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_4117244
_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 G N3 O3), 14.5(H2 O)'
_chemical_formula_sum            'C51 H83 F3 N9 O23.5'
_chemical_formula_weight         1255.26
_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                115.640(3)
_cell_angle_beta                 103.505(3)
_cell_angle_gamma                102.530(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8743(6)
_cell_length_b                   15.9086(6)
_cell_length_c                   16.5542(11)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      3.02
_cell_volume                     2984.8(3)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48264
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         3.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  0.9908
_exptl_absorpt_correction_T_min  0.9794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       Block
_exptl_crystal_F_000             1334
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     917
_refine_ls_number_reflns         15713
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+2.1320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1601
_reflns_number_gt                11326
_reflns_number_total             15713
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja208647n_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-10
;
_cod_original_formula_sum        'C51 H83 F3 N9 O23.50'
_cod_database_code               4117244