#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:40:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178719 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/30/4083060.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_4083060
loop_
_publ_author_name
'Carter, Tyler J.'
'Wang, Justin Y.'
'Szymczak, Nathaniel K.'
_publ_section_title
;
 Manganese-Mediated Hydride Delivery to a Borazine by Stepwise Reduction
 and Protonation
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1540
_journal_paper_doi               10.1021/om500157m
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C9 H19 B3 Mn N3 O3'
_chemical_formula_sum            'C9 H19 B3 Mn N3 O3'
_chemical_formula_weight         304.64
_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                 106.407(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9006(2)
_cell_length_b                   14.2192(3)
_cell_length_c                   12.3119(9)
_cell_measurement_reflns_used    16808
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.10
_cell_measurement_theta_min      4.90
_cell_volume                     1494.74(13)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12'
_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      85(2)
_diffrn_detector_area_resol_mean 29.257
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn944+ CCD'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'micro-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43158
_diffrn_reflns_theta_full        68.20
_diffrn_reflns_theta_max         68.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.219
_exptl_absorpt_correction_T_max  0.705
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_ls_extinction_coef       0.0030(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0513
_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)+(0.0865P)²+1.1035P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1467
_reflns_number_gt                2641
_reflns_number_total             2738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500157m_si_002.cif
_cod_data_source_block           5TJC19
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1494.74(12)
_cod_original_sg_symbol_H-M      P(2)1/n
_cod_database_code               4083060
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
Mn1 Mn 0.17311(5) 0.32570(3) 0.46679(4) 0.0220(2) Uani 1 1 d .
O2 O 0.5171(3) 0.33496(16) 0.5522(2) 0.0381(6) Uani 1 1 d .
O1 O 0.1457(3) 0.34258(15) 0.69956(18) 0.0337(5) Uani 1 1 d .
N3 N -0.0588(3) 0.27346(15) 0.38712(19) 0.0225(5) Uani 1 1 d .
O3 O 0.1470(3) 0.53160(14) 0.42267(19) 0.0365(5) Uani 1 1 d .
C8 C 0.3825(4) 0.33226(19) 0.5186(3) 0.0298(7) Uani 1 1 d .
N1 N 0.1582(3) 0.26632(16) 0.30433(19) 0.0239(5) Uani 1 1 d .
N2 N -0.0691(3) 0.37005(15) 0.21774(19) 0.0242(5) Uani 1 1 d .
C6 C -0.1423(3) 0.2347(2) 0.4652(2) 0.0284(6) Uani 1 1 d .
H6A H -0.2358 0.2034 0.4224 0.043 Uiso 1 1 calc R
H6B H -0.1694 0.2848 0.5083 0.043 Uiso 1 1 calc R
H6C H -0.0757 0.1906 0.5157 0.043 Uiso 1 1 calc R
B2 B 0.0889(4) 0.3412(2) 0.2252(3) 0.0263(7) Uani 1 1 d .
B1 B 0.0656(4) 0.2088(2) 0.3659(3) 0.0257(7) Uani 1 1 d .
C4 C -0.1445(4) 0.4420(2) 0.1343(2) 0.0307(6) Uani 1 1 d .
H4A H -0.2562 0.4374 0.1188 0.046 Uiso 1 1 calc R
H4B H -0.1159 0.4323 0.0655 0.046 Uiso 1 1 calc R
H4C H -0.1107 0.5033 0.1640 0.046 Uiso 1 1 calc R
C2 C 0.3032(3) 0.2202(2) 0.2930(3) 0.0313(7) Uani 1 1 d .
H2A H 0.2803 0.1874 0.2221 0.047 Uiso 1 1 calc R
H2B H 0.3409 0.1764 0.3540 0.047 Uiso 1 1 calc R
H2C H 0.3817 0.2671 0.2956 0.047 Uiso 1 1 calc R
C5 C -0.3015(3) 0.3862(2) 0.3068(3) 0.0308(6) Uani 1 1 d .
H5A H -0.2957 0.4535 0.3040 0.046 Uiso 1 1 calc R
H5B H -0.3237 0.3676 0.3756 0.046 Uiso 1 1 calc R
H5C H -0.3833 0.3641 0.2431 0.046 Uiso 1 1 calc R
C7 C 0.1560(4) 0.33766(19) 0.6075(3) 0.0283(7) Uani 1 1 d .
C1 C 0.0377(4) 0.0989(2) 0.3458(3) 0.0320(7) Uani 1 1 d .
H1A H -0.0273 0.0881 0.2701 0.048 Uiso 1 1 calc R
H1B H -0.0130 0.0743 0.3990 0.048 Uiso 1 1 calc R
H1C H 0.1366 0.0679 0.3561 0.048 Uiso 1 1 calc R
C3 C 0.1831(4) 0.3894(2) 0.1499(3) 0.0389(8) Uani 1 1 d .
H3A H 0.2933 0.3803 0.1839 0.058 Uiso 1 1 calc R
H3B H 0.1602 0.4554 0.1440 0.058 Uiso 1 1 calc R
H3C H 0.1535 0.3617 0.0757 0.058 Uiso 1 1 calc R
B3 B -0.1411(4) 0.3427(2) 0.3031(3) 0.0235(6) Uani 1 1 d .
C9 C 0.1552(3) 0.4523(2) 0.4389(2) 0.0271(6) Uani 1 1 d .
H1 H 0.175(3) 0.220(3) 0.482(3) 0.030(9) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 '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
C7 Mn1 C8 90.85(14)
C7 Mn1 C9 93.51(13)
C8 Mn1 C9 92.41(12)
C7 Mn1 B1 119.40(13)
C8 Mn1 B1 119.86(13)
C9 Mn1 B1 130.99(12)
C7 Mn1 N1 160.45(11)
C8 Mn1 N1 97.87(12)
C9 Mn1 N1 103.51(11)
B1 Mn1 N1 41.34(11)
C7 Mn1 N3 98.11(12)
C8 Mn1 N3 161.18(11)
C9 Mn1 N3 103.44(11)
B1 Mn1 N3 41.47(10)
N1 Mn1 N3 68.86(8)
B3 N3 C6 117.8(2)
B3 N3 B1 121.9(2)
C6 N3 B1 114.3(2)
B3 N3 Mn1 108.30(17)
C6 N3 Mn1 115.21(17)
B1 N3 Mn1 68.59(14)
O2 C8 Mn1 178.9(3)
B2 N1 C2 118.2(2)
B2 N1 B1 123.0(2)
C2 N1 B1 114.8(2)
B2 N1 Mn1 103.85(17)
C2 N1 Mn1 115.77(17)
B1 N1 Mn1 69.06(15)
B3 N2 B2 120.4(2)
B3 N2 C4 119.4(2)
B2 N2 C4 119.1(2)
N2 B2 N1 118.1(3)
N2 B2 C3 120.7(3)
N1 B2 C3 121.2(3)
N1 B1 N3 106.7(2)
N1 B1 C1 122.5(3)
N3 B1 C1 122.2(3)
N1 B1 Mn1 69.60(15)
N3 B1 Mn1 69.94(14)
C1 B1 Mn1 151.7(2)
O1 C7 Mn1 177.9(2)
N2 B3 N3 117.6(3)
N2 B3 C5 120.9(3)
N3 B3 C5 121.5(3)
O3 C9 Mn1 178.7(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mn1 C7 1.789(3)
Mn1 C8 1.794(3)
Mn1 C9 1.830(3)
Mn1 B1 2.133(3)
Mn1 N1 2.140(2)
Mn1 N3 2.152(2)
O2 C8 1.152(4)
O1 C7 1.165(4)
N3 B3 1.465(4)
N3 C6 1.478(4)
N3 B1 1.517(4)
O3 C9 1.144(4)
N1 B2 1.457(4)
N1 C2 1.489(3)
N1 B1 1.508(4)
N2 B3 1.431(4)
N2 B2 1.443(4)
N2 C4 1.471(3)
B2 C3 1.572(5)
B1 C1 1.591(4)
C5 B3 1.568(4)
