Ligand-directed assembly of trinuclear and one-dimensional heterotrimetallic CuIILnIIIFeIIIcomplexes: unusual antiferromagnetic CuIIFeIIIcoupling via cyano bridges
Liu, Mei-Jiao; Hu, Kong-Qiu; Liu, Cai-Ming; Cui, Ai-Li; Kou, Hui-Zhong; New J. Chem. 40 (2016) 8643–; doi:10.1039/C6NJ01887D

data_7055731
_publ_section_title
;
 Ligand-directed assembly of trinuclear and one-dimensional
 heterotrimetallic CuIILnIIIFeIIIcomplexes: unusual antiferromagnetic
 CuIIFeIIIcoupling via cyano bridges
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              8643
_journal_paper_doi               10.1039/C6NJ01887D
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C25 H26 Cu Fe N8 O7.54 Tb, 1.46(O), 2(H2 O)'
_chemical_formula_sum            'C25 H34 Cu Fe N8 O11 Tb'
_chemical_formula_weight         900.91
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-12 deposited with the CCDC.
2016-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.12(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.889(3)
_cell_length_b                   12.035(2)
_cell_length_c                   22.242(8)
_cell_measurement_reflns_used    24818
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.455
_cell_measurement_theta_min      3.165
_cell_volume                     3330.7(16)
_computing_cell_refinement       'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_data_collection       'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_data_reduction        'crystalstructure 3.6.0 (Rigaku, 2004)'
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.77
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31991
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.364
_diffrn_reflns_theta_min         3.274
_exptl_absorpt_coefficient_mu    3.230
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.090
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR; Higashi, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.948
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7598
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0423P)^2^+2.1690P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6148
_reflns_number_total             7598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj01887d2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055730--7055736.cif.
;
_cod_original_cell_volume        3330.6(16)
_cod_database_code               7055731
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Cu1, Cu1'}
3. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq, Uanis(O7W) \\sim Ueq, Uanis(O6W) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Cu1) = Uanis(Cu1')
4. Others
 Sof(N2')=1-FVAR(1)
 Sof(N2)=FVAR(1)
 Sof(Cu1')=Sof(O1W')=1-FVAR(2)
 Sof(Cu1)=Sof(O1W)=FVAR(2)
 Sof(O6W')=1-FVAR(3)
 Sof(O6W)=FVAR(3)
5.a Riding coordinates:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB), O7W(H7WA,H7WB)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C25(H25A,H25B), C26(H26A,H26B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C10(H10), C21(H21), C24(H24), C27(H27), C28(H28)
5.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              57010
_olex2_submission_special_instructions 'No special instructions were received'