Metal-mediated generation of triazapentadienate-terminated di- and trinuclear μ2-pyrazolate NiII species and control of their nuclearity
Andrusenko, Elena V.; Kabin, Evgeniy V.; Novikov, Alexander S.; Bokach, Nadezhda A.; Starova, Galina L.; Kukushkin, Vadim Yu.; New J. Chem. 41 (2017) 316–; doi:10.1039/C6NJ02962K

data_7055866
_publ_section_title
;
 Metal-mediated generation of triazapentadienate-terminated di- and
 trinuclear \m2-pyrazolate NiII species and control of their nuclearity
;
_journal_issue                   1
_journal_name_full               'New J. Chem.'
_journal_page_first              316
_journal_paper_doi               10.1039/C6NJ02962K
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C18 H30 N10 Ni2 O4'
_chemical_formula_sum            'C18 H30 N10 Ni2 O4'
_chemical_formula_weight         567.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-02
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2016-07-11 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                78.021(5)
_cell_angle_beta                 75.628(5)
_cell_angle_gamma                86.402(5)
_cell_formula_units_Z            2
_cell_length_a                   8.1705(4)
_cell_length_b                   10.6165(7)
_cell_length_c                   14.8093(8)
_cell_measurement_reflns_used    2987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7020
_cell_measurement_theta_min      3.2400
_cell_volume                     1217.20(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.9831
_diffrn_measured_fraction_theta_max 0.9831
_diffrn_measurement_details
;
  1 omega   -7.00   23.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -99.0000  -60.0000 30

  2 omega  -67.00  -40.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777 -178.0000   60.0000 27

  3 omega  -93.00  -66.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777 -178.0000   90.0000 27

  4 omega  -37.00   51.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777   57.0000  -60.0000 88

  5 omega  -22.00    9.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -99.0000    0.0000 31

  6 omega   -3.00   88.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152   57.0000 -120.0000 91

  7 omega  -50.00   38.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152  -57.0000  -30.0000 88

  8 omega  -39.00   36.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152  -77.0000   90.0000 75
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0346081000
_diffrn_orient_matrix_UB_12      0.0632853000
_diffrn_orient_matrix_UB_13      -0.0059967000
_diffrn_orient_matrix_UB_21      0.0576646000
_diffrn_orient_matrix_UB_22      0.0164040000
_diffrn_orient_matrix_UB_23      -0.0450285000
_diffrn_orient_matrix_UB_31      -0.0592404000
_diffrn_orient_matrix_UB_32      -0.0197783000
_diffrn_orient_matrix_UB_33      -0.0219414000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10684
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.57
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.592
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tables
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0417
_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/[\s^2^(Fo^2^)+(0.0265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                3850
_reflns_number_total             4942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj02962k2.cif
_cod_data_source_block           eva274
_cod_depositor_comments
'Adding full bibliography for 7055865--7055869.cif.'
_cod_database_code               7055866
_chemical_oxdiff_formula         'c16 h17 n2 cl1 ni1'
_reflns_odcompleteness_completeness 98.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32