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_4512403
_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'
_chemical_formula_sum            'C23 H26 N2 O4'
_chemical_formula_weight         394.46
_chemical_name_common            'anhydrous brucine'
_chemical_name_systematic
;
anhydrous brucine
;
_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   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 115.88(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.323(2)
_cell_length_b                   12.764(3)
_cell_length_c                   10.191(2)
_cell_measurement_reflns_used    350
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      37.1466
_cell_measurement_theta_min      2.7078
_cell_volume                     974.1(4)
_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      273(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_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  0.1146
_diffrn_reflns_av_unetI/netI     0.4113
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8752
_diffrn_reflns_point_group_measured_fraction_full 0.832
_diffrn_reflns_point_group_measured_fraction_max 0.620
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.323
_diffrn_reflns_theta_min         2.657
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       needle
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.131
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 370 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   3.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.673
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         6728
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.673
_refine_ls_R_factor_all          0.3255
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0057P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0707
_reflns_Friedel_coverage         0.430
_reflns_Friedel_fraction_full    0.660
_reflns_Friedel_fraction_max     0.386
_reflns_number_gt                1364
_reflns_number_total             6728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501437g_si_002.cif
_cod_data_source_block           1dehydrated
_cod_depositor_comments
'Adding full bibliography for 4512402--4512403.cif.'
_cod_database_code               4512403
_shelxl_version_number           2014-3
_shelx_res_checksum              56507
_shelx_hkl_checksum              15720