#------------------------------------------------------------------------------
#$Date: 2025-08-18 18:33:07 +0300 (Mon, 18 Aug 2025) $
#$Revision: 301779 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/03/1540385.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_1540385
loop_
_publ_author_name
'Eisenhart, Reed J.'
'Clouston, Laura J.'
'Lu, Connie C.'
_publ_section_title
;
 Configuring Bonds between First-Row Transition Metals.
;
_journal_issue                   11
_journal_name_full               'Accounts of chemical research'
_journal_page_first              2885
_journal_page_last               2894
_journal_paper_doi               10.1021/acs.accounts.5b00336
_journal_volume                  48
_journal_year                    2015
_chemical_formula_moiety         'C39 H60 B Cr F4 N4 Ni P3'
_chemical_formula_sum            'C39 H60 B Cr F4 N4 Ni P3'
_chemical_formula_weight         875.34
_chemical_name_common            '[NiCr][BF4]'
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.4121(8)
_cell_length_b                   12.4121(8)
_cell_length_c                   57.067(4)
_cell_measurement_reflns_used    2989
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.995
_cell_measurement_theta_min      2.308
_cell_volume                     7613.9(9)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            20420
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.8402
_exptl_absorpt_correction_T_min  0.8402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;

Unmodelable electron density was removed using PLATON SQUEEZE.Two molecules of disordered THF was removed from the asymmetric unit.
;
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0439P)²+3.6769P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                2346
_reflns_number_total             2989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ar5b00336_si_002.cif
_cod_data_source_block           12182s_NiCrL1BF4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1540381--1540386.cif.
;
_cod_original_cell_volume        7613.8(8)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               1540385
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Ni1 Ni 0.6667 0.3333 0.404071(9) 0.02481(16) Uani 1 3 d S
Cr1 Cr 0.6667 0.3333 0.446340(11) 0.02545(18) Uani 1 3 d S
P1 P 0.87109(6) 0.41371(6) 0.404153(11) 0.03019(18) Uani 1 1 d .
N1 N 0.6667 0.3333 0.48376(6) 0.0269(8) Uani 1 3 d S
N2 N 0.53003(18) 0.17259(18) 0.45048(3) 0.0298(5) Uani 1 1 d .
C1 C 0.5466(2) 0.2267(2) 0.49112(4) 0.0308(6) Uani 1 1 d .
C2 C 0.5008(2) 0.2093(2) 0.51350(4) 0.0354(6) Uani 1 1 d .
H2A H 0.5454 0.2698 0.5252 0.042 Uiso 1 1 calc R
C3 C 0.3898(3) 0.1040(3) 0.51899(5) 0.0404(7) Uani 1 1 d .
H3A H 0.3578 0.0915 0.5345 0.049 Uiso 1 1 calc R
C4 C 0.3256(3) 0.0169(3) 0.50181(5) 0.0414(7) Uani 1 1 d .
H4A H 0.2503 -0.0566 0.5057 0.050 Uiso 1 1 calc R
C5 C 0.3690(2) 0.0347(2) 0.47902(5) 0.0377(6) Uani 1 1 d .
H5A H 0.3232 -0.0259 0.4674 0.045 Uiso 1 1 calc R
C6 C 0.4808(2) 0.1423(2) 0.47313(4) 0.0310(6) Uani 1 1 d .
C7 C 0.4590(2) 0.0817(2) 0.43226(4) 0.0349(6) Uani 1 1 d .
H7A H 0.3765 0.0749 0.4305 0.042 Uiso 1 1 calc R
H7B H 0.4458 -0.0010 0.4369 0.042 Uiso 1 1 calc R
C8 C 0.9256(2) 0.3374(3) 0.38321(4) 0.0370(6) Uani 1 1 d .
H8A H 0.8857 0.2486 0.3883 0.044 Uiso 1 1 calc R
C9 C 1.0653(3) 0.3853(3) 0.38318(5) 0.0559(9) Uani 1 1 d .
H9A H 1.0927 0.3820 0.3991 0.084 Uiso 1 1 calc R
H9B H 1.1095 0.4714 0.3776 0.084 Uiso 1 1 calc R
H9C H 1.0833 0.3333 0.3728 0.084 Uiso 1 1 calc R
C10 C 0.8773(3) 0.3343(3) 0.35835(4) 0.0468(7) Uani 1 1 d .
H10A H 0.7877 0.3037 0.3589 0.070 Uiso 1 1 calc R
H10B H 0.8931 0.2787 0.3485 0.070 Uiso 1 1 calc R
H10C H 0.9203 0.4183 0.3517 0.070 Uiso 1 1 calc R
C11 C 0.9893(2) 0.5818(2) 0.40213(5) 0.0396(7) Uani 1 1 d .
H11A H 1.0724 0.5903 0.4053 0.048 Uiso 1 1 calc R
C12 C 0.9647(3) 0.6522(3) 0.42127(5) 0.0523(8) Uani 1 1 d .
H12A H 0.9547 0.6102 0.4363 0.078 Uiso 1 1 calc R
H12B H 0.8886 0.6541 0.4176 0.078 Uiso 1 1 calc R
H12C H 1.0349 0.7374 0.4222 0.078 Uiso 1 1 calc R
C13 C 0.9962(3) 0.6389(3) 0.37812(5) 0.0503(8) Uani 1 1 d .
H13A H 1.0494 0.7295 0.3791 0.075 Uiso 1 1 calc R
H13B H 0.9125 0.6183 0.3731 0.075 Uiso 1 1 calc R
H13C H 1.0313 0.6057 0.3667 0.075 Uiso 1 1 calc R
B1 B 0.3333 0.6667 0.42303(10) 0.0399(13) Uani 1 3 d S
F1 F 0.3333 0.6667 0.39905(5) 0.0563(8) Uani 1 3 d S
F2 F 0.3041(2) 0.75317(18) 0.43134(3) 0.0710(6) Uani 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 0.0033 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'
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'
Cr Cr 0.3209 0.6236 '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'
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
P1 Ni1 P1 120.0 2_655 .
P1 Ni1 P1 120.0 2_655 3_665
P1 Ni1 P1 120.0 . 3_665
P1 Ni1 Cr1 89.88(2) 2_655 .
P1 Ni1 Cr1 89.88(2) . .
P1 Ni1 Cr1 89.88(2) 3_665 .
N2 Cr1 N2 118.45(3) 2_655 3_665
N2 Cr1 N2 118.44(3) 2_655 .
N2 Cr1 N2 118.44(3) 3_665 .
N2 Cr1 N1 82.79(6) 2_655 .
N2 Cr1 N1 82.79(6) 3_665 .
N2 Cr1 N1 82.77(6) . .
N2 Cr1 Ni1 97.21(6) 2_655 .
N2 Cr1 Ni1 97.21(6) 3_665 .
N2 Cr1 Ni1 97.23(6) . .
N1 Cr1 Ni1 180.0 . .
C7 P1 C8 101.22(12) 2_655 .
C7 P1 C11 99.21(12) 2_655 .
C8 P1 C11 104.41(13) . .
C7 P1 Ni1 108.99(9) 2_655 .
C8 P1 Ni1 113.45(9) . .
C11 P1 Ni1 126.08(9) . .
C1 N1 C1 112.24(14) 3_665 2_655
C1 N1 C1 112.24(14) 3_665 .
C1 N1 C1 112.24(14) 2_655 .
C1 N1 Cr1 106.53(15) 3_665 .
C1 N1 Cr1 106.53(15) 2_655 .
C1 N1 Cr1 106.54(15) . .
C6 N2 C7 115.8(2) . .
C6 N2 Cr1 116.31(16) . .
C7 N2 Cr1 127.32(15) . .
C2 C1 C6 121.6(2) . .
C2 C1 N1 124.1(2) . .
C6 C1 N1 114.4(2) . .
C1 C2 C3 120.0(2) . .
C1 C2 H2A 120.0 . .
C3 C2 H2A 120.0 . .
C4 C3 C2 119.5(2) . .
C4 C3 H3A 120.2 . .
C2 C3 H3A 120.2 . .
C3 C4 C5 121.2(3) . .
C3 C4 H4A 119.4 . .
C5 C4 H4A 119.4 . .
C4 C5 C6 119.9(2) . .
C4 C5 H5A 120.1 . .
C6 C5 H5A 120.1 . .
N2 C6 C1 117.6(2) . .
N2 C6 C5 124.7(2) . .
C1 C6 C5 117.8(2) . .
N2 C7 P1 110.34(16) . 3_665
N2 C7 H7A 109.6 . .
P1 C7 H7A 109.6 3_665 .
N2 C7 H7B 109.6 . .
P1 C7 H7B 109.6 3_665 .
H7A C7 H7B 108.1 . .
C9 C8 C10 111.3(2) . .
C9 C8 P1 115.86(19) . .
C10 C8 P1 111.88(19) . .
C9 C8 H8A 105.6 . .
C10 C8 H8A 105.6 . .
P1 C8 H8A 105.6 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C12 C11 C13 111.0(2) . .
C12 C11 P1 109.09(18) . .
C13 C11 P1 114.01(19) . .
C12 C11 H11A 107.5 . .
C13 C11 H11A 107.5 . .
P1 C11 H11A 107.5 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
F1 B1 F2 110.1(2) . 3_565
F1 B1 F2 110.1(2) . 2_665
F2 B1 F2 108.8(2) 3_565 2_665
F1 B1 F2 110.1(2) . .
F2 B1 F2 108.8(2) 3_565 .
F2 B1 F2 108.8(2) 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 P1 2.2140(6) 2_655
Ni1 P1 2.2141(7) .
Ni1 P1 2.2141(7) 3_665
Ni1 Cr1 2.4122(8) .
Cr1 N2 1.8785(19) 2_655
Cr1 N2 1.8785(19) 3_665
Cr1 N2 1.879(2) .
Cr1 N1 2.135(3) .
P1 C7 1.840(2) 2_655
P1 C8 1.850(3) .
P1 C11 1.860(3) .
N1 C1 1.475(3) 3_665
N1 C1 1.475(3) 2_655
N1 C1 1.475(3) .
N2 C6 1.399(3) .
N2 C7 1.462(3) .
C1 C2 1.371(3) .
C1 C6 1.401(3) .
C2 C3 1.380(4) .
C2 H2A 0.9500 .
C3 C4 1.380(4) .
C3 H3A 0.9500 .
C4 C5 1.383(4) .
C4 H4A 0.9500 .
C5 C6 1.403(3) .
C5 H5A 0.9500 .
C7 P1 1.840(2) 3_665
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.526(4) .
C8 C10 1.533(4) .
C8 H8A 1.0000 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.522(4) .
C11 C13 1.525(4) .
C11 H11A 1.0000 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
B1 F1 1.368(6) .
B1 F2 1.378(3) 3_565
B1 F2 1.378(3) 2_665
B1 F2 1.378(3) .
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_4
P1 Ni1 Cr1 N2 -134.98(6) 2_655 2_655
P1 Ni1 Cr1 N2 -14.98(6) . 2_655
P1 Ni1 Cr1 N2 105.02(6) 3_665 2_655
P1 Ni1 Cr1 N2 -14.98(7) 2_655 3_665
P1 Ni1 Cr1 N2 105.02(7) . 3_665
P1 Ni1 Cr1 N2 -134.97(7) 3_665 3_665
P1 Ni1 Cr1 N2 105.02(6) 2_655 .
P1 Ni1 Cr1 N2 -134.98(6) . .
P1 Ni1 Cr1 N2 -14.97(6) 3_665 .
P1 Ni1 Cr1 N1 -87(8) 2_655 .
P1 Ni1 Cr1 N1 33(8) . .
P1 Ni1 Cr1 N1 153(8) 3_665 .
P1 Ni1 P1 C7 112.69(10) 2_655 2_655
P1 Ni1 P1 C7 -66.90(10) 3_665 2_655
Cr1 Ni1 P1 C7 22.90(9) . 2_655
P1 Ni1 P1 C8 -135.37(10) 2_655 .
P1 Ni1 P1 C8 45.04(11) 3_665 .
Cr1 Ni1 P1 C8 134.83(10) . .
P1 Ni1 P1 C11 -4.70(12) 2_655 .
P1 Ni1 P1 C11 175.70(10) 3_665 .
Cr1 Ni1 P1 C11 -94.50(11) . .
N2 Cr1 N1 C1 106.18(12) 2_655 3_665
N2 Cr1 N1 C1 -13.82(12) 3_665 3_665
N2 Cr1 N1 C1 -133.82(12) . 3_665
Ni1 Cr1 N1 C1 58(100) . 3_665
N2 Cr1 N1 C1 -13.82(12) 2_655 2_655
N2 Cr1 N1 C1 -133.82(12) 3_665 2_655
N2 Cr1 N1 C1 106.18(12) . 2_655
Ni1 Cr1 N1 C1 -62(100) . 2_655
N2 Cr1 N1 C1 -133.82(11) 2_655 .
N2 Cr1 N1 C1 106.18(11) 3_665 .
N2 Cr1 N1 C1 -13.82(11) . .
Ni1 Cr1 N1 C1 178(100) . .
N2 Cr1 N2 C6 90.17(17) 2_655 .
N2 Cr1 N2 C6 -65.3(2) 3_665 .
N1 Cr1 N2 C6 12.45(16) . .
Ni1 Cr1 N2 C6 -167.55(16) . .
N2 Cr1 N2 C7 -98.7(2) 2_655 .
N2 Cr1 N2 C7 105.8(2) 3_665 .
N1 Cr1 N2 C7 -176.5(2) . .
Ni1 Cr1 N2 C7 3.5(2) . .
C1 N1 C1 C2 -50.3(3) 3_665 .
C1 N1 C1 C2 77.3(3) 2_655 .
Cr1 N1 C1 C2 -166.5(2) . .
C1 N1 C1 C6 129.5(3) 3_665 .
C1 N1 C1 C6 -103.0(3) 2_655 .
Cr1 N1 C1 C6 13.3(2) . .
C6 C1 C2 C3 2.9(4) . .
N1 C1 C2 C3 -177.4(2) . .
C1 C2 C3 C4 -0.2(4) . .
C2 C3 C4 C5 -1.6(4) . .
C3 C4 C5 C6 0.6(4) . .
C7 N2 C6 C1 179.6(2) . .
Cr1 N2 C6 C1 -8.3(3) . .
C7 N2 C6 C5 -1.8(4) . .
Cr1 N2 C6 C5 170.4(2) . .
C2 C1 C6 N2 175.0(2) . .
N1 C1 C6 N2 -4.7(3) . .
C2 C1 C6 C5 -3.8(4) . .
N1 C1 C6 C5 176.5(2) . .
C4 C5 C6 N2 -176.7(2) . .
C4 C5 C6 C1 2.0(4) . .
C6 N2 C7 P1 -175.23(17) . 3_665
Cr1 N2 C7 P1 13.6(3) . 3_665
C7 P1 C8 C9 -61.0(2) 2_655 .
C11 P1 C8 C9 41.7(2) . .
Ni1 P1 C8 C9 -177.59(19) . .
C7 P1 C8 C10 170.03(19) 2_655 .
C11 P1 C8 C10 -87.3(2) . .
Ni1 P1 C8 C10 53.4(2) . .
C7 P1 C11 C12 -67.5(2) 2_655 .
C8 P1 C11 C12 -171.68(19) . .
Ni1 P1 C11 C12 54.2(2) . .
C7 P1 C11 C13 167.8(2) 2_655 .
C8 P1 C11 C13 63.6(2) . .
Ni1 P1 C11 C13 -70.5(2) . .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.008 0.485 -0.002 1943 504 ' '
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168302607
