Hydrogen bonding in brucinium dihydrogen citrate trihydrate at 130 K
Graham Smith; Urs D. Wermuth; Jonathan M. White; Acta Crystallographica Section C 61 (2005) o621–o624; doi:10.1107/S0108270105028222

data_2015221
_publ_section_title
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 Hydrogen bonding in brucinium dihydrogen citrate trihydrate at 130 K
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_journal_coeditor_code           TA1515
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o621
_journal_page_last               o624
_journal_paper_doi               10.1107/S0108270105028222
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C23 H27 N2 O4 2+, C6 H7 O7 2-, 3H2 O'
_chemical_formula_moiety         'C23 H27 N2 O4 2+, C6 H7 O7 2-, 3H2 O'
_chemical_formula_sum            'C29 H40 N2 O14'
_chemical_formula_weight         640.63
_chemical_melting_point          492(2)
_chemical_name_common            'brucinium dihydrogen citrate trihydrate'
_chemical_name_systematic
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2,3-dimethoxy-10-oxostrychnidinium dihydrogencitrate trihydrate
;
_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 (Sheldrick, 1997)'
_cell_angle_alpha                75.775(2)
_cell_angle_beta                 80.917(2)
_cell_angle_gamma                81.553(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2355(8)
_cell_length_b                   9.6894(8)
_cell_length_c                   17.1446(15)
_cell_measurement_reflns_used    2391
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.25
_cell_volume                     1459.1(2)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON
_computing_structure_refinement
'SHELXL97 (Sheldrick, 1997) in WinGX  (Farrugia, 1999)'
_computing_structure_solution
'SHELXS97 (Sheldrick, 1997) in WinGX (Farrugia, 1999)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7737
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         5129
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0266P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                4354
_reflns_number_total             5129
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            ta1515.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '489.9--494.1' was changed to
'492(2)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '489.9--494.1' was changed to
'492(2)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2015221
_cod_database_fobs_code          2015221