93(9) . . y
C2 Mo B3 114.35(10) . . y
C4 Mo B3 146.06(10) . . y
C5 Mo B3 146.31(9) . . y
B5 Mo B3 75.26(10) . . ?
C1 Mo B3 72.01(9) . . ?
B4 Mo B3 43.81(9) . . ?
B2 Mo B3 43.25(8) . . ?
B5 C1 B6 113.30(19) . . ?
B5 C1 B2 112.68(18) . . ?
B6 C1 B2 62.37(15) . . ?
B5 C1 B10 62.60(16) . . ?
B6 C1 B10 61.62(16) . . ?
B2 C1 B10 112.69(19) . . ?
B5 C1 Mo 68.08(12) . . ?
B6 C1 Mo 128.51(16) . . ?
B2 C1 Mo 70.01(11) . . ?
B10 C1 Mo 127.08(16) . . ?
N B2 C1 122.45(19) . . y
N B2 B7 117.83(19) . . y
C1 B2 B7 105.95(18) . . ?
N B2 B6 114.06(19) . . y
C1 B2 B6 58.65(15) . . ?
B7 B2 B6 60.27(15) . . ?
N B2 B3 125.33(19) . . y
C1 B2 B3 107.77(18) . . ?
B7 B2 B3 60.38(14) . . ?
B6 B2 B3 109.39(18) . . ?
N B2 Mo 109.64(14) . . y
C1 B2 Mo 68.05(12) . . ?
B7 B2 Mo 124.04(15) . . ?
B6 B2 Mo 123.28(16) . . ?
B3 B2 Mo 68.83(12) . . ?
B2 B3 B7 59.25(14) . . ?
B2 B3 B8 105.46(18) . . ?
B7 B3 B8 59.07(15) . . ?
B2 B3 B4 107.14(18) . . ?
B7 B3 B4 107.07(19) . . ?
B8 B3 B4 59.02(15) . . ?
B2 B3 Mo 67.92(12) . . ?
B7 B3 Mo 122.20(15) . . ?
B8 B3 Mo 120.66(16) . . ?
B4 B3 Mo 67.06(12) . . ?
B8 B4 B9 59.41(16) . . ?
B8 B4 B3 60.42(15) . . ?
B9 B4 B3 107.5(2) . . ?
B8 B4 B5 105.26(19) . . ?
B9 B4 B5 58.15(15) . . ?
B3 B4 B5 106.23(18) . . ?
B8 B4 Mo 123.74(16) . . ?
B9 B4 Mo 120.36(17) . . ?
B3 B4 Mo 69.13(12) . . ?
B5 B4 Mo 65.91(12) . . ?
C1 B5 B9 105.3(2) . . ?
C1 B5 B10 59.15(15) . . ?
B9 B5 B10 59.83(16) . . ?
C1 B5 B4 106.08(19) . . ?
B9 B5 B4 59.18(16) . . ?
B10 B5 B4 107.7(2) . . ?
C1 B5 Mo 69.83(12) . . ?
B9 B5 Mo 123.40(17) . . ?
B10 B5 Mo 125.54(18) . . ?
B4 B5 Mo 68.18(12) . . ?
C1 B6 B10 59.38(15) . . ?
C1 B6 B11 106.0(2) . . ?
B10 B6 B11 60.25(16) . . ?
C1 B6 B2 58.98(14) . . ?
B10 B6 B2 108.1(2) . . ?
B11 B6 B2 107.73(19) . . ?
C1 B6 B7 105.67(18) . . ?
B10 B6 B7 108.5(2) . . ?
B11 B6 B7 60.20(15) . . ?
B2 B6 B7 59.58(15) . . ?
B2 B7 B8 107.69(19) . . ?
B2 B7 B6 60.14(15) . . ?
B8 B7 B6 107.33(19) . . ?
B2 B7 B11 107.70(19) . . ?
B8 B7 B11 59.65(15) . . ?
B6 B7 B11 59.60(15) . . ?
B2 B7 B3 60.37(14) . . ?
B8 B7 B3 60.81(15) . . ?
B6 B7 B3 109.28(19) . . ?
B11 B7 B3 109.30(19) . . ?
B11 B8 B9 60.49(17) . . ?
B11 B8 B7 60.48(15) . . ?
B9 B8 B7 108.3(2) . . ?
B11 B8 B4 110.3(2) . . ?
B9 B8 B4 60.83(16) . . ?
B7 B8 B4 109.15(18) . . ?
B11 B8 B3 109.41(18) . . ?
B9 B8 B3 108.71(19) . . ?
B7 B8 B3 60.11(14) . . ?
B4 B8 B3 60.56(15) . . ?
B8 B9 B10 108.0(2) . . ?
B8 B9 B5 109.07(19) . . ?
B10 B9 B5 60.22(16) . . ?
B8 B9 B11 59.66(16) . . ?
B10 B9 B11 59.80(16) . . ?
B5 B9 B11 108.2(2) . . ?
B8 B9 B4 59.76(16) . . ?
B10 B9 B4 110.82(19) . . ?
B5 B9 B4 62.67(16) . . ?
B11 B9 B4 108.8(2) . . ?
C1 B10 B6 59.00(15) . . ?
C1 B10 B11 105.65(19) . . ?
B6 B10 B11 60.17(16) . . ?
C1 B10 B9 104.68(19) . . ?
B6 B10 B9 107.9(2) . . ?
B11 B10 B9 60.32(16) . . ?
C1 B10 B5 58.25(15) . . ?
B6 B10 B5 107.59(19) . . ?
B11 B10 B5 108.4(2) . . ?
B9 B10 B5 59.96(16) . . ?
B8 B11 B6 107.98(19) . . ?
B8 B11 B10 108.2(2) . . ?
B6 B11 B10 59.59(16) . . ?
B8 B11 B9 59.85(16) . . ?
B6 B11 B9 107.1(2) . . ?
B10 B11 B9 59.88(17) . . ?
B8 B11 B7 59.87(15) . . ?
B6 B11 B7 60.20(15) . . ?
B10 B11 B7 107.95(19) . . ?
B9 B11 B7 107.29(19) . . ?
O2 C2 Mo 177.8(2) . . y
O3 C3 Mo 178.5(2) . . y
H4A C4 C5 139(2) . . y
H4A C4 Mo 147(2) . . y
C5 C4 Mo 74.44(16) . . y
C4 C5 C6 140.9(2) . . y
C4 C5 Mo 69.34(15) . . y
C6 C5 Mo 149.79(19) . . y
C5 C6 C9 108.7(2) . . ?
C5 C6 C8 108.2(2) . . ?
C9 C6 C8 109.6(2) . . ?
C5 C6 C7 110.4(2) . . ?
C9 C6 C7 109.7(2) . . ?
C8 C6 C7 110.2(2) . . ?
C10 N C12 108.3(2) . . ?
C10 N C11 105.8(2) . . ?
C12 N C11 106.3(2) . . ?
C10 N B2 112.30(18) . . ?
C12 N B2 112.3(2) . . ?
C11 N B2 111.37(18) . . ?
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
Mo C3 1.995(3) . y
Mo C2 2.002(3) . y
Mo C4 2.044(3) . y
Mo C5 2.104(2) . y
Mo B5 2.357(3) . y
Mo C1 2.385(2) . y
Mo B4 2.396(3) . y
Mo B2 2.416(3) . y
Mo B3 2.431(3) . y
C1 B5 1.703(4) . ?
C1 B6 1.712(4) . ?
C1 B2 1.718(4) . ?
C1 B10 1.719(3) . ?
B2 N 1.613(3) . y
B2 B7 1.766(4) . ?
B2 B6 1.776(4) . ?
B2 B3 1.786(3) . ?
B3 B7 1.787(4) . ?
B3 B8 1.799(4) . ?
B3 B4 1.802(4) . ?
B4 B8 1.774(4) . ?
B4 B9 1.793(4) . ?
B4 B5 1.854(4) . ?
B5 B9 1.773(4) . ?
B5 B10 1.778(4) . ?
B6 B10 1.758(4) . ?
B6 B11 1.768(4) . ?
B6 B7 1.779(4) . ?
B7 B8 1.768(4) . ?
B7 B11 1.779(4) . ?
B8 B11 1.764(4) . ?
B8 B9 1.767(4) . ?
B9 B10 1.771(4) . ?
B9 B11 1.779(4) . ?
B10 B11 1.769(4) . ?
C2 O2 1.138(3) . y
C3 O3 1.139(3) . y
C4 H4A 0.88(3) . y
C4 C5 1.291(4) . y
C5 C6 1.503(3) . y
C6 C9 1.534(4) . ?
C6 C8 1.534(4) . ?
C6 C7 1.535(4) . ?
N C10 1.497(3) . ?
N C12 1.498(3) . ?
N C11 1.505(3) . ?
