Furosemide Cocrystals: Structures, Hydrogen Bonding, and Implications for Properties
Harriss, Bethany I.; Vella-Zarb, Liana; Wilson, Claire; Evans, Ivana Radosavljevic; Crystal Growth & Design 14 (2014) 783–; doi:10.1021/cg401662d

data_4509915
_publ_section_title
;
 Furosemide Cocrystals: Structures, Hydrogen Bonding, and Implications for
 Properties
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              783
_journal_paper_doi               10.1021/cg401662d
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C19 H18 Cl1 N3 O7 S1'
_chemical_formula_sum            'C19 H18 Cl N3 O7 S'
_chemical_formula_weight         467.89
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 122.37(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.823(5)
_cell_length_b                   4.7607(10)
_cell_length_c                   18.427(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1987.4(10)
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.087
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17604
_diffrn_reflns_theta_full        25.560
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.123
_diffrn_source                   synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.347
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.61
_refine_ls_extinction_coef       125.549
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9886
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4461
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.0010421
_refine_ls_shift/su_mean         0.0000333
_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: 
 6.02 7.90 2.37 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1274
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1274
_reflns_limit_h_max              29
_reflns_limit_h_min              -34
_reflns_limit_k_max              6
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                2560
_reflns_number_total             4469
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.35
_oxford_diffrn_Wilson_scale      18.90
_oxford_refine_ls_r_factor_ref   0.0592
_oxford_refine_ls_scale          0.2674(3)
_oxford_reflns_number_all        4461
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            cg401662d_si_005.cif
_cod_data_source_block           global
_cod_original_cell_volume        1987.3(10)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C19 H18 Cl1 N3 O7 S1'
_cod_database_code               4509915