Water‒Halogen Interactions in Chlorine and Bromine Clathrate Hydrates: An Example of Multidirectional Halogen Bonding
Udachin, Konstantin A.; Alavi, Saman; Ripmeester, John A.; The Journal of Physical Chemistry C 117 (2013) 14176–; doi:10.1021/jp402399r

data_1512147
_publ_section_title
;
 Water--Halogen Interactions in Chlorine and Bromine Clathrate Hydrates:
 An Example of Multidirectional Halogen Bonding
;
_journal_issue                   27
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              14176
_journal_paper_doi               10.1021/jp402399r
_journal_volume                  117
_journal_year                    2013
_chemical_formula_sum            'Br38.27 H344 O172'
_chemical_formula_weight         6156.91
_chemical_name_common            'Bromine hydrate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           136
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4n 2n'
_symmetry_space_group_name_H-M   'P 42/m n m'
_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            1
_cell_length_a                   23.0436(9)
_cell_length_b                   23.0436(9)
_cell_length_c                   12.0745(7)
_cell_measurement_temperature    173.0(1)
_cell_volume                     6411.7(5)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'ATOMS V.5.0'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.0(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       '\w 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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24788
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.059
_exptl_absorpt_correction_T_max  0.3127
_exptl_absorpt_correction_T_min  0.1955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3059
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.166
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.00020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         2549
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+4.4023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                1868
_reflns_number_total             2549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp402399r_si_001.cif
_cod_data_source_block           koss12
_cod_original_sg_symbol_H-M      P4(2)/mnm
_cod_original_formula_sum        'H344 Br38.27 O172'
_cod_database_code               1512147