A 1:1 complex between deoxycholate and tris(hydroxymethyl)methylammonium
Tusvik, Per Helge; Mostad, Arvid; Dalhus, Bjørn; Rosenqvist, Einar; Acta Crystallographica Section C 55 (1999) 1113–1115; doi:10.1107/S0108270199004370

data_2008703
_publ_section_title
;
 A 1:1 complex between deoxycholate and
 tris(hydroxymethyl)methylammonium
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1113
_journal_page_last               1115
_journal_paper_doi               10.1107/S0108270199004370
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C4 H12 N O3 +, C24 H39 O4 -, 3H2 O'
_chemical_formula_structural     'C28 H57 N O10'
_chemical_formula_sum            'C28 H57 N O10'
_chemical_formula_weight         567.75
_chemical_name_common
;
deoxycholic acid, tris(hydroxymethyl) amino methane, water
;
_chemical_name_systematic
;
tris(hydroxymethyl)methyl ammonium 3\a,12\a-dihydroxy-5\b-cholan-24-oate
trihydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.0480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.16730(10)
_cell_length_b                   10.1932(2)
_cell_length_c                   15.4592(2)
_cell_measurement_reflns_used    7716
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.33
_cell_measurement_theta_min      1.35
_cell_volume                     1566.86(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_sigmaI/netI    0.035
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24971
_diffrn_reflns_theta_max         36.33
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         12832
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_restrained_S_obs      1.039
_refine_ls_R_factor_all          0.042
_refine_ls_R_factor_obs          0.035
_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^)+(0.0396P)^2^+0.1891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.092
_refine_ls_wR_factor_obs         0.084
_reflns_number_observed          11732
_reflns_number_total             12833
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            os1052.cif
_cod_data_source_block           per1
_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^)+(0.0396P)^2^+0.1891P] 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^)+(0.0396P)^2^+0.1891P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2008703
_cod_database_fobs_code          2008703