# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_jyy104
_database_code_depnum_ccdc_archive 'CCDC 1541587'
_audit_update_record             
;
2017-04-01 deposited with the CCDC.
2017-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Ni(tmepe)2(BF4)2
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H64 B2 F8 Ni O8 P4'
_chemical_formula_weight         885.00

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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                   19.1558(19)
_cell_length_b                   12.2650(12)
_cell_length_c                   19.1620(19)
_cell_angle_alpha                90
_cell_angle_beta                 110.6513(11)
_cell_angle_gamma                90
_cell_volume                     4212.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9931
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      28.92

_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_F_000             1864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.444
_exptl_crystal_size_mid          0.423
_exptl_crystal_size_min          0.345
_exptl_absorpt_coefficient_mu    0.689
_shelx_estimated_absorpt_T_min   0.750
_shelx_estimated_absorpt_T_max   0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6939
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25493
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.012
_diffrn_reflns_theta_max         29.013
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5299
_reflns_number_gt                4615
_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       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0822P)²+8.3673P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5299
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1426
_refine_ls_wR_factor_gt          0.1366
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_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
Ni1 Ni 0.2500 0.7500 0.5000 0.01925(12) Uani 1 2 d S . P A .
C1 C 0.27013(13) 0.9328(2) 0.38350(13) 0.0308(5) Uani 1 1 d . . . . .
H1A H 0.2332 0.9844 0.3901 0.037 Uiso 1 1 calc R U . . .
H1B H 0.3038 0.9736 0.3638 0.037 Uiso 1 1 calc R U . . .
C2 C 0.23064(12) 0.8424(2) 0.32964(12) 0.0296(5) Uani 1 1 d . . . . .
H2A H 0.2668 0.8041 0.3119 0.036 Uiso 1 1 calc R U . . .
H2B H 0.1911 0.8741 0.2858 0.036 Uiso 1 1 calc R U . . .
P1 P 0.32369(3) 0.86917(5) 0.47259(3) 0.02389(14) Uani 1 1 d . . . . .
C11 C 0.39945(12) 0.7922(2) 0.45909(13) 0.0313(5) Uani 1 1 d . . . . .
H11A H 0.4342 0.7691 0.5087 0.038 Uiso 1 1 calc R U . . .
H11B H 0.3780 0.7252 0.4308 0.038 Uiso 1 1 calc R U . . .
C12 C 0.44467(13) 0.8504(3) 0.41876(13) 0.0376(6) Uani 1 1 d . . . . .
H12A H 0.4548 0.9266 0.4366 0.045 Uiso 1 1 calc R U . . .
H12B H 0.4930 0.8129 0.4288 0.045 Uiso 1 1 calc R U . . .
O11 O 0.40280(10) 0.84909(19) 0.34122(10) 0.0442(5) Uani 1 1 d . . . . .
C13 C 0.44435(16) 0.8997(4) 0.30150(16) 0.0559(9) Uani 1 1 d . . . . .
H13A H 0.4529 0.9765 0.3162 0.084 Uiso 1 1 calc R U . . .
H13B H 0.4164 0.8949 0.2478 0.084 Uiso 1 1 calc R U . . .
H13C H 0.4924 0.8625 0.3132 0.084 Uiso 1 1 calc R U . . .
C14 C 0.36890(13) 0.98470(19) 0.53135(13) 0.0316(5) Uani 1 1 d . . . . .
H14A H 0.4015 0.9576 0.5808 0.038 Uiso 1 1 calc R U . . .
H14B H 0.4006 1.0235 0.5083 0.038 Uiso 1 1 calc R U . . .
C15 C 0.31172(15) 1.0641(2) 0.54156(15) 0.0400(6) Uani 1 1 d . . . . .
H15A H 0.2937 1.1141 0.4983 0.048 Uiso 1 1 calc R U . . .
H15B H 0.2684 1.0234 0.5450 0.048 Uiso 1 1 calc R U . . .
O12 O 0.34632(12) 1.12486(16) 0.60817(11) 0.0458(5) Uani 1 1 d . . . . .
C16 C 0.2926(2) 1.1941(3) 0.6234(2) 0.0594(8) Uani 1 1 d . . . . .
H16A H 0.2730 1.2472 0.5830 0.089 Uiso 1 1 calc R U . . .
H16B H 0.3167 1.2327 0.6706 0.089 Uiso 1 1 calc R U . . .
H16C H 0.2516 1.1495 0.6270 0.089 Uiso 1 1 calc R U . . .
P2 P 0.18915(3) 0.74537(4) 0.37690(3) 0.02288(14) Uani 1 1 d . . . . .
C21 C 0.17783(16) 0.6220(2) 0.32048(13) 0.0383(6) Uani 1 1 d . . . . .
H21A H 0.1602 0.5626 0.3452 0.046 Uiso 1 1 calc R U . . .
H21B H 0.1384 0.6353 0.2715 0.046 Uiso 1 1 calc R U . . .
C22 C 0.2469(2) 0.5835(3) 0.3075(2) 0.0603(9) Uani 1 1 d . . . . .
H22A H 0.2367 0.5134 0.2800 0.072 Uiso 1 1 calc R U . . .
H22B H 0.2617 0.6376 0.2770 0.072 Uiso 1 1 calc R U . . .
O21 O 0.30502(13) 0.56976(19) 0.37674(16) 0.0623(7) Uani 1 1 d . . . . .
C23 C 0.3738(3) 0.5367(4) 0.3671(4) 0.116(2) Uani 1 1 d . . . . .
H23A H 0.3709 0.4593 0.3538 0.174 Uiso 1 1 calc R U . . .
H23B H 0.4158 0.5486 0.4138 0.174 Uiso 1 1 calc R U . . .
H23C H 0.3811 0.5800 0.3272 0.174 Uiso 1 1 calc R U . . .
C24A C 0.0927(10) 0.7883(11) 0.3543(12) 0.034(4) Uani 0.540(6) 1 d . . P A 1
H24A H 0.0705 0.8021 0.3000 0.040 Uiso 0.540(6) 1 calc R U P A 1
H24B H 0.0643 0.7283 0.3663 0.040 Uiso 0.540(6) 1 calc R U P A 1
C25A C 0.0839(3) 0.8974(4) 0.3986(5) 0.0318(11) Uani 0.540(6) 1 d . . P A 1
H25A H 0.0318 0.9035 0.3971 0.038 Uiso 0.540(6) 1 calc R U P A 1
H25B H 0.1171 0.8924 0.4515 0.038 Uiso 0.540(6) 1 calc R U P A 1
O22A O 0.1025(2) 0.9906(3) 0.3654(2) 0.0449(11) Uani 0.540(6) 1 d . . P A 1
C26A C 0.0919(4) 1.0873(5) 0.4057(5) 0.069(2) Uani 0.540(6) 1 d . . P A 1
H26A H 0.0398 1.0912 0.4025 0.104 Uiso 0.540(6) 1 calc R U P A 1
H26B H 0.1044 1.1529 0.3833 0.104 Uiso 0.540(6) 1 calc R U P A 1
H26C H 0.1245 1.0824 0.4581 0.104 Uiso 0.540(6) 1 calc R U P A 1
C24B C 0.0906(11) 0.7903(17) 0.3482(15) 0.040(6) Uani 0.460(6) 1 d . . P A 2
H24C H 0.0662 0.7730 0.2946 0.048 Uiso 0.460(6) 1 calc R U P A 2
H24D H 0.0660 0.7454 0.3757 0.048 Uiso 0.460(6) 1 calc R U P A 2
C25B C 0.0767(3) 0.8957(5) 0.3580(4) 0.0357(14) Uani 0.460(6) 1 d . . P A 2
H25C H 0.0228 0.9069 0.3477 0.043 Uiso 0.460(6) 1 calc R U P A 2
H25D H 0.0920 0.9428 0.3240 0.043 Uiso 0.460(6) 1 calc R U P A 2
O22B O 0.1189(3) 0.9212(3) 0.4337(3) 0.0349(11) Uani 0.460(6) 1 d . . P A 2
C26B C 0.1031(4) 1.0275(7) 0.4549(5) 0.059(2) Uani 0.460(6) 1 d . . P A 2
H26D H 0.1234 1.0827 0.4304 0.088 Uiso 0.460(6) 1 calc R U P A 2
H26E H 0.1260 1.0356 0.5092 0.088 Uiso 0.460(6) 1 calc R U P A 2
H26F H 0.0489 1.0370 0.4398 0.088 Uiso 0.460(6) 1 calc R U P A 2
B1 B 0.09514(17) 0.7152(3) 0.11365(16) 0.0360(6) Uani 1 1 d . . . . .
F1 F 0.08729(10) 0.77565(14) 0.17141(9) 0.0454(4) Uani 1 1 d . . . . .
F2 F 0.04209(11) 0.63226(16) 0.09690(12) 0.0647(6) Uani 1 1 d . . . . .
F3 F 0.16617(11) 0.66945(17) 0.13816(14) 0.0654(6) Uani 1 1 d . . . . .
F4 F 0.08286(16) 0.7806(2) 0.05221(11) 0.0784(7) Uani 1 1 d . . . . .


_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
Ni1 P1 2.2199(5) 7_566 ?
Ni1 P1 2.2199(5) . ?
Ni1 P2 2.2330(6) . ?
Ni1 P2 2.2331(6) 7_566 ?
C1 C2 1.522(3) . ?
C1 P1 1.828(2) . ?
C2 P2 1.837(2) . ?
P1 C11 1.825(2) . ?
P1 C14 1.827(2) . ?
C11 C12 1.526(3) . ?
C12 O11 1.418(3) . ?
O11 C13 1.423(3) . ?
C14 C15 1.529(4) . ?
C15 O12 1.424(3) . ?
O12 C16 1.441(4) . ?
P2 C24A 1.821(18) . ?
P2 C21 1.828(3) . ?
P2 C24B 1.85(2) . ?
C21 C22 1.506(5) . ?
C22 O21 1.410(5) . ?
O21 C23 1.452(4) . ?
C24A C25A 1.63(2) . ?
C25A O22A 1.414(6) . ?
O22A C26A 1.467(8) . ?
C24B C25B 1.35(2) . ?
C25B O22B 1.425(8) . ?
O22B C26B 1.429(8) . ?
B1 F4 1.375(4) . ?
B1 F1 1.384(3) . ?
B1 F3 1.391(4) . ?
B1 F2 1.393(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
P1 Ni1 P1 180.0 7_566 . ?
P1 Ni1 P2 95.429(19) 7_566 . ?
P1 Ni1 P2 84.572(19) . . ?
P1 Ni1 P2 84.572(19) 7_566 7_566 ?
P1 Ni1 P2 95.43(2) . 7_566 ?
P2 Ni1 P2 180.00(3) . 7_566 ?
C2 C1 P1 107.64(16) . . ?
C1 C2 P2 109.62(15) . . ?
C11 P1 C14 105.13(11) . . ?
C11 P1 C1 107.53(11) . . ?
C14 P1 C1 103.43(11) . . ?
C11 P1 Ni1 107.26(8) . . ?
C14 P1 Ni1 124.58(8) . . ?
C1 P1 Ni1 107.93(7) . . ?
C12 C11 P1 116.83(19) . . ?
O11 C12 C11 108.23(19) . . ?
C12 O11 C13 109.8(2) . . ?
C15 C14 P1 111.57(16) . . ?
O12 C15 C14 108.7(2) . . ?
C15 O12 C16 110.5(2) . . ?
C24A P2 C21 101.5(6) . . ?
C24A P2 C2 105.9(4) . . ?
C21 P2 C2 103.10(12) . . ?
C21 P2 C24B 100.0(8) . . ?
C2 P2 C24B 103.5(6) . . ?
C24A P2 Ni1 110.6(7) . . ?
C21 P2 Ni1 123.69(9) . . ?
C2 P2 Ni1 110.41(7) . . ?
C24B P2 Ni1 113.8(9) . . ?
C22 C21 P2 115.4(2) . . ?
O21 C22 C21 109.2(2) . . ?
C22 O21 C23 111.4(4) . . ?
C25A C24A P2 113.4(11) . . ?
O22A C25A C24A 109.9(7) . . ?
C25A O22A C26A 108.3(5) . . ?
C25B C24B P2 118.4(14) . . ?
C24B C25B O22B 106.4(12) . . ?
C25B O22B C26B 112.9(5) . . ?
F4 B1 F1 109.8(3) . . ?
F4 B1 F3 112.1(3) . . ?
F1 B1 F3 108.4(2) . . ?
F4 B1 F2 109.8(2) . . ?
F1 B1 F2 107.4(2) . . ?
F3 B1 F2 109.3(2) . . ?

_refine_diff_density_max         1.189
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.088

