Ambient temperature crystallisation of a lamellar gallium fluorophosphate from the synthesis solution of microporous ULM-5
Livage, Carine; Millange, Franck; Loiseau, Thierry; Simon, Nathalie; Férey, Gérard; Walton, Richard I.; O’Hare, Dermot; Chemical Communications  (2001) 994–; doi:10.1039/b102753k

data_7114941
_publ_section_title
;
 Ambient temperature crystallisation of a lamellar gallium fluorophosphate
 from the synthesis solution of microporous ULM-5
;
_journal_issue                   11
_journal_name_full               'Chemical Communications'
_journal_page_first              994
_journal_paper_doi               10.1039/b102753k
_journal_year                    2001
_chemical_compound_source        'synthesised by authors'
_chemical_formula_moiety         'C12 H52 F2 Ga3 N4 O23.50 P4'
_chemical_formula_sum            'C12 H52 F2 Ga3 N4 O23.5 P4'
_chemical_formula_weight         999.62
_chemical_name_common
'Ga3F2(OH)4(H2PO4)(HPO4)3 [H3N(CH2)6NH3]2 3.5H2O'
_chemical_name_systematic
; 
? 
;
_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                 95.91(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2007(15)
_cell_length_b                   14.417(4)
_cell_length_c                   23.195(6)
_cell_measurement_reflns_used    4263
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.67
_cell_volume                     3393.0(14)
_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      296(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  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20065
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.659
_exptl_absorpt_correction_T_max  0.8578
_exptl_absorpt_correction_T_min  0.6616
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       0.00019(8)
_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   1.026
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_obs          0.0562
_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^)+(0.0620P)^2^+16.0021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1564
_refine_ls_wR_factor_obs         0.1319
_reflns_number_observed          4263
_reflns_number_total             6931
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b102753k.txt
_cod_data_source_block           final
_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^)+(0.0620P)^2^+16.0021P] 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^)+(0.0620P)^2^+16.0021P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C12 H52 F2 Ga3 N4 O23.50 P4'
_cod_database_code               7114941