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_7043557
_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         'C12 H22 N8 Ni O2'
_chemical_formula_sum            'C12 H22 N8 Ni O2'
_chemical_formula_weight         369.08
_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
_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                90
_cell_angle_beta                 91.976(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.5790(3)
_cell_length_b                   14.3346(7)
_cell_length_c                   8.3734(4)
_cell_measurement_reflns_used    5751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.1828
_cell_measurement_theta_min      2.8128
_cell_volume                     789.20(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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 16.2096
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -53.00   -4.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.4031  -77.0000  -30.0000 49

  2 omega  -72.00  -46.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.4031  178.0000   30.0000 26

  3 omega  -20.00   66.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968  -99.0000  -90.0000 86

  4 omega   13.00   97.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968   19.0000    0.0000 84

  5 omega    3.00   89.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968   77.0000 -180.0000 86

  6 omega  -44.00   57.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968  -77.0000   60.0000 101

  7 omega  -42.00   57.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968  -77.0000  -30.0000 99

  8 omega   35.00  102.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968  178.0000  -90.0000 67

  9 omega   -2.00   82.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968   77.0000  -90.0000 84

 10 omega   -4.00   88.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968   77.0000   90.0000 92

 11 omega   19.00   99.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4968   38.0000   60.0000 80
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0800594000
_diffrn_orient_matrix_UB_12      -0.0261058000
_diffrn_orient_matrix_UB_13      -0.0327524000
_diffrn_orient_matrix_UB_21      0.0234606000
_diffrn_orient_matrix_UB_22      -0.0194311000
_diffrn_orient_matrix_UB_23      0.0764234000
_diffrn_orient_matrix_UB_31      -0.0683693000
_diffrn_orient_matrix_UB_32      -0.0372332000
_diffrn_orient_matrix_UB_33      -0.0167887000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13141
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.818
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       needle
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0272P)^2^+0.4648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1688
_reflns_number_total             1820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01960b2.cif
_cod_data_source_block           3
_cod_original_cell_volume        789.21(7)
_cod_database_code               7043557
_chemical_oxdiff_formula         'Ni N4 C12 H12 O2'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'