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_7232558
_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 O3 Y'
_chemical_formula_sum            'C45 H69 O3 Y'
_chemical_formula_weight         746.91
_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             2018-06-25
_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                76.182(4)
_cell_angle_beta                 86.604(3)
_cell_angle_gamma                80.933(3)
_cell_formula_units_Z            10
_cell_length_a                   9.6910(6)
_cell_length_b                   25.0295(17)
_cell_length_c                   45.485(3)
_cell_measurement_reflns_used    9062
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.32
_cell_measurement_theta_min      2.31
_cell_volume                     10577.0(12)
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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  0.0870
_diffrn_reflns_av_unetI/netI     0.1105
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            279802
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.671
_diffrn_reflns_theta_min         0.847
_exptl_absorpt_coefficient_mu    1.414
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0686 before and 0.0589 after correction. The Ratio of minimum to maximum transmission is 0.8617. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       block
_exptl_crystal_F_000             4020
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.905
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2311
_refine_ls_number_reflns         64948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+4.1334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                37286
_reflns_number_total             64948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00184k2.cif
_cod_data_source_block           100k_orig
_cod_depositor_comments
'Adding full bibliography for 7232556--7232561.cif.'
_cod_database_code               7232558
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.602
_shelx_estimated_absorpt_t_min   0.484
_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), C18B(H18B), C20B(H20B), C33B(H33B), C35B(H35B), C3C(H3C), C5C(H5C),
 C18C(H18C), C20C(H20C), C33C(H33C), C35C(H35C), C3D(H3D), C5D(H5D), C18D(H18D),
  C20D(H20D), C33D(H33D), C35D(H35D), C3E(H3E), C5E(H5E), C18E(H18E),
 C20E(H20E), C33E(H33E), C35E(H35E)
2.b Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C11A(H11A,
 H11B,H11C), C13A(H13A,H13B,H13C), C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C),
 C23A(H23A,H23B,H23C), C24A(H24A,H24B,H24C), C25A(H25A,H25B,H25C), C26A(H26A,
 H26B,H26C), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C30A(H30A,H30B,H30C),
 C38A(H38A,H38B,H38C), C39A(H39A,H39B,H39C), C40A(H40A,H40B,H40C), C41A(H41A,
 H41B,H41C), C43A(H43A,H43B,H43C), C44A(H44A,H44B,H44C), C45A(H45A,H45B,H45C),
 C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F), C11B(H11D,H11E,
 H11F), C13B(H13D,H13E,H13F), C14B(H14D,H14E,H14F), C15B(H15D,H15E,H15F),
 C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F), C25B(H25D,H25E,H25F), C26B(H26D,
 H26E,H26F), C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F),
 C38B(H38D,H38E,H38F), C39B(H39D,H39E,H39F), C40B(H40D,H40E,H40F), C41B(H41D,
 H41E,H41F), C43B(H43D,H43E,H43F), C44B(H44D,H44E,H44F), C45B(H45D,H45E,H45F),
 C8C(H8CA,H8CB,H8CC), C9C(H9CA,H9CB,H9CC), C10C(H10G,H10H,H10I), C11C(H11G,H11H,
 H11I), C13C(H13G,H13H,H13I), C14C(H14G,H14H,H14I), C15C(H15G,H15H,H15I),
 C23C(H23G,H23H,H23I), C24C(H24G,H24H,H24I), C25C(H25G,H25H,H25I), C26C(H26G,
 H26H,H26I), C28C(H28G,H28H,H28I), C29C(H29G,H29H,H29I), C30C(H30G,H30H,H30I),
 C38C(H38G,H38H,H38I), C39C(H39G,H39H,H39I), C40C(H40G,H40H,H40I), C41C(H41G,
 H41H,H41I), C43C(H43G,H43H,H43I), C44C(H44G,H44H,H44I), C45C(H45G,H45H,H45I),
 C8D(H8DA,H8DB,H8DC), C9D(H9DA,H9DB,H9DC), C10D(H10J,H10K,H10L), C11D(H11J,H11K,
 H11L), C13D(H13J,H13K,H13L), C14D(H14J,H14K,H14L), C15D(H15J,H15K,H15L),
 C23D(H23J,H23K,H23L), C24D(H24J,H24K,H24L), C25D(H25J,H25K,H25L), C26D(H26J,
 H26K,H26L), C28D(H28J,H28K,H28L), C29D(H29J,H29K,H29L), C30D(H30J,H30K,H30L),
 C38D(H38J,H38K,H38L), C39D(H39J,H39K,H39L), C40D(H40J,H40K,H40L), C41D(H41J,
 H41K,H41L), C43D(H43J,H43K,H43L), C44D(H44J,H44K,H44L), C45D(H45J,H45K,H45L),
 C8E(H8EA,H8EB,H8EC), C9E(H9EA,H9EB,H9EC), C10E(H10M,H10N,H10O), C11E(H11M,H11N,
 H11O), C13E(H13M,H13N,H13O), C14E(H14M,H14N,H14O), C15E(H15M,H15N,H15O),
 C23E(H23M,H23N,H23O), C24E(H24M,H24N,H24O), C25E(H25M,H25N,H25O), C26E(H26M,
 H26N,H26O), C28E(H28M,H28N,H28O), C29E(H29M,H29N,H29O), C30E(H30M,H30N,H30O),
 C38E(H38M,H38N,H38O), C39E(H39M,H39N,H39O), C40E(H40M,H40N,H40O), C41E(H41M,
 H41N,H41O), C43E(H43M,H43N,H43O), C44E(H44M,H44N,H44O), C45E(H45M,H45N,H45O)
;
_shelx_res_checksum              77224
_olex2_submission_special_instructions 'No special instructions were received'