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_7227735
_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 H58 Cu5 N4 O22 Sm2, 2(F6 P), 2(C2 H6 O), 2(H2 O)'
_chemical_formula_sum            'C50 H74 Cu5 F12 N4 O26 P2 Sm2'
_chemical_formula_weight         2055.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                63.49(3)
_cell_angle_beta                 84.78(3)
_cell_angle_gamma                71.57(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5555(19)
_cell_length_b                   14.872(3)
_cell_length_c                   14.873(3)
_cell_measurement_reflns_used    5097
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.9624
_cell_measurement_theta_min      2.6475
_cell_volume                     1791.2(9)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.9948
_diffrn_measured_fraction_theta_max 0.9948
_diffrn_measurement_details
;
scan:
    Number of images: 90
               Slice: -120.0000 - 60.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 50.0328
              2theta: -29.8929
scan:
    Number of images: 80
               Slice: -120.0000 - 40.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 50.0328
              2theta: -29.8929
scan:
    Number of images: 70
               Slice: -120.0000 - 20.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 50.0328
              2theta: -29.8929
;
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
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_diffrn_orient_matrix_UB_11      -0.1087
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_diffrn_orient_matrix_UB_21      -0.0087
_diffrn_orient_matrix_UB_22      -0.0686
_diffrn_orient_matrix_UB_23      0.0298
_diffrn_orient_matrix_UB_31      0.0373
_diffrn_orient_matrix_UB_32      0.0532
_diffrn_orient_matrix_UB_33      0.0450
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_max       11
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_diffrn_reflns_theta_min         2.25
_diffrn_source                   'Rotating Anode'
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_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    3.221
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7665
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.9055
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1019.6733
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.2726
_refine_diff_density_min         -2.0354
_refine_diff_density_rms         0.2181
_refine_ls_d_res_high            0.8407
_refine_ls_d_res_low             9.0495
_refine_ls_goodness_of_fit_ref   1.0134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    57
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6285
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.0108
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0335
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0799P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
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_reflns_limit_k_max              17
_reflns_limit_k_min              -15
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                5528
_reflns_number_total             6285
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6ce02519f2.cif
_cod_data_source_block           cusm_sq_d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7227732--7227739.cif.
;
_cod_original_cell_volume        1791.1(9)
_cod_database_code               7227735
_diffrn_number_total             8434
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H7 of O7, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H12a of O12, All O(H,H) groups
2. Restrained distances
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
5.a Riding coordinates:
 O12(H12a), O7(H7)
5.b Free rotating group:
 O13(H13a,H13b)
5.c Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), C10(H10)
5.d Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C11(H11a,H11b), C24(H24a,H24b)
5.e Me refined with riding coordinates:
 C1(H1a,H1b,H1c)
5.f Aromatic/amide H refined with riding coordinates:
 C4(H4), C14(H14), C16(H16), C15(H15), C5(H5), C6(H6a), C12(H12)
5.g Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C25(H25a,H25b,H25c), C21(H21a,H21b,H21c), C23(H23a,H23b,
 H23c)
;
_olex2_submission_special_instructions 'No special instructions were received'