Sodium and potassium salts of bumetanide trihydrate: Impact of counterion on structure, aqueous solubility and dehydration kinetics
Ong, Winston; Cheung, Eugene Y.; Schultz, Karen A.; Smith, Cartney; Bourassa, James; Hickey, Magali B.; CrystEngComm 14 (2012) 2428–; doi:10.1039/c2ce06631a

data_7207652
_publ_section_title
;
 Sodium and potassium salts of bumetanide trihydrate: Impact of counterion
 on structure, aqueous solubility and dehydration kinetics
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              2428
_journal_paper_doi               10.1039/c2ce06631a
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C17 H25 K1 N2 O8 S1'
_chemical_formula_sum            'C17 H25 K N2 O8 S'
_chemical_formula_weight         456.56
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 102.160(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.797(2)
_cell_length_b                   5.4342(3)
_cell_length_c                   17.5936(9)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4280.3(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_max       72
_diffrn_reflns_limit_h_min       -72
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            92568
_diffrn_reflns_theta_full        34.615
_diffrn_reflns_theta_max         34.615
_diffrn_reflns_theta_min         1.819
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.573
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.82
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0355
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         9113
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.0010833
_refine_ls_shift/su_mean         0.0006254
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
9.67 12.5 3.74
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0788
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0788
_reflns_limit_h_max              70
_reflns_limit_h_min              -72
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                7515
_reflns_number_total             9128
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.08
_oxford_diffrn_Wilson_scale      23.63
_oxford_refine_ls_r_factor_ref   0.0477
_oxford_refine_ls_scale          0.21833(6)
_oxford_reflns_number_all        9113
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c2ce06631a.txt
_cod_data_source_block           1
_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.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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      'C 1 2/c 1 '
_cod_original_formula_sum        'C17 H25 K1 N2 O8 S1'
_cod_database_code               7207652