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_7232560
_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 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-25 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                92.202(2)
_cell_angle_beta                 97.768(2)
_cell_angle_gamma                91.001(2)
_cell_formula_units_Z            4
_cell_length_a                   9.6480(4)
_cell_length_b                   17.7941(7)
_cell_length_c                   25.1982(10)
_cell_measurement_reflns_used    9713
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      2.45
_cell_volume                     4282.0(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.980
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            105269
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.612
_diffrn_reflns_theta_min         0.816
_exptl_absorpt_coefficient_mu    1.098
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0850 before and 0.0559 after correction. The Ratio of minimum to maximum transmission is 0.7875. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       Block
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.360
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     925
_refine_ls_number_reflns         19495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+4.3757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15993
_reflns_number_total             19495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00184k2.cif
_cod_data_source_block           ce_100k
_cod_depositor_comments
'Adding full bibliography for 7232556--7232561.cif.'
_cod_database_code               7232560
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.668
_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.a Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C5A(H5A), C18A(H18A), C20A(H20A), C33A(H33A), C35A(H35A), C3B(H3B),
 C5B(H5B), C20B(H20B), C18B(H18B), C33B(H33B), C35B(H35B)
2.b Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C10A(H10A,H10B,H10C), C9A(H9AA,H9AB,H9AC), C11A(H11A,
 H11B,H11C), C15A(H15A,H15B,H15C), C14A(H14A,H14B,H14C), C13A(H13A,H13B,H13C),
 C25A(H25A,H25B,H25C), C24A(H24A,H24B,H24C), C23A(H23A,H23B,H23C), C26A(H26A,
 H26B,H26C), C30A(H30A,H30B,H30C), C29A(H29A,H29B,H29C), C28A(H28A,H28B,H28C),
 C39A(H39A,H39B,H39C), C40A(H40A,H40B,H40C), C38A(H38A,H38B,H38C), C41A(H41A,
 H41B,H41C), C44A(H44A,H44B,H44C), C45A(H45A,H45B,H45C), C43A(H43A,H43B,H43C),
 C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F), C11B(H11D,H11E,
 H11F), C15B(H15D,H15E,H15F), C14B(H14D,H14E,H14F), C13B(H13D,H13E,H13F),
 C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F), C28B(H28D,H28E,H28F), C26B(H26D,
 H26E,H26F), C25B(H25D,H25E,H25F), C24B(H24D,H24E,H24F), C23B(H23D,H23E,H23F),
 C39B(H39D,H39E,H39F), C40B(H40D,H40E,H40F), C38B(H38D,H38E,H38F), C41B(H41D,
 H41E,H41F), C45B(H45D,H45E,H45F), C44B(H44D,H44E,H44F), C43B(H43D,H43E,H43F)
;
_shelx_res_checksum              98787
_olex2_submission_special_instructions 'No special instructions were received'