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_7702141
_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 Ho6 N24 O18)'
_chemical_formula_sum            'C30 H54 Fe Ho3 N12 O9'
_chemical_formula_weight         1277.49
_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     direct
_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                   16.276(3)
_cell_length_b                   18.779(3)
_cell_length_c                   14.043(3)
_cell_measurement_reflns_used    7628
_cell_measurement_temperature    150
_cell_measurement_theta_max      21.95
_cell_measurement_theta_min      2.20
_cell_volume                     4292.2(14)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.619
_diffrn_measured_fraction_theta_max 1.000
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.619
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            29300
_diffrn_reflns_point_group_measured_fraction_full 0.619
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         21.255
_diffrn_reflns_theta_min         1.811
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.862
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.5551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0979 before and 0.0628 after correction.
The Ratio of minimum to maximum transmission is 0.7454.
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    1.977
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2468
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0234
_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^)+(0.0193P)^2^+19.7941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2246
_reflns_number_total             2477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02541f1.cif
_cod_data_source_block           C30H54N12O9Ho3Fe
_cod_original_cell_volume        4292.2(13)
_cod_database_code               7702141
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.735
_shelx_estimated_absorpt_t_min   0.512
_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: H3a(0.5) H3b(0.5) H2a(0.5) H2b(0.5) H1a(0.5) H1b(0.5)
3.a Rotating group:
 O3(H3a,H3b), O2(H2a,H2b), O1(H1a,H1b)
3.b Ternary CH refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C10(H10), C16(H16)
3.c Idealised Me refined as rotating group:
 C20(H20a,H20b,H20c), C19(H19a,H19b,H19c), C9(H9a,H9b,H9c), C17(H17a,H17b,
 H17c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c)
;
_shelx_res_checksum              79862
_shelx_fab_checksum              82808
_olex2_submission_special_instructions 'No special instructions were received'