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_7034830
_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      triclinic
_space_group_IT_number           1
_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             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                101.4820(10)
_cell_angle_beta                 95.4070(10)
_cell_angle_gamma                90.4790(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2637(4)
_cell_length_b                   12.0257(5)
_cell_length_c                   12.1769(5)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      3.02
_cell_volume                     1322.96(10)
_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, 2008)'
_diffrn_ambient_temperature      101.1
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0285
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35776
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.859
_diffrn_reflns_theta_min         2.927
_exptl_absorpt_coefficient_mu    3.533
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            reddish-brown
_exptl_crystal_colour_primary    reddish-brown
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_description       needle
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 5064 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.014(9)
_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     761
_refine_ls_number_reflns         12428
_refine_ls_number_restraints     411
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0179P)^2^+1.0670P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0498
_reflns_Friedel_coverage         0.987
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                10969
_reflns_number_total             12428
_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_database_code               7034830
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.933
_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.a Ternary CH refined with riding coordinates:
 C30(H30), C31(H31), C39(H39), C38(H38)
3.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C42(H42A,H42B), C40(H40A,
 H40B), C41(H41A,H41B), C44(H44A,H44B), C43(H43A,H43B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C12(H12), C15(H15), C16(H16), C19(H19), C20(H20),
 C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C36(H36), C35(H35), C37(H37)
3.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C26(H26A,H26B,
 H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'