A robust two-dimensional hydrogen-bonded network for the predictable assembly of ternary co-crystals of furosemide
Srirambhatla, Vijay K.; Kraft, Arno; Watt, Stephen; Powell, Anthony V.; CrystEngComm 16 (2014) 9979–; doi:10.1039/C4CE01692K

data_7218161
_publ_section_related_literature
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? 
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_publ_section_title
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 A robust two-dimensional hydrogen-bonded network for the predictable
 assembly of ternary co-crystals of furosemide
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_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              9979
_journal_paper_doi               10.1039/C4CE01692K
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C12 H11 Cl N2 O5 S, C10 H8 N2, 0.5(C6 H6 O2)'
_chemical_formula_sum            'C25 H22 Cl N4 O6 S'
_chemical_formula_weight         541.98
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             12-06-08
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                83.633(3)
_cell_angle_beta                 89.624(3)
_cell_angle_gamma                72.794(3)
_cell_formula_units_Z            2
_cell_length_a                   6.9302(4)
_cell_length_b                   9.9356(6)
_cell_length_c                   18.6298(11)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1217.34(13)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.981
_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  0.024
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
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_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21940
_diffrn_reflns_theta_full        25.162
_diffrn_reflns_theta_max         28.922
_diffrn_reflns_theta_min         1.100
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.9854
_exptl_absorpt_correction_T_min  0.9768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5405
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.0009833
_refine_ls_shift/su_mean         0.0000484
_refine_ls_structure_factor_coef F
_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: 
 0.263 0.296 0.132 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0477
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0366
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                5405
_reflns_number_total             6308
_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   0.0436
_oxford_refine_ls_scale          0.11443(13)
_oxford_reflns_number_all        6292
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'x84313_0m in P-1'
_cod_data_source_file            c4ce01692k2.cif
_cod_data_source_block           FUS-BP-HYDQ(1)
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7218156--7218161.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7218161
_iucr_refine_instruction_details_constraints
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BLOCK SCALE X'S, U'S 
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RIDE C   (  24,X'S) H   (  24,X'S) 
RIDE N   (   1,X'S) H   (   7,X'S) H   (   6,X'S) 
RIDE N   (   2,X'S) H   (   2,X'S) 
RIDE O   (   1,X'S) H   (   1,X'S) 
RIDE C   (   3,X'S) H   (   3,X'S) 
RIDE C   (   5,X'S) H   (   5,X'S) 
RIDE C   (   8,X'S) H   (   8,X'S) H   (   9,X'S) 
RIDE C   (  10,X'S) H   (  10,X'S) 
RIDE C   (  11,X'S) H   (  11,X'S) 
RIDE C   (  12,X'S) H   (  12,X'S) 
RIDE C   (  13,X'S) H   (  13,X'S) 
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RIDE C   (  15,X'S) H   (  15,X'S) 
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RIDE C   (  19,X'S) H   (  19,X'S) 
RIDE C   (  20,X'S) H   (  20,X'S) 
RIDE C   (  21,X'S) H   (  21,X'S) 
RIDE C   (  22,X'S) H   (  22,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;