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_7055868
_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         'C8 H16 N6 Ni O4'
_chemical_formula_sum            'C8 H16 N6 Ni O4'
_chemical_formula_weight         318.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-16
_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                90.00
_cell_angle_beta                 98.159(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8999(5)
_cell_length_b                   5.7496(3)
_cell_length_c                   11.1292(5)
_cell_measurement_reflns_used    1446
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6140
_cell_measurement_theta_min      6.4640
_cell_volume                     627.07(5)
_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    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 0.9640
_diffrn_measured_fraction_theta_max 0.9640
_diffrn_measurement_details
;
  1 omega  -46.00  -17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1287   38.0000    0.0000 29

  2 omega  -48.00  -21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1287  -38.0000  120.0000 27

  3 omega    3.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1287   38.0000    0.0000 30

  4 omega -109.00  -81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1287  -38.0000  120.0000 28

  5 omega   83.00  119.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.1287   77.0000 -120.0000 36

  6 omega   14.00   80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.1287   77.0000 -120.0000 66

  7 omega   65.00  128.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.1287  178.0000 -180.0000 63

  8 omega   36.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000    0.0000 54

  9 omega   36.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -180.0000 30

 10 omega   35.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -30.0000 56

 11 omega   47.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   60.0000 43

 12 omega   87.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -180.0000 25

 13 omega   37.00   64.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000 -150.0000 27

 14 omega   48.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000   60.0000 61

 15 omega   70.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000 -180.0000 27

 16 omega   36.00   61.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 25

 17 omega   90.00  131.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   30.0000 41

 18 omega   58.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000    0.0000 47

 19 omega   49.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -90.0000 49

 20 omega   61.00  111.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000    0.0000  -60.0000 50
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0308506000
_diffrn_orient_matrix_UB_12      0.2624070000
_diffrn_orient_matrix_UB_13      -0.0120635000
_diffrn_orient_matrix_UB_21      0.1260613000
_diffrn_orient_matrix_UB_22      0.0522610000
_diffrn_orient_matrix_UB_23      0.0940404000
_diffrn_orient_matrix_UB_31      0.0888374000
_diffrn_orient_matrix_UB_32      0.0167765000
_diffrn_orient_matrix_UB_33      -0.1026000000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2615
_diffrn_reflns_theta_full        75.87
_diffrn_reflns_theta_max         75.87
_diffrn_reflns_theta_min         6.46
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.470
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63693
_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            red
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0608P)^2^+0.1536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                1140
_reflns_number_total             1263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj02962k2.cif
_cod_data_source_block           eva312
_cod_depositor_comments
'Adding full bibliography for 7055865--7055869.cif.'
_cod_original_cell_volume        627.06(5)
_cod_database_code               7055868
_chemical_oxdiff_formula         'ni i N4 C10 H15'
_reflns_odcompleteness_completeness 90.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95