The Devil is in the Detail: A Rare H-Bonding Motif in New Forms of Docetaxel
Vella-Zarb, Liana; Dinnebier, Robert E.; Baisch, Ulrich; Crystal Growth & Design 13 (2013) 4402–; doi:10.1021/cg400814a

data_4510772
_publ_section_title
;
 The Devil is in the Detail: A Rare H-Bonding Motif in New Forms of
 Docetaxel
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4402
_journal_paper_doi               10.1021/cg400814a
_journal_volume                  13
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C43 H53 N O14, C H3.5 O, H2 O'
_chemical_formula_sum            'C44 H58.5 N O16'
_chemical_formula_weight         857.41
_chemical_name_systematic        'Docetaxel dihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2012-12-24
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.213(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.287(2)
_cell_length_b                   32.938(8)
_cell_length_c                   12.780(3)
_cell_measurement_reflns_used    4960
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      2.37
_cell_volume                     4330.3(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XM, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.627
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.688900
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_Laue_measured_fraction_full 0.627
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10423
_diffrn_reflns_point_group_measured_fraction_full 0.622
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         21.257
_diffrn_reflns_theta_min         1.544
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1346 before and 0.0843 after correction.
The Ratio of minimum to maximum transmission is 0.6174.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       plate
_exptl_crystal_F_000             1830
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1973 quotients [(I+)-I(-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.3(10)
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1139
_refine_ls_number_reflns         10423
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0501P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1558
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.616
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                5929
_reflns_number_total             10423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg400814a_si_002.cif
_cod_data_source_block           doceEt2W
_cod_original_cell_volume        4330.2(17)
_cod_original_formula_sum        'C44 H58.50 N O16'
_cod_database_code               4510772
_diffrn_reflns_sigmai/neti       0.1850
_shelx_estimated_absorpt_t_max   1.000
_shelx_estimated_absorpt_t_min   0.995
_shelxl_version_number           2012-4