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_7034827
_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 Eu N5 O13'
_chemical_formula_sum            'C22 H24 Cu Eu N5 O13'
_chemical_formula_weight         781.96
_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
(compiled 2014.12.26 svn.r3119 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                101.5260(10)
_cell_angle_beta                 95.2070(10)
_cell_angle_gamma                90.3530(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2709(5)
_cell_length_b                   12.0444(7)
_cell_length_c                   12.2012(7)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.92
_cell_volume                     1329.02(13)
_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      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0267
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36979
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.338
_diffrn_reflns_theta_min         3.180
_exptl_absorpt_coefficient_mu    3.216
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            reddish-brown
_exptl_crystal_colour_primary    reddish-brown
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_description       needle
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.159
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 5489 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.014(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         13151
_refine_ls_number_restraints     411
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0161P)^2^+1.1649P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0479
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                11772
_reflns_number_total             13151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00789e2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7034824--7034836.cif.'
_cod_database_code               7034827
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.938
_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:
 C1(H1), C2(H2), C3(H3), C7(H7)
3.b Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C53(H53A,H53B), C52(H52A,H52B), C49(H49A,H49B), C48(H48A,
 H48B), C54(H54A,H54B), C56(H56A,H56B), C57(H57A,H57B)
3.c Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C1AA(H1AA), C4(H4), C14(H14), C15(H15), C16(H16), C20(H20),
 C22(H22), C23(H23), C25(H25), C27(H27), C29(H29), C30(H30), C32(H32), C28(H28),
  C31(H31)
3.d Idealised Me refined as rotating group:
 C3AA(H3AA,H3AB,H3AC), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'