Temperature-controlled polymorphism of chiral Cu(II)-Ln(III) dinuclear complexes exhibiting slow magnetic relaxation.
Wen, He-Rui; Bao, Jun; Liu, Sui-Jun; Liu, Cai-Ming; Zhang, Cai-Wei; Tang, Yun-Zhi; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11191–11201; doi:10.1039/c5dt00789e

data_7034832
_publ_section_title
;
 Temperature-controlled polymorphism of chiral Cu(II)-Ln(III) dinuclear
 complexes exhibiting slow magnetic relaxation.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11191
_journal_page_last               11201
_journal_paper_doi               10.1039/c5dt00789e
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H24 Cu N5 O13 Tb'
_chemical_formula_sum            'C22 H24 Cu N5 O13 Tb'
_chemical_formula_weight         788.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-04-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-21 deposited with the CCDC.
2015-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.352(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2823(6)
_cell_length_b                   15.2642(8)
_cell_length_c                   15.8767(9)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.321
_cell_measurement_theta_min      2.298
_cell_volume                     2636.6(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26414
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.341
_diffrn_reflns_theta_min         1.872
_exptl_absorpt_coefficient_mu    3.545
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.2011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1638 before and 0.0785 after correction.
The Ratio of minimum to maximum transmission is 0.2698.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.429
_refine_diff_density_min         -3.030
_refine_diff_density_rms         0.223
_refine_ls_abs_structure_details
;
 Flack x determined using 4359 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.060(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         11327
_refine_ls_number_restraints     392
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0622
_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^)+(0.1103P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1574
_reflns_Friedel_coverage         0.840
_reflns_Friedel_fraction_full    0.926
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                10492
_reflns_number_total             11327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00789e2.cif
_cod_data_source_block           6'
_cod_depositor_comments
'Adding full bibliography for 7034824--7034836.cif.'
_cod_original_cell_volume        2636.6(2)
_cod_database_code               7034832
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.537
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(O23A)=1-FVAR(1)
 Sof(O23)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C26(H26), C25(H25), C2(H2)
4.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C34(H34A,H34B), C12(H12A,H12B), C28(H28A,H28B), C3(H3A,H3B),
 C1(H1A,H1B), C23(H23A,H23B), C44(H44A,H44B)
4.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C21(H21), C42(H42), C19(H19), C41(H41), C40(H40), C16(H16),
 C13(H13), C33(H33), C32(H32), C31(H31), C30(H30), C7(H7), C6(H6), C27(H27),
 C5(H5)
4.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C11(H11A,H11B,H11C), C4(H4A,H4B,H4C), C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'