Metal-mediated Reactions between Dialkylcyanamides and Acetamidoxime Generate Unusual (Nitrosoguanidinate)Nickel(II) Complexes
Bikbaeva, Zarina M.; Novikov, Alexander S.; Suslonov, Vitalii V.; Bokach, Nadezhda A.; Kukushkin, Vadim Yu.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01960B

data_7043558
_publ_section_title
;
 Metal-mediated Reactions between Dialkylcyanamides and Acetamidoxime
 Generate Unusual (Nitrosoguanidinate)Nickel(II) Complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01960B
_journal_year                    2017
_chemical_formula_moiety         'C10 H18 N8 Ni O2'
_chemical_formula_sum            'C10 H18 N8 Ni O2'
_chemical_formula_weight         341.03
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-01-29 deposited with the CCDC.
2017-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                75.399(13)
_cell_angle_beta                 81.175(12)
_cell_angle_gamma                81.118(14)
_cell_formula_units_Z            1
_cell_length_a                   6.7068(10)
_cell_length_b                   6.7518(12)
_cell_length_c                   7.8797(10)
_cell_measurement_reflns_used    1074
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.1820
_cell_measurement_theta_min      5.8320
_cell_volume                     338.70(9)
_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, 2015)'
_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 0.978
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega  -67.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3104   57.0000   90.0000 97

  2 omega -108.00  -21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3104  -57.0000  -60.0000 87

  3 omega -130.00  -36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3104 -178.0000   90.0000 94

  4 omega   67.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000   60.0000 40

  5 omega   58.00   92.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000  120.0000 34

  6 omega   46.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  150.0000 29

  7 omega   47.00   87.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   30.0000 40

  8 omega   54.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000  -60.0000 52

  9 omega   66.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000 -120.0000 32

 10 omega   95.00  121.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000 -180.0000 26

 11 omega   48.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -120.0000 48

 12 omega   94.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000  -60.0000 84

 13 omega  146.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000    0.0000 30

 14 omega  132.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   30.0000 44

 15 omega  121.00  147.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   60.0000 26

 16 omega   88.00  123.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   30.0000 35

 17 omega   87.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000    0.0000 25

 18 omega   40.00   94.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000    0.0000 54

 19 omega   42.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000    0.0000 63

 20 omega   40.00   99.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000 -180.0000 59

 21 omega   49.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000 -180.0000 34

 22 omega   43.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -180.0000 54

 23 omega   81.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  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      0.1651904000
_diffrn_orient_matrix_UB_12      -0.0853190000
_diffrn_orient_matrix_UB_13      -0.1307944000
_diffrn_orient_matrix_UB_21      -0.1187560000
_diffrn_orient_matrix_UB_22      -0.1834763000
_diffrn_orient_matrix_UB_23      0.0174007000
_diffrn_orient_matrix_UB_31      -0.1159625000
_diffrn_orient_matrix_UB_32      0.1244109000
_diffrn_orient_matrix_UB_33      -0.1549267000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2391
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.923
_diffrn_reflns_theta_min         5.845
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.262
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88160
_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            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       needle
_exptl_crystal_F_000             178
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0470P)^2^+0.0773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0991
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1219
_reflns_number_total             1368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01960b2.cif
_cod_data_source_block           4
_cod_database_code               7043558
_chemical_oxdiff_formula         'Ni cl C25 H20 N4 S'
_reflns_odcompleteness_completeness 97.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     75.12
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B)
;
_olex2_submission_special_instructions 'No special instructions were received'