Compartmental ligand approach for constructing 3d‒4f heterometallic [CuII5LnIII2] clusters: synthesis and magnetostructural properties
Jiang, Lin; Liu, Bin; Zhao, Hao-Wen; Tian, Jin-Lei; Liu, Xin; Yan, Shi-Ping; CrystEngComm 19 (2017) 1816–; doi:10.1039/C6CE02519F

data_7227738
_publ_section_title
;
 Compartmental ligand approach for constructing 3d--4f heterometallic
 [CuII5LnIII2] clusters: synthesis and magnetostructural properties
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1816
_journal_paper_doi               10.1039/C6CE02519F
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety
'C46 H62 Cu5 Gd2 N4 O22, 2(N O3), 4(C2 H6 O), 2(C2 H5 O)'
_chemical_formula_sum            'C58 H96 Cu5 Gd2 N6 O34'
_chemical_formula_weight         2053.61
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-14 deposited with the CCDC.
2017-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.813(3)
_cell_length_b                   16.135(3)
_cell_length_c                   19.072(4)
_cell_measurement_reflns_used    7566
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7560
_cell_measurement_theta_min      3.3810
_cell_volume                     3793.2(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16876
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.187
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2062
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.471
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8626
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+4.8365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                6761
_reflns_number_total             8626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce02519f2.cif
_cod_data_source_block           jlgd
_cod_depositor_comments
'Adding full bibliography for 7227732--7227739.cif.'
_cod_original_cell_volume        3793.0(13)
_cod_database_code               7227738
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C27-O16
 2.35 with sigma of 0.01
 O16-C26
 1.3 with sigma of 0.01
 C27-C26
 1.52 with sigma of 0.01
3.a Riding coordinates:
 O16(H16A)
3.b Ternary CH refined with riding coordinates:
 C10(H10), N1(H1), N2(H2)
3.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C8(H8A,H8B), C11(H11A,H11B), C9(H9A,H9B), C28(H28A,H28B),
 C26(H26A,H26B)
3.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C5(H5), C6(H6A), C16(H16), C4(H4), C24(H24)
3.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C23(H23A,H23B,
 H23C), C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C)
3.f Idealised tetrahedral OH refined as rotating group:
 O17(H17), O15(H15A)
;
_olex2_submission_special_instructions 'No special instructions were received'