Packing Interactions in Hydrated and Anhydrous Forms of the Antibiotic Ciprofloxacin: a Solid-State NMR, X-ray Diffraction, and Computer Simulation Study
Mafra, Luís; Santos, Sérgio M.; Siegel, Renée; Alves, Inês; Paz, Filipe A. Almeida; Dudenko, Dmytro; Spiess, Hans W.; Journal of the American Chemical Society 134 (2012) 71–74; doi:10.1021/ja208647n

data_4117243
_publ_contact_author_address
; Department of Chemistry
  University of Aveiro
  CICECO
  3810-193
  Aveiro
  Portugal

  Present address:
  Max-Planck-Insitut fur Polymerforschung
  Ackermannweg 10
  55128 Mainz
  Germany
;
_publ_contact_author_email       lmafra@ua.pt
_publ_contact_author_fax         '+351 234 370084'
_publ_contact_author_name        'Dr Luis Mafra'
_publ_contact_author_phone       '+351 234 370200'
_publ_section_title
;
 Packing Interactions in Hydrated and Anhydrous Forms of the Antibiotic
 Ciprofloxacin: a Solid-State NMR, X-ray Diffraction, and Computer
 Simulation Study
;
_journal_coden_ASTM              JACSAT
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              71
_journal_page_last               74
_journal_paper_doi               10.1021/ja208647n
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         '3(C17 H18 F N3 O3), 11(H2 O)'
_chemical_formula_sum            'C17 H25.333 F N3 O6.667'
_chemical_formula_weight         397.40
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '13 June 2011'
_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_cell_angle_alpha                111.4970(10)
_cell_angle_beta                 105.9840(10)
_cell_angle_gamma                106.1990(10)
_cell_formula_units_Z            6
_cell_length_a                   13.8921(4)
_cell_length_b                   15.0770(5)
_cell_length_c                   16.2208(5)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.84
_cell_measurement_theta_min      3.10
_cell_volume                     2751.22(16)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT+ (Bruker, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       '\w / \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46833
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         3.53
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.9942
_exptl_absorpt_correction_T_min  0.9838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       Block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         14677
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.9375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                9932
_reflns_number_total             14677
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja208647n_si_001.cif
_cod_data_source_block           2
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-10
;
_cod_original_cell_volume        2751.22(15)
_cod_database_code               4117243