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_1520082
_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         'C59.5 H78 Co2 Dy2 N8 O22, 2(C H4 O)'
_chemical_formula_sum            'C61.5 H86 Co2 Dy2 N8 O24'
_chemical_formula_weight         1764.24
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-02-11
_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                67.4228(15)
_cell_angle_beta                 86.9557(13)
_cell_angle_gamma                89.2403(12)
_cell_formula_units_Z            4
_cell_length_a                   14.0680(2)
_cell_length_b                   21.3940(3)
_cell_length_c                   26.2804(4)
_cell_measurement_reflns_used    52126
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.2910
_cell_measurement_theta_min      1.7660
_cell_volume                     7292.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_details
;
  1 omega  -78.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000  -72.0000  150.0000 100

  2 omega  -71.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000  -72.0000  -30.0000 93

  3 omega  -22.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000   72.0000   90.0000 93

  4 omega  -93.00  -14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000    0.0000  -30.0000 79

  5 omega  -32.00   -7.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000   54.0000  -60.0000 25

  6 omega   -5.00   20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000  -72.0000    0.0000 25

  7 omega -109.00   53.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000    0.0000    0.0000 162

  8 omega -109.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000  -72.0000 -180.0000 131

  9 omega  -78.00  -52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000  -72.0000   30.0000 26
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0073870000
_diffrn_orient_matrix_UB_12      -0.0189409000
_diffrn_orient_matrix_UB_13      0.0287355000
_diffrn_orient_matrix_UB_21      0.0344841000
_diffrn_orient_matrix_UB_22      0.0202528000
_diffrn_orient_matrix_UB_23      0.0053875000
_diffrn_orient_matrix_UB_31      -0.0361349000
_diffrn_orient_matrix_UB_32      0.0228117000
_diffrn_orient_matrix_UB_33      0.0013941000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            117090
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         29.418
_diffrn_reflns_theta_min         1.599
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.551
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79432
_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    1.607
_exptl_crystal_description       plate
_exptl_crystal_F_000             3556
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.01
_refine_diff_density_max         6.752
_refine_diff_density_min         -4.744
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1666
_refine_ls_number_reflns         36189
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+147.9280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.1945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29530
_reflns_number_total             36189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01813g2.cif
_cod_data_source_block           2014ncs0839
_cod_depositor_comments
;
Adding full bibliography for 1520082--1520087.cif.

2019-07-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C123 H172 Co4 Dy4 N16 O48'
_cod_original_formula_weight         3528.48
_cod_original_formula_moiety         '2(C59.5 H78 Co2 Dy2 N8 O22), 4(C H4 O)'
_cod_original_formula_units_Z            2
_cod_database_code               1520082
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         Dy2Co2C48H60N6O10
_reflns_odcompleteness_completeness 89.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.35
_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) groups
2. Restrained distances
 C141-C143
 1.53 with sigma of 0.02
 C151-C152
 1.53 with sigma of 0.02
 C153-C151
 1.53 with sigma of 0.02
 C151-C154
 1.53 with sigma of 0.02
 C105-C106
 1.53 with sigma of 0.02
 C105-C108
 1.53 with sigma of 0.02
 C105-C107
 1.53 with sigma of 0.02
 C128-O127
 1.43 with sigma of 0.02
 C124-O123
 1.43 with sigma of 0.02
 C126-O125
 1.43 with sigma of 0.02
 O0AA-C2AA
 1.43 with sigma of 0.02
3. Rigid bond restraints
 C46, C47, C48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C106, C107, C108
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O127, C128
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C105, C106, C107, C108
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C45, C46, C47, C48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O125, C126
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C128, O127, C124, O123, C126, O125
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C46 \\sim C47 \\sim C48: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C106 \\sim C107 \\sim C108: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O127 \\sim C128: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C105 \\sim C106 \\sim C107 \\sim C108: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C45 \\sim C46 \\sim C47 \\sim C48: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O125 \\sim C126: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C128 \\sim O127 \\sim C124 \\sim O123 \\sim O125 \\sim C126: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C55) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C110) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C55) \\sim Ueq, Uanis(C110) \\sim Ueq: with sigma of 0.2 and sigma for
terminal atoms of 0.3
Uiso(C47) = Uiso(C46) = Uiso(C48)
Uanis(C111) = Uanis(C110) = Uanis(C113) = Uanis(C112)
Uanis(C57) = Uanis(C55) = Uanis(C58) = Uanis(C56)
Uanis(O42) = Uanis(N8) = Uanis(O43) = Uanis(O44)
5. Rigid body (RIGU) restrains
 C46, C47, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C106, C107, C108
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O127, C128
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C105, C106, C107, C108
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C45, C46, C47, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O125, C126
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C45, C46, C47, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C105, C106, C107, C108
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O127, C128, C126, O125, C124, O123
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C45(0.5) C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) C47(0.5) H47A(0.5)
 H47B(0.5) H47C(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C55(0.5) C105(0.5)
 C106(0.5) H10J(0.5) H10K(0.5) H10L(0.5) C107(0.5) H10M(0.5) H10N(0.5)
 H10O(0.5) C108(0.5) H10P(0.5) H10Q(0.5) H10R(0.5) C110(0.5) C144(0.5)
 H14A(0.5) H14B(0.5) H14C(0.5) C143(0.5) H14E(0.5) H14F(0.5) H14D(0.5)
 C142(0.5) H14G(0.5) H14H(0.5) H14I(0.5) C141(0.5) C153(0.5) H15A(0.5)
 H15B(0.5) H15C(0.5) C151(0.5) C154(0.5) H15D(0.5) H15E(0.5) H15F(0.5)
 C152(0.5) H15G(0.5) H15H(0.5) H15I(0.5)
7.a Riding coordinates:
 C1(H1A,H1B,H1C)
7.b Me refined with riding coordinates:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C80(H80A,H80B,H80C),
 C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C101(H10A,H10B,H10C), C102(H10D,H10E,
 H10F), C103(H10G,H10H,H10I), C106(H10J,H10K,H10L), C107(H10M,H10N,H10O),
 C108(H10P,H10Q,H10R), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C113(H11J,
 H11K,H11L), C116(H11M,H11N,H11O), C117(H11P,H11Q,H11R), C118(H11S,H11T,H11U),
 C119(H11V,H11W,H11X), C120(H12D,H12E,H12F), C126(H12G,H12H,H12I), C124(H12J,
 H12K,H12L), C128(H12M,H12N,H12O), C144(H14A,H14B,H14C), C143(H14E,H14F,H14D),
 C142(H14G,H14H,H14I), C153(H15A,H15B,H15C), C154(H15D,H15E,H15F), C152(H15G,
 H15H,H15I), C2AA(H2AA,H2AB,H2AC)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C14(H14), C0AA(H0AA), C16(H16), C17(H17),
 C18(H18), C22(H22), C23(H23), C24(H24), C27(H27), C33(H33), C34(H34), C35(H35),
  C36(H36), C37(H37), C63(H63), C64(H64), C65(H65), C68(H68), C74(H74),
 C75(H75), C76(H76), C77(H77), C78(H78), C82(H82), C83(H83), C84(H84), C87(H87),
  C93(H93), C94(H94), C95(H95), C96(H96), C97(H97)
7.d Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C)
7.e Idealised tetrahedral OH refined as rotating group:
 O125(H125), O123(H123), O127(H127), O0AA(H0AB)
;
_olex2_submission_special_instructions 'No special instructions were received'