Synthesis and Characterization of Subcell−Supercell Related Ethylenediamine-Pillared Zinc Hydroxysulfates
Rujiwatra, Apinpus; Mander, Gavin J.; Kepert, Cameron J.; Rosseinsky, Matthew J.; Crystal Growth & Design 5 (2005) 183–; doi:10.1021/cg034242x

data_4504857
_publ_contact_author
;
      Apinpus Rujiwatra
      Department of Chemistry
    Faculty of Science
    Chiang Mai University
    Chiang Mai  50200
      Thailand 
;
_publ_section_title
;
 Synthesis and Characterization of Subcell&#x2212;Supercell Related
 Ethylenediamine-Pillared Zinc Hydroxysulfates
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              183
_journal_paper_doi               10.1021/cg034242x
_journal_volume                  5
_journal_year                    2005
_chemical_compound_source
;
 'hydrothermal synthesis at 180 deg C for 3 days'
;
_chemical_formula_moiety         '(CNH4)7 (SO4)7 (OH)42 Zn28 (H2O)18'
_chemical_formula_sum            'C7 H106 N7 O88 S7 Zn28'
_chemical_formula_weight         3752.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   21.926(2)
_cell_length_b                   21.926(2)
_cell_length_c                   10.5643(9)
_cell_measurement_reflns_used    6444
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.98
_cell_measurement_theta_min      3.33
_cell_volume                     4398.4(7)
_computing_cell_refinement       'LSCELL (Clegg, 1997)'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SAINT'
_computing_molecular_graphics    X-STEP/DIAMOND
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment
;
 'In thin film of perfluorpolyether oil on glass fibre'
;
_diffrn_ambient_temperature      150(2)
_diffrn_crystal_treatment        'Flash cooled in nitrogen stream'
_diffrn_detector_area_resol_mean 8.912
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Brucker AXS SMART CCD diffractometer'
_diffrn_measurement_method       'omega rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.69230
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            30736
_diffrn_reflns_theta_full        29.37
_diffrn_reflns_theta_max         29.37
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    7.542
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.832452
_exptl_absorpt_correction_type   Multiscans
_exptl_absorpt_process_details
;
 Mean and maximum errors in direction cosine check functions 
 are 0.001 and 0.003 respectively. 9323 reflections were 
 employed for parameter determination. R(int)= 0.1025 and 
 R(int) = 0.0279 before and after the  refinements with 
 final corrected 30736 reflections. The settings for 
 parameter refinements are (Intensity/sigma)threshold = 5.000 and 
 (Intensity + sigma)/(Mean intensity) threshold = 0.2500. 
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.805
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             3633
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.972
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         8089
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0792P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1555
_reflns_number_gt                3835
_reflns_number_total             8089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg034242xsi20031203_072537.cif
_cod_data_source_block           rehydrated_phase_of_Zn8(SO4)2(OH)12(en).6(H2O)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4398.5(7)
_cod_database_code               4504857