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_7034829
_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 Gd N5 O13'
_chemical_formula_sum            'C22 H24 Cu Gd N5 O13'
_chemical_formula_weight         787.25
_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                 105.682(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2871(18)
_cell_length_b                   15.301(2)
_cell_length_c                   15.918(3)
_cell_measurement_reflns_used    9279
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.90
_cell_volume                     2646.8(7)
_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      296.16
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.976
_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  0.0565
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            65917
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.780
_diffrn_reflns_theta_min         2.973
_exptl_absorpt_coefficient_mu    3.365
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.835
_refine_diff_density_min         -1.781
_refine_diff_density_rms         0.195
_refine_ls_abs_structure_details
;
 Flack x determined using 4694 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.150(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         15291
_refine_ls_number_restraints     399
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+27.3435P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1442
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.867
_reflns_number_gt                11738
_reflns_number_total             15291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00789e2.cif
_cod_data_source_block           5'
_cod_depositor_comments
'Adding full bibliography for 7034824--7034836.cif.'
_cod_database_code               7034829
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.583
_shelx_estimated_absorpt_t_min   0.525
_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), C29(H29), C31(H31), C32(H32)
3.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C33(H33A,H33B), C34(H34A,H34B), C38(H38A,H38B), C36(H36A,
 H36B), C35(H35A,H35B), C40(H40A,H40B), C39(H39A,H39B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C12(H12), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C28(H28), C44(H44), C42(H42), C43(H43)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C41(H41A,H41B,H41C)
;
_olex2_submission_special_instructions 'No special instructions were received'