Cubane shaped clusters, precursors for aluminophosphate frameworks: a solid state multinuclear NMR study, in time and frequency domains
Azaïs, Thierry; Bonhomme, Christian; Bonhomme-Coury, Laure; Vaissermann, Jacqueline; Millot, Yannick; Man, Pascal P.; Bertani, Philippe; Hirschinger, Jérôme; Livage, Jacques; Journal of the Chemical Society, Dalton Transactions  (2002) 609–; doi:10.1039/b104774b

data_7702653
_publ_section_title
;
 Cubane shaped clusters, precursors for aluminophosphate frameworks: a
 solid state multinuclear NMR study, in time and frequency domains
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              609
_journal_paper_doi               10.1039/b104774b
_journal_year                    2002
_chemical_compound_source
;
?
;
_chemical_formula_moiety
' (C24 H76 Al4 O28 P4) 4+, 4 (Br 1-),4(C2 H6 O1) '
_chemical_formula_sum            'C32 H100 Al4 Br4 O32 P4'
_chemical_formula_weight         1548.4
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.425(4)
_cell_length_b                   15.425(6)
_cell_length_c                   14.712(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    163
_cell_measurement_theta_max      14.2
_cell_measurement_theta_min      14
_cell_volume                     3500.4(19)
_diffrn_ambient_temperature      163
_diffrn_measurement_device       'Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.06
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1743
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        12.13
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.49
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'colourless '
_exptl_crystal_density_diffrn    1.45
_exptl_crystal_description       block
_exptl_crystal_F_000             1558.61
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.71
_refine_ls_extinction_coef       34.4
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.0369
_refine_ls_hydrogen_treatment
;
H atoms placed geometrically after each cycle
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         1347
_refine_ls_R_factor_obs          0.0589
_refine_ls_shift/esd_max         0.343220
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0726
_reflns_number_observed          1347
_reflns_number_total             1616
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            b104774b.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Tetragonal' was changed to
'tetragonal' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_atom_sites_solution_primary' value 'Direct_Methods' was
changed to 'direct'.

data item '_atom_sites_solution_hydrogens' value 'Geometric' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3500(2)
_cod_original_sg_symbol_H-M      'I -4 '
_cod_original_formula_sum        ' C32 H100 Al4 Br4 O32 P4  '
_cod_database_code               7702653