Invariom modeling of ceftazidime pentahydrate: molecular properties from a 200 second synchrotron microcrystal experiment
Schürmann, C. J.; Pröpper, K.; Wagner, T.; Dittrich, B.; Acta Crystallographica Section B 68 (2012) 313–317; doi:10.1107/S0108768112017831

data_2105122
_publ_contact_author
;
Dittrich, Birger, Institute of inorganic chemistry,
Georg-August-University Goettingen, Tammannstr. 4,
D-37077 Goettingen, Germany.
;
_publ_section_title
;
 Invariom modeling of ceftazidime pentahydrate: molecular properties from
 a 200 second synchrotron microcrystal experiment
;
_journal_coeditor_code           GW5017
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              313
_journal_page_last               317
_journal_paper_doi               10.1107/S0108768112017831
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         'C22 H22 N6 O7 S2, 5(H2 O)'
_chemical_formula_sum            'C22 H32 N6 O12 S2'
_chemical_formula_weight         636.68
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_method           'XD routine XDCIF'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4.0
_cell_length_a                   8.9716(5)
_cell_length_b                   10.3943(7)
_cell_length_c                   31.5444(12)
_cell_measurement_reflns_used    12106
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      1.9
_cell_volume                     2941.6(3)
_computing_publication_material  'enCIFer 1.3, CCDC, 2008'
_computing_structure_refinement  'Koritsanszky et al, (2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.71
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Pilatus 6M'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           'monochromated synchrotron radiation'
_diffrn_radiation_wavelength     0.65000
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            22933
_diffrn_reflns_theta_full        0.952
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6472
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2008/2, multi-scan. (G. M. Sheldrick, 2008)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.4376
_exptl_crystal_description       triangle
_exptl_crystal_F_000             192.0
_exptl_crystal_size_max          0.008
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.003
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.571
_refine_ls_abs_structure_details
;
An invariom refinement was performed (Dittrich, Acta Cryst. A62, 217)
to improve the standard uncertainty of the Flack parameter
(Flack, Acta Cryst, A39, 876) compared to an independent-atom refinement.
After using non-spherical scattering factors the standard uncertainty is
reduced and a reliable assignment (Flack, J. Appl. Cryst. (2000). 33, 1143)
of absolute structure is possible.
;
_refine_ls_abs_structure_Flack   0.01(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.5191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6506
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
     calc w1 = Fo*sqrt(w2) + sqrt(Fo^2^w2^2^ + sqrt(w2^2^))
     where
     calc w2 = q/[s^2^(Fo^2^) + (0.05 P)^2^ + 0.00 P + 0.00 + 0.00 sin(th)]
     where P = (0.3333 Fo^2^ + 0.6667 Fc^2^)
           q = 1.0
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                6506
_reflns_number_total             8486
_reflns_threshold_expression     F>4(\s)F
_cod_data_source_file            gw5017.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P21 21 21'
_cod_database_code               2105122
_cod_database_fobs_code          2105122