# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_PDJHK1a
_database_code_depnum_ccdc_archive 'CCDC 1906434'
loop_
_audit_author_name
_audit_author_address
'Phil Jeffrey'
;Princeton University
United States of America
;
_audit_update_record             
;
2019-03-29 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;
_chemical_name_systematic        
"Tetracarbonyl-(2,2'-bipyridine)-manganese hexafluoroantimonate dichloromethane solvate"
_chemical_name_common            HK1a
_chemical_formula_moiety         'C14 H8 N2 O4 Mn+, F6Sb-, (CH2Cl2)'
_chemical_formula_sum            'C15 H10 Cl2 F6 Mn N2 O4 Sb'
_chemical_formula_iupac          ?
_chemical_formula_weight         643.84

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_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'

_cell_length_a                   10.8094(7)
_cell_length_b                   17.2883(10)
_cell_length_c                   11.0181(7)
_cell_angle_alpha                90
_cell_angle_beta                 92.010(2)
_cell_angle_gamma                90
_cell_volume                     2057.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9839
_cell_measurement_theta_min      2.5945
_cell_measurement_theta_max      31.1019
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'translucent pale yellow'
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.141
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1240

_exptl_absorpt_coefficient_mu    2.265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_T_max  0.74

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'I\mS microfocus source'
_diffrn_source_type              ?

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?

_diffrn_measurement_device_type  'Bruker Photon 100 CMOS'
_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean 10.4167

_diffrn_reflns_number            66616
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15

_refine_special_details          
;
;

_reflns_number_total             6287
_reflns_number_gt                5735
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1027
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_restrained_S_all      1.206
_refine_ls_number_reflns         6287
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0238P)²+11.4660P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.428
_refine_diff_density_min         -1.402
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'Bruker Instrument Service vV6.2.6'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb Sb1 0.71168(2) 0.25218(2) 0.68374(2) 0.01672(7) Uani d . . . 1 . .
Mn Mn1 0.73502(5) 0.30675(3) 0.16828(5) 0.01170(10) Uani d . . . 1 . .
Cl Cl1 0.28170(10) 0.44249(6) 0.64549(10) 0.0286(2) Uani d . . . 1 . .
F F1 0.5620(2) 0.30530(17) 0.6987(3) 0.0339(6) Uani d . . . 1 . .
O O1 0.5505(3) 0.37093(18) 0.3377(3) 0.0258(6) Uani d . . . 1 . .
N N1 0.6844(3) 0.39072(17) 0.0452(3) 0.0141(5) Uani d . . . 1 . .
C C1 0.5908(3) 0.3859(2) -0.0375(3) 0.0175(7) Uani d . . . 1 . .
H H1 0.540881 0.34067 -0.039681 0.021 Uiso calc U . R 1 . .
Cl Cl2 0.33534(12) 0.52021(7) 0.42044(10) 0.0353(3) Uani d . . . 1 . .
F F2 0.6245(2) 0.17046(14) 0.6068(2) 0.0283(5) Uani d . . . 1 . .
O O2 0.5537(3) 0.18905(17) 0.0799(3) 0.0238(6) Uani d . . . 1 . .
N N2 0.8554(3) 0.39332(17) 0.2176(3) 0.0156(5) Uani d . . . 1 . .
C C2 0.5641(4) 0.4449(2) -0.1203(3) 0.0216(7) Uani d . . . 1 . .
H H2 0.497255 0.439887 -0.178163 0.026 Uiso calc U . R 1 . .
F F3 0.8587(2) 0.19645(15) 0.6693(3) 0.0345(6) Uani d . . . 1 . .
O O3 0.8252(3) 0.19245(17) 0.3523(3) 0.0256(6) Uani d . . . 1 . .
C C3 0.6363(4) 0.5106(2) -0.1170(4) 0.0244(8) Uani d . . . 1 . .
H H3 0.619604 0.551665 -0.172466 0.029 Uiso calc U . R 1 . .
F F4 0.7970(2) 0.33317(15) 0.7636(2) 0.0276(5) Uani d . . . 1 . .
O O4 0.9145(3) 0.24961(19) -0.0146(3) 0.0253(6) Uani d . . . 1 . .
C C4 0.7332(4) 0.5162(2) -0.0323(4) 0.0217(7) Uani d . . . 1 . .
H H4 0.783728 0.561184 -0.02886 0.026 Uiso calc U . R 1 . .
F F5 0.6873(3) 0.20547(17) 0.8348(2) 0.0377(7) Uani d . . . 1 . .
C C5 0.7557(3) 0.4555(2) 0.0475(3) 0.0167(6) Uani d . . . 1 . .
F F6 0.7354(3) 0.29941(16) 0.5346(2) 0.0365(7) Uani d . . . 1 . .
C C6 0.8544(3) 0.4563(2) 0.1436(3) 0.0171(6) Uani d . . . 1 . .
C C7 0.9389(4) 0.5161(2) 0.1609(4) 0.0245(8) Uani d . . . 1 . .
H H7 0.93942 0.55837 0.10585 0.029 Uiso calc U . R 1 . .
C C8 1.0224(4) 0.5137(2) 0.2591(5) 0.0294(9) Uani d . . . 1 . .
H H8 1.080845 0.554184 0.272232 0.035 Uiso calc U . R 1 . .
C C9 1.0192(4) 0.4514(2) 0.3375(4) 0.0265(8) Uani d . . . 1 . .
H H9 1.073837 0.449198 0.406882 0.032 Uiso calc U . R 1 . .
C C10 0.9356(4) 0.3923(2) 0.3138(4) 0.0207(7) Uani d . . . 1 . .
H H10 0.934729 0.349296 0.367431 0.025 Uiso calc U . R 1 . .
C C11 0.6199(3) 0.3465(2) 0.2759(3) 0.0163(6) Uani d . . . 1 . .
C C12 0.6229(3) 0.2349(2) 0.1130(3) 0.0156(6) Uani d . . . 1 . .
C C13 0.7926(3) 0.2369(2) 0.2825(3) 0.0172(6) Uani d . . . 1 . .
C C14 0.8504(3) 0.2708(2) 0.0530(3) 0.0149(6) Uani d . . . 1 . .
C C15 0.3455(4) 0.4324(2) 0.5016(4) 0.0249(8) Uani d . . . 1 . .
H H15A 0.300625 0.391422 0.455315 0.03 Uiso calc U . R 1 . .
H H15B 0.43338 0.416671 0.511346 0.03 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sb1 F6 . 1.860(3) ?
Sb1 F3 . 1.870(3) ?
Sb1 F1 . 1.873(2) ?
Sb1 F5 . 1.876(3) ?
Sb1 F4 . 1.878(2) ?
Sb1 F2 . 1.883(2) ?
Mn1 C12 . 1.826(4) ?
Mn1 C13 . 1.836(4) ?
Mn1 C11 . 1.879(4) ?
Mn1 C14 . 1.914(4) ?
Mn1 N2 . 2.044(3) ?
Mn1 N1 . 2.048(3) ?
Cl1 C15 . 1.760(4) ?
O1 C11 . 1.113(5) ?
N1 C1 . 1.341(5) ?
N1 C5 . 1.359(4) ?
C1 C2 . 1.391(5) ?
C1 H1 . 0.95 ?
Cl2 C15 . 1.763(4) ?
O2 C12 . 1.140(4) ?
N2 C10 . 1.345(5) ?
N2 C6 . 1.360(5) ?
C2 C3 . 1.379(6) ?
C2 H2 . 0.95 ?
O3 C13 . 1.135(5) ?
C3 C4 . 1.381(6) ?
C3 H3 . 0.95 ?
O4 C14 . 1.098(5) ?
C4 C5 . 1.386(5) ?
C4 H4 . 0.95 ?
C5 C6 . 1.477(5) ?
C6 C7 . 1.389(5) ?
C7 C8 . 1.384(7) ?
C7 H7 . 0.95 ?
C8 C9 . 1.383(7) ?
C8 H8 . 0.95 ?
C9 C10 . 1.384(5) ?
C9 H9 . 0.95 ?
C10 H10 . 0.95 ?
C15 H15A . 0.99 ?
C15 H15B . 0.99 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
F6 Sb1 F3 . . 90.41(13) ?
F6 Sb1 F1 . . 90.49(14) ?
F3 Sb1 F1 . . 178.36(12) ?
F6 Sb1 F5 . . 179.44(14) ?
F3 Sb1 F5 . . 90.00(14) ?
F1 Sb1 F5 . . 89.11(14) ?
F6 Sb1 F4 . . 90.33(13) ?
F3 Sb1 F4 . . 91.11(12) ?
F1 Sb1 F4 . . 90.26(12) ?
F5 Sb1 F4 . . 89.28(12) ?
F6 Sb1 F2 . . 90.81(13) ?
F3 Sb1 F2 . . 89.35(11) ?
F1 Sb1 F2 . . 89.27(11) ?
F5 Sb1 F2 . . 89.58(12) ?
F4 Sb1 F2 . . 178.77(12) ?
C12 Mn1 C13 . . 89.23(16) ?
C12 Mn1 C11 . . 90.75(16) ?
C13 Mn1 C11 . . 91.38(16) ?
C12 Mn1 C14 . . 89.88(15) ?
C13 Mn1 C14 . . 91.61(15) ?
C11 Mn1 C14 . . 176.95(15) ?
C12 Mn1 N2 . . 174.91(14) ?
C13 Mn1 N2 . . 95.84(14) ?
C11 Mn1 N2 . . 89.63(14) ?
C14 Mn1 N2 . . 89.47(14) ?
C12 Mn1 N1 . . 95.89(14) ?
C13 Mn1 N1 . . 174.79(15) ?
C11 Mn1 N1 . . 89.48(14) ?
C14 Mn1 N1 . . 87.48(13) ?
N2 Mn1 N1 . . 79.04(12) ?
C1 N1 C5 . . 118.5(3) ?
C1 N1 Mn1 . . 125.7(2) ?
C5 N1 Mn1 . . 115.7(2) ?
N1 C1 C2 . . 122.3(4) ?
N1 C1 H1 . . 118.8 ?
C2 C1 H1 . . 118.8 ?
C10 N2 C6 . . 118.3(3) ?
C10 N2 Mn1 . . 125.9(3) ?
C6 N2 Mn1 . . 115.8(2) ?
C3 C2 C1 . . 118.8(4) ?
C3 C2 H2 . . 120.6 ?
C1 C2 H2 . . 120.6 ?
C2 C3 C4 . . 119.4(4) ?
C2 C3 H3 . . 120.3 ?
C4 C3 H3 . . 120.3 ?
C3 C4 C5 . . 119.2(4) ?
C3 C4 H4 . . 120.4 ?
C5 C4 H4 . . 120.4 ?
N1 C5 C4 . . 121.7(4) ?
N1 C5 C6 . . 114.6(3) ?
C4 C5 C6 . . 123.7(3) ?
N2 C6 C7 . . 121.5(4) ?
N2 C6 C5 . . 114.4(3) ?
C7 C6 C5 . . 124.1(4) ?
C8 C7 C6 . . 119.5(4) ?
C8 C7 H7 . . 120.2 ?
C6 C7 H7 . . 120.2 ?
C9 C8 C7 . . 118.8(4) ?
C9 C8 H8 . . 120.6 ?
C7 C8 H8 . . 120.6 ?
C8 C9 C10 . . 119.2(4) ?
C8 C9 H9 . . 120.4 ?
C10 C9 H9 . . 120.4 ?
N2 C10 C9 . . 122.5(4) ?
N2 C10 H10 . . 118.7 ?
C9 C10 H10 . . 118.7 ?
O1 C11 Mn1 . . 178.5(3) ?
O2 C12 Mn1 . . 178.8(3) ?
O3 C13 Mn1 . . 178.0(4) ?
O4 C14 Mn1 . . 178.5(3) ?
Cl1 C15 Cl2 . . 110.6(2) ?
Cl1 C15 H15A . . 109.5 ?
Cl2 C15 H15A . . 109.5 ?
Cl1 C15 H15B . . 109.5 ?
Cl2 C15 H15B . . 109.5 ?
H15A C15 H15B . . 108.1 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C5 N1 C1 C2 . . . . -0.2(5) ?
Mn1 N1 C1 C2 . . . . -178.3(3) ?
N1 C1 C2 C3 . . . . -0.2(6) ?
C1 C2 C3 C4 . . . . 0.2(6) ?
C2 C3 C4 C5 . . . . 0.1(6) ?
C1 N1 C5 C4 . . . . 0.5(5) ?
Mn1 N1 C5 C4 . . . . 178.8(3) ?
C1 N1 C5 C6 . . . . 178.5(3) ?
Mn1 N1 C5 C6 . . . . -3.2(4) ?
C3 C4 C5 N1 . . . . -0.4(6) ?
C3 C4 C5 C6 . . . . -178.3(3) ?
C10 N2 C6 C7 . . . . 4.2(5) ?
Mn1 N2 C6 C7 . . . . -174.4(3) ?
C10 N2 C6 C5 . . . . -174.5(3) ?
Mn1 N2 C6 C5 . . . . 6.9(4) ?
N1 C5 C6 N2 . . . . -2.4(4) ?
C4 C5 C6 N2 . . . . 175.6(3) ?
N1 C5 C6 C7 . . . . 178.9(3) ?
C4 C5 C6 C7 . . . . -3.1(6) ?
N2 C6 C7 C8 . . . . -3.2(6) ?
C5 C6 C7 C8 . . . . 175.4(4) ?
C6 C7 C8 C9 . . . . 0.0(6) ?
C7 C8 C9 C10 . . . . 2.0(6) ?
C6 N2 C10 C9 . . . . -2.2(6) ?
Mn1 N2 C10 C9 . . . . 176.3(3) ?
C8 C9 C10 N2 . . . . -0.9(6) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C4 H4 F2 2_655 0.95 2.31 3.200(4) 155.1 ?
C15 H15B O1 . 0.99 2.46 3.095(5) 121.4 ?
C15 H15B Cl2 3_666 0.99 2.81 3.620(5) 139.9 ?
C15 H15A F5 4_565 0.99 2.44 3.430(5) 177.5 ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dichloromethane/Hexane'
_chemical_properties_physical    Light-sensitive,Photo-sensitive
