Polymorphs Related by an Enantiotropic Phase Transition but Having Only Order–Disorder-Level Conformational Differences in a Spiro-Conjugated Imidazolidine Ring Compound
Suzuki, Mitsuaki; Maeda, Yutaka; Akita, Motoko; Teramae, Hiroyuki; Kobayashi, Keiji; Crystal Growth & Design 14 (2014) 6302–; doi:10.1021/cg501060w

data_4512174
_publ_section_title
;
 Polymorphs Related by an Enantiotropic Phase Transition but Having Only
 Order--Disorder-Level Conformational Differences in a Spiro-Conjugated
 Imidazolidine Ring Compound
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              6302
_journal_paper_doi               10.1021/cg501060w
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C15 H18 N2 O2'
_chemical_formula_sum            'C15 H18 N2 O2'
_chemical_formula_weight         258.31
_chemical_melting_point          371
_chemical_name_common            SCID_200K
_chemical_name_systematic
;
 1,3-diethyl-spiro[imidazolidine-2,2'-[2H]indene]-1',3'-dione   
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   15.3886(8)
_cell_length_b                   29.0676(15)
_cell_length_c                   9.4210(5)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    200
_cell_measurement_theta_max      33.61
_cell_measurement_theta_min      2.53
_cell_volume                     4214.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            28906
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.142
_diffrn_reflns_theta_min         1.401
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.270
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         8148
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1083P)^2^+1.5766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2047
_refine_ls_wR_factor_ref         0.2206
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6409
_reflns_number_total             8148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501060w_si_006.cif
_cod_data_source_block           ms0120a
_cod_depositor_comments
'Adding full bibliography for 4512171--4512176.cif.'
_cod_database_code               4512174
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.978
_shelxl_version_number           2014-1
_shelx_res_checksum              28347
_shelx_hkl_checksum              67675