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_7055865
_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         'C28 H44 N14 Ni3 O4'
_chemical_formula_sum            'C28 H44 N14 Ni3 O4'
_chemical_formula_weight         816.90
_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     iterative
_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                107.345(4)
_cell_angle_beta                 98.847(4)
_cell_angle_gamma                99.464(4)
_cell_formula_units_Z            1
_cell_length_a                   8.6286(4)
_cell_length_b                   8.7296(4)
_cell_length_c                   12.6607(5)
_cell_measurement_reflns_used    3053
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.3220
_cell_measurement_theta_min      3.0820
_cell_volume                     876.82(7)
_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
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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    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9992
_diffrn_measurement_details
;
  1 omega  -40.00    4.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777   38.0000  120.0000 44

  2 omega  -23.00   24.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -99.0000 -150.0000 47

  3 omega  -91.00  -35.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777 -178.0000  120.0000 56

  4 omega   -9.00   24.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -99.0000  -60.0000 33

  5 omega  -51.00   41.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152  -38.0000  -30.0000 92

  6 omega    0.00   87.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152   57.0000  150.0000 87

  7 omega   21.00   73.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152   57.0000  -60.0000 52

  8 omega  -50.00   40.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152  -57.0000  120.0000 90

  9 omega  -25.00    5.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152  -99.0000  -60.0000 30
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0489097000
_diffrn_orient_matrix_UB_12      0.0675447000
_diffrn_orient_matrix_UB_13      -0.0080172000
_diffrn_orient_matrix_UB_21      0.0694748000
_diffrn_orient_matrix_UB_22      -0.0175851000
_diffrn_orient_matrix_UB_23      0.0276327000
_diffrn_orient_matrix_UB_31      0.0080115000
_diffrn_orient_matrix_UB_32      -0.0524734000
_diffrn_orient_matrix_UB_33      -0.0527694000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9512
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.51
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.650
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98600
_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            violet
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tables
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0435
_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/[\s^2^(Fo^2^)+(0.0329P)^2^+0.5851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                3004
_reflns_number_total             3884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj02962k2.cif
_cod_data_source_block           eva269
_cod_depositor_comments
'Adding full bibliography for 7055865--7055869.cif.'
_cod_original_cell_volume        876.83(6)
_cod_database_code               7055865
_chemical_oxdiff_formula         'ni cl2 N8 C6 h12'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32