Unusual Ligand Isomerization Dictated by Coordination Requirements of the Metal Ion: A Double-Bond Shift in Cu(II)-Assisted Template Condensation between Diacetylpyridine and a Tripodal Tetramine
Elena V. Rybak-Akimova; Alexander Y. Nazarenko; Svetlana S. Silchenko; Inorganic Chemistry 38 (1999) 2974–2980; doi:10.1021/ic990027n

data_4322085
_publ_section_title
;
 Unusual Ligand Isomerization Dictated by Coordination Requirements of the
 Metal Ion: A Double-Bond Shift in Cu(II)-Assisted Template Condensation
 between Diacetylpyridine and a Tripodal Tetramine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2974
_journal_page_last               2980
_journal_paper_doi               10.1021/ic990027n
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C18 H30 Cl2 Cu N5 O8.5'
_chemical_formula_weight         586.91
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.03(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.676(4)
_cell_length_b                   9.238(2)
_cell_length_c                   17.460(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2493.4(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4222
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    1.145
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.089
_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     361
_refine_ls_number_reflns         3315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.077
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1067P)^2^+2.8595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1764
_reflns_number_gt                2351
_reflns_number_total             3315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990027n_2.cif
_cod_data_source_block           lena1d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1067P)^2^+2.8595P] 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^)+(0.1067P)^2^+2.8595P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C18 H30 Cl2 Cu N5 O8.50'
_cod_database_code               4322085