#------------------------------------------------------------------------------
#$Date: 2024-04-05 01:35:02 +0200 (Fri 05 de Apr de 2024) $
#$Revision: 290978 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/52/7715216.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_7715216
loop_
_publ_author_name
'Luff, Martin S.'
'Walther, Luis'
'Finze, Maik'
'Radius, Udo'
_publ_section_title
;
 NHC-ligated nickel(II) cyanoborate complexes and salts.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5391
_journal_page_last               5400
_journal_paper_doi               10.1039/d4dt00231h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C26 H44 B2 N8 Ni'
_chemical_formula_sum            'C26 H44 B2 N8 Ni'
_chemical_formula_weight         549.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-01-24 deposited with the CCDC.	2024-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                69.393(6)
_cell_angle_beta                 85.022(5)
_cell_angle_gamma                74.058(5)
_cell_formula_units_Z            1
_cell_length_a                   8.9341(5)
_cell_length_b                   9.5418(6)
_cell_length_c                   10.1375(6)
_cell_measurement_reflns_used    10775
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9530
_cell_measurement_theta_min      2.3510
_cell_volume                     777.74(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.810
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1178
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13816
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.079
_diffrn_reflns_theta_min         2.146
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.290
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       block
_exptl_crystal_F_000             294
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.290
_refine_diff_density_max         0.656
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         4040
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1563P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2095
_refine_ls_wR_factor_ref         0.2283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3206
_reflns_number_total             4040
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00231h2.cif
_cod_data_source_block           Compound_trans_15b
_cod_depositor_comments
'Adding full bibliography for 7715213--7715230.cif.'
_cod_database_code               7715216
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.790
_shelx_estimated_absorpt_t_max   0.834
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_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
Ni01 Ni 0.500000 0.500000 0.500000 0.0412(2) Uani 1 2 d S . P . .
H1 H 0.579(5) 0.131(5) 0.239(4) 0.062 Uiso 1 1 d . U . . .
H1A H 0.435(4) 0.045(5) 0.379(4) 0.062 Uiso 1 1 d . U . . .
C1 C 0.7049(3) 0.3633(3) 0.5573(3) 0.0351(5) Uani 1 1 d . . . . .
N2 N 0.8259(2) 0.3390(2) 0.47169(19) 0.0262(4) Uani 1 1 d . . . . .
C3 C 0.9509(2) 0.2213(2) 0.5476(2) 0.0268(4) Uani 1 1 d . . . . .
C4 C 0.9045(3) 0.1732(3) 0.6827(2) 0.0344(5) Uani 1 1 d . . . . .
N5 N 0.7521(2) 0.2637(3) 0.6859(2) 0.0424(6) Uani 1 1 d . . . . .
C6 C 0.8206(3) 0.4358(3) 0.3199(2) 0.0352(5) Uani 1 1 d . . . . .
H6 H 0.711034 0.501424 0.299257 0.042 Uiso 1 1 calc R U . . .
C7 C 0.9220(4) 0.5476(4) 0.2914(3) 0.0565(9) Uani 1 1 d . . . . .
H00N H 1.031708 0.489045 0.305184 0.085 Uiso 1 1 calc R U . . .
H00O H 0.894560 0.605920 0.356396 0.085 Uiso 1 1 calc R U . . .
H00P H 0.905099 0.619762 0.194074 0.085 Uiso 1 1 calc R U . . .
C8 C 0.8528(4) 0.3408(4) 0.2235(3) 0.0518(8) Uani 1 1 d . . . . .
H00K H 0.824833 0.409560 0.126393 0.078 Uiso 1 1 calc R U . . .
H00L H 0.790750 0.264903 0.252987 0.078 Uiso 1 1 calc R U . . .
H00M H 0.963643 0.286403 0.228818 0.078 Uiso 1 1 calc R U . . .
C9_11 C 0.6759(7) 0.1945(9) 0.8331(7) 0.0378(13) Uiso 0.415(6) 1 d D U P A 1
H9_11 H 0.737829 0.084855 0.878710 0.045 Uiso 0.415(6) 1 calc R U P A 1
C10_11 C 0.701(2) 0.2887(14) 0.9177(15) 0.041(2) Uani 0.415(6) 1 d D U P A 1
H10A_11 H 0.666719 0.246388 1.014606 0.061 Uiso 0.415(6) 1 calc R U P A 1
H10B_11 H 0.641471 0.396810 0.875027 0.061 Uiso 0.415(6) 1 calc R U P A 1
H10C_11 H 0.812242 0.283939 0.918311 0.061 Uiso 0.415(6) 1 calc R U P A 1
C11_11 C 0.5148(8) 0.1925(8) 0.8137(7) 0.0358(13) Uani 0.415(6) 1 d D U P A 1
H11A_11 H 0.468634 0.152105 0.906008 0.054 Uiso 0.415(6) 1 calc R U P A 1
H11B_11 H 0.515373 0.125846 0.758821 0.054 Uiso 0.415(6) 1 calc R U P A 1
H11C_11 H 0.453329 0.298133 0.763442 0.054 Uiso 0.415(6) 1 calc R U P A 1
C9_12 C 0.6405(5) 0.2822(4) 0.8005(4) 0.0277(9) Uani 0.585(6) 1 d D U P A 2
H9_12 H 0.544898 0.364782 0.755974 0.033 Uiso 0.585(6) 1 calc R U P A 2
C10_12 C 0.6999(14) 0.3281(9) 0.9086(10) 0.0358(15) Uani 0.585(6) 1 d D U P A 2
H10A_12 H 0.619084 0.339738 0.978662 0.054 Uiso 0.585(6) 1 calc R U P A 2
H10B_12 H 0.727139 0.426763 0.862616 0.054 Uiso 0.585(6) 1 calc R U P A 2
H10C_12 H 0.792467 0.247704 0.955440 0.054 Uiso 0.585(6) 1 calc R U P A 2
C11_12 C 0.5950(8) 0.1274(6) 0.8661(6) 0.0507(13) Uani 0.585(6) 1 d D U P A 2
H11A_12 H 0.513365 0.137035 0.935952 0.076 Uiso 0.585(6) 1 calc R U P A 2
H11B_12 H 0.686419 0.044738 0.912150 0.076 Uiso 0.585(6) 1 calc R U P A 2
H11C_12 H 0.556279 0.102167 0.792026 0.076 Uiso 0.585(6) 1 calc R U P A 2
C12 C 1.1047(3) 0.1648(3) 0.4857(3) 0.0392(6) Uani 1 1 d . . . . .
H00A H 1.091497 0.106699 0.426740 0.059 Uiso 1 1 calc R U . . .
H12 H 1.179519 0.097185 0.561786 0.059 Uiso 1 1 calc R U . . .
H00D H 1.143608 0.253835 0.428034 0.059 Uiso 1 1 calc R U . . .
C13 C 0.9952(4) 0.0524(4) 0.8085(3) 0.0545(8) Uani 1 1 d . . . . .
H00E H 1.094490 -0.001169 0.777771 0.082 Uiso 1 1 calc R U . . .
H00F H 0.935383 -0.022809 0.857516 0.082 Uiso 1 1 calc R U . . .
H00G H 1.015027 0.102035 0.872571 0.082 Uiso 1 1 calc R U . . .
B1_2 B 0.4605(3) 0.1551(3) 0.2925(3) 0.0314(5) Uani 1 1 d . . . . .
C2_2 C 0.4612(3) 0.2776(3) 0.3662(3) 0.0344(5) Uani 1 1 d . . . . .
N3_2 N 0.4685(2) 0.3627(3) 0.4201(2) 0.0395(5) Uani 1 1 d . . . . .
C4_2 C 0.3350(3) 0.2294(3) 0.1687(2) 0.0339(5) Uani 1 1 d . . . . .
N5_2 N 0.2467(3) 0.2784(4) 0.0782(3) 0.0562(7) 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'
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
_geom_angle_publ_flag
N3_2 Ni01 N3_2 180.00(12) 2_666 . ?
N3_2 Ni01 C1 92.02(9) 2_666 . ?
N3_2 Ni01 C1 87.98(9) . . ?
N3_2 Ni01 C1 87.98(9) 2_666 2_666 ?
N3_2 Ni01 C1 92.01(9) . 2_666 ?
C1 Ni01 C1 180.0 . 2_666 ?
N5 C1 N2 105.8(2) . . ?
N5 C1 Ni01 127.7(2) . . ?
N2 C1 Ni01 126.30(19) . . ?
C1 N2 C3 110.61(19) . . ?
C1 N2 C6 121.6(2) . . ?
C3 N2 C6 127.73(19) . . ?
C4 C3 N2 106.4(2) . . ?
C4 C3 C12 128.7(2) . . ?
N2 C3 C12 124.9(2) . . ?
C3 C4 N5 106.4(2) . . ?
C3 C4 C13 128.5(3) . . ?
N5 C4 C13 125.1(2) . . ?
C1 N5 C4 110.8(2) . . ?
C1 N5 C9_12 114.6(2) . . ?
C4 N5 C9_12 134.3(2) . . ?
C1 N5 C9_11 137.7(3) . . ?
C4 N5 C9_11 110.0(3) . . ?
N2 C6 C8 112.9(2) . . ?
N2 C6 C7 111.1(2) . . ?
C8 C6 C7 113.7(3) . . ?
N2 C6 H6 106.2 . . ?
C8 C6 H6 106.2 . . ?
C7 C6 H6 106.2 . . ?
C6 C7 H00N 109.5 . . ?
C6 C7 H00O 109.5 . . ?
H00N C7 H00O 109.5 . . ?
C6 C7 H00P 109.5 . . ?
H00N C7 H00P 109.5 . . ?
H00O C7 H00P 109.5 . . ?
C6 C8 H00K 109.5 . . ?
C6 C8 H00L 109.5 . . ?
H00K C8 H00L 109.5 . . ?
C6 C8 H00M 109.5 . . ?
H00K C8 H00M 109.5 . . ?
H00L C8 H00M 109.5 . . ?
C11_11 C9_11 C10_11 118.0(9) . . ?
C11_11 C9_11 N5 110.7(5) . . ?
C10_11 C9_11 N5 103.9(8) . . ?
C11_11 C9_11 H9_11 107.9 . . ?
C10_11 C9_11 H9_11 107.9 . . ?
N5 C9_11 H9_11 107.9 . . ?
C9_11 C10_11 H10A_11 109.5 . . ?
C9_11 C10_11 H10B_11 109.5 . . ?
H10A_11 C10_11 H10B_11 109.5 . . ?
C9_11 C10_11 H10C_11 109.5 . . ?
H10A_11 C10_11 H10C_11 109.5 . . ?
H10B_11 C10_11 H10C_11 109.5 . . ?
C9_11 C11_11 H11A_11 109.5 . . ?
C9_11 C11_11 H11B_11 109.5 . . ?
H11A_11 C11_11 H11B_11 109.5 . . ?
C9_11 C11_11 H11C_11 109.5 . . ?
H11A_11 C11_11 H11C_11 109.5 . . ?
H11B_11 C11_11 H11C_11 109.5 . . ?
N5 C9_12 C10_12 114.7(6) . . ?
N5 C9_12 C11_12 106.2(3) . . ?
C10_12 C9_12 C11_12 112.2(5) . . ?
N5 C9_12 H9_12 107.8 . . ?
C10_12 C9_12 H9_12 107.8 . . ?
C11_12 C9_12 H9_12 107.8 . . ?
C9_12 C10_12 H10A_12 109.5 . . ?
C9_12 C10_12 H10B_12 109.5 . . ?
H10A_12 C10_12 H10B_12 109.5 . . ?
C9_12 C10_12 H10C_12 109.5 . . ?
H10A_12 C10_12 H10C_12 109.5 . . ?
H10B_12 C10_12 H10C_12 109.5 . . ?
C9_12 C11_12 H11A_12 109.5 . . ?
C9_12 C11_12 H11B_12 109.5 . . ?
H11A_12 C11_12 H11B_12 109.5 . . ?
C9_12 C11_12 H11C_12 109.5 . . ?
H11A_12 C11_12 H11C_12 109.5 . . ?
H11B_12 C11_12 H11C_12 109.5 . . ?
C3 C12 H00A 109.5 . . ?
C3 C12 H12 109.5 . . ?
H00A C12 H12 109.5 . . ?
C3 C12 H00D 109.5 . . ?
H00A C12 H00D 109.5 . . ?
H12 C12 H00D 109.5 . . ?
C4 C13 H00E 109.5 . . ?
C4 C13 H00F 109.5 . . ?
H00E C13 H00F 109.5 . . ?
C4 C13 H00G 109.5 . . ?
H00E C13 H00G 109.5 . . ?
H00F C13 H00G 109.5 . . ?
C4_2 B1_2 C2_2 110.30(19) . . ?
C4_2 B1_2 H1 105.5(19) . . ?
C2_2 B1_2 H1 107(2) . . ?
C4_2 B1_2 H1A 112.0(19) . . ?
C2_2 B1_2 H1A 107.8(19) . . ?
H1 B1_2 H1A 114(3) . . ?
N3_2 C2_2 B1_2 177.0(2) . . ?
C2_2 N3_2 Ni01 174.3(2) . . ?
N5_2 C4_2 B1_2 177.6(3) . . ?
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
Ni01 N3_2 1.855(2) 2_666 ?
Ni01 N3_2 1.855(2) . ?
Ni01 C1 1.931(2) . ?
Ni01 C1 1.931(2) 2_666 ?
C1 N5 1.335(3) . ?
C1 N2 1.348(3) . ?
N2 C3 1.397(3) . ?
N2 C6 1.487(3) . ?
C3 C4 1.350(3) . ?
C3 C12 1.502(3) . ?
C4 N5 1.402(3) . ?
C4 C13 1.498(3) . ?
N5 C9_12 1.491(4) . ?
N5 C9_11 1.582(7) . ?
C6 C8 1.514(4) . ?
C6 C7 1.520(4) . ?
C6 H6 1.0000 . ?
C7 H00N 0.9800 . ?
C7 H00O 0.9800 . ?
C7 H00P 0.9800 . ?
C8 H00K 0.9800 . ?
C8 H00L 0.9800 . ?
C8 H00M 0.9800 . ?
C9_11 C11_11 1.476(9) . ?
C9_11 C10_11 1.511(12) . ?
C9_11 H9_11 1.0000 . ?
C10_11 H10A_11 0.9800 . ?
C10_11 H10B_11 0.9800 . ?
C10_11 H10C_11 0.9800 . ?
C11_11 H11A_11 0.9800 . ?
C11_11 H11B_11 0.9800 . ?
C11_11 H11C_11 0.9800 . ?
C9_12 C10_12 1.498(8) . ?
C9_12 C11_12 1.543(6) . ?
C9_12 H9_12 1.0000 . ?
C10_12 H10A_12 0.9800 . ?
C10_12 H10B_12 0.9800 . ?
C10_12 H10C_12 0.9800 . ?
C11_12 H11A_12 0.9800 . ?
C11_12 H11B_12 0.9800 . ?
C11_12 H11C_12 0.9800 . ?
C12 H00A 0.9800 . ?
C12 H12 0.9800 . ?
C12 H00D 0.9800 . ?
C13 H00E 0.9800 . ?
C13 H00F 0.9800 . ?
C13 H00G 0.9800 . ?
B1_2 C4_2 1.586(3) . ?
B1_2 C2_2 1.596(3) . ?
B1_2 H1 1.15(4) . ?
B1_2 H1A 1.17(4) . ?
C2_2 N3_2 1.144(3) . ?
C4_2 N5_2 1.142(3) . ?
