Facile Ni(II)/Ketoxime-Mediated Conversion of Organonitriles into Imidoylamidine Ligands. Synthesis of Imidoylamidines and Acetyl Amides
Maximilian N. Kopylovich; Armando J. L. Pombeiro; Andreas Fischer; Lars Kloo; Vadim Yu. Kukushkin; Inorganic Chemistry 42 (2003) 7239–7248; doi:10.1021/ic0349813

data_4312447
_publ_contact_author_address
;
Department of Chemistry
St. Petersburg State University
198504 Stary Petergof
Russian Federation
;
_publ_contact_author_email       kukushkin@VK2100.spb.edu
_publ_contact_author_name        'Vadim Yu. Kukushkin'
_publ_section_title
;
 Facile Ni(II)/Ketoxime-Mediated Conversion of Organonitriles into
 Imidoylamidine Ligands. Synthesis of Imidoylamidines and Acetyl Amides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7239
_journal_page_last               7248
_journal_paper_doi               10.1021/ic0349813
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C16 H35 Cl N6 Ni O '
_chemical_formula_sum            'C16 H35 Cl N6 Ni O'
_chemical_formula_weight         421.660
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.5984(4)
_cell_length_b                   11.0714(2)
_cell_length_c                   14.7694(2)
_cell_measurement_reflns_used    49914
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      4.21
_cell_volume                     4349.32(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.00548
_diffrn_orient_matrix_UB_12      0.00292
_diffrn_orient_matrix_UB_13      -0.03708
_diffrn_orient_matrix_UB_21      0.03935
_diffrn_orient_matrix_UB_22      0.08130
_diffrn_orient_matrix_UB_23      0.00060
_diffrn_orient_matrix_UB_31      0.06014
_diffrn_orient_matrix_UB_32      -0.02903
_diffrn_orient_matrix_UB_33      -0.01117
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26672
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         4.21
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         9128
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+3.1600*P+(0.0292P)^2^+0.0000sin\q/\l]
 where P = 0.00000Fo^2^ + 1.00000Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                8213
_reflns_number_total             9128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0349813si20030818_063355_3.cif
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P c a 21 '
_cod_original_formula_sum        'C16 H35 Cl N6 Ni O '
_cod_database_code               4312447