New coordination networks containing trinuclear lanthanide complexes and hexacyanometallates.
Escobedo-Cruz, Francisco V; Hughbanks, Timothy; Dalton transactions (Cambridge, England : 2003) 47 (2018) 6831–6841; doi:10.1039/c7dt02541f

data_7702150
_publ_section_title
;
 New coordination networks containing trinuclear lanthanide complexes and
 hexacyanometallates.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6831
_journal_page_last               6841
_journal_paper_doi               10.1039/c7dt02541f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.5(C60 H108 Fe2 N24 O18 Tb6)'
_chemical_formula_sum            'C30 H54 Fe N12 O9 Tb3'
_chemical_formula_weight         1259.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.359(3)
_cell_length_b                   18.917(3)
_cell_length_c                   14.106(2)
_cell_measurement_reflns_used    6546
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.19
_cell_volume                     4365.3(12)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker-Axs ApexII'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.822
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.822
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37251
_diffrn_reflns_point_group_measured_fraction_full 0.822
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.558
_diffrn_reflns_theta_min         2.153
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.186
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0929 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.7996.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2444
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0187P)^2^+11.9238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2864
_reflns_number_total             3353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02541f1.cif
_cod_data_source_block           C30H54N12O9Tb3Fe
_cod_original_cell_volume        4365.1(13)
_cod_database_code               7702150
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H1a(0.5) H1b(0.5) H2a(0.5) H2b(0.5) H3a(0.5) H3b(0.5)
3.a Rotating group:
 O1(H1a,H1b), O2(H2a,H2b), O3(H3a,H3b)
3.b Ternary CH refined with riding coordinates:
 C8AA(H8AA), C12(H12), C0AA(H0AA), C1AA(H1AA), C9AA(H9AA), C4AA(H4AA)
3.c Idealised Me refined as rotating group:
 C2AA(H2Aa,H2Ab,H2Ac), C3AA(H3Aa,H3Ab,H3Ac), C14(H14a,H14b,H14c), C5AA(H5Aa,
 H5Ab,H5Ac), C13(H13a,H13b,H13c), C6AA(H6Aa,H6Ab,H6Ac)
;
_shelx_res_checksum              74528
_shelx_fab_checksum              64771
_olex2_submission_special_instructions 'No special instructions were received'