Low-density hydrogen-bonded networks in crystals and at the air/water interface
Plaut, David J.; Lund, Kristian M.; Ward, Michael D.; Chemical Communications  (2000) 769–; doi:10.1039/a910252n

data_7110834
_publ_section_title
;
 Low-density hydrogen-bonded networks in crystals and at the air/water
 interface
;
_journal_issue                   9
_journal_name_full               'Chemical Communications'
_journal_page_first              769
_journal_paper_doi               10.1039/a910252n
_journal_year                    2000
_chemical_compound_source        'D. Plaut, Prof. M. Ward'
_chemical_formula_sum            'C36 H69 N3 O7'
_chemical_formula_weight         655.94
_chemical_name_common
'tris-ditertbutylammoniumtrimesate acetone clathrate  '
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.641(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7487(6)
_cell_length_b                   18.492(2)
_cell_length_c                   23.164(2)
_cell_measurement_reflns_used    4905
_cell_measurement_temperature    173(2)
_cell_volume                     4090.0(6)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Siemens'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Platform CCD, Siemens'
_diffrn_measurement_method       'omega-scans, area detector'
_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  0.0828
_diffrn_reflns_av_sigmaI/netI    0.1048
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30377
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.882464
_exptl_absorpt_correction_type   'SADABS, G. Sheldrick (1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0069(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   0.903
_refine_ls_goodness_of_fit_obs   1.166
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7227
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.903
_refine_ls_restrained_S_obs      1.166
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_obs          0.0600
_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^)+(0.0906P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1752
_refine_ls_wR_factor_obs         0.1478
_reflns_number_observed          3305
_reflns_number_total             7227
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a910252nsup1.cif
_cod_data_source_block           99150
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0906P)^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^)+(0.0906P)^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_original_cell_volume        4090.0(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7110834