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_7044779
_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            'C76 H80 Cl6 N12 O2.5 P3 Pt3'
_chemical_formula_weight         2092.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.819(5)
_cell_length_b                   15.689(5)
_cell_length_c                   29.119(5)
_cell_measurement_reflns_used    15937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.99
_cell_measurement_theta_min      5.056
_cell_volume                     9054(4)
_computing_cell_refinement
'SAINT V7.12A (Bruker Nonius 2004) in Apex2 suite'
_computing_data_collection       'Apex2  V.1.0-27 (Bruker Nonius, 2005)'
_computing_data_reduction
'SAINT and XPREP Version 6.14 COPYRIGHT(c) 2003 Bruker-AXS'
_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 0.985
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       'omega-phi scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            77741
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.337
_diffrn_reflns_theta_min         2.055
_exptl_absorpt_coefficient_mu    4.901
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       prism
_exptl_crystal_F_000             4084
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.221
_refine_diff_density_min         -2.809
_refine_diff_density_rms         0.206
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.082(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     914
_refine_ls_number_reflns         16475
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+118.4683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1504
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                14042
_reflns_number_total             16475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03418k3.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_formula_sum        'C76 H80 Cl6 N12 O2.50 P3 Pt3'
_cod_database_code               7044779
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.351
_shelx_estimated_absorpt_t_max   0.640
_shelx_res_checksum              79815
_shelx_fab_checksum              94945