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_7000416
_publ_section_title
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 Ionothermal synthesis of two novel metal organophosphonates
;
_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         Ga2F(C4H9PO3)4H2.5(C7N2H11)0.5
_chemical_formula_sum            'C16 H38.5 F Ga2 O12 P4'
_chemical_formula_weight         705.29
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.103(3)
_cell_angle_beta                 99.824(5)
_cell_angle_gamma                95.923(5)
_cell_formula_units_Z            2
_cell_length_a                   11.892(4)
_cell_length_b                   12.388(4)
_cell_length_c                   13.868(4)
_cell_measurement_reflns_used    2076
_cell_measurement_temperature    30(2)
_cell_measurement_theta_max      20.4
_cell_measurement_theta_min      1.5
_cell_volume                     1861.3(10)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10871
_diffrn_reflns_theta_full        20.39
_diffrn_reflns_theta_max         20.39
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    1.492
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             726.0
_exptl_crystal_size_max          0.0625
_exptl_crystal_size_mid          0.0125
_exptl_crystal_size_min          0.0125
_platon_squeeze_details
;
;
_refine_diff_density_max         1.338
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0164P)^2^+35.0559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.1808
_reflns_number_gt                3512
_reflns_number_total             4379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813731e.txt
_cod_data_source_block           abssq
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_cell_measurement_temperature' value '-243(2)' was changed to
'30(2)' - it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1861.3(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C16 H38.50 F Ga2 O12 P4'
_cod_database_code               7000416