Ionothermal synthesis of two novel metal organophosphonates
Byrne, Peter J.; Wragg, David S.; Warren, John E.; Morris, Russell E.; Dalton Transactions  (2009) 795–799; doi:10.1039/b813731e

data_7000415
_publ_section_title
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 Ionothermal synthesis of two novel metal organophosphonates
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_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              795
_journal_page_last               799
_journal_paper_doi               10.1039/b813731e
_journal_year                    2009
_chemical_formula_moiety         Al5F((C4H9)PO3)6(OH)2(C8N4H6)2
_chemical_formula_sum            'C32 H68 Al5 F N4 O20 P6'
_chemical_formula_weight         1168.62
_chemical_name_systematic
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?
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_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_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            3
_cell_length_a                   12.5125(18)
_cell_length_b                   12.5125(18)
_cell_length_c                   29.518(8)
_cell_measurement_reflns_used    1855
_cell_measurement_temperature    30(2)
_cell_measurement_theta_max      23.67
_cell_measurement_theta_min      2.20
_cell_volume                     4002.3(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      30(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'silicon (111)'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67030
_diffrn_reflns_av_R_equivalents  0.1160
_diffrn_reflns_av_sigmaI/netI    0.1667
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            24131
_diffrn_reflns_theta_full        24.51
_diffrn_reflns_theta_max         24.51
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.982
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.0501
_exptl_crystal_size_mid          0.0167
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.26(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         10550
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1743
_reflns_number_gt                6201
_reflns_number_total             10550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813731e.txt
_cod_data_source_block           absnew
_cod_depositor_comments
;
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P3(2) '
_cod_database_code               7000415