New complexes with pyrazole-containing ligands and different metallic centres. Comparative study of their fluxional behaviour involving M‒N bond rupture
José Elguero; Ana Guerrero; Felipe Gómez de la Torre; Antonio de la Hoz; Félix A. Jalón; Blanca R. Manzano; Ana Rodríguez; New J. Chem. 25 (2001) 1050–1060; doi:10.1039/b102318g

data_7051136
_publ_section_title
;
 New complexes with pyrazole-containing ligands and different metallic
 centres. Comparative study of their fluxional behaviour involving M--N
 bond rupture
;
_journal_issue                   8
_journal_name_full               'New J. Chem.'
_journal_page_first              1050
_journal_page_last               1060
_journal_paper_doi               10.1039/b102318g
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C12 H11 F3 N4 O3 Pd S'
_chemical_formula_weight         454.71
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.511(8)
_cell_angle_beta                 79.73(2)
_cell_angle_gamma                81.53(2)
_cell_formula_units_Z            2
_cell_length_a                   7.623(4)
_cell_length_b                   10.1347(8)
_cell_length_c                   11.9270(10)
_cell_measurement_temperature    293(2)
_cell_volume                     828.6(5)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XRAY80 (Stewart, 1976)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3989
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.20
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.296
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.322
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3989
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.178
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w==1/[\s^2^(Fo^2^)+(0.1405P)^2^+0.4788P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.2064
_reflns_number_gt                3029
_reflns_number_total             3989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102318g.txt
_cod_data_source_block           20
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w==1/[\s^2^(Fo^2^)+(0.1405P)^2^+0.4788P] where P==(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w==1/[\s^2^(Fo^2^)+(0.1405P)^2^+0.4788P] where P==(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        828.6(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051136