Structural changes of hexamethylenetetramine and undecanedioic acid co-crystal (HMT-C11) as a function of the temperature
Pinheiro, Carlos Basílio; Gardon, Manuel; Chapuis, Gervais; Acta Crystallographica Section B 59 (2003) 416–427; doi:10.1107/S0108768103007754

data_2103906
_publ_section_title
;
 Structural changes of hexamethylenetetramine and undecanedioic acid
 co-crystal (HMT-C11) as a function of the temperature
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              416
_journal_page_last               427
_journal_paper_doi               10.1107/S0108768103007754
_journal_volume                  59
_journal_year                    2003
_chemical_formula_sum            'C17 H32 N4 O4'
_chemical_formula_weight         356.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-B 2b 2'
_symmetry_space_group_name_H-M   'B m m b'
_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                   9.3593(19)
_cell_length_b                   29.257(6)
_cell_length_c                   7.2982(15)
_cell_measurement_reflns_used    3000
_cell_measurement_temperature    323(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3.54
_cell_volume                     1998.4(7)
_computing_cell_refinement       'kM4 - Oxford Diffraction'
_computing_data_collection       'kM4 - Oxford Diffraction'
_computing_data_reduction        Xprep
_computing_molecular_graphics    XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      323(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford CCD'
_diffrn_measurement_method       oscillation
_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  0.1360
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10013
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelets
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.144
_refine_diff_density_min         -0.129
_refine_ls_extinction_coef       0.0029(2)
_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   1.193
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         958
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1351P)^2^+0.2969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2296
_refine_ls_wR_factor_ref         0.2438
_reflns_number_gt                741
_reflns_number_total             958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            na0146.cif
_cod_data_source_block           324K
_cod_original_sg_symbol_H-M      Bmmb
_cod_database_code               2103906
_cod_database_fobs_code          2103906