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_7055869
_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         'C36 H36 N14 Ni3 O4'
_chemical_formula_sum            'C36 H36 N14 Ni3 O4'
_chemical_formula_weight         904.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-09-07 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.089(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6333(12)
_cell_length_b                   14.8982(4)
_cell_length_c                   11.0132(5)
_cell_measurement_reflns_used    4038
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.3220
_cell_measurement_theta_min      2.9400
_cell_volume                     2072.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega  -48.00   30.00   1.0000    4.9500
omega____ theta____ kappa____ phi______ frames
    -      -41.3104   38.0000  150.0000 78

  2 omega  -53.00  -19.00   1.0000    4.9500
omega____ theta____ kappa____ phi______ frames
    -      -41.3104  -38.0000 -150.0000 34

  3 omega -120.00   -5.00   1.0000    4.9500
omega____ theta____ kappa____ phi______ frames
    -      -41.3104  -19.0000  -30.0000 115

  4 omega   61.00   88.00   1.0000    4.9500
omega____ theta____ kappa____ phi______ frames
    -       41.3104  178.0000  -30.0000 27

  5 omega   59.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000  -90.0000 26

  6 omega   39.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -30.0000 58

  7 omega  138.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  150.0000 40

  8 omega   54.00   79.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000  150.0000 25

  9 omega   37.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -180.0000 38

 10 omega   48.00  108.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000   90.0000 60

 11 omega   43.00  105.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000    0.0000 62

 12 omega  119.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000  -90.0000 58

 13 omega   37.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   90.0000 51

 14 omega  101.00  140.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  120.0000 39

 15 omega   53.00   79.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000  120.0000 26

 16 omega  151.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  120.0000 27

 17 omega  102.00  127.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  125.0000  150.0000 25

 18 omega  152.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  125.0000  150.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0828900000
_diffrn_orient_matrix_UB_12      -0.0220322000
_diffrn_orient_matrix_UB_13      0.0596059000
_diffrn_orient_matrix_UB_21      -0.0709042000
_diffrn_orient_matrix_UB_22      0.0764871000
_diffrn_orient_matrix_UB_23      -0.0803769000
_diffrn_orient_matrix_UB_31      -0.0544646000
_diffrn_orient_matrix_UB_32      -0.0658540000
_diffrn_orient_matrix_UB_33      -0.1129658000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9619
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.992
_diffrn_reflns_theta_min         3.499
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.044
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       prism
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3845
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0573
_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/[\s^2^(Fo^2^)+(0.1254P)^2^+1.0017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.1857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3305
_reflns_number_total             3845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj02962k2.cif
_cod_data_source_block           eva-775a
_cod_depositor_comments
'Adding full bibliography for 7055865--7055869.cif.'
_cod_database_code               7055869
_chemical_oxdiff_formula         'C34 H29 N5 O2 Ni'
_reflns_odcompleteness_completeness 97.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     75.12
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-H2 = N3-H3
 0.86 with sigma of 0.02
 H1AC-H2
 2.1 with sigma of 0.02
3. Others
 Fixed Sof: C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C2(0.75) H2A(0.75) H2B(0.75)
 H2C(0.75) C4A(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5) C1A(0.25) H1AA(0.25)
 H1AB(0.25) H1AC(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C6(H6), C10(H10), C18(H18), C19(H19), C9(H9), C14(H14),
 C12(H12), C11(H11)
4.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C2(H2A,H2B,H2C), C4A(H4AA,H4AB,H4AC), C1A(H1AA,H1AB,H1AC)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'