Reversible temperature-induced polymorphic phase transitions of [Y(OAr)3] and [Ce(OAr)3] (Ar = 2,6-tBu2-4-MeC6H2): interconversions between pyramidal and planar geometries
Haddow, Mairi F.; Newland, Robert J.; Tegner, Bengt E.; Mansell, Stephen M.; CrystEngComm 21 (2019) 2884–; doi:10.1039/C9CE00184K

data_7232556
_publ_section_title
;
 Reversible temperature-induced polymorphic phase transitions of [Y(OAr)3]
 and [Ce(OAr)3] (Ar = 2,6-tBu2-4-MeC6H2): interconversions between
 pyramidal and planar geometries
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              2884
_journal_paper_doi               10.1039/C9CE00184K
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C45 H69 Ce O3'
_chemical_formula_sum            'C45 H69 Ce O3'
_chemical_formula_weight         798.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-10-25 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                70.569(4)
_cell_angle_beta                 84.308(6)
_cell_angle_gamma                83.265(5)
_cell_formula_units_Z            2
_cell_length_a                   9.7009(11)
_cell_length_b                   15.2187(15)
_cell_length_c                   15.7698(14)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.74
_cell_measurement_theta_min      2.44
_cell_volume                     2175.9(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37311
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.695
_diffrn_reflns_theta_min         2.277
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0762 before and 0.0494 after correction. The Ratio of minimum to maximum transmission is 0.7791. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       Block
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         9961
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0521P)^2^+0.5855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6782
_reflns_number_total             9961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00184k2.cif
_cod_data_source_block           ce_200k
_cod_depositor_comments
'Adding full bibliography for 7232556--7232561.cif.'
_cod_database_code               7232556
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.672
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29B-C27 \\sim C29A-C27 \\sim C28B-C27 \\sim C28A-C27 \\sim C30B-C27 \\sim
C30A-C27
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C29B, C29A, C28B, C28A, C30A, C30B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29A, C29B, C28B, C28A, C30A, C30B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Ce1B(0.5) Ce1A(0.5) C28B(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
 C30A(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C29A(0.5) H29A(0.5) H29B(0.5)
 H29C(0.5) C28A(0.5) H28D(0.5) H28E(0.5) H28F(0.5) C29B(0.5) H29D(0.5)
 H29E(0.5) H29F(0.5) C30B(0.5) H30D(0.5) H30E(0.5) H30F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C18(H18), C33(H33), C35(H35)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C26(H26A,H26B,
 H26C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C40(H40A,
 H40B,H40C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C43(H43A,H43B,H43C), C28B(H28A,H28B,
 H28C), C30A(H30A,H30B,H30C), C29A(H29A,H29B,H29C), C28A(H28D,H28E,H28F),
 C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F)
;
_shelx_res_checksum              6788
_olex2_submission_special_instructions 'No special instructions were received'