A family of one-dimensional lanthanide complexes bridged by two distinct carboxylate ligands with the Dy analogue displaying magnetic relaxation behaviour
Zhu, Wen-Hua; Xiong, Xia; Gao, Chen; Li, Shan; Zhang, Yan; Wang, Juan; Zhang, Chi; Powell, Annie K.; Gao, Song; Dalton Transactions 46 (2017) 14114–14121; doi:10.1039/C7DT02736B

data_1546898
_publ_section_title
;
 A family of one-dimensional lanthanide complexes bridged by two distinct
 carboxylate ligands with the Dy analogue displaying magnetic relaxation
 behaviour
;
_journal_issue                   41
_journal_name_full               'Dalton Transactions'
_journal_page_first              14114
_journal_page_last               14121
_journal_paper_doi               10.1039/C7DT02736B
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         '0.5(C40 H36 Er2 N2 O18), H2 O'
_chemical_formula_sum            'C20 H20 Er N O10'
_chemical_formula_weight         601.63
_chemical_name_common            '[Er(INNO)(Bza)2(H2O)2]H2O,12nov24i'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-08-26 deposited with the CCDC.
2017-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.332(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.312(3)
_cell_length_b                   14.376(2)
_cell_length_c                   9.5785(15)
_cell_measurement_reflns_used    4856
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.277
_cell_measurement_theta_min      2.502
_cell_volume                     2242.4(6)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.926
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8809
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.360
_diffrn_reflns_theta_min         1.890
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.797
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.501
_refine_diff_density_min         -2.187
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3413
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0220P)^2^+6.0820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3019
_reflns_number_total             3413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02736b3.cif
_cod_data_source_block           Er(6)
_cod_original_cell_volume        2242.5(6)
_cod_database_code               1546898
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.450
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H6B of H5A
 At 1 times of:
  H6A of H5A
2. Shared sites
{N1, C12}
{O3, H1}
3. Restrained distances
 O5-H5B = O5-H5A
 0.96 with sigma of 0.02
 H5B-H5A
 1.52 with sigma of 0.02
 O6-H6B = O6-H6A
 0.96 with sigma of 0.02
 H6B-H6A
 1.52 with sigma of 0.02
 H5A-H1_$2
 2 with sigma of 0.02
 H5A-H6B
 2 with sigma of 0.02
 H6B-O5
 2.2 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C12)
Uanis(O3) = Uanis(H1)
5. Others
 Fixed Sof: N1(0.5) O3(0.5) H1(0.5) C12(0.5) O6(0.5) H6A(0.5) H6B(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C11(H11)
;
_shelx_res_checksum              73495
_olex2_submission_special_instructions 'No special instructions were received'