Experimental Charge-Density Study of the Intra- and Intermolecular Bonding in TKX-50.
Tidey, Jeremiah P.; Zhurov, Vladimir V.; Gianopoulos, Christopher G.; Zhurova, Elizabeth A.; Pinkerton, A. Alan; The journal of physical chemistry. A 121 (2017) 8962–8972; doi:10.1021/acs.jpca.7b09367

data_1548377
_publ_section_title
;
 Experimental Charge-Density Study of the Intra- and Intermolecular
 Bonding in TKX-50.
;
_journal_issue                   46
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              8962
_journal_page_last               8972
_journal_paper_doi               10.1021/acs.jpca.7b09367
_journal_volume                  121
_journal_year                    2017
_chemical_formula_moiety         'C2 H8 N10 O4'
_chemical_formula_sum            'C2 H8 N10 O4'
_chemical_formula_weight         236.18
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 95.571(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.49040(10)
_cell_length_b                   11.4912(3)
_cell_length_c                   6.45560(10)
_cell_measurement_reflns_used    74492
_cell_measurement_temperature    20.0(1)
_cell_measurement_theta_max      70.848
_cell_measurement_theta_min      3.546
_cell_volume                     405.368(14)
_computing_cell_refinement       'Otwinowski & Minor (1997)'
_computing_data_collection       'CrystalClear, (2005)'
_computing_data_reduction
;
Zhurova et al,(1999), Zhurov et al,(2008), Blessing, (1995,1997)
;
_computing_molecular_graphics    'Volkov et al, (2006), Stash, (2002,2005)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_computing_structure_solution    'Sheldrick (2008)'
_diffrn_ambient_temperature      20.0(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device       'Rigaku R-axis Rapid'
_diffrn_measurement_method       w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0136
_diffrn_reflns_av_unetI/netI     0.0074
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            74492
_diffrn_reflns_theta_full        46.366
_diffrn_reflns_theta_max         70.848
_diffrn_reflns_theta_min         3.546
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_description       block
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.111
_refine_diff_density_min         -0.080
_refine_diff_density_rms         0.019
_refine_ls_extinction_coef       0.521(3)
_refine_ls_extinction_expression
;
Becker, P.J. & Coppens, P. (1974) Acta Cryst., A30, 129-153.
;
_refine_ls_extinction_method     'Becker-Coppens type 1 Lorentzian isotropic'
_refine_ls_goodness_of_fit_ref   1.333
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         7072
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.007
_refine_ls_R_factor_gt           0.007
_refine_ls_R_Fsqd_factor         0.008
_refine_ls_shift/su_max          0.000000004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
calc w1 = [Fo*sqrt(w2) + sqrt(Fo^2^w2^2^ + sqrt(w2^2^))]^2^
where
     calc w2 = q/[s^2^(Fo^2^) + (0.00 P)^2^ + 0.00 P + 0.00 + 0.00 sin(th)]
     where P = (0.3333 Fo^2^ + 0.6667 Fc^2^)
           q = 1.0
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.005
_reflns_number_gt                7072
_reflns_number_total             7716
_reflns_threshold_expression
;
 I>3\s, non-overlapped & non-partial reflections
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_cod_data_source_file            jp7b09367_si_001.cif
_cod_data_source_block           TKX_He
_cod_database_code               1548377
_atom_site_anharm_details
;
The atomic anharmonic pdf is approximated by a Gram-Charlier expansion
about the harmonic pdf, according to the expression :
 
      P(u) = (1 + Cijk*Hijk/3! + Dijkl*Hijkl/4!)*P(0)
 
The coefficients Cijk and Dijkl are refined in the least squares procedure.
The reported coefficients Cijk are multiplied by 1000 and Dijkl by 10000.
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