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_4507657
_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             2013-01-02T14:21:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.989(3)
_cell_angle_beta                 105.20(3)
_cell_angle_gamma                90.13(2)
_cell_formula_units_Z            4
_cell_length_a                   11.120(3)
_cell_length_b                   12.377(3)
_cell_length_c                   14.302(3)
_cell_measurement_reflns_used    142
_cell_measurement_temperature    252.0(2)
_cell_measurement_theta_max      52.0
_cell_measurement_theta_min      4.6
_cell_volume                     1899.2(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      252.0(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.079
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10052
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         4.05
_diffrn_standards_number         27
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.2
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         6319
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.847
_refine_ls_R_factor_all          0.117
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0959P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1632
_reflns_number_gt                2913
_reflns_number_total             6319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400016z_si_002.cif
_cod_data_source_block           dp(cpp)m_H_252K
_cod_original_cell_volume        1899.3(8)
_cod_database_code               4507657