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_1520086
_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         'C84 H117 Co2 Dy5 N6 O37, 4(C2 H3 N)'
_chemical_formula_sum            'C92 H129 Co2 Dy5 N10 O37'
_chemical_formula_weight         2897.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.3983(4)
_cell_length_b                   17.1091(3)
_cell_length_c                   23.8614(6)
_cell_measurement_reflns_used    52276
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5020
_cell_measurement_theta_min      2.5290
_cell_volume                     11593.5(4)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_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(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -107.00   73.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000   -8.0000  -17.0000 360

  2 omega  -81.50   22.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000  -72.0000 -115.0000 207

  3 omega  -68.00   22.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000  -72.0000   81.0000 180

  4 omega  -92.50  -30.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000  -40.0000  -17.0000 125

  5 omega  -32.00  -16.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000   72.0000 -148.0000 32

  6 omega -107.00    1.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000   -8.0000   49.0000 216
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_orient_matrix_UB_11      -0.0068975000
_diffrn_orient_matrix_UB_12      -0.0003373000
_diffrn_orient_matrix_UB_13      0.0285786000
_diffrn_orient_matrix_UB_21      0.0153304000
_diffrn_orient_matrix_UB_22      0.0318413000
_diffrn_orient_matrix_UB_23      0.0054487000
_diffrn_orient_matrix_UB_31      -0.0184664000
_diffrn_orient_matrix_UB_32      0.0265328000
_diffrn_orient_matrix_UB_33      -0.0061608000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1091
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            150674
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.528
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    3.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65009
_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    1.660
_exptl_crystal_description       block
_exptl_crystal_F_000             5724
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.679
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         13272
_refine_ls_number_restraints     1593
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0911
_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^)+(0.0410P)^2^+279.9541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2129
_refine_ls_wR_factor_ref         0.2165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11412
_reflns_number_total             13272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01813g2.cif
_cod_data_source_block           2014ncs0911z
_cod_depositor_comments
'Adding full bibliography for 1520082--1520087.cif.'
_cod_original_cell_volume        11593.6(4)
_cod_database_code               1520086
_chemical_oxdiff_formula         'C78 H108 Co2 Dy5 N9 O38'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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
 N401-C401 = N441-C441
 1.16 with sigma of 0.02
 C401-C402 = C441-C442
 1.54 with sigma of 0.02
 C422-C421
 1.54 with sigma of 0.02
 C421-N421
 1.16 with sigma of 0.02
 O322-O323 \\sim O322-O321
 with sigma of 0.04
 N321-O322 \\sim N321-O323 \\sim N321-O321
 with sigma of 0.02
3. Restrained planarity
 O321, O322, O323, N321
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: Dy1(0.5) O321(0.5) O322(0.5) O323(0.5) N321(0.5) N401(0.5)
 C401(0.5) C402(0.5) H40A(0.5) H40B(0.5) H40C(0.5)
8.a Ternary CH refined with riding coordinates:
 O1(H1), O2(H2), O3(H3)
8.b Me refined with riding coordinates:
 C422(H42A,H42B,H42C)
8.c Aromatic/amide H refined with riding coordinates:
 C107(H107), C108(H108), C109(H109), C110(H110), C111(H111), C114(H114),
 C118(H118), C119(H119), C120(H120)
8.d Idealised Me refined as rotating group:
 C112(H11A,H11B,H11C), C113(H11D,H11E,H11F), C121(H12A,H12B,H12C), C203(H20A,
 H20B,H20C), C204(H20D,H20E,H20F), C205(H20G,H20H,H20I), C223(H22A,H22B,H22C),
 C224(H22D,H22E,H22F), C225(H22G,H22H,H22I), C243(H24A,H24B,H24C), C244(H24D,
 H24E,H24F), C245(H24G,H24H,H24I), C263(H26A,H26B,H26C), C264(H26D,H26E,H26F),
 C265(H26G,H26H,H26I), C402(H40A,H40B,H40C), C442(H44A,H44B,H44C)
;
_shelx_res_checksum              82463
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_original_sample_id W10D43BB
_olex2_submission_special_instructions 'No special instructions were received'