Isomerization of a lanthanide complex using a humming top guest template: a solid-to-solid reaction
Mills, Michelle B.; Hollingshead, Andrew G.; Maahs, Adam C.; Soldatov, Dmitriy V.; Preuss, Kathryn E.; CrystEngComm 17 (2015) 7816–; doi:10.1039/C5CE01680K

data_7223169
_publ_section_title
;
 Isomerization of a lanthanide complex using a humming top guest template:
 a solid-to-solid reaction
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              7816
_journal_paper_doi               10.1039/C5CE01680K
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety
'C27 H9 Br2 Ce F18 N6 O6 S4, 0.5(C18 H15 Cl2 Sb)'
_chemical_formula_sum            'C36 H16.5 Br2 Ce Cl F18 N6 O6 S4 Sb0.5'
_chemical_formula_weight         1495.56
_chemical_name_common            '[Ce(hfac)3(BrPyDTDA)2]*0.5{SbPh3Cl2}'
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-07-27 deposited with the CCDC.
2015-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   36.8971(5)
_cell_length_b                   30.3093(4)
_cell_length_c                   17.87564(19)
_cell_measurement_reflns_used    30666
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.4490
_cell_measurement_theta_min      2.8370
_cell_volume                     19990.8(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3693
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            99135
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         2.847
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.988
_exptl_crystal_description       prism
_exptl_crystal_F_000             11504
_exptl_crystal_recrystallization_method Sublimation
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         5.159
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details
;
 Flack x determined using 5929 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.013(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         15221
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+180.7032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1275
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                13354
_reflns_number_total             15221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01680k2.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C36 H16.50 Br2 Ce Cl F18 N6 O6 S4 Sb0.50'
_cod_database_code               7223169
_shelx_estimated_absorpt_t_min   0.575
_shelx_estimated_absorpt_t_max   0.860
_shelxl_version_number           2013-4
_shelx_res_checksum              51312