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_7055867
_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         'C38 H38 N10 Ni2 O4'
_chemical_formula_sum            'C38 H38 N10 Ni2 O4'
_chemical_formula_weight         816.20
_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
_audit_creation_date             2015-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-04 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3458(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.83295(18)
_cell_length_b                   39.2516(5)
_cell_length_c                   16.3620(3)
_cell_measurement_reflns_used    22589
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.0250
_cell_measurement_theta_min      3.5270
_cell_volume                     7498.7(2)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -44.00   23.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000  -90.0000 67

  2 omega -113.00  -39.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787 -178.0000  -30.0000 74

  3 omega -116.00  -22.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -38.0000  120.0000 94

  4 omega   58.00   87.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787 -178.0000   60.0000 29

  5 omega  146.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  -30.0000 31

  6 omega   73.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  150.0000 34

  7 omega   93.00  119.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   60.0000 26

  8 omega   40.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -49.0000   15.6305 60

  9 omega   85.00  120.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  -30.0000 35

 10 omega   42.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   60.0000 49

 11 omega  123.00  162.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000    0.0000 39

 12 omega   38.00   64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  150.0000 26

 13 omega   39.00   74.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000    0.0000 35

 14 omega   47.00   73.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -60.0000 26

 15 omega   74.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -60.0000 34

 16 omega   62.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -150.0000 30

 17 omega   31.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -60.0000 26

 18 omega   30.00   70.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -90.0000 40

 19 omega   46.00   72.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000   30.0000 26

 20 omega   77.00  113.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000   30.0000 36

 21 omega   37.00   89.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -22.0000   85.8885 52

 22 omega   38.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -60.0000 47

 23 omega  103.00  132.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000  -30.0000 29

 24 omega  108.00  134.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000    0.0000 26

 25 omega  137.00  164.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000    0.0000 27

 26 omega   90.00  127.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -180.0000 37

 27 omega   62.00   88.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  150.0000 26

 28 omega  124.00  150.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000 -150.0000 26

 29 omega   32.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -17.0000 -101.0673 51

 30 omega  143.00  173.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   60.0000 30

 31 omega  108.00  135.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  120.0000 27

 32 omega   72.00   98.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -30.0000 26

 33 omega  111.00  136.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000 -180.0000 25

 34 omega   57.00   82.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  120.0000 25

 35 omega  -48.00  -22.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000 -180.0000 26

 36 omega   11.00   36.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000 -180.0000 25

 37 omega -114.00  -86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -38.0000   90.0000 28

 38 omega  -78.00  -15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -38.0000  -30.0000 63

 39 omega  -67.00  -41.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -57.0000 -180.0000 26

 40 omega   55.00  126.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787 -178.0000   30.0000 71

 41 omega   87.00  113.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -120.0000 26

 42 omega   38.00   73.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -120.0000 35

 43 omega   71.00   97.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -57.0000   64.3313 26

 44 omega  125.00  175.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000 -120.0000 50

 45 omega   97.00  124.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000 -120.0000 27

 46 omega  130.00  157.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000 -120.0000 27

 47 omega   84.00  123.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   30.0000 39

 48 omega  103.00  129.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000  -30.0000 26

 49 omega   40.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -60.0000 26

 50 omega   74.00  105.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000   60.0000 31

 51 omega   47.00   79.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  120.0000 32

 52 omega   60.00   87.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  120.0000 27

 53 omega   33.00   62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000 -180.0000 29

 54 omega   79.00  105.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -60.0000 26

 55 omega  106.00  132.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  -30.0000 26

 56 omega   91.00  149.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   90.0000 58

 57 omega   86.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   30.0000 25

 58 omega   86.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  150.0000 26

 59 omega  147.00  173.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  150.0000 26

 60 omega   83.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   90.0000 38

 61 omega  123.00  149.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   90.0000 26

 62 omega   62.00   87.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  120.0000 25

 63 omega   92.00  133.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000 -180.0000 41

 64 omega   87.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   30.0000 25

 65 omega  105.00  148.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000  150.0000 43

 66 omega  144.00  172.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  -60.0000 28

 67 omega   97.00  129.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  -60.0000 32
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0885369000
_diffrn_orient_matrix_UB_12      0.0249094000
_diffrn_orient_matrix_UB_13      0.0465271000
_diffrn_orient_matrix_UB_21      0.0025042000
_diffrn_orient_matrix_UB_22      0.0197289000
_diffrn_orient_matrix_UB_23      -0.0810764000
_diffrn_orient_matrix_UB_31      -0.0977305000
_diffrn_orient_matrix_UB_32      0.0230632000
_diffrn_orient_matrix_UB_33      0.0191552000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_number            14876
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.495
_diffrn_reflns_theta_min         3.545
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.697
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69553
_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            orange
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       prism
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         1.613
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     981
_refine_ls_number_reflns         14876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+3.0578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11882
_reflns_number_total             14876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj02962k2.cif
_cod_data_source_block           eva_717
_cod_depositor_comments
;
Adding full bibliography for 7055865--7055869.cif.

2017-11-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        7498.68(19)
_cod_original_formula_moiety     '2(C38 H38 N10 Ni2 O4)'
_cod_original_formula_sum        'C76 H76 N20 Ni4 O8'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1632.40
_cod_database_code               7055867
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         '2(C38 H38 N10 Ni2 O4)'
_reflns_odcompleteness_completeness 94.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N9(H9), N10(H10), C7(H7), C16(H16), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), N2A(H2A), N3A(H3A), N9A(H9A), N10A(H10A),
 C7A(H7A), C16A(H16A), C19A(H19A), C20A(H20A), C21A(H21A), C22A(H22A),
 C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C27A(H27A), C28A(H28A),
 C29A(H29A), C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A),
 C35A(H35A), C36A(H36A), C37A(H37A), C38A(H38A)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C),
 C1A(H1AA,H1AB,H1AC), C4A(H4AA,H4AB,H4AC), C11A(H11D,H11E,H11F), C13A(H13D,H13E,
 H13F)
;
_olex2_submission_special_instructions 'No special instructions were received'