# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Mn2Li(BH4)5*C4H10O5
_database_code_depnum_ccdc_archive 'CCDC 985621'
_audit_update_record             
;
2014-02-06 deposited with the CCDC.
2015-02-10 downloaded from the CCDC.
;

#=============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            
;
lithium dimanganese pentaborohydride bis(diethyl ether)
;
_chemical_formula_moiety         'B5 H20 Mn2, 2(C4 H10 O), Li'
_chemical_formula_sum            'C8 H40 B5 Li Mn2 O2'
_chemical_formula_weight         339.27


loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080
0.00800 0.00600
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560
0.00200 0.00200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304
0.00000 0.00000
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
mn 11.28190 5.34090 7.35730 0.34320 3.01930 17.86740 2.24410 83.75430 1.08960
0.29500 0.72900
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
b 2.05450 23.21850 1.33260 1.02100 1.09790 60.34980 0.70680 0.14030 -0.19320
0.00000 0.00100
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
li 1.12820 3.95460 0.75080 1.05240 0.61750 85.39050 0.46530 168.26100 0.03770
0.00000 0.00000
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5

#=============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
x,y,z
-x,y,-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
-x+1/2,-y+1/2,-z
x+1/2,-y+1/2,z+1/2

_cell_length_a                   21.7106(3)
_cell_length_b                   7.72944(12)
_cell_length_c                   14.02422(19)
_cell_angle_alpha                90.00000
_cell_angle_beta                 110.8649(14)
_cell_angle_gamma                90.00000
_cell_volume                     2199.09(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    ?
_cell_special_details            
; ?
;
# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to 
# equatorial plane
_pd_spec_size_equat              ? # parallel to 
# scattering vector
# in transmission
_pd_spec_size_thick              ? # parallel to 
# scattering vector
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the 
# container.
; 
Sample in 0.5 mm glass capillary was mounted in argon-filled glovebox
;
_pd_spec_mount_mode              transmission

_pd_spec_shape                   cylinder
_pd_char_colour                  yellow

#=============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; 
Using LaB6 standard
;

_diffrn_ambient_temperature      ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.827420
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ? # Not in version 2.0.1
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             728.0
_exptl_absorpt_coefficient_mu    1.138
_pd_meas_scan_method             fixed
_pd_meas_special_details         
;  ?
;

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        4994
_pd_meas_2theta_range_min        0.04690
_pd_meas_2theta_range_max        36.06976
_pd_meas_2theta_range_inc        0.007216

#=============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_proc_ls_profile_function     ?
_pd_proc_ls_background_function  ?
_pd_proc_ls_pref_orient_corr     
; ?
;

#  The following profile R-factors are NOT CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These are the current CIF standard

_pd_proc_ls_prof_R_factor        3.8975
_pd_proc_ls_prof_wR_factor       5.3471
_pd_proc_ls_prof_wR_expected     0.5179

#  The following profile R-factors are CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These items are not in the current CIF standard, but are defined above

_pd_proc_ls_prof_cR_factor       10.5242
_pd_proc_ls_prof_cwR_factor      11.2901
_pd_proc_ls_prof_cwR_expected    1.0936

#  The following items are not in the CIF standard, but are defined above

_pd_proc_ls_prof_chi2            106.5897
_pd_proc_ls_prof_echi2           108.6613


#  Items related to LS refinement

_refine_ls_R_I_factor            5.0528
_refine_ls_number_reflns         569
_refine_ls_number_parameters     24
_refine_ls_number_restraints     77
_refine_ls_shift/su_max          0.01
_refine_ls_goodness_of_fit_all   10.3242

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        0.0549
_pd_proc_2theta_range_max        36.0778
_pd_proc_2theta_range_inc        0.007216
_pd_proc_wavelength              0.827420


_pd_block_diffractogram_id       ? # The id used for the block containing
# the powder pattern profile (section 11)

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       ?
_computing_structure_solution    FOX
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    ?
_computing_publication_material  ?

#=============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type # Not in version 2.0.1
_atom_site_type_symbol
O1 0.96728(7) 0.32937(19) 0.13545(11) 0.152(3) 1.00000 Uiso O
C1 1.05134(7) 0.24798(19) 0.08280(11) 0.152(3) 1.00000 Uiso C
H1A 1.07727(7) 0.15625(19) 0.07039(11) 0.152(3) 1.00000 Uiso H
H1B 1.08030(7) 0.33328(19) 0.12622(11) 0.152(3) 1.00000 Uiso H
H1C 1.02607(7) 0.30170(19) 0.01847(11) 0.152(3) 1.00000 Uiso H
C2 1.00590(7) 0.18048(19) 0.13230(11) 0.152(3) 1.00000 Uiso C
H2A 1.03007(7) 0.12084(19) 0.19293(11) 0.152(3) 1.00000 Uiso H
H2B 0.97691(7) 0.09591(19) 0.08814(11) 0.152(3) 1.00000 Uiso H
C3 0.90820(7) 0.34049(19) 0.05170(11) 0.152(3) 1.00000 Uiso C
H3A 0.88999(7) 0.45188(19) 0.05300(11) 0.152(3) 1.00000 Uiso H
H3B 0.91486(7) 0.32795(19) -0.01435(11) 0.152(3) 1.00000 Uiso H
C4 0.86081(7) 0.20791(19) 0.06109(11) 0.152(3) 1.00000 Uiso C
H4A 0.82010(7) 0.21479(19) 0.00525(11) 0.152(3) 1.00000 Uiso H
H4B 0.85354(7) 0.22195(19) 0.12428(11) 0.152(3) 1.00000 Uiso H
H4C 0.87973(7) 0.09325(19) 0.06139(11) 0.152(3) 1.00000 Uiso H
Mn1 0.70722(10) 0.2375(4) 0.31312(15) 0.0564(6) 1.00000 Uiso Mn
B1 0.5959(3) 0.1998(7) 0.2601(4) 0.089(3) 1.00000 Uiso B
H11 0.6280(3) 0.3055(7) 0.3083(4) 0.089(3) 1.00000 Uiso H
H12 0.6211(3) 0.1407(7) 0.2099(4) 0.089(3) 1.00000 Uiso H
H13 0.5876(3) 0.0966(7) 0.3114(4) 0.089(3) 1.00000 Uiso H
H14 0.5468(3) 0.2563(7) 0.2108(4) 0.089(3) 1.00000 Uiso H
B2 0.7398(3) 0.4916(7) 0.7344(4) 0.089(3) 1.00000 Uiso B
H21 0.7665(3) 0.5324(7) 0.8162(4) 0.089(3) 1.00000 Uiso H
H22 0.7711(3) 0.3956(7) 0.7112(4) 0.089(3) 1.00000 Uiso H
H23 0.6912(3) 0.4295(7) 0.7273(4) 0.089(3) 1.00000 Uiso H
H24 0.7304(3) 0.6090(7) 0.6831(4) 0.089(3) 1.00000 Uiso H
B3 0.75000 0.75000 0.00000 0.089(3) 1.00000 Uiso B
H31 0.71908(16) 0.7408(4) 0.0497(2) 0.089(3) 0.50000 Uiso H
H32 0.73703(16) 0.8724(4) -0.0468(2) 0.089(3) 0.50000 Uiso H
H33 0.80388(16) 0.7521(4) 0.0495(2) 0.089(3) 0.50000 Uiso H
H34 0.73990(16) 0.6341(4) -0.0523(2) 0.089(3) 0.50000 Uiso H
Li1 0.00000 0.50000 0.25000 0.24(3) 1.00000 Uiso Li


_geom_special_details            ?

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
O1 C2 1.434(2) 1_555 ?
O1 C3 1.3996(17) 1_555 ?
O1 Li1 2.0030(14) 1_655 ?
C1 H1A 0.959(2) 1_555 ?
C1 H1B 0.9634(19) 1_555 ?
C1 H1C 0.9668(19) 1_555 ?
C1 C2 1.488(2) 1_555 ?
C2 H2A 0.9450(19) 1_555 ?
C2 H2B 0.9640(19) 1_555 ?
C3 H3A 0.950(2) 1_555 ?
C3 H3B 0.992(2) 1_555 ?
C3 C4 1.491(2) 1_555 ?
C4 H4A 0.9509(17) 1_555 ?
C4 H4B 0.960(2) 1_555 ?
C4 H4C 0.976(2) 1_555 ?
Mn1 B1 2.280(7) 1_555 ?
Mn1 H11 1.777(7) 1_555 ?
Mn1 H12 2.055(6) 1_555 ?
Mn1 B2 2.581(7) 4_564 ?
Mn1 B2 2.334(7) 7_656 ?
Mn1 H21 2.187(7) 4_564 ?
Mn1 H22 1.229(7) 7_656 ?
Mn1 H23 2.782(7) 7_656 ?
Mn1 H24 2.375(7) 4_564 ?
Mn1 B3 2.4509(20) 4_565 ?
Mn1 H31 2.017(3) 6_645 ?
Mn1 H32 2.023(4) 4_565 ?
Mn1 H33 2.028(4) 6_645 ?
Mn1 H34 2.024(4) 4_565 ?
B1 H11 1.129(7) 1_555 ?
B1 H12 1.130(10) 1_555 ?
B1 H13 1.131(8) 1_555 ?
B1 H14 1.131(8) 1_555 ?
B1 Li1 2.555(6) 5_545 ?
B2 H21 1.130(7) 1_555 ?
B2 H22 1.129(9) 1_555 ?
B2 H23 1.131(9) 1_555 ?
B2 H24 1.131(8) 1_555 ?
B3 H31 1.129(4) 1_555 ?
B3 H32 1.128(3) 1_555 ?
B3 H33 1.128(3) 1_555 ?
B3 H34 1.129(3) 1_555 ?
Li1 H13 1.936(6) 5_455 ?
Li1 H14 2.378(6) 5_455 ?


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
C2 O1 C3 113.24(17) 1_555 1_555 ?
H1A C1 H1B 109.1(3) 1_555 1_555 ?
H1A C1 H1C 108.8(3) 1_555 1_555 ?
H1A C1 C2 110.8(3) 1_555 1_555 ?
H1B C1 H1C 108.8(2) 1_555 1_555 ?
H1B C1 C2 109.7(2) 1_555 1_555 ?
H1C C1 C2 109.6(2) 1_555 1_555 ?
O1 C2 C1 103.01(20) 1_555 1_555 ?
O1 C2 H2A 120.5(2) 1_555 1_555 ?
O1 C2 H2B 108.0(2) 1_555 1_555 ?
C1 C2 H2A 110.0(2) 1_555 1_555 ?
C1 C2 H2B 109.1(2) 1_555 1_555 ?
H2A C2 H2B 105.9(2) 1_555 1_555 ?
O1 C3 H3A 107.6(2) 1_555 1_555 ?
O1 C3 H3B 112.5(2) 1_555 1_555 ?
O1 C3 C4 109.80(17) 1_555 1_555 ?
H3A C3 H3B 107.8(3) 1_555 1_555 ?
H3A C3 C4 108.4(2) 1_555 1_555 ?
H3B C3 C4 110.5(3) 1_555 1_555 ?
C3 C4 H4A 110.9(2) 1_555 1_555 ?
C3 C4 H4B 110.4(3) 1_555 1_555 ?
C3 C4 H4C 108.8(2) 1_555 1_555 ?
H4A C4 H4B 110.1(3) 1_555 1_555 ?
H4A C4 H4C 108.7(2) 1_555 1_555 ?
H4B C4 H4C 107.8(3) 1_555 1_555 ?
H11 B1 H12 109.4(9) 1_555 1_555 ?
H11 B1 H13 109.5(9) 1_555 1_555 ?
H11 B1 H14 109.4(8) 1_555 1_555 ?
H12 B1 H13 109.5(10) 1_555 1_555 ?
H12 B1 H14 109.6(10) 1_555 1_555 ?
H13 B1 H14 109.4(8) 1_555 1_555 ?
H21 B2 H22 109.4(9) 1_555 1_555 ?
H21 B2 H23 109.4(8) 1_555 1_555 ?
H21 B2 H24 109.5(8) 1_555 1_555 ?
H22 B2 H23 109.5(10) 1_555 1_555 ?
H22 B2 H24 109.6(9) 1_555 1_555 ?
H23 B2 H24 109.5(9) 1_555 1_555 ?
Mn1 H22 B2 163.5(9) 7_656 1_555 ?
H31 B3 H32 109.4(5) 1_555 1_555 ?
H31 B3 H33 109.6(5) 1_555 1_555 ?
H31 B3 H34 109.3(5) 1_555 1_555 ?
H32 B3 H33 109.6(4) 1_555 1_555 ?
H32 B3 H34 109.7(4) 1_555 1_555 ?
H33 B3 H34 109.3(4) 1_555 1_555 ?




# The following lines are used to test the character set of files sent by     
# network email or other means. They are not part of the CIF data set.        
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789              
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ 
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NaMn2BH4
_database_code_depnum_ccdc_archive 'CCDC 985622'
_audit_update_record             
;
2014-02-06 deposited with the CCDC.
2015-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            
'sodium dimanganese pentaborohydride bis(diethyl ether)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H40 B5 Mn2 Na O2'
_chemical_formula_sum            'C8 H40 B5 Mn2 Na O2'
_chemical_formula_weight         355.32

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   14.5133(6)
_cell_length_b                   7.4487(3)
_cell_length_c                   10.7119(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.338(5)
_cell_angle_gamma                90
_cell_volume                     1121.96(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1847
_cell_measurement_theta_min      3.0661
_cell_measurement_theta_max      25.2524

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_F_000             380
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    1.136
_shelx_estimated_absorpt_T_min   0.805
_shelx_estimated_absorpt_T_max   0.925
_exptl_absorpt_correction_T_min  0.54282
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 air-sensitive, crystal was mounted in argon-filled glovebox
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rigaku UltraX 18 rotating anode'
_diffrn_radiation_monochromator  'Xenocs Fox3D mirror'
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '111 images, ΔΦ 1.5° '
_diffrn_detector_area_resol_mean 6.666
_diffrn_reflns_number            4030
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.897
_diffrn_reflns_theta_max         26.045
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             2093
_reflns_number_gt                1808
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_max     0.899
_reflns_Friedel_fraction_full    0.946

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0959P)²+1.2554P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   diffmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 722 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2093
_refine_ls_number_parameters     115
_refine_ls_number_restraints     59
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0557
_refine_ls_wR_factor_ref         0.1545
_refine_ls_wR_factor_gt          0.1459
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.64376(5) 0.7750(2) 0.41977(8) 0.0417(4) Uani 1 1 d . . . . .
Na1 Na 0.5000 0.4893(7) 0.0000 0.0705(13) Uani 1 2 d S T P . .
B1 B 0.7658(6) 0.5376(13) 0.4823(10) 0.052(2) Uani 1 1 d D . . . .
H11 H 0.780(4) 0.650(5) 0.419(4) 0.062 Uiso 1 1 d D U . . .
H12 H 0.6895(18) 0.546(8) 0.491(6) 0.062 Uiso 1 1 d D U . . .
H13 H 0.777(4) 0.403(4) 0.440(5) 0.062 Uiso 1 1 d D U . . .
H14 H 0.815(4) 0.550(8) 0.582(3) 0.062 Uiso 1 1 d D U . . .
B2 B 0.5864(8) 0.7091(17) 0.1943(11) 0.069(3) Uani 1 1 d D . . . .
H21 H 0.614(4) 0.620(7) 0.127(5) 0.083 Uiso 1 1 d D U . . .
H22 H 0.587(5) 0.633(8) 0.286(4) 0.083 Uiso 1 1 d D U . . .
H23 H 0.634(4) 0.831(6) 0.219(6) 0.083 Uiso 1 1 d D U . . .
H24 H 0.512(2) 0.753(9) 0.147(5) 0.083 Uiso 1 1 d D U . . .
B3 B 0.5000 0.796(3) 0.5000 0.056(3) Uani 1 2 d DS T P . .
H31 H 0.507(5) 0.887(9) 0.418(5) 0.067 Uiso 1 1 d D U . . .
H32 H 0.433(3) 0.713(9) 0.467(6) 0.067 Uiso 1 1 d D U . . .
O1 O 0.4047(5) 0.2750(16) 0.0622(6) 0.0899(17) Uani 1 1 d D U . . .
C1 C 0.4448(7) 0.303(2) 0.2903(10) 0.084(4) Uani 1 1 d D U . . .
H1A H 0.5122 0.2844 0.2940 0.126 Uiso 1 1 calc R U . . .
H1B H 0.4311 0.2598 0.3702 0.126 Uiso 1 1 calc R U . . .
H1C H 0.4299 0.4315 0.2800 0.126 Uiso 1 1 calc R U . . .
C2 C 0.3846(8) 0.2009(16) 0.1770(10) 0.093(3) Uani 1 1 d D U . . .
H2A H 0.4007 0.0715 0.1844 0.112 Uiso 1 1 calc R U . . .
H2B H 0.3162 0.2147 0.1742 0.112 Uiso 1 1 calc R U . . .
C3 C 0.3647(10) 0.1528(18) -0.0383(14) 0.121(5) Uani 1 1 d D U . . .
H3A H 0.3599 0.0330 -0.0004 0.145 Uiso 1 1 calc R U . . .
H3B H 0.4079 0.1420 -0.0963 0.145 Uiso 1 1 calc R U . . .
C4 C 0.2710(11) 0.206(2) -0.1137(16) 0.150(7) Uani 1 1 d D U . . .
H4A H 0.2348 0.2586 -0.0566 0.225 Uiso 1 1 calc R U . . .
H4B H 0.2372 0.1010 -0.1573 0.225 Uiso 1 1 calc R U . . .
H4C H 0.2778 0.2955 -0.1781 0.225 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Mn1 B2 2.403(11) . ?
Mn1 B1 2.443(9) 4_656 ?
Mn1 B3 2.4505(15) . ?
Mn1 B1 2.475(9) . ?
Mn1 H11 2.19(6) . ?
Mn1 H12 1.92(6) . ?
Mn1 H22 1.80(6) . ?
Mn1 H23 2.16(7) . ?
Mn1 H31 2.15(9) . ?
Na1 O1 2.316(10) . ?
Na1 O1 2.316(10) 2_655 ?
Na1 B2 2.700(11) . ?
Na1 B2 2.700(11) 2_655 ?
Na1 H21 2.10(6) . ?
Na1 H24 2.49(6) . ?
B1 H11 1.124(12) . ?
B1 H12 1.134(12) . ?
B1 H13 1.127(12) . ?
B1 H14 1.132(12) . ?
B2 H21 1.129(12) . ?
B2 H22 1.132(12) . ?
B2 H23 1.132(12) . ?
B2 H24 1.126(12) . ?
B3 H31 1.133(14) . ?
B3 H32 1.133(14) . ?
O1 C3 1.420(11) . ?
O1 C2 1.442(10) . ?
C1 C2 1.513(11) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.455(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

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
B2 Mn1 B1 127.6(4) . 4_656 ?
B2 Mn1 B3 104.6(3) . . ?
B1 Mn1 B3 102.2(4) 4_656 . ?
B2 Mn1 B1 99.9(4) . . ?
B1 Mn1 B1 100.57(6) 4_656 . ?
B3 Mn1 B1 124.4(4) . . ?
B2 Mn1 H11 90.0(14) . . ?
B1 Mn1 H11 87.2(13) 4_656 . ?
B3 Mn1 H11 151.2(6) . . ?
B1 Mn1 H11 27.0(3) . . ?
B2 Mn1 H12 102.6(19) . . ?
B1 Mn1 H12 116.4(16) 4_656 . ?
B3 Mn1 H12 99.2(9) . . ?
B1 Mn1 H12 26.2(6) . . ?
H11 Mn1 H12 52.9(6) . . ?
B2 Mn1 H22 26.7(7) . . ?
B1 Mn1 H22 154.1(9) 4_656 . ?
B3 Mn1 H22 93.2(19) . . ?
B1 Mn1 H22 87.3(18) . . ?
H11 Mn1 H22 89(2) . . ?
H12 Mn1 H22 81(2) . . ?
B2 Mn1 H23 28.1(4) . . ?
B1 Mn1 H23 99.7(5) 4_656 . ?
B3 Mn1 H23 119.0(17) . . ?
B1 Mn1 H23 105.9(18) . . ?
H11 Mn1 H23 85(2) . . ?
H12 Mn1 H23 120(2) . . ?
H22 Mn1 H23 54.4(9) . . ?
B2 Mn1 H31 89.0(17) . . ?
B1 Mn1 H31 95.1(19) 4_656 . ?
B3 Mn1 H31 27.5(4) . . ?
B1 Mn1 H31 151.3(7) . . ?
H11 Mn1 H31 178(2) . . ?
H12 Mn1 H31 125.2(11) . . ?
H22 Mn1 H31 89(3) . . ?
H23 Mn1 H31 95(2) . . ?
O1 Na1 O1 92.8(5) . 2_655 ?
O1 Na1 B2 113.1(3) . . ?
O1 Na1 B2 116.3(3) 2_655 . ?
O1 Na1 B2 116.3(3) . 2_655 ?
O1 Na1 B2 113.1(3) 2_655 2_655 ?
B2 Na1 B2 105.4(6) . 2_655 ?
O1 Na1 H21 124.3(17) . . ?
O1 Na1 H21 94.1(8) 2_655 . ?
B2 Na1 H21 23.2(7) . . ?
B2 Na1 H21 111.1(18) 2_655 . ?
O1 Na1 H24 108.3(15) . . ?
O1 Na1 H24 140.5(5) 2_655 . ?
B2 Na1 H24 24.6(3) . . ?
B2 Na1 H24 87.4(11) 2_655 . ?
H21 Na1 H24 46.4(8) . . ?
Mn1 B1 Mn1 163.9(4) 4_646 . ?
Mn1 B1 H11 134(3) 4_646 . ?
Mn1 B1 H11 62(3) . . ?
Mn1 B1 H12 116(3) 4_646 . ?
Mn1 B1 H12 48(3) . . ?
H11 B1 H12 109.7(15) . . ?
Mn1 B1 H13 49(3) 4_646 . ?
Mn1 B1 H13 134(3) . . ?
H11 B1 H13 110.3(15) . . ?
H12 B1 H13 109.1(15) . . ?
Mn1 B1 H14 61(3) 4_646 . ?
Mn1 B1 H14 116(3) . . ?
H11 B1 H14 109.5(15) . . ?
H12 B1 H14 108.9(14) . . ?
H13 B1 H14 109.4(15) . . ?
Mn1 B2 Na1 151.4(5) . . ?
Mn1 B2 H21 132(3) . . ?
Na1 B2 H21 47(3) . . ?
Mn1 B2 H22 46(3) . . ?
Na1 B2 H22 106(3) . . ?
H21 B2 H22 109.6(15) . . ?
Mn1 B2 H23 64(3) . . ?
Na1 B2 H23 144(3) . . ?
H21 B2 H23 109.2(15) . . ?
H22 B2 H23 108.8(15) . . ?
Mn1 B2 H24 117(3) . . ?
Na1 B2 H24 67(3) . . ?
H21 B2 H24 109.8(15) . . ?
H22 B2 H24 109.8(15) . . ?
H23 B2 H24 109.6(15) . . ?
Mn1 B3 Mn1 172.6(9) . 2_656 ?
Mn1 B3 H31 61(4) . . ?
Mn1 B3 H31 124(4) 2_656 . ?
Mn1 B3 H32 127(4) . . ?
Mn1 B3 H32 48(4) 2_656 . ?
H31 B3 H32 108.8(18) . . ?
C3 O1 C2 105.6(11) . . ?
C3 O1 Na1 112.7(8) . . ?
C2 O1 Na1 140.4(6) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C1 107.0(8) . . ?
O1 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
O1 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
O1 C3 C4 113.3(11) . . ?
O1 C3 H3A 108.9 . . ?
C4 C3 H3A 108.9 . . ?
O1 C3 H3B 108.9 . . ?
C4 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 O1 C2 C1 167.3(11) . . . . ?
Na1 O1 C2 C1 2.1(17) . . . . ?
C2 O1 C3 C4 97.3(16) . . . . ?
Na1 O1 C3 C4 -92.8(15) . . . . ?

_refine_diff_density_max         0.565
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.076

_shelxl_version_number           2014-1



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Mn_pyr_long_ba
_database_code_depnum_ccdc_archive 'CCDC 985623'
_audit_update_record             
;
2014-02-06 deposited with the CCDC.
2015-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'manganese bisborohydride tris(pyridine)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H23 B2 Mn N3'
_chemical_formula_sum            'C15 H23 B2 Mn N3'
_chemical_formula_weight         321.92

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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'

_cell_length_a                   12.3618(4)
_cell_length_b                   15.5064(5)
_cell_length_c                   9.2859(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.126(4)
_cell_angle_gamma                90
_cell_volume                     1746.53(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3680
_cell_measurement_theta_min      2.8394
_cell_measurement_theta_max      26.0437

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_F_000             676
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.751
_shelx_estimated_absorpt_T_min   0.801
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_T_min  0.94888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 air-sensitive, crystal was mounted in argon-filled glovebox
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rigaku UltraX 18 rotating anode'
_diffrn_radiation_monochromator  'Xenocs Fox3D mirror'
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '110 images, ΔΦ 1.5° '
_diffrn_detector_area_resol_mean 6.666
_diffrn_reflns_number            5423
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.845
_diffrn_reflns_theta_max         26.100
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1702
_reflns_number_gt                1549
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   diffmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1702
_refine_ls_number_parameters     109
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1330
_refine_ls_wR_factor_gt          0.1264
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.5000 0.69086(2) 0.7500 0.0228(2) Uani 1 2 d S T P . .
C5 C 0.59710(18) 0.76898(14) 0.4765(2) 0.0294(5) Uani 1 1 d . . . . .
H5 H 0.5844 0.8225 0.5200 0.035 Uiso 1 1 calc R U . . .
N1 N 0.57341(16) 0.69609(10) 0.5427(2) 0.0267(4) Uani 1 1 d . . . . .
C1 C 0.59435(19) 0.62153(15) 0.4806(2) 0.0340(5) Uani 1 1 d . . . . .
H1 H 0.5799 0.5691 0.5264 0.041 Uiso 1 1 calc R U . . .
C3 C 0.6584(2) 0.69303(14) 0.2848(3) 0.0366(6) Uani 1 1 d . . . . .
H3 H 0.6865 0.6919 0.1965 0.044 Uiso 1 1 calc R U . . .
C4 C 0.63883(18) 0.77040(16) 0.3490(2) 0.0319(5) Uani 1 1 d . . . . .
H4 H 0.6538 0.8236 0.3061 0.038 Uiso 1 1 calc R U . . .
B1 B 0.33074(17) 0.62031(15) 0.6131(2) 0.0232(5) Uani 1 1 d D . . . .
H1B H 0.3410(17) 0.6913(5) 0.610(2) 0.035 Uiso 1 1 d D U . . .
H1C H 0.3255(15) 0.5920(11) 0.5007(11) 0.035 Uiso 1 1 d D U . . .
H1D H 0.2535(10) 0.6027(12) 0.6543(18) 0.035 Uiso 1 1 d D U . . .
H1A H 0.4036(11) 0.5894(11) 0.6896(16) 0.035 Uiso 1 1 d D U . . .
C2 C 0.6363(2) 0.61719(17) 0.3520(3) 0.0393(6) Uani 1 1 d . . . . .
H2 H 0.6496 0.5630 0.3111 0.047 Uiso 1 1 calc R U . . .
N2 N 0.5000 0.83571(16) 0.7500 0.0244(5) Uani 1 2 d S T P . .
C6 C 0.41962(16) 0.87992(14) 0.6644(2) 0.0310(5) Uani 1 1 d . . . . .
H6 H 0.3622 0.8488 0.6033 0.037 Uiso 1 1 calc R U . . .
C7 C 0.4164(2) 0.96904(16) 0.6610(4) 0.0628(9) Uani 1 1 d . . . . .
H7 H 0.3583 0.9990 0.5991 0.075 Uiso 1 1 calc R U . . .
C8 C 0.5000 1.0125(2) 0.7500 0.091(2) Uani 1 2 d S T P . .
H8 H 0.5000 1.0738 0.7500 0.109 Uiso 1 2 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Mn1 N2 2.246(3) . ?
Mn1 N1 2.2823(19) . ?
Mn1 N1 2.2823(19) 2_656 ?
Mn1 B1 2.483(2) . ?
Mn1 B1 2.483(2) 2_656 ?
C5 N1 1.346(3) . ?
C5 C4 1.380(3) . ?
N1 C1 1.340(3) . ?
C1 C2 1.392(3) . ?
C3 C4 1.382(3) . ?
C3 C2 1.383(3) . ?
N2 C6 1.336(2) . ?
N2 C6 1.336(2) 2_656 ?
C6 C7 1.383(3) . ?
C7 C8 1.369(3) . ?
C8 C7 1.369(3) 2_656 ?

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
N2 Mn1 N1 87.96(4) . . ?
N2 Mn1 N1 87.96(4) . 2_656 ?
N1 Mn1 N1 175.92(8) . 2_656 ?
N2 Mn1 B1 116.14(5) . . ?
N1 Mn1 B1 90.96(6) . . ?
N1 Mn1 B1 90.83(6) 2_656 . ?
N2 Mn1 B1 116.14(6) . 2_656 ?
N1 Mn1 B1 90.83(6) . 2_656 ?
N1 Mn1 B1 90.96(6) 2_656 2_656 ?
B1 Mn1 B1 127.72(11) . 2_656 ?
N1 C5 C4 123.8(2) . . ?
C1 N1 C5 116.8(2) . . ?
C1 N1 Mn1 118.29(14) . . ?
C5 N1 Mn1 124.92(13) . . ?
N1 C1 C2 123.1(2) . . ?
C4 C3 C2 118.5(2) . . ?
C5 C4 C3 118.8(2) . . ?
C3 C2 C1 119.0(2) . . ?
C6 N2 C6 118.2(3) . 2_656 ?
C6 N2 Mn1 120.88(14) . . ?
C6 N2 Mn1 120.88(14) 2_656 . ?
N2 C6 C7 122.8(2) . . ?
C8 C7 C6 117.6(3) . . ?
C7 C8 C7 121.1(4) 2_656 . ?

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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 C5 N1 C1 1.3(3) . . . . ?
C4 C5 N1 Mn1 -178.25(16) . . . . ?
C5 N1 C1 C2 -1.4(4) . . . . ?
Mn1 N1 C1 C2 178.27(18) . . . . ?
N1 C5 C4 C3 -0.4(3) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
C4 C3 C2 C1 0.6(4) . . . . ?
N1 C1 C2 C3 0.4(4) . . . . ?
C6 N2 C6 C7 0.0(2) 2_656 . . . ?
Mn1 N2 C6 C7 -180.0(2) . . . . ?
N2 C6 C7 C8 0.0(4) . . . . ?
C6 C7 C8 C7 0.01(19) . . . 2_656 ?

_refine_diff_density_max         0.538
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.062

_shelxl_version_number           2014-1



