"Swollen" Macrocycles: Palladium(II)-Directed Template Syntheses of Pendant-Arm 14-, 16-, and 18-Membered Macrocycles
Monica Rossignoli; Christine C. Allen; Trevor W. Hambley; Geoffrey A. Lawrance; Marcel Maeder; Inorganic Chemistry 35 (1996) 4961–4966; doi:10.1021/ic951628r

data_4323877
_publ_contact_author
;
        Prof. Geoffrey A. Lawrance
        Department of Chemistry
        University of Newcastle
        Callaghan 2308
        Australia
;
_publ_section_title
;
 "Swollen" Macrocycles: Palladium(II)-Directed Template Syntheses of
 Pendant-Arm 14-, 16-, and 18-Membered Macrocycles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4961
_journal_page_last               4966
_journal_paper_doi               10.1021/ic951628r
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C12 H26 Cl2 N6 O12 Pd'
_chemical_formula_weight         623.69
_chemical_name_common            '[Pd(dino[14]mac](ClO~4~)~2~'
_chemical_name_systematic
;
 (6,13-Dimethyl-6,13-dinitro-1,4,8,11-tetraazacyclotetradecane)palladium(II) 
 perchlorate 
;
_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_date             96-04-03
_audit_creation_method           from_xtal_archive_file_using_SHELXL
_cell_angle_alpha                69.04(3)
_cell_angle_beta                 68.60(3)
_cell_angle_gamma                71.53(3)
_cell_formula_units_Z            1
_cell_length_a                   8.105(3)
_cell_length_b                   8.370(2)
_cell_length_c                   9.437(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     543.7(4)
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_data_reduction        'Enraf-Nonius Structure Determination Package'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4 (Enfraf-Nonius)'
_diffrn_measurement_method       \w-0.33\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    3.9879
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1903
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        -0.47
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.79
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_meas      2.01
_exptl_crystal_density_method    flotation
_exptl_crystal_description       plate
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    noref
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_refine_ls_number_reflns         1902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.258
_refine_ls_restrained_S_obs      1.065
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_obs          0.0351
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1379
_refine_ls_wR_factor_obs         0.1154
_reflns_number_observed          1856
_reflns_number_total             1903
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic951628r_1.cif
_cod_data_source_block           (I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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^)+(0.1000P)^2^+0.0000P] 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        543.7(3)
_cod_database_code               4323877