Cyclic water pentamers in triclinic crystals of brucinium <small>L</small>-glycerate
Białońska, Agata; Ciunik, Zbigniew; Popek, Tomasz; Lis, Tadeusz; Acta Crystallographica Section C 61 (2005) o88–o91; doi:10.1107/S0108270104031853

data_2014757
_publ_section_title
;
 Cyclic water pentamers in triclinic crystals of brucinium
 <small>L</small>-glycerate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o88
_journal_page_last               o91
_journal_paper_doi               10.1107/S0108270104031853
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C23 H27 N2 O4 + , C3 H5 O4 - , 4.75H2 O'
_chemical_formula_moiety         'C23 H27 N2 O4 + , C3 H5 O4 - , 4.75H2 O'
_chemical_formula_sum            'C26 H41.5 N2 O12.75'
_chemical_formula_weight         586.11
_chemical_name_common            'brucinium L-glycerate 4.75 hydrate'
_chemical_name_systematic
;
brucinium L-glycerate 4.75 hydrate
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                77.21(3)
_cell_angle_beta                 87.36(3)
_cell_angle_gamma                81.57(3)
_cell_formula_units_Z            2
_cell_length_a                   9.308(3)
_cell_length_b                   9.578(3)
_cell_length_c                   16.130(4)
_cell_measurement_reflns_used    6626
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      3.37
_cell_volume                     1387.1(7)
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2001)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2001)'
_computing_data_reduction        CrysAlisRED
_computing_molecular_graphics    'SHELXTL-NT (Bruker, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Kuma KM4 CCD'
_diffrn_measurement_method       \w
_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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16810
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         3.37
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             627
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         6655
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.043P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                5944
_reflns_number_total             6655
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sx1156.cif
_cod_data_source_block           I
_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 
;
_cod_original_formula_sum        'C26 H41.50 N2 O12.75'
_cod_database_code               2014757
_cod_database_fobs_code          2014757