Preparation and characterization of terdentate [C,N,N] acetophenone and acetylpyridine hydrazone platinacycles. A DFT insight into the reaction mechanism
Marcos, Ismael; Ojea, Vicente; Vazquez-Garcia, Digna; Fernández Sánchez, Jesús José; Fernández, Alberto; Lopez-Torres, Margarita; Lado, Jorge; VILA, JOSE M; Dalton Transactions  (2017) –; doi:10.1039/C7DT03418K

data_7044778
_publ_section_title
;
 Preparation and characterization of terdentate [C,N,N] acetophenone and
 acetylpyridine hydrazone platinacycles. A DFT insight into the reaction
 mechanism
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03418K
_journal_year                    2017
_chemical_formula_sum            'C16 H19 Cl N4 O Pt S'
_chemical_formula_weight         545.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-07 deposited with the CCDC.
2017-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.124(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.197(5)
_cell_length_b                   7.101(5)
_cell_length_c                   12.014(3)
_cell_measurement_reflns_used    1958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      3.34
_cell_volume                     858.9(8)
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_collection       'BRUKER APEX2'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13106
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_min         2.023
_exptl_absorpt_coefficient_mu    8.456
_exptl_absorpt_correction_T_max  0.5181
_exptl_absorpt_correction_T_min  0.3325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS G. Sheldrick'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_description       plate
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.689
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         1902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+1.5823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1729
_reflns_number_total             1902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03418k3.cif
_cod_data_source_block           shelx
_cod_database_code               7044778
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.283
_shelx_estimated_absorpt_t_max   0.551
_shelx_res_checksum              52308