Amidrazone Complexes from a Cascade Platinum(II)-Mediated Reaction between Amidoximes and Dialkylcyanamides
Dmitrii S. Bolotin; Nadezhda A. Bokach; Andreii S. Kritchenkov; Matti Haukka; Vadim Yu. Kukushkin; Inorganic Chemistry 52 (2013) 6378–6389; doi:10.1021/ic4000878

data_4335010
_publ_section_title
;
 Amidrazone Complexes from a Cascade Platinum(II)-Mediated Reaction
 between Amidoximes and Dialkylcyanamides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6378
_journal_page_last               6389
_journal_paper_doi               10.1021/ic4000878
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C20 H26 Cl N7 O Pt, 2(C H3 N O2)'
_chemical_formula_sum            'C22 H32 Cl N9 O5 Pt'
_chemical_formula_weight         733.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.4880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9394(3)
_cell_length_b                   12.2397(4)
_cell_length_c                   20.1196(5)
_cell_measurement_reflns_used    9217
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.34
_cell_measurement_theta_min      2.49
_cell_volume                     2406.76(12)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics
'CrystaMaker (CrystalMaker Software ltd., 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '62mm x 62mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            31406
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    5.998
_exptl_absorpt_correction_T_max  0.3642
_exptl_absorpt_correction_T_min  0.2049
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.21
_platon_squeeze_details
;
Nitromethane solvent was disordered and therefore omitted from the final 
refinement and treated as a diffuse contribution using the SQUEEZE procedure as 
implemented in PLATON (A. Spek, 2003)
;
_refine_diff_density_max         1.617
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.377
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         6946
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.377
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+11.7790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                6578
_reflns_number_total             6946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4000878_si_002_3.cif
_cod_data_source_block           5g
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4335010