Azamacrocycles and the azaoxacryptand 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane as structure-directing agents in the synthesis of microporous metalloaluminophosphates
Maple, Martin J.; Philp, Eilidh F.; Slawin, Alexandra M. Z.; Lightfoot, Philip; Cox, Paul A.; Wright, Paul A.; Journal of Materials Chemistry 11 (2001) 98–104; doi:10.1039/b003430o

data_7203984
_publ_section_title
;
 Azamacrocycles and the azaoxacryptand
 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane as
 structure-directing agents in the synthesis of microporous
 metalloaluminophosphates
;
_journal_coden_ASTM              JMACEP
_journal_issue                   1
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              98
_journal_page_last               104
_journal_paper_doi               10.1039/b003430o
_journal_volume                  11
_journal_year                    2001
_chemical_compound_source        -
_chemical_formula_analytical     'C10 H25 Al Co N4 O8 P2'
_chemical_formula_moiety         'C10 H24 N4.Co.Al.P O4.P O3 (OH)'
_chemical_formula_structural     'C10 H25 Al Co N4 O8 P2'
_chemical_formula_sum            'C10 H25 Al Co N4 O8 P2'
_chemical_formula_weight         477.19
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.3230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9780(8)
_cell_length_b                   14.7200(8)
_cell_length_c                   8.4792(5)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      168
_cell_measurement_theta_min      12
_cell_volume                     1849.77(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CCD
_diffrn_measurement_method       'phi and omega scans'
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7991
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.775120
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    -
_exptl_crystal_description       prism
_exptl_crystal_F_000             988
_exptl_crystal_size_max          .28
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .25
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.984
_refine_ls_goodness_of_fit_obs   1.042
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         2617
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.176
_refine_ls_restrained_S_obs      1.041
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_obs          0.0285
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0818
_refine_ls_wR_factor_obs         0.0643
_reflns_number_observed          2100
_reflns_number_total             2659
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b003430o.txt
_cod_data_source_block           eppw3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/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_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '-' was changed to '?' - the value is
undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value '-' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1849.8(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7203984