#------------------------------------------------------------------------------
#$Date: 2018-07-10 12:13:45 +0300 (Tue, 10 Jul 2018) $
#$Revision: 208944 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/59/7115933.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_7115933
loop_
_publ_author_name
'Peili Zhang'
'Mei Wang'
'Yong Yang'
'Dehua Zheng'
'Kai Han'
'Licheng Sun'
_publ_section_title
;
 Highly efficient molecular nickel catalysts for electrochemical hydrogen
 production from neutral water
;
_journal_name_full               Chem.Commun.
_journal_page_first              14153
_journal_paper_doi               10.1039/C4cc05511J
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C25 H21 B2 F8 N6 Ni'
_chemical_formula_weight         644.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           190
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_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                   18.058(4)
_cell_length_b                   18.058(4)
_cell_length_c                   14.612(3)
_cell_measurement_temperature    296(2)
_cell_volume                     4126.5(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25339
_diffrn_reflns_theta_full        28.40
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.790
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1956
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.98(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1176P)²+0.7356P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.1834
_reflns_number_gt                2569
_reflns_number_total             3587
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc05511j2.cif
_cod_data_source_block           ok
_cod_depositor_comments
;

2018-06-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C150 H126 B12 F50 N36 Ni6'
_cod_original_formula_weight         3864.73
_cod_original_formula_units_Z            1
_cod_original_sg_symbol_H-M      P6cc
_cod_database_code               7115933
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+y, -x, -z+1/2'
'-y, x-y, z'
'x, y, -z+1/2'
'-x+y, -x, z'
'-y, x-y, -z+1/2'
'y, x, z+1/2'
'x-y, -y, -z'
'-x, -x+y, z+1/2'
'y, x, -z'
'x-y, -y, z+1/2'
'-x, -x+y, -z'
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 0.30308(5) 0.28662(5) 0.2500 0.0375(2) Uani 1 2 d S
N1 N 0.3150(2) 0.2075(2) 0.1543(2) 0.0423(8) Uani 1 1 d .
N3 N 0.4343(3) 0.3400(3) 0.2500 0.0375(10) Uani 1 2 d S
N4 N 0.3314(2) 0.3833(2) 0.3446(3) 0.0433(9) Uani 1 1 d .
N6 N 0.1736(4) 0.2265(4) 0.2500 0.0546(15) Uani 1 2 d S
C1 C 0.3957(4) 0.5410(4) 0.4260(4) 0.0708(16) Uani 1 1 d .
H1A H 0.4176 0.5945 0.4530 0.085 Uiso 1 1 calc R
C2 C 0.3109(4) 0.4915(4) 0.4105(5) 0.0714(18) Uani 1 1 d .
H2A H 0.2737 0.5102 0.4286 0.086 Uiso 1 1 calc R
C3 C 0.2880(4) 0.1173(4) 0.0254(4) 0.0641(16) Uani 1 1 d .
H3A H 0.2525 0.0865 -0.0231 0.077 Uiso 1 1 calc R
C4 C 0.3644(5) 0.1189(4) 0.0398(4) 0.0657(16) Uani 1 1 d .
H4A H 0.3805 0.0884 0.0014 0.079 Uiso 1 1 calc R
C6 C 0.2657(4) 0.1622(3) 0.0840(3) 0.0531(13) Uani 1 1 d .
H6A H 0.2143 0.1612 0.0745 0.064 Uiso 1 1 calc R
C7 C 0.0078(6) 0.1356(7) 0.2500 0.095(4) Uani 1 2 d S
C11 C 0.4160(4) 0.1653(3) 0.1106(4) 0.0537(12) Uani 1 1 d .
H11A H 0.4679 0.1675 0.1208 0.064 Uiso 1 1 calc R
C14 C 0.1021(4) 0.1878(5) 0.2500 0.0551(18) Uani 1 2 d S
C15 C 0.4384(4) 0.2596(4) 0.2500 0.0392(13) Uani 1 2 d S
H15A H 0.4975 0.2711 0.2500 0.047 Uiso 1 2 calc SR
C16 C 0.4494(4) 0.5100(3) 0.4005(4) 0.0554(13) Uani 1 1 d .
H16A H 0.5081 0.5426 0.4101 0.067 Uiso 1 1 calc R
C17 C 0.2798(4) 0.4142(4) 0.3684(4) 0.0590(15) Uani 1 1 d .
H17A H 0.2216 0.3820 0.3557 0.071 Uiso 1 1 calc R
C20 C 0.4143(3) 0.4304(3) 0.3609(3) 0.0443(10) Uani 1 1 d .
C22 C 0.3894(3) 0.2089(3) 0.1666(3) 0.0409(9) Uani 1 1 d .
C23 C 0.4688(3) 0.3929(3) 0.3337(4) 0.0470(11) Uani 1 1 d .
H23A H 0.5268 0.4386 0.3224 0.056 Uiso 1 1 calc R
H23B H 0.4703 0.3580 0.3832 0.056 Uiso 1 1 calc R
F17 F 0.0651(8) 0.0651(8) 0.0000 0.41(2) Uani 1 2 d S
F19 F 0.0000 0.0000 0.073(2) 0.69(6) Uani 1 3 d S
B5 B 0.0000 0.0000 0.0000 0.061(4) Uani 1 6 d S
F9 F 0.0593(6) 0.3392(7) 0.1762(4) 0.174(4) Uani 1 1 d .
F11 F 0.1277(8) 0.4494(9) 0.2500 0.252(9) Uani 1 2 d S
F12 F -0.0139(4) 0.3874(4) 0.2500 0.0919(18) Uani 1 2 d S
B3 B 0.0509(7) 0.3714(7) 0.2500 0.064(2) Uani 1 2 d S
F1 F 0.6217(3) 0.3709(3) 0.1323(3) 0.0946(13) Uani 1 1 d .
F4 F 0.6667 0.3333 0.0080(5) 0.0842(19) Uani 1 3 d S
B1 B 0.6667 0.3333 0.1033(7) 0.046(2) Uani 1 3 d S
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'
F F 0.0171 0.0103 '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'
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
N6 Ni1 N3 176.2(2) . .
N6 Ni1 N4 100.56(17) . .
N3 Ni1 N4 82.24(14) . .
N6 Ni1 N4 100.56(17) . 4
N3 Ni1 N4 82.23(14) . 4
N4 Ni1 N4 83.3(2) . 4
N6 Ni1 N1 96.85(17) . .
N3 Ni1 N1 80.37(15) . .
N4 Ni1 N1 162.59(15) . .
N4 Ni1 N1 93.62(15) 4 .
N6 Ni1 N1 96.85(17) . 4
N3 Ni1 N1 80.37(15) . 4
N4 Ni1 N1 93.62(15) . 4
N4 Ni1 N1 162.59(15) 4 4
N1 Ni1 N1 84.2(2) . 4
C6 N1 C22 117.9(4) . .
C6 N1 Ni1 132.0(4) . .
C22 N1 Ni1 110.0(3) . .
C23 N3 C23 111.0(5) . 4
C23 N3 C15 114.7(3) . .
C23 N3 C15 114.7(3) 4 .
C23 N3 Ni1 108.4(3) . .
C23 N3 Ni1 108.4(3) 4 .
C15 N3 Ni1 98.6(3) . .
C20 N4 C17 118.8(4) . .
C20 N4 Ni1 112.6(3) . .
C17 N4 Ni1 126.0(4) . .
C14 N6 Ni1 174.9(6) . .
C2 C1 C16 118.4(5) . .
C2 C1 H1A 120.8 . .
C16 C1 H1A 120.8 . .
C1 C2 C17 120.3(5) . .
C1 C2 H2A 119.8 . .
C17 C2 H2A 119.8 . .
C6 C3 C4 118.5(5) . .
C6 C3 H3A 120.8 . .
C4 C3 H3A 120.8 . .
C11 C4 C3 119.8(5) . .
C11 C4 H4A 120.1 . .
C3 C4 H4A 120.1 . .
N1 C6 C3 122.7(6) . .
N1 C6 H6A 118.7 . .
C3 C6 H6A 118.7 . .
C4 C11 C22 118.4(5) . .
C4 C11 H11A 120.8 . .
C22 C11 H11A 120.8 . .
N6 C14 C7 179.3(9) . .
N3 C15 C22 106.8(3) . 4
N3 C15 C22 106.8(3) . .
C22 C15 C22 107.1(5) 4 .
N3 C15 H15A 111.9 . .
C22 C15 H15A 111.9 4 .
C22 C15 H15A 111.9 . .
C20 C16 C1 118.9(5) . .
C20 C16 H16A 120.5 . .
C1 C16 H16A 120.5 . .
N4 C17 C2 121.5(6) . .
N4 C17 H17A 119.2 . .
C2 C17 H17A 119.2 . .
N4 C20 C16 122.0(5) . .
N4 C20 C23 116.7(4) . .
C16 C20 C23 121.3(5) . .
N1 C22 C11 122.7(5) . .
N1 C22 C15 113.4(4) . .
C11 C22 C15 123.9(4) . .
N3 C23 C20 110.5(4) . .
N3 C23 H23A 109.6 . .
C20 C23 H23A 109.6 . .
N3 C23 H23B 109.6 . .
C20 C23 H23B 109.6 . .
H23A C23 H23B 108.1 . .
B5 F17 F19 42.3(9) . 8
B5 F17 F19 42.3(9) . .
F19 F17 F19 84.6(18) 8 .
B5 F19 F17 47.7(9) . .
B5 F19 F17 47.7(9) . 3
F17 F19 F17 79.7(14) . 3
B5 F19 F17 47.7(9) . 5
F17 F19 F17 79.7(14) . 5
F17 F19 F17 79.7(14) 3 5
F19 B5 F19 179.998(1) . 8
F19 B5 F17 90.0 . .
F19 B5 F17 89.999(1) 8 .
F19 B5 F17 90.0 . 3
F19 B5 F17 90.002(1) 8 3
F17 B5 F17 120.0 . 3
F19 B5 F17 90.0 . 5
F19 B5 F17 90.0 8 5
F17 B5 F17 120.0 . 5
F17 B5 F17 120.0 3 5
F9 B3 F9 116.4(10) . 4
F9 B3 F12 114.6(6) . .
F9 B3 F12 114.6(6) 4 .
F9 B3 F11 100.1(8) . .
F9 B3 F11 100.1(8) 4 .
F12 B3 F11 108.4(10) . .
F1 B1 F1 110.7(5) 3_655 .
F1 B1 F1 110.7(5) 3_655 5_665
F1 B1 F1 110.7(5) . 5_665
F1 B1 F4 108.2(5) 3_655 .
F1 B1 F4 108.2(5) . .
F1 B1 F4 108.2(5) 5_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N6 2.027(6) .
Ni1 N3 2.063(5) .
Ni1 N4 2.080(4) .
Ni1 N4 2.080(4) 4
Ni1 N1 2.086(4) .
Ni1 N1 2.086(4) 4
N1 C6 1.336(6) .
N1 C22 1.343(6) .
N3 C23 1.484(5) .
N3 C23 1.484(5) 4
N3 C15 1.491(8) .
N4 C20 1.323(6) .
N4 C17 1.349(6) .
N6 C14 1.119(9) .
C1 C2 1.351(9) .
C1 C16 1.392(8) .
C1 H1A 0.9300 .
C2 C17 1.363(9) .
C2 H2A 0.9300 .
C3 C6 1.371(8) .
C3 C4 1.381(10) .
C3 H3A 0.9300 .
C4 C11 1.363(9) .
C4 H4A 0.9300 .
C6 H6A 0.9300 .
C7 C14 1.479(11) .
C11 C22 1.378(7) .
C11 H11A 0.9300 .
C15 C22 1.515(6) 4
C15 C22 1.515(6) .
C15 H15A 0.9800 .
C16 C20 1.376(7) .
C16 H16A 0.9300 .
C17 H17A 0.9300 .
C20 C23 1.499(7) .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
F17 B5 1.176(14) .
F17 F19 1.59(2) 8
F17 F19 1.59(2) .
F19 B5 1.07(3) .
F19 F17 1.59(2) 3
F19 F17 1.59(2) 5
B5 F19 1.07(3) 8
B5 F17 1.176(14) 3
B5 F17 1.176(14) 5
F9 B3 1.269(8) .
F11 B3 1.398(17) .
F12 B3 1.339(12) .
B3 F9 1.269(8) 4
F1 B1 1.359(5) .
F4 B1 1.392(13) .
B1 F1 1.359(5) 3_655
B1 F1 1.360(5) 5_665
