Uniaxial Negative Thermal Expansion in an Organic Complex Caused by Sliding of Layers
Bhattacharya, Suman; Saha, Binoy K.; Crystal Growth & Design 12 (2012) 4716–; doi:10.1021/cg300980s

data_4506848
_publ_section_title
;
 Uniaxial Negative Thermal Expansion in an Organic Complex Caused by
 Sliding of Layers
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4716
_journal_paper_doi               10.1021/cg300980s
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C9 H6 O6, C8 H11 N1, H2O'
_chemical_formula_sum            'C17 H19 N O7'
_chemical_formula_weight         349.33
_chemical_name_common            BTA.DMA.H2O-165
_chemical_name_systematic
;
 benzene-1,3,5-tricarboxylic acid, 2,6-dimethylaniline, hydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-30
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.157(6)
_cell_angle_beta                 102.521(9)
_cell_angle_gamma                95.439(9)
_cell_formula_units_Z            4
_cell_length_a                   8.3768(13)
_cell_length_b                   13.7290(10)
_cell_length_c                   14.5547(10)
_cell_measurement_reflns_used    5604
_cell_measurement_temperature    165(2)
_cell_measurement_theta_max      29.3226
_cell_measurement_theta_min      2.5921
_cell_volume                     1626.2(3)
_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
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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_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      165(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_details
;
  1 omega  -34.00   -8.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -37.0000  120.0000 26

  2 omega  -20.00   18.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397 -100.0000  -50.0000 38

  3 omega  -92.00  -65.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  179.0000  -60.0000 27

  4 omega  -11.00   81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1366   77.0000  -90.0000 92

  5 omega  -32.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1366    0.0000  -90.0000 124

  6 omega  -24.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1366 -100.0000  124.0000 86
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0246320000
_diffrn_orient_matrix_UB_12      0.0172542000
_diffrn_orient_matrix_UB_13      0.0474024000
_diffrn_orient_matrix_UB_21      0.0799522000
_diffrn_orient_matrix_UB_22      -0.0138748000
_diffrn_orient_matrix_UB_23      0.0018397000
_diffrn_orient_matrix_UB_31      0.0239659000
_diffrn_orient_matrix_UB_32      0.0469501000
_diffrn_orient_matrix_UB_33      -0.0155479000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13511
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.39
_diffrn_reflns_theta_min         2.60
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         8974
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0478
_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/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                5047
_reflns_number_total             8974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300980s_si_001.cif
_cod_data_source_block           BTA.DMA.H2O-165
_cod_database_code               4506848