Rerefinement of (μ-1,7,11,17-tetraoxa-2,6,12,16-tetraazacycloeicosane-κ^4^<i>N</i>^1^,<i>N</i>^17^:<i>N</i>^7^,<i>N</i>^11^)bis[dichlorozinc(II)]
Kuksa, Vladimir A.; Wardell, Solange M. S. V; Lin, Paul Kong Thoo; Howie, R. Alan; Acta Crystallographica Section E 58 (2002) m68–m69; doi:10.1107/S1600536802001654

data_2200856
_publ_section_title
;Rerefinement of
 (\m-1,7,11,17-tetraoxa-2,6,12,16-tetraazacycloeicosane-\k^4^<i>N</i>^1^,<i>N</i>^17^:<i>N</i>^7^,<i>N</i>^11^)bis[dichlorozinc(II)]
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m68
_journal_page_last               m69
_journal_paper_doi               10.1107/S1600536802001654
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Zn2 Cl4 (C12 H28 N4 O4)]'
_chemical_formula_moiety         'C12 H28 Cl4 N4 O4 Zn2'
_chemical_formula_sum            'C12 H28 Cl4 N4 O4 Zn2'
_chemical_formula_weight         564.92
_chemical_name_systematic
;
(\m-1,7,11,17-tetraoxa-2,6,12,16-tetraazacycloeicosane-
\k^4^N^1^,N^17^:N^7^,N^11^)bis[dichlorozinc(II)]
;
_chemical_temperature_decomposition 428
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.4120(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4925(4)
_cell_length_b                   7.2697(2)
_cell_length_c                   19.2129(6)
_cell_measurement_reflns_used    12531
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.62
_cell_volume                     2172.59(11)
_computing_cell_refinement       MADNES
_computing_data_collection       'MADNES  (Pflugrath & Messerschmidt, 1989)'
_computing_data_reduction        'ABSMAD (Karaulov, 1992)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full .986
_diffrn_measured_fraction_theta_max .986
_diffrn_measurement_device_type  'Delft Instruments FAST'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0432
_diffrn_reflns_av_sigmaI/netI    .0324
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12531
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.724
_exptl_absorpt_correction_T_max  .665
_exptl_absorpt_correction_T_min  .589
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .15
_refine_diff_density_max         .473
_refine_diff_density_min         -.478
_refine_ls_extinction_coef       .0027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          .0403
_refine_ls_R_factor_gt           .0310
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0469P)^2^+1.0443P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .0785
_refine_ls_wR_factor_ref         .0841
_reflns_number_gt                2096
_reflns_number_total             2470
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6145.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '428
(dec.)'. The value '428 (dec.)' was changed to '428'.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '428
(dec.)'. The value '428 (dec.)' was changed to '428'.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2172.59(10)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               2200856
_cod_database_fobs_code          2200856