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_1520087
_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         'C52 H72 Co2 Dy2 N8 O22, 2(N O3)'
_chemical_formula_sum            'C52 H72 Co2 Dy2 N10 O28'
_chemical_formula_weight         1728.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-03-18
_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                 115.817(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.6279(17)
_cell_length_b                   12.2953(5)
_cell_length_c                   26.851(2)
_cell_measurement_temperature    293(2)
_cell_volume                     7319.2(10)
_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      293.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.859
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            21059
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.113
_diffrn_reflns_theta_min         3.501
_exptl_absorpt_coefficient_mu    2.545
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.565
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         8459
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+14.7874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6233
_reflns_number_total             8459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01813g2.cif
_cod_data_source_block           w14d24bb
_cod_depositor_comments
'Adding full bibliography for 1520082--1520087.cif.'
_cod_original_cell_volume        7319.1(9)
_cod_database_code               1520087
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H1 of O1, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H8 of O8, All O(H,H) groups
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.01
 C25-H8
 1.893932 with sigma of 0.02
 Dy1-H8
 2.920322 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O12, N5, O13, O14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Rotating group:
 O2(H2A,H2B)
4.b Ternary CH refined with riding coordinates:
 O1(H1)
4.c Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
4.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8A), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19)
4.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              70094
_olex2_submission_special_instructions 'No special instructions were received'