Structural and Thermodynamic Insight into Solid State Phase Transition Mechanism of a 1,3,3′-Triketone
Stilinović, Vladimir; Kaitner, Branko; Crystal Growth & Design 13 (2013) 1703–; doi:10.1021/cg400016z

data_4507660
_publ_section_title
;
 Structural and Thermodynamic Insight into Solid State Phase Transition
 Mechanism of a 1,3,3&#x2032;-Triketone
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1703
_journal_paper_doi               10.1021/cg400016z
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C19 H32 O3'
_chemical_formula_sum            'C19 H32 O3'
_chemical_formula_weight         308.45
_chemical_name_systematic
;
dipivaloyl-3-cyclopentylpropanoylmethane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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             2013-01-02T15:32:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                85.208(13)
_cell_angle_beta                 79.191(13)
_cell_angle_gamma                87.602(12)
_cell_formula_units_Z            2
_cell_length_a                   5.6643(8)
_cell_length_b                   11.4320(18)
_cell_length_c                   14.604(2)
_cell_measurement_reflns_used    232
_cell_measurement_temperature    245.0(2)
_cell_measurement_theta_max      52.0
_cell_measurement_theta_min      4.6
_cell_volume                     925.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      245.0(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur CCD
diffractometer
;
_diffrn_measurement_method       '\w scan'
_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  0.0248
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5277
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.95
_diffrn_standards_number         27
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1281
_reflns_number_gt                2029
_reflns_number_total             3218
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400016z_si_002.cif
_cod_data_source_block           dp(cpp)m_L_245K
_cod_database_code               4507660