Discrete Cuboidal 15- and 16-Membered Water Clusters in Brucine 3.86-Hydrate, Water Release and Its Consequences
Białońska, Agata; Ciunik, Zbigniew; Ilczyszyn, Maria M.; Siczek, Miłosz; Crystal Growth & Design 14 (2014) 6537–; doi:10.1021/cg501437g

data_4512402
_publ_section_title
;
 Discrete Cuboidal 15- and 16-Membered Water Clusters in Brucine
 3.86-Hydrate, Water Release and Its Consequences
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              6537
_journal_paper_doi               10.1021/cg501437g
_journal_volume                  14
_journal_year                    2014
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C23 H26 N2 o4, 3.86(H2 O)'
_chemical_formula_sum            'C23 H33.67 N2 O7.86'
_chemical_formula_weight         463.89
_chemical_name_common            'brucine 3.86-hydrate'
_chemical_name_systematic
;
brucine 3.86-hydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 122.56(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.070(5)
_cell_length_b                   12.353(2)
_cell_length_c                   17.111(3)
_cell_measurement_reflns_used    1689
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.44
_cell_measurement_theta_min      3.20
_cell_volume                     4466(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21t (release 14-08-2012 CrysAlis171 .NET)
(compiled Aug 14 2012,18:12:40)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21t (release 14-08-2012 CrysAlis171 .NET)
(compiled Aug 14 2012,18:12:40)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21t (release 14-08-2012 CrysAlis171 .NET)
(compiled Aug 14 2012,18:12:40)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
SHELXS-2013 (Sheldrick, G. M. (2008). <i>Acta Cryst.</i> <b>A64</b>, 112-122.)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15588
_diffrn_reflns_point_group_measured_fraction_full 0.721
_diffrn_reflns_point_group_measured_fraction_max 0.654
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.481
_diffrn_reflns_theta_min         3.330
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       needle
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1079 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.7(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         7408
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0410P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.361
_reflns_Friedel_fraction_full    0.422
_reflns_Friedel_fraction_max     0.363
_reflns_number_gt                5255
_reflns_number_total             7408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501437g_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4512402--4512403.cif.'
_cod_original_cell_volume        4466.2(19)
_cod_database_code               4512402
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2014-3
_shelx_res_checksum              23294
_shelx_hkl_checksum              55002