Anisotropic thermal expansion in 18-crown-6·2 H2O·2 HNO3
Calleja, Maria; Mason, Sax A.; Prince, Paul D.; Steed, Jonathan W.; Wilkinson, Clive; New Journal of Chemistry 27 (2003) 28–; doi:10.1039/b207292k

data_7050439
_publ_section_title
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 Anisotropic thermal expansion in 18-crown-6&#x00B7;2 H2O&#x00B7;2 HNO3
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_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              28
_journal_paper_doi               10.1039/b207292k
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C12 H30 N2 O14'
_chemical_formula_weight         426.38
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.314(6)
_cell_angle_beta                 67.323(7)
_cell_angle_gamma                87.935(8)
_cell_formula_units_Z            1
_cell_length_a                   7.5600(15)
_cell_length_b                   7.9619(15)
_cell_length_c                   9.7801(17)
_cell_measurement_reflns_used    213
_cell_measurement_temperature    250(2)
_cell_volume                     518.44(17)
_computing_data_reduction        Racer
_computing_molecular_graphics    'XSeed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.740
_diffrn_measured_fraction_theta_max 0.740
_diffrn_measurement_device_type  'Instrument D9'
_diffrn_radiation_monochromator  Cu220
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ILL reactor'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.83900
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1312
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.79
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   'Face index'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             68
_exptl_crystal_size_max          4.0
_exptl_crystal_size_mid          2.6
_exptl_crystal_size_min          1.7
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.019(2)
_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_ref   1.091
_refine_ls_hydrogen_treatment    refined
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         1154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0198P)^2^+1.0611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                910
_reflns_number_total             1154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207292k.txt
_cod_data_source_block           250kdata(250K-HNO3-H2O-18crown6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050439