Palladium(II) chloride complexes with 1,2,4-triazolo[1,5-a]pyrimidines: X-ray, 15N‒1H NMR and 15N CP MAS studies
Szłyk, Edward; Grodzicki, Antoni; Pazderski, Leszek; Wojtczak, Andrzej; Chatłas, Janusz; Wrzeszcz, Grzegorz; Sitkowski, Jerzy; Kamieński, Bohdan; Journal of the Chemical Society, Dalton Transactions  (2000) 867–; doi:10.1039/a908469j

data_7009075
_publ_section_title
;
 Palladium(II) chloride complexes with
 1,2,4-triazolo[1,5-a]pyrimidines: X-ray, 15N--1H NMR and 15N CP MAS
 studies
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              867
_journal_paper_doi               10.1039/a908469j
_journal_year                    2000
_chemical_formula_sum            'C27 H43 Cl2 N8 O0.5 Pd'
_chemical_formula_weight         655.02
_chemical_name_systematic
; 
 ? 
;
_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                75.342(4)
_cell_angle_beta                 81.431(4)
_cell_angle_gamma                79.665(4)
_cell_formula_units_Z            2
_cell_length_a                   10.7430(6)
_cell_length_b                   11.0134(5)
_cell_length_c                   14.1340(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1582.16(14)
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Kuma KM4'
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6874
_diffrn_reflns_theta_full        80.24
_diffrn_reflns_theta_max         80.24
_diffrn_reflns_theta_min         3.25
_diffrn_standards_decay_%        0.24
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.563
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.100
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0028(2)
_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   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.436
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+0.4281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                5262
_reflns_number_total             6498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908469j.txt
_cod_data_source_block           pddbtp
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+0.4281P] 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^)+(0.0727P)^2^+0.4281P] 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        1582.16(13)
_cod_database_code               7009075