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_1520085
_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         'C116 H148 Co4 Dy4 N12 O34, C4 H6 N2'
_chemical_formula_sum            'C120 H154 Co4 Dy4 N14 O34'
_chemical_formula_weight         3222.28
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           175
_space_group_name_Hall           '-P 6'
_space_group_name_H-M_alt        'P 6/m'
_symmetry_space_group_name_Hall  '-P 6'
_symmetry_space_group_name_H-M   'P 6/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-02-10
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   27.7587(6)
_cell_length_b                   27.7587(6)
_cell_length_c                   22.5433(9)
_cell_measurement_temperature    100
_cell_volume                     15043.4(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1782
_diffrn_reflns_av_unetI/netI     0.1016
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            108985
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.328
_exptl_absorpt_coefficient_mu    1.845
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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    1.067
_exptl_crystal_description       plate
_exptl_crystal_F_000             4848
_exptl_crystal_size_max          0.048
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         10477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0789P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6100
_reflns_number_total             10477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01813g2.cif
_cod_data_source_block           2014ncs0912z
_cod_depositor_comments
'Adding full bibliography for 1520082--1520087.cif.'
_cod_original_cell_volume        15043.4(9)
_cod_database_code               1520085
_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. Rigid bond restraints
 C14, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
: 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
4. Rigid body (RIGU) restrains
 C14, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C13(0.5) H13A(0.5)
 H13B(0.5) H13C(0.5) C14(0.5) C19(0.5) H19(0.5) C18(0.5) H18(0.5) C17(0.5)
 H17(0.5) C16(0.5) H16(0.5) C15(0.5) H15(0.5) C22(0.5) H22A(0.5) H22B(0.5)
 H22C(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C24(0.5) H24A(0.5) H24B(0.5)
 H24C(0.5) H31A(0.5) H31B(0.5) H31C(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5)
 C18A(0.5) H18A(0.5) C17A(0.5) H17A(0.5) C16A(0.5) H16A(0.5) C15A(0.5)
 H15A(0.5) C14A(0.5) C19A(0.5) H19A(0.5) C12A(0.5) H12D(0.5) H12E(0.5)
 H12F(0.5) C13A(0.5) H13D(0.5) H13E(0.5) H13F(0.5) C23A(0.5) H23D(0.5)
 H23E(0.5) H23F(0.5) C24A(0.5) H24D(0.5) H24E(0.5) H24F(0.5) C22A(0.5)
 H22D(0.5) H22E(0.5) H22F(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
6.a Ternary CH refined with riding coordinates:
 O1(H1)
6.b Aromatic/amide H refined with riding coordinates:
 C3AA(H3AA), C4(H4), C5(H5), C8(H8), C19(H19), C18(H18), C17(H17), C16(H16),
 C15(H15), C18A(H18A), C17A(H17A), C16A(H16A), C15A(H15A), C19A(H19A)
6.c Fitted pentagon refined as free rotating group:
 C11(C9,C10,N2,N3)
6.d Fitted hexagon refined as free rotating group:
 C14(C19,C18,C17,C16,C15), C18A(C17A,C16A,C15A,C14A,C19A)
6.e Idealised Me refined as rotating group:
 C1AA(H1AA,H1AB,H1AC), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C0AA(H0AA,H0AB,H0AC), C12A(H12D,H12E,H12F), C13A(H13D,H13E,H13F),
 C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F), C22A(H22D,H22E,H22F), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C)
;
_olex2_submission_special_instructions 'No special instructions were received'