Synthesis and Characterization of a Novel Germanate Material Containing 16-Ring Channels and Templated by a Simple Primary Amine
Attfield, Martin P.; Al-Ebini, Yousef; Pritchard, Robin G.; Andrews, Ellen M.; Charlesworth, Richard J.; Hung, Wan; Masheder, Ben J.; Royal, Drew S.; Chemistry of Materials 19 (2007) 316–; doi:10.1021/cm062241x

data_4001289
_publ_contact_author             'Attfield, Martin P.'
_publ_section_title
;
 Synthesis and Characterization of a Novel Germanate Material Containing
 16-Ring Channels and Templated by a Simple Primary Amine
;
_journal_issue                   2
_journal_name_full               'Chemistry of Materials'
_journal_page_first              316
_journal_paper_doi               10.1021/cm062241x
_journal_volume                  19
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'4(Ge9 H3 O21), 2(C3 H10 N O), 8(C3 H10 N), 2(O2), O2'
_chemical_formula_sum            'C30 H112 Ge36 N10 O92'
_chemical_formula_weight         4699.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           108
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      108
_symmetry_space_group_name_Hall  'I 4 -2c'
_symmetry_space_group_name_H-M   'I 4 c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-09-13T13:56:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.9728(6)
_cell_length_b                   24.9728(6)
_cell_length_c                   9.8957(2)
_cell_measurement_reflns_used    3565
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2
_cell_measurement_wavelength     0.71073
_cell_volume                     6171.4(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Nonius Kappa CCD detector diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       1
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3425
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    8.727
_exptl_absorpt_correction_T_max  0.648
_exptl_absorpt_correction_T_min  0.215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(RBlessing, 1995, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4500
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         1804
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0598
_reflns_number_gt                1578
_reflns_number_total             1804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm062241xsi20060918_015610.cif
_cod_data_source_block           C30H112Ge36N10O92
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_database_code               4001289