Single molecule magnet behaviour in a {Dy4P2} octahedron.
Zangana, Karzan H.; Moreno Pineda, Eufemio; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12522–12525; doi:10.1039/c5dt01786f

data_7035396
_publ_section_title
;
 Single molecule magnet behaviour in a {Dy4P2} octahedron.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12522
_journal_page_last               12525
_journal_paper_doi               10.1039/c5dt01786f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'2(C45 H69 Co3 N3 O13), C28 H58 Gd4 N6 O34 P2, 2(C2 H3 N)'
_chemical_formula_sum            'C122 H202 Co6 Gd4 N14 O60 P2'
_chemical_formula_weight         3869.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-22 deposited with the CCDC.
2015-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9131(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7554(2)
_cell_length_b                   19.4689(4)
_cell_length_c                   36.4118(7)
_cell_measurement_reflns_used    18772
_cell_measurement_temperature    128.0(4)
_cell_measurement_theta_max      28.7950
_cell_measurement_theta_min      3.2110
_cell_volume                     8254.0(3)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      128.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -3.00   94.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7892   37.0000   90.0000 97

  2 omega   35.00   76.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7892  178.0000  -60.0000 41

  3 omega   65.00   91.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7892  178.0000  -90.0000 26

  4 omega   -3.00   94.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7892   37.0000    0.0000 97

  5 omega   -1.00   77.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7892   57.0000  150.0000 78

  6 omega  -80.00  -41.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0235  124.0000    4.0000 39

  7 omega  -94.00  -15.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0235  147.0000  169.0000 79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0050262000
_diffrn_orient_matrix_UB_12      0.0208792000
_diffrn_orient_matrix_UB_13      0.0160824000
_diffrn_orient_matrix_UB_21      0.0012856000
_diffrn_orient_matrix_UB_22      0.0297437000
_diffrn_orient_matrix_UB_23      -0.0111933000
_diffrn_orient_matrix_UB_31      -0.0607420000
_diffrn_orient_matrix_UB_32      0.0023639000
_diffrn_orient_matrix_UB_33      -0.0016296000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            64303
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.080
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.274
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70264
_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.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       needle
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.273
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1053
_refine_ls_number_reflns         16879
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0120P)^2^+15.5354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12988
_reflns_number_total             16879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01786f2.cif
_cod_data_source_block           Gd4P4
_cod_depositor_comments
'Adding full bibliography for 7035395--7035396.cif.'
_cod_database_code               7035396
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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,H) groups
2. Restrained distances
 C9A-C7 \\sim C7-C10A \\sim C10A-C7 \\sim C7-C8A \\sim C8A-C7 \\sim C7-C9A
 with sigma of 0.02
 C8A-C9A \\sim C9A-C10A \\sim C9A-C10A \\sim C10A-C8A \\sim C10A-C8A \\sim
C8A-C9A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8A) = Uanis(C8)
4. Rigid body (RIGU) restrains
 C27, C28, C29, C30, C28A, C29A, C30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22, C23, C24, C25, C23A, C24A, C25A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C8, C9, C10, C8A, C9A, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(2)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(2)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C10A)=Sof(H10F)=Sof(H10G)=Sof(H10H)=1-FVAR(3)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10C)=Sof(H10D)=Sof(H10E)=FVAR(3)
6.a Rotating group:
 O109(H10A,H10B)
6.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F), C28A(H28D,
 H28E,H28F), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C2P(H2PA,H2PB,H2PC),
 C3(H3A,H3B,H3C), C3P(H3PA,H3PB,H3PC), C4(H4A,H4B,H4C), C4P(H4PA,H4PB,H4PC),
 C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10C,H10D,H10E),
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10F,H10G,H10H), C57(H57A,H57B,
 H57C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2013-07-05
_olex2_submission_special_instructions 'No special instructions were received'