# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1477206'
_audit_update_record             
;
2016-04-29 deposited with the CCDC.
2016-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Cobalt Bis-hydridotris(3,5-dimethylpyrazole)borate '
_chemical_name_common            Co(Tp*)2
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H44 B2 Co N12'
_chemical_formula_sum            'C30 H44 B2 Co N12'
_chemical_formula_weight         653.32

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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8252(14)
_cell_length_b                   10.8259(17)
_cell_length_c                   11.028(3)
_cell_angle_alpha                106.446(3)
_cell_angle_beta                 108.868(3)
_cell_angle_gamma                109.701(2)
_cell_volume                     842.8(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2472
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      26.16

_exptl_crystal_description       strip
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.34
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             345
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5541
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         27.52
_reflns_number_total             3837
_reflns_number_gt                3274
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0714P)²+0.1439P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3837
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1258
_refine_ls_wR_factor_gt          0.1167
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001

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
Co1 Co 0.5000 0.5000 0.5000 0.03743(14) Uani 1 2 d S . .
N1 N 0.2785(2) 0.28980(18) 0.18506(17) 0.0424(4) Uani 1 1 d . . .
N2 N 0.2603(2) 0.36664(19) 0.29747(17) 0.0447(4) Uani 1 1 d . . .
N3 N 0.6023(2) 0.45967(19) 0.25892(17) 0.0418(4) Uani 1 1 d . . .
N4 N 0.6447(2) 0.56542(18) 0.38646(18) 0.0446(4) Uani 1 1 d . . .
N5 N 0.5316(2) 0.24847(18) 0.32480(17) 0.0407(4) Uani 1 1 d . . .
N6 N 0.5540(2) 0.31869(18) 0.45944(17) 0.0435(4) Uani 1 1 d . . .
C1 C 0.0929(4) 0.1248(3) -0.0763(2) 0.0649(7) Uani 1 1 d . . .
H1A H 0.1846 0.1772 -0.0977 0.097 Uiso 1 1 calc R . .
H1B H -0.0249 0.0960 -0.1491 0.097 Uiso 1 1 calc R . .
H1C H 0.1011 0.0395 -0.0730 0.097 Uiso 1 1 calc R . .
C2 C 0.1208(3) 0.2210(2) 0.0650(2) 0.0478(5) Uani 1 1 d . . .
C3 C -0.0032(3) 0.2528(3) 0.0999(3) 0.0563(6) Uani 1 1 d . . .
H3 H -0.1241 0.2200 0.0385 0.068 Uiso 1 1 calc R . .
C4 C 0.0908(3) 0.3443(2) 0.2463(2) 0.0508(5) Uani 1 1 d . . .
C5 C 0.0182(3) 0.4094(3) 0.3387(3) 0.0667(7) Uani 1 1 d . . .
H5A H 0.1168 0.4797 0.4316 0.100 Uiso 1 1 calc R . .
H5B H -0.0666 0.3334 0.3473 0.100 Uiso 1 1 calc R . .
H5C H -0.0419 0.4567 0.2961 0.100 Uiso 1 1 calc R . .
C6 C 0.5666(4) 0.0412(3) 0.1870(3) 0.0664(7) Uani 1 1 d . . .
H6A H 0.4435 -0.0132 0.1122 0.100 Uiso 1 1 calc R . .
H6B H 0.6086 -0.0253 0.2072 0.100 Uiso 1 1 calc R . .
H6C H 0.6423 0.0990 0.1573 0.100 Uiso 1 1 calc R . .
C7 C 0.5750(3) 0.1392(2) 0.3183(2) 0.0469(5) Uani 1 1 d . . .
C8 C 0.6266(3) 0.1390(2) 0.4490(2) 0.0528(5) Uani 1 1 d . . .
H8 H 0.6645 0.0762 0.4758 0.063 Uiso 1 1 calc R . .
C9 C 0.6110(3) 0.2514(2) 0.5340(2) 0.0484(5) Uani 1 1 d . . .
C10 C 0.6511(5) 0.2972(3) 0.6869(3) 0.0699(7) Uani 1 1 d . . .
H10A H 0.7800 0.3432 0.7462 0.105 Uiso 1 1 calc R . .
H10B H 0.5925 0.2129 0.6996 0.105 Uiso 1 1 calc R . .
H10C H 0.6067 0.3649 0.7130 0.105 Uiso 1 1 calc R . .
C11 C 0.6760(4) 0.4358(3) 0.0549(3) 0.0673(7) Uani 1 1 d . . .
H11A H 0.6591 0.3403 0.0442 0.101 Uiso 1 1 calc R . .
H11B H 0.7836 0.4861 0.0484 0.101 Uiso 1 1 calc R . .
H11C H 0.5727 0.4269 -0.0192 0.101 Uiso 1 1 calc R . .
C12 C 0.6954(3) 0.5205(3) 0.1975(2) 0.0498(5) Uani 1 1 d . . .
C13 C 0.8019(4) 0.6661(3) 0.2875(3) 0.0594(6) Uani 1 1 d . . .
H13 H 0.8832 0.7354 0.2743 0.071 Uiso 1 1 calc R . .
C14 C 0.7646(3) 0.6903(2) 0.4030(3) 0.0518(5) Uani 1 1 d . . .
C15 C 0.8445(4) 0.8322(3) 0.5312(3) 0.0728(8) Uani 1 1 d . . .
H15A H 0.8050 0.8142 0.5988 0.109 Uiso 1 1 calc R . .
H15B H 0.8050 0.8964 0.5024 0.109 Uiso 1 1 calc R . .
H15C H 0.9747 0.8767 0.5743 0.109 Uiso 1 1 calc R . .
B1 B 0.4651(3) 0.2989(3) 0.2091(2) 0.0423(5) Uani 1 1 d . . .
H1 H 0.4476 0.2282 0.1063 0.051 Uiso 1 1 d R . .


_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
Co1 N6 2.1334(16) 2_666 ?
Co1 N6 2.1334(16) . ?
Co1 N2 2.1465(17) 2_666 ?
Co1 N2 2.1465(17) . ?
Co1 N4 2.1509(17) . ?
Co1 N4 2.1509(17) 2_666 ?
N1 C2 1.340(3) . ?
N1 N2 1.375(2) . ?
N1 B1 1.544(3) . ?
N2 C4 1.321(3) . ?
N3 C12 1.347(3) . ?
N3 N4 1.374(2) . ?
N3 B1 1.550(3) . ?
N4 C14 1.324(3) . ?
N5 C7 1.351(3) . ?
N5 N6 1.375(2) . ?
N5 B1 1.548(3) . ?
N6 C9 1.333(3) . ?
C1 C2 1.494(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.384(3) . ?
C3 C4 1.397(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.506(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.496(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.365(3) . ?
C8 C9 1.389(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.495(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.498(3) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.366(4) . ?
C13 C14 1.392(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.500(3) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
B1 H1 1.1005 . ?

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
N6 Co1 N6 180.0 2_666 . ?
N6 Co1 N2 86.61(7) 2_666 2_666 ?
N6 Co1 N2 93.39(7) . 2_666 ?
N6 Co1 N2 93.39(7) 2_666 . ?
N6 Co1 N2 86.61(7) . . ?
N2 Co1 N2 180.0 2_666 . ?
N6 Co1 N4 93.51(6) 2_666 . ?
N6 Co1 N4 86.49(6) . . ?
N2 Co1 N4 92.49(7) 2_666 . ?
N2 Co1 N4 87.51(7) . . ?
N6 Co1 N4 86.49(6) 2_666 2_666 ?
N6 Co1 N4 93.51(6) . 2_666 ?
N2 Co1 N4 87.51(7) 2_666 2_666 ?
N2 Co1 N4 92.49(7) . 2_666 ?
N4 Co1 N4 180.000(1) . 2_666 ?
C2 N1 N2 109.81(17) . . ?
C2 N1 B1 130.34(17) . . ?
N2 N1 B1 119.77(16) . . ?
C4 N2 N1 107.11(17) . . ?
C4 N2 Co1 135.49(15) . . ?
N1 N2 Co1 117.21(12) . . ?
C12 N3 N4 109.77(18) . . ?
C12 N3 B1 130.91(18) . . ?
N4 N3 B1 119.32(15) . . ?
C14 N4 N3 106.62(16) . . ?
C14 N4 Co1 135.84(15) . . ?
N3 N4 Co1 117.40(12) . . ?
C7 N5 N6 109.36(16) . . ?
C7 N5 B1 130.40(17) . . ?
N6 N5 B1 120.24(15) . . ?
C9 N6 N5 106.52(16) . . ?
C9 N6 Co1 136.44(14) . . ?
N5 N6 Co1 117.01(12) . . ?
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 . . ?
N1 C2 C3 107.52(19) . . ?
N1 C2 C1 123.5(2) . . ?
C3 C2 C1 129.0(2) . . ?
C2 C3 C4 105.8(2) . . ?
C2 C3 H3 127.1 . . ?
C4 C3 H3 127.1 . . ?
N2 C4 C3 109.7(2) . . ?
N2 C4 C5 122.7(2) . . ?
C3 C4 C5 127.6(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N5 C7 C8 108.00(18) . . ?
N5 C7 C6 123.3(2) . . ?
C8 C7 C6 128.7(2) . . ?
C7 C8 C9 106.19(19) . . ?
C7 C8 H8 126.9 . . ?
C9 C8 H8 126.9 . . ?
N6 C9 C8 109.93(19) . . ?
N6 C9 C10 122.5(2) . . ?
C8 C9 C10 127.6(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C13 107.5(2) . . ?
N3 C12 C11 123.4(2) . . ?
C13 C12 C11 129.2(2) . . ?
C12 C13 C14 106.4(2) . . ?
C12 C13 H13 126.8 . . ?
C14 C13 H13 126.8 . . ?
N4 C14 C13 109.8(2) . . ?
N4 C14 C15 122.4(2) . . ?
C13 C14 C15 127.8(2) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 B1 N5 109.81(16) . . ?
N1 B1 N3 108.57(16) . . ?
N5 B1 N3 109.67(17) . . ?
N1 B1 H1 107.3 . . ?
N5 B1 H1 111.2 . . ?
N3 B1 H1 110.3 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.055
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'CH2Cl2 and iPrOH'
_exptl_crystal_preparation       'Magnetic properties'
