Crystal Structures of a Series of Novel Alkylammonium Phosphates and Their Formation in Aluminophosphate Synthesis Mixtures
Scott R. J. Oliver; Alan J. Lough; Geoffrey A. Ozin; Inorganic Chemistry 37 (1998) 5021–5028; doi:10.1021/ic980069w

data_4323014
_publ_section_title
;
 Crystal Structures of a Series of Novel Alkylammonium Phosphates and
 Their Formation in Aluminophosphate Synthesis Mixtures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5021
_journal_page_last               5028
_journal_paper_doi               10.1021/ic980069w
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C8 H22 N O4 P'
_chemical_formula_weight         227.24
_chemical_name_systematic
; 
 ? 
;
_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                 90.66
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.554
_cell_length_b                   34.652(3)
_cell_length_c                   7.3280(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1156.32(19)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2291
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.230
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_F_000             496
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0085(14)
_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   1.201
_refine_ls_goodness_of_fit_obs   1.208
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.382
_refine_ls_restrained_S_obs      1.208
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_obs          0.0474
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+1.8917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1542
_refine_ls_wR_factor_obs         0.1184
_reflns_number_observed          1596
_reflns_number_total             2031
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980069w_2.cif
_cod_data_source_block           s9548,_octylammonium_dihydrogen_phosphate_(ODP)
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+1.8917P] 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^)+(0.0332P)^2^+1.8917P] 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        1156.3(2)
_cod_original_formula_sum        'C8 H4 H18 N O4 P'
_cod_database_code               4323014