A new family of high nuclearity Co(II)/Dy(III) coordination clusters possessing robust and unseen topologies.
Berkoff, Benjamin; Griffiths, Kieran; Abdul-Sada, Alaa; Tizzard, Graham J.; Coles, Simon J.; Escuer, Albert; Kostakis, George E.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12788–12795; doi:10.1039/c5dt01813g

data_1520084
_publ_section_title
;
 A new family of high nuclearity Co(II)/Dy(III) coordination clusters
 possessing robust and unseen topologies.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12788
_journal_page_last               12795
_journal_paper_doi               10.1039/c5dt01813g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'2(C116 H148 Co4 Dy4 N12 O34), C78 H108 Co2 Dy5 N9 O37'
_chemical_formula_sum            'C310 H404 Co10 Dy13 N33 O105'
_chemical_formula_weight         8974.44
_chemical_name_systematic
;
 ?
;
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-24 deposited with the CCDC.
2015-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                73.030(2)
_cell_angle_beta                 88.444(3)
_cell_angle_gamma                89.026(3)
_cell_formula_units_Z            1
_cell_length_a                   13.7063(10)
_cell_length_b                   25.9590(18)
_cell_length_c                   32.551(2)
_cell_measurement_temperature    100
_cell_volume                     11072.8(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1105
_diffrn_reflns_av_unetI/netI     0.1045
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            156032
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.148
_exptl_absorpt_coefficient_mu    2.594
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       needle
_exptl_crystal_F_000             4463
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.661
_refine_diff_density_min         -2.277
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2116
_refine_ls_number_reflns         44922
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0760
_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^)+(0.1280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1931
_refine_ls_wR_factor_ref         0.2120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27561
_reflns_number_total             44922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01813g2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 1520082--1520087.cif.'
_cod_original_cell_volume        11072.7(14)
_cod_database_code               1520084
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N14-C131
 1.46 with sigma of 0.02
 N14-C12
 1.46 with sigma of 0.02
 C145-C143
 1.53 with sigma of 0.02
 C1F-C143
 1.53 with sigma of 0.02
3. Rigid bond restraints
 C145
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C145: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C49, C50, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C45, C46, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C144, C145, C146
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C148, C149, C150, C151
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, C50, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C45, C46, C47, C54, C56, C57, C58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C145
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C1F(0.5) H1FA(0.5) H1FB(0.5) H1FC(0.5) Dy7(0.5) O45(0.5) O46(0.5)
 O47(0.5) N17(0.5) C12(0.5) C1E(0.5) H1E(0.5) C1D(0.5) H1D(0.5) C1C(0.5)
 H1CA(0.5) C1B(0.5) H1BB(0.5) C1A(0.5) H1AA(0.5) C134(0.5) H134(0.5) C135(0.5)
 H135(0.5) C136(0.5) H136(0.5) C131(0.5) C132(0.5) H132(0.5) C133(0.5)
 H133(0.5) C145(0.5) H14J(0.5) H14K(0.5) H14L(0.5)
7.a Ternary CH refined with riding coordinates:
 O1BA(H1BA), O76(H76), O6AA(H6AA), O104(H104)
7.b Me refined with riding coordinates:
 C59(H59A,H59B,H59C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C88(H88A,H88B,
 H88C), C99(H99A,H99B,H99C), C100(H10A,H10B,H10C), C101(H10D,H10E,H10F),
 C104(H10G,H10H,H10I), C105(H10J,H10K,H10L), C106(H10M,H10N,H10O), C109(H10P,
 H10Q,H10R), C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C114(H11G,H11H,H11I),
 C115(H11J,H11K,H11L), C116(H11M,H11N,H11O), C1(H1A,H1B,H1C), C11(H11P,H11Q,
 H11R), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C), C57(H57A,H57B,H57C), C157(H15A,H15B,H15C),
 C1F(H1FA,H1FB,H1FC), C118(H11S,H11T,H11U), C128(H12A,H12B,H12C), C129(H12D,
 H12E,H12F), C139(H13A,H13B,H13C), C140(H14A,H14B,H14C), C141(H14D,H14E,H14F),
 C144(H14G,H14H,H14I), C145(H14J,H14K,H14L), C146(H14M,H14N,H14O), C149(H14P,
 H14Q,H14R), C150(H15D,H15E,H15F), C151(H15G,H15H,H15I), C154(H15J,H15K,H15L),
 C155(H15M,H15N,H15O), C156(H15P,H15Q,H15R)
7.c Aromatic/amide H refined with riding coordinates:
 C61(H61), C62(H62), C63(H63), C66(H66), C73(H73), C74(H74), C75(H75),
 C76(H76A), C77(H77), C80(H80), C81(H81), C82(H82), C85(H85), C92(H92),
 C93(H93), C94(H94), C95(H95), C96(H96), C3(H3), C4(H4), C4BA(H4BA), C5(H5),
 C8(H8), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23),
 C24(H24), C27(H27), C34(H34), C35(H35), C36(H36), C37(H37), C1E(H1E), C1D(H1D),
  C1C(H1CA), C1B(H1BB), C1A(H1AA), C120(H120), C121(H121), C122(H122),
 C125(H125), C134(H134), C135(H135), C136(H136), C132(H132), C133(H133)
7.d Fitted hexagon refined as free rotating group:
 C12(C1E,C1D,C1C,C1B,C1A), C134(C135,C136,C131,C132,C133)
7.e Idealised Me refined as rotating group:
 C78(H78A,H78B,H78C), C89(H89A,H89B,H89C), C56(H56A,H56B,H56C), C58(H58A,H58B,
 H58C)
;
_shelx_res_checksum              49905
_olex2_submission_special_instructions 'No special instructions were received'