#------------------------------------------------------------------------------
#$Date: 2014-06-05 16:58:55 +0300 (Thu, 05 Jun 2014) $
#$Revision: 115653 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/03/4510390.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4510390
loop_
_publ_author_name
'Bia\/lo\'nska, Agata'
'Ciunik, Zbigniew'
_publ_section_title
;
Seventeen-Membered Water Cluster Resulting from Recognition of Solvated
Anions on Brucinium Corrugated Layers
;
_journal_issue 5
_journal_name_full 'Crystal Growth & Design'
_journal_page_first 2621
_journal_paper_doi 10.1021/cg500310n
_journal_volume 14
_journal_year 2014
_chemical_absolute_configuration rm
_chemical_formula_moiety 'C23 H27 N2 O4, C10 H9 N2 O5, 4.8(H2 O)'
_chemical_formula_sum 'C33 H45.6 N4 O13.8'
_chemical_formula_weight 719.13
_chemical_name_systematic
;
brucinium N-(4-nitrobenzoyl)-L-alaninate 4.8-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-2013
_cell_angle_alpha 90
_cell_angle_beta 104.98(3)
_cell_angle_gamma 90
_cell_formula_units_Z 16
_cell_length_a 31.826(6)
_cell_length_b 12.510(3)
_cell_length_c 35.668(3)
_cell_measurement_reflns_used 10237
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.8510
_cell_measurement_theta_min 3.0210
_cell_volume 13718(5)
_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). Acta Cryst. A64, 112-122.)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type 'Xcalibur, Sapphire2'
_diffrn_measurement_method '\w scan'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.1466
_diffrn_reflns_av_unetI/netI 0.2488
_diffrn_reflns_limit_h_max 53
_diffrn_reflns_limit_h_min -54
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 56
_diffrn_reflns_limit_l_min -60
_diffrn_reflns_number 126236
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 37.164
_diffrn_reflns_theta_min 2.910
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 0.109
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.393
_exptl_crystal_description plate
_exptl_crystal_F_000 6112
_exptl_crystal_size_max 0.620
_exptl_crystal_size_mid 0.160
_exptl_crystal_size_min 0.060
_refine_diff_density_max 0.369
_refine_diff_density_min -0.274
_refine_diff_density_rms 0.062
_refine_ls_abs_structure_details
;
Flack x determined using 3307 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack 0.2(8)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.955
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 2097
_refine_ls_number_reflns 52899
_refine_ls_number_restraints 337
_refine_ls_restrained_S_all 0.953
_refine_ls_R_factor_all 0.2900
_refine_ls_R_factor_gt 0.0954
_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^)+(0.0567P)^2^]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1553
_refine_ls_wR_factor_ref 0.2321
_reflns_Friedel_coverage 0.528
_reflns_number_gt 16741
_reflns_number_total 52899
_reflns_threshold_expression 'I > 2\s(I)'
_[local]_cod_data_source_file cg500310n_si_001.cif
_[local]_cod_data_source_block b4nbla(2)
_[local]_cod_chemical_formula_sum_orig 'C33 H45.60 N4 O13.80'
_cod_depositor_comments
'Adding full bibliography for 4510389--4510390.cif.'
_cod_database_code 4510390
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.935
_shelx_estimated_absorpt_t_max 0.993
_diffrn_reflns_laue_measured_fraction_max 0.948
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.750
_diffrn_reflns_point_group_measured_fraction_full 0.861
_reflns_friedel_fraction_max 0.537
_reflns_friedel_fraction_full 0.710
_shelxl_version_number 2013-2
_shelx_hkl_file
;
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