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_7055736
_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
'C48 H48 Cu2 Fe N10 O9 Tb, 4.5(O), 1.5(C2 H3 N)'
_chemical_formula_sum            'C51 H63.5 Cu2 Fe N11.5 O13.5 Tb'
_chemical_formula_weight         1395.48
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-12
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.134(11)
_cell_length_b                   23.479(12)
_cell_length_c                   26.843(14)
_cell_measurement_reflns_used    2976
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      7.57
_cell_volume                     13320(12)
_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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_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  0.1520
_diffrn_reflns_av_unetI/netI     0.0894
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            119161
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.559
_diffrn_reflns_theta_min         3.010
_exptl_absorpt_coefficient_mu    1.955
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.504
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Higashi, T. (1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       strip
_exptl_crystal_F_000             5656
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.821
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         15222
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1085P)^2^+0.5830P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.2171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7925
_reflns_number_total             15222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj01887d2.cif
_cod_data_source_block           5
_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        13319(12)
_cod_original_formula_sum        'C51 H63.50 Cu2 Fe N11.50 O13.50 Tb'
_cod_database_code               7055736
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3W) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C100)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C76) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Others
 Sof(O6WA)=1-FVAR(1)
 Sof(O6W)=FVAR(1)
 Fixed Sof: C103(0.5) N11(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 N12(0.25) C105(0.25) H10G(0.25) H10H(0.25) H10I(0.25) C104(0.25) C108(0.25)
 H10J(0.25) H10K(0.25) H10L(0.25) N14(0.25) C102(0.25) O3W(0.5) C10(0.5)
 H10M(0.5) H10N(0.5) H10O(0.5) C11(0.5) N13(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C31(H31A,H31B), C37(H37A,H37B), C92(H92A,H92B)
4.b Me refined with riding coordinates:
 C41(H41A,H41B,H41C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C66(H66A,H66B,
 H66C), C70(H70A,H70B,H70C), C14(H14A,H14B,H14C), C105(H10G,H10H,H10I),
 C108(H10J,H10K,H10L)
4.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C40(H40), C46(H46), C50(H50), C51(H51), C52(H52), C57(H57),
 C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C74(H74), C76(H76), C80(H80),
  C83(H83)
4.d Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C101(H10A,H10B,H10C), C100(H10D,H10E,H10F), C10(H10M,
 H10N,H10O)
;
_shelx_res_checksum              56030
_olex2_submission_special_instructions 'No special instructions were received'