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_7043560
_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         'C6 H14 N8 Ni O2'
_chemical_formula_sum            'C6 H14 N8 Ni O2'
_chemical_formula_weight         288.96
_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   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                 96.885(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.4378(10)
_cell_length_b                   6.6766(12)
_cell_length_c                   15.437(2)
_cell_measurement_reflns_used    768
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.0010
_cell_measurement_theta_min      5.7370
_cell_volume                     556.41(16)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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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 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -45.00   32.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000  120.0000 77

  2 omega -129.00  -36.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  178.0000 -150.0000 93

  3 omega  -58.00  -14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -38.0000  150.0000 44

  4 omega   25.00   55.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787  -99.0000 -180.0000 30

  5 omega   54.00   87.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   60.0000 33

  6 omega  117.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -60.0000 25

  7 omega   39.00   96.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -60.0000 57

  8 omega   85.00  170.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  -90.0000 85

  9 omega   82.00  141.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   90.0000 59

 10 omega   45.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  120.0000 27

 11 omega   52.00   79.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   30.0000 27

 12 omega   42.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000 -120.0000 26

 13 omega   74.00  115.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000 -120.0000 41

 14 omega  117.00  163.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000    0.0000 46

 15 omega   85.00  125.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -180.0000 40

 16 omega   41.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000    0.0000 30

 17 omega  132.00  169.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   30.0000 37

 18 omega   81.00  108.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   30.0000 27

 19 omega   76.00  141.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000 -120.0000 65

 20 omega  -48.00   14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000 -150.0000 62

 21 omega  -49.00  -20.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000  -60.0000 29

 22 omega  -12.00   15.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000  -60.0000 27
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1568927000
_diffrn_orient_matrix_UB_12      0.1721068000
_diffrn_orient_matrix_UB_13      0.0443337000
_diffrn_orient_matrix_UB_21      0.2371362000
_diffrn_orient_matrix_UB_22      -0.1033853000
_diffrn_orient_matrix_UB_23      -0.0228275000
_diffrn_orient_matrix_UB_31      -0.0218647000
_diffrn_orient_matrix_UB_32      0.1144791000
_diffrn_orient_matrix_UB_33      -0.0871860000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            2788
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.492
_diffrn_reflns_theta_min         5.774
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.624
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74293
_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            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       needle
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         1105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0626P)^2^+0.3647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                878
_reflns_number_total             1105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01960b2.cif
_cod_data_source_block           1
_cod_original_cell_volume        556.40(17)
_cod_database_code               7043560
_chemical_oxdiff_formula         'C6 H12 N6 O4 cl2 ni1'
_reflns_odcompleteness_completeness 94.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'