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_4323013
_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            'C10 H25 N2 O4 P'
_chemical_formula_weight         268.29
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.569(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.197(3)
_cell_length_b                   5.9923(13)
_cell_length_c                   16.580(3)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10.84
_cell_measurement_theta_min      4.74
_cell_volume                     1394.8(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.1256
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2850
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.90
_diffrn_standards_decay_%        11.18
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0045(22)
_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   0.868
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_obs          0.0610
_refine_ls_shift/esd_max         0.147
_refine_ls_shift/esd_mean        0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1559
_refine_ls_wR_factor_obs         0.1380
_reflns_number_observed          1488
_reflns_number_total             2737
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980069w_1.cif
_cod_data_source_block
s9633,_cyclopentylammonium_monohydrogen_phosphate_(CMP)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' 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^)+(0.0798P)^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^)+(0.0798P)^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        1394.7(5)
_cod_database_code               4323013