Crystal structures with a challenge: high-pressure crystallisation of ciprofloxacin sodium salts and their recovery to ambient pressure
Fabbiani, Francesca P. A.; Dittrich, Birger; Florence, Alastair J.; Gelbrich, Thomas; Hursthouse, Michael B.; Kuhs, Werner F.; Shankland, Norman; Sowa, Heidrun; CrystEngComm 11 (2009) 1396–; doi:10.1039/b822987b

data_7200855
_publ_section_title
;
 Crystal structures with a challenge: high-pressure crystallisation of
 ciprofloxacin sodium salts and their recovery to ambient pressure
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1396
_journal_paper_doi               10.1039/b822987b
_journal_volume                  11
_journal_year                    2009
_chemical_compound_source
;
recovery of 2 to ambient pressure
;
_chemical_formula_moiety         'C17 H17.50 F1 N3 O3, Na0.50, 5(H2O)'
_chemical_formula_sum            'C17 H27.5 F N3 Na0.5 O8'
_chemical_formula_weight         432.41
_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   geom
_atom_sites_solution_primary
;
starting coordinates for cipro moiety taken
from the structure of 4
;
_cell_angle_alpha                85.247(14)
_cell_angle_beta                 99.498(13)
_cell_angle_gamma                93.272(14)
_cell_formula_units_Z            2
_cell_length_a                   9.391(8)
_cell_length_b                   9.570(8)
_cell_length_c                   11.095(9)
_cell_measurement_reflns_used    1144
_cell_measurement_temperature    100
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     979.1(14)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    MERCURY
_computing_publication_material
'CRYSTALS (Betteridge et al., 2003), PLATON, XCIF, ENCIFER'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Starting from fract. coordinates of 2'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Bruker Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.103
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6358
_diffrn_reflns_theta_full        19.420
_diffrn_reflns_theta_max         19.816
_diffrn_reflns_theta_min         1.866
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'based on symmetry-related measuraments'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             458
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.54
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8956
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         1772
_refine_ls_number_restraints     331
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.000103
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.12P)^2^ + 3.51P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2300
_refine_ls_wR_factor_gt          0.1971
_refine_ls_wR_factor_ref         0.2300
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              9
_reflns_limit_k_min              -8
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_gt                1061
_reflns_number_total             1773
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.56
_oxford_diffrn_Wilson_scale      5.37
_oxford_refine_ls_r_factor_ref   0.1286
_oxford_refine_ls_scale          0.544(3)
_oxford_reflns_number_all        1772
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            b822987b.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        979.2(14)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C17 H27.50 F1 N3 Na0.50 O8'
_cod_database_code               7200855