#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/02/4110216.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_4110216
loop_
_publ_author_name
'Matthew J. Horner'
'K. Travis Holman'
'Michael D. Ward'
_publ_section_title
;
 Architectural Diversity and Elastic Networks in Hydrogen-Bonded Host
 Frameworks: From Molecular Jaws to Cylinders
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14640
_journal_page_last               14660
_journal_paper_doi               10.1021/ja0741574
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C14 H18 Br N3 O4 S'
_chemical_formula_weight         404.28
_chemical_name_common            'guanidinium sulfonate chlathrate'
_chemical_name_systematic
; 
 ? 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7431(4)
_cell_length_b                   11.2471(6)
_cell_length_c                   19.8076(12)
_cell_measurement_reflns_used    5714
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      2.75
_cell_volume                     1724.99(17)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker (or Siemens)'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'XSEED, L. Barbour; http://www.xseed.com'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SMART platform CCD, Bruker (or Siemens)'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9078
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    2.526
_exptl_absorpt_correction_T_max  0.8235
_exptl_absorpt_correction_T_min  0.3708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       plate
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0391P)²+0.5227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0684
_reflns_number_gt                2740
_reflns_number_total             3031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0741574si20070910_040750_15.cif
_cod_data_source_block           G4BBS_anisole
_cod_database_code               4110216
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Br1 Br 0.74590(5) 0.97545(2) 0.863398(13) 0.03299(10) Uani 1 1 d .
S1 S 0.75665(12) 0.79586(5) 1.17123(3) 0.02252(14) Uani 1 1 d .
O1 O 0.5992(3) 0.7254(2) 1.18072(12) 0.0266(6) Uani 1 1 d .
N1 N 0.5957(3) 0.4938(3) 1.25059(14) 0.0302(8) Uani 1 1 d .
H1A H 0.4968 0.4605 1.2615 0.036 Uiso 1 1 calc R
H1B H 0.5969 0.5615 1.2283 0.036 Uiso 1 1 calc R
C1 C 0.7561(5) 0.8423(2) 1.08587(12) 0.0224(5) Uani 1 1 d .
O2 O 0.9133(3) 0.7261(2) 1.18058(12) 0.0285(6) Uani 1 1 d .
N2 N 0.8931(3) 0.4948(2) 1.25366(14) 0.0275(7) Uani 1 1 d .
H2A H 0.8944 0.5639 1.2329 0.033 Uiso 1 1 calc R
H2B H 0.9908 0.4604 1.2651 0.033 Uiso 1 1 calc R
C2 C 0.8448(4) 0.7796(3) 1.03646(16) 0.0279(7) Uani 1 1 d .
H2 H 0.9079 0.7103 1.0483 0.033 Uiso 1 1 calc R
O3 O 0.7546(3) 0.90458(14) 1.21132(9) 0.0274(4) Uani 1 1 d .
N3 N 0.7419(4) 0.34004(17) 1.30153(11) 0.0274(5) Uani 1 1 d .
H3A H 0.6431 0.3065 1.3125 0.033 Uiso 1 1 calc R
H3B H 0.8399 0.3060 1.3129 0.033 Uiso 1 1 calc R
C3 C 0.8417(4) 0.8174(3) 0.97013(16) 0.0310(7) Uani 1 1 d .
H3 H 0.9030 0.7747 0.9364 0.037 Uiso 1 1 calc R
C4 C 0.7483(5) 0.9183(2) 0.95338(12) 0.0239(5) Uani 1 1 d .
C5 C 0.6558(4) 0.9805(3) 1.00177(16) 0.0297(7) Uani 1 1 d .
H5 H 0.5905 1.0486 0.9895 0.036 Uiso 1 1 calc R
C6 C 0.6597(4) 0.9424(3) 1.06807(16) 0.0297(7) Uani 1 1 d .
H6 H 0.5966 0.9843 1.1016 0.036 Uiso 1 1 calc R
C7 C 0.7429(5) 0.4422(2) 1.26779(12) 0.0240(5) Uani 1 1 d .
O1S O 0.2753(4) 1.1947(2) 0.86832(11) 0.0504(7) Uani 1 1 d .
C1S C 0.2790(4) 1.1656(3) 0.93545(16) 0.0351(8) Uani 1 1 d .
C2S C 0.3543(4) 1.2347(3) 0.98530(17) 0.0350(8) Uani 1 1 d .
H2S H 0.4114 1.3066 0.9738 0.042 Uiso 1 1 calc R
C3S C 0.3461(4) 1.1984(3) 1.05188(17) 0.0389(8) Uani 1 1 d .
H3S H 0.3967 1.2461 1.0862 0.047 Uiso 1 1 calc R
C4S C 0.2656(6) 1.0943(3) 1.06881(17) 0.0436(8) Uani 1 1 d .
H4S H 0.2604 1.0699 1.1147 0.052 Uiso 1 1 calc R
C5S C 0.1919(4) 1.0246(3) 1.0190(2) 0.0444(9) Uani 1 1 d .
H5S H 0.1365 0.9522 1.0310 0.053 Uiso 1 1 calc R
C6S C 0.1977(4) 1.0591(3) 0.95184(19) 0.0414(9) Uani 1 1 d .
H6S H 0.1473 1.0110 0.9177 0.050 Uiso 1 1 calc R
C7S C 0.3792(6) 1.2941(4) 0.84780(19) 0.0627(12) Uani 1 1 d .
H7S1 H 0.3418 1.3655 0.8721 0.094 Uiso 1 1 calc R
H7S2 H 0.3661 1.3067 0.7991 0.094 Uiso 1 1 calc R
H7S3 H 0.5007 1.2778 0.8582 0.094 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O2 S1 O3 113.05(15)
O2 S1 O1 112.65(10)
O3 S1 O1 111.98(15)
O2 S1 C1 106.40(16)
O3 S1 C1 105.85(10)
O1 S1 C1 106.25(15)
C2 C1 C6 119.7(2)
C2 C1 S1 121.5(2)
C6 C1 S1 118.7(2)
C3 C2 C1 120.4(3)
C2 C3 C4 119.3(3)
C3 C4 C5 121.2(2)
C3 C4 Br1 120.6(2)
C5 C4 Br1 118.3(2)
C6 C5 C4 119.3(3)
C5 C6 C1 120.1(3)
N1 C7 N3 120.2(4)
N1 C7 N2 120.1(2)
N3 C7 N2 119.6(3)
C1S O1S C7S 116.7(3)
O1S C1S C2S 124.5(3)
O1S C1S C6S 115.0(3)
C2S C1S C6S 120.5(3)
C3S C2S C1S 119.7(3)
C4S C3S C2S 120.5(3)
C3S C4S C5S 119.9(3)
C4S C5S C6S 120.8(3)
C5S C6S C1S 118.6(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Br1 C4 1.895(2)
S1 O2 1.457(2)
S1 O3 1.4581(17)
S1 O1 1.466(2)
S1 C1 1.769(2)
N1 C7 1.323(4)
C1 C2 1.388(4)
C1 C6 1.396(4)
N2 C7 1.334(4)
C2 C3 1.381(4)
N3 C7 1.329(3)
C3 C4 1.386(4)
C4 C5 1.386(4)
C5 C6 1.382(4)
O1S C1S 1.370(4)
O1S C7S 1.436(4)
C1S C2S 1.385(5)
C1S C6S 1.391(4)
C2S C3S 1.382(5)
C3S C4S 1.368(5)
C4S C5S 1.383(5)
C5S C6S 1.387(5)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660382
