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_7055733
_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 Gd N10 O9, 5(O), 2.5(C2 H3 N)'
_chemical_formula_sum            'C53 H67.5 Cu2 Fe Gd N12.5 O14'
_chemical_formula_weight         1443.87
_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             2016-08-11
_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                   21.1918(9)
_cell_length_b                   23.3200(8)
_cell_length_c                   26.6459(12)
_cell_measurement_reflns_used    8327
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.04
_cell_volume                     13168.2(9)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_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      173.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1456
_diffrn_reflns_av_unetI/netI     0.0999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            78394
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.414
_diffrn_reflns_theta_min         2.894
_exptl_absorpt_coefficient_mu    1.914
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       strip
_exptl_crystal_F_000             5776
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.962
_refine_diff_density_min         -2.131
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         13377
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1608
_refine_ls_R_factor_gt           0.0922
_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^)+(0.0576P)^2^+326.9834P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8162
_reflns_number_total             13377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj01887d2.cif
_cod_data_source_block           compelx-4
_cod_depositor_comments
'Adding full bibliography for 7055730--7055736.cif.'
_cod_original_formula_sum        'C53 H67.50 Cu2 Fe Gd N12.50 O14'
_cod_database_code               7055733
_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(C111) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(N15) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: N12(0.75) C104(0.75) C105(0.75) H10G(0.75) H10H(0.75) H10I(0.75)
 C110(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C111(0.5) N15(0.5) C102(0.5) H10J(0.5)
 H10K(0.5) H10L(0.5) C103(0.5) N11(0.5) C106(0.75) C107(0.75) H10M(0.75)
 H10N(0.75) H10O(0.75) N13(0.75)
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), C70(H70A,H70B,
 H70C), C110(H11A,H11B,H11C), C102(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), C66(H66A,H66B,H66C), C101(H10A,H10B,H10C), C100(H10D,
 H10E,H10F), C105(H10G,H10H,H10I), C107(H10M,H10N,H10O)
;
_shelx_res_checksum              10005
_olex2_submission_special_instructions 'No special instructions were received'