A cationic zinc(II) complex of a new ligand based on <i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylstreptamine 2,4,6-orthoformate as the chloride salt
Jones, Peter G.; Kirby, Anthony J.; Beckmann, Claus; Acta Crystallographica Section E 59 (2003) m168–m170; doi:10.1107/S1600536803005889

data_2201811
_publ_section_title
;
 A cationic zinc(II) complex of a new ligand based on
 <i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylstreptamine
 2,4,6-orthoformate as the chloride salt
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m168
_journal_page_last               m170
_journal_paper_doi               10.1107/S1600536803005889
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Zn2 (C13 H22 N3 O4)2] Cl2'
_chemical_formula_moiety         'C26 H44 N6 O8 Zn2 2+, 2Cl 1-'
_chemical_formula_sum            'C26 H44 Cl2 N6 O8 Zn2'
_chemical_formula_weight         770.31
_chemical_name_systematic
;
rac-Bis[\m-(1R,2S,12R,13s,15s,17S,18r)-14,16,19-trioxa-
3,7,11-triazatetracyclo[13.3.1.0^2,13^.0^12,17^]nonadecan-18-olato-
1\k^3^N^3^,N^7^,N^11^:2\k^2^O^18^]dizinc(II) dichloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.849(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.706(2)
_cell_length_b                   9.2379(16)
_cell_length_c                   13.050(2)
_cell_measurement_reflns_used    56
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      10
_cell_volume                     1487.2(4)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992)'
_computing_molecular_graphics    'XP (Siemens, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe STADI-4'
_diffrn_measurement_method       \w/\q
_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  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3862
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         3.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.853
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   '\y scans'
_exptl_absorpt_process_details   '(XEMP; Siemens, 1994)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.437
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3416
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0324P)^2^+1.1834P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                3146
_reflns_number_total             3416
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6251.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (13 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1487.3(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2201811
_cod_database_fobs_code          2201811