Molecular Tectonics. Disruption of Self-Association in Melts Derived from Hydrogen-Bonded Solids
Danielle Boils; Marie-Eve Perron; Francis Monchamp; Hugues Duval; Thierry Maris; James D. Wuest; Macromolecules 37 (2004) 7351–7357; doi:10.1021/ma035977d

data_1501599
_publ_section_title
;
 Molecular Tectonics. Disruption of Self-Association in Melts Derived from
 Hydrogen-Bonded Solids
;
_journal_name_full               Macromolecules
_journal_page_first              7351
_journal_page_last               7357
_journal_paper_doi               10.1021/ma035977d
_journal_volume                  37
_journal_year                    2004
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C69 H100 N24, 10(C4 H8 O2)'
_chemical_formula_sum            'C109 H180 N24 O20'
_chemical_formula_weight         2146.77
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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            2
_cell_length_a                   11.8715(3)
_cell_length_b                   11.8715(3)
_cell_length_c                   40.004(2)
_cell_measurement_reflns_used    29551
_cell_measurement_temperature    226(2)
_cell_measurement_theta_max      72.14
_cell_measurement_theta_min      2.16
_cell_volume                     5637.9(3)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'UdMX (local program)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      226(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            36656
_diffrn_reflns_theta_full        58.88
_diffrn_reflns_theta_max         58.88
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  2880
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.8600
_exptl_absorpt_correction_T_min  0.2100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2324
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), 1960 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.3(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         4045
_refine_ls_number_restraints     450
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0868
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1511P)^2^+5.6939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2183
_refine_ls_wR_factor_ref         0.2195
_reflns_number_gt                3953
_reflns_number_total             4045
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            deposit.cif
_cod_data_source_block           jiw300
_cod_original_cell_volume        5637.9(4)
_cod_original_sg_symbol_H-M      I-4
_cod_database_code               1501599