Hydrogen-bonding patterns in bis(trimethoprim) dipicolinate pentahydrate
Madhukar Hemamalini; Packianathan Thomas Muthiah; Gabriele Bocelli; Andrea Cantoni; Acta Crystallographica Section E 61 (2005) o2368–o2371; doi:10.1107/S1600536805020167

data_2206479
_publ_section_title
;
 Hydrogen-bonding patterns in bis(trimethoprim) dipicolinate
 pentahydrate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2368
_journal_page_last               o2371
_journal_paper_doi               10.1107/S1600536805020167
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '2C14 H19 N4 O3 + , C7 H3 N O4 2- , 5H2 O'
_chemical_formula_moiety         '2C14 H19 N4 O3 + , C7 H3 N O4 2- , 5H2 O'
_chemical_formula_sum            'C35 H51 N9 O15'
_chemical_formula_weight         837.85
_chemical_name_common            'Trimethoprim dipicolinate pentahydrate'
_chemical_name_systematic
;
(2,4-diamino-5-(3',4',5'-trimethoxybenzyl)pyrimidinium
dipicolinate pentahydrate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.23(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.713(2)
_cell_length_b                   12.025(3)
_cell_length_c                   35.703(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      3.12
_cell_volume                     4158.7(14)
_computing_cell_refinement       'MolEN (Fair, 1990)'
_computing_data_collection       'FEBO (Belletti, 1996)'
_computing_data_reduction        MolEN
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and PLATON (Spek, 2003)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Philips PW1100'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9210
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  60
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.9802
_exptl_absorpt_correction_T_min  0.9610
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(SHELXA; Sheldrick, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.351
_refine_ls_extinction_coef       0.0032(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001Fc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9074
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1425
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0728P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1595
_reflns_number_gt                4170
_reflns_number_total             9074
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6416.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2206479
_cod_database_fobs_code          2206479