cis‒trans isomerism and rotational isomerism in triazene-1-oxide bis-chelates of palladium(II)
Zbigniew Ciunik; Juliusz A. Wolny; Mikołaj F. Rudolf; Stanisław Wołowiec; J. Chem. Soc., Dalton Trans.  (2002) 885–895; doi:10.1039/b106652h

data_7011022
_publ_section_title
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 cis--trans isomerism and rotational isomerism in triazene-1-oxide
 bis-chelates of palladium(II)
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_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              885
_journal_page_last               895
_journal_paper_doi               10.1039/b106652h
_journal_year                    2002
_chemical_formula_sum            'C18 H24 N6 O2 Pd'
_chemical_formula_weight         462.83
_space_group_IT_number           2
_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                88.08(3)
_cell_angle_beta                 74.01(3)
_cell_angle_gamma                65.39(3)
_cell_formula_units_Z            2
_cell_length_a                   9.098(2)
_cell_length_b                   9.918(2)
_cell_length_c                   13.036(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1023.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.862
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7009
_diffrn_reflns_theta_full        28.90
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.8357
_exptl_absorpt_correction_T_min  0.7071
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.625
_refine_diff_density_min         -1.644
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1038P)^2^+2.1631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1907
_reflns_number_gt                3952
_reflns_number_total             4659
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106652h.txt
_cod_data_source_block           cmpd_7
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1038P)^2^+2.1631P] 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^)+(0.1038P)^2^+2.1631P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        1023.6(4)
_cod_database_code               7011022