A multinuclear solid state NMR, density functional theory and X-Ray diffraction study of hydrogen bonding in Group I hydrogen dibenzoates
Rees, Gregory J.; Day, Stephen P.; Lari, Alberth; Howes, Andrew P.; Iuga, Dinu; Pitak, Mateusz B.; Coles, Simon J.; Threlfall, Terry L.; Light, Mark E.; Smith, Mark E.; Quigley, David; Wallis, John D.; Hanna, John V.; CrystEngComm 15 (2013) 8823–; doi:10.1039/c3ce41258j

data_7211119
_publ_section_title
;
 A multinuclear solid state NMR, density functional theory and X-Ray
 diffraction study of hydrogen bonding in Group I hydrogen dibenzoates
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              8823
_journal_paper_doi               10.1039/c3ce41258j
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C14 H11 Cs O4'
_chemical_formula_weight         376.14
_chemical_name_systematic
; 
cesium hemibenzoate orthorhombic phase
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_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                   28.3393(19)
_cell_length_b                   7.0215(3)
_cell_length_c                   6.9066(4)
_cell_measurement_reflns_used    3550
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0716
_cell_measurement_theta_min      2.8675
_cell_volume                     1374.31(14)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9832
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7535
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    2.700
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0088P)^2^+2.2155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0540
_reflns_number_gt                1389
_reflns_number_total             1664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41258j.txt
_cod_data_source_block           csortho
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7211119