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_7034831
_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 Dy N5 O13'
_chemical_formula_sum            'C22 H24 Cu Dy N5 O13'
_chemical_formula_weight         792.50
_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                101.5640(10)
_cell_angle_beta                 95.7150(10)
_cell_angle_gamma                90.5080(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2947(2)
_cell_length_b                   12.0714(3)
_cell_length_c                   12.1819(3)
_cell_measurement_temperature    138(2)
_cell_volume                     1331.83(5)
_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      138.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            43323
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.174
_diffrn_reflns_theta_min         3.183
_exptl_absorpt_coefficient_mu    3.659
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            reddish-brown
_exptl_crystal_colour_primary    reddish-brown
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       needle
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.351
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 5287 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.031(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         11647
_refine_ls_number_restraints     364
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0189
_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^)+(0.0064P)^2^+1.9530P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0440
_reflns_Friedel_coverage         0.972
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                11068
_reflns_number_total             11647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00789e2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7034824--7034836.cif.'
_cod_database_code               7034831
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.930
_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:
 C14(H14), C9(H9), C31(H31), C36(H36)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C35(H35A,H35B), C34(H34A,H34B), C10(H10A,
 H10B), C32(H32A,H32B), C11(H11A,H11B), C33(H33A,H33B)
3.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C39(H39), C17(H17), C8(H8), C37(H37), C30(H30), C19(H19), C25(H25),
 C3(H3), C15(H15), C41(H41), C40(H40), C26(H26), C18(H18), C4(H4), C5(H5)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C44(H44A,H44B,H44C), C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'