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_4509916
_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
'C12 H11 Cl N2 O5 S, C12 H11 Cl N2 O5 S, C6 H6 N2 O'
_chemical_formula_sum            'C30 H28 Cl2 N6 O11 S2'
_chemical_formula_weight         783.60
_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                 94.353(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.0178(11)
_cell_length_b                   38.527(8)
_cell_length_c                   17.031(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    120
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     3282.9(13)
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_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  0.085
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24388
_diffrn_reflns_theta_full        24.969
_diffrn_reflns_theta_max         24.969
_diffrn_reflns_theta_min         1.310
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1615.904
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.00
_refine_diff_density_min         -1.06
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9181
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         5701
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0977
_refine_ls_shift/su_max          0.0002741
_refine_ls_shift/su_mean         0.0000214
_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: 
 34.1 36.7 19.4 5.52 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1369
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1369
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              45
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                4232
_reflns_number_total             5720
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.1307
_oxford_refine_ls_scale          0.3507(4)
_oxford_reflns_number_all        5701
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            cg401662d_si_004.cif
_cod_data_source_block           global
_cod_original_cell_volume        3283.0(12)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4509916
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE 
CONT CL(1,X'S,U'S) UNTIL C(54) 
CONT O(100,X'S,U[ISO]) UNTIL C(201) 
CONT O(26,X'S,U[ISO]) UNTIL N(31) 
CONT  H   ( 481,X'S, U[ISO]) 
CONT  H   ( 482,X'S, U[ISO]) 
CONT  H   ( 211,X'S, U[ISO]) 
CONT  H   ( 212,X'S, U[ISO]) 
CONT  H   ( 14,X'S, U[ISO]) 
CONT  H   ( 35,X'S, U[ISO]) 
RIDE C   (   3,X'S) H   (   3,X'S) 
RIDE N   (   5,X'S) H   (   5,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (  16,X'S) H   (  16,X'S) 
RIDE C   (  32,X'S) H   (  32,X'S) 
RIDE C   (  38,X'S) H   (  38,X'S) 
RIDE N   (  39,X'S) H   (  39,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  43,X'S) H   (  43,X'S) 
RIDE C   (  44,X'S) H   (  44,X'S) 
RIDE C   (  45,X'S) H   (  45,X'S) 
RIDE C   (  50,X'S) H   (  50,X'S) 
RIDE C   (  51,X'S) H   (  51,X'S) 
RIDE C   (  53,X'S) H   (  53,X'S) 
RIDE C   (  54,X'S) H   (  54,X'S) 
RIDE C   ( 200,X'S) H   ( 200,X'S) 
RIDE C   ( 201,X'S) H   ( 201,X'S) 
RIDE C   ( 202,X'S) H   ( 202,X'S) 
RIDE C   ( 101,X'S) H   ( 101,X'S) 
RIDE C   ( 103,X'S) H   ( 103,X'S) 
RIDE C   ( 102,X'S) H   ( 102,X'S) 
EQUIV PART(2001,OCC) PART(2002,OCC) 
WEIGHT -1 PART(2002,OCC) 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
END                                                                             
;