Crystal Structures of Nitronium Tetranitratogallate and Its Reversible Solid-State Phase Transition Mediated by Nonmerohedral Twinning
Daniel G. Colombo; Victor G. Young,; Wayne L. Gladfelter; Inorganic Chemistry 39 (2000) 4621–4624; doi:10.1021/ic0002418

data_4321396
_publ_contact_author
; Prof. Wayne Gladfelter
  Department of Chemistry
  University of Minnesota
  207 Pleasant St S.E.
  Minneapolis
  Minnesota
  USA
;
_publ_contact_author_email       gladfelt@chem.umn.edu
_publ_contact_author_fax         (612)626-7541
_publ_contact_author_phone       (612)624-4391
_publ_section_title
;
 Crystal Structures of Nitronium Tetranitratogallate and Its Reversible
 Solid-State Phase Transition Mediated by Nonmerohedral Twinning
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4621
_journal_page_last               4624
_journal_paper_doi               10.1021/ic0002418
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        'D. Columbo / Prof. W. Gladfelter'
_chemical_formula_analytical     'Ga N5 O14'
_chemical_formula_moiety         'Ga N5 O14'
_chemical_formula_structural     '[NO2][Ga(NO3)4]'
_chemical_formula_sum            'Ga N5 O14'
_chemical_formula_weight         363.77
_chemical_name_common            1
_chemical_name_systematic        ' Nitronium Tetranitratogallate'
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2774(3)
_cell_length_b                   9.2774(3)
_cell_length_c                   6.1149(2)
_cell_measurement_reflns_used    2979
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      3.1
_cell_volume                     526.31(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens SMART platform CCD'
_diffrn_measurement_method       multi-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2945
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    2.718
_exptl_absorpt_correction_T_max  0.337
_exptl_absorpt_correction_T_min  0.149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Blessing, A51, 33-38, 1995'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.295
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(2)
_refine_ls_extinction_coef       0.0513(42)
_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   1.052
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0570
_refine_ls_wR_factor_ref         0.0570
_reflns_number_gt                765
_reflns_number_total             767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0002418_1.cif
_cod_data_source_block           1
_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^)+(0.0293P)^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^)+(0.0293P)^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_database_code               4321396