Synthesis and SMM behaviour of trinuclear versus dinuclear 3d-5f uranyl(v)-cobalt(ii) cation-cation complexes.
Chatelain, Lucile; Tuna, Floriana; Pécaut, Jacques; Mazzanti, Marinella; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5498–5502; doi:10.1039/c6dt04558h

data_7041725
_publ_section_title
;
 Synthesis and SMM behaviour of trinuclear versus dinuclear 3d-5f
 uranyl(v)-cobalt(ii) cation-cation complexes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5498
_journal_page_last               5502
_journal_paper_doi               10.1039/c6dt04558h
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
'C37 H39 Co N7 O4 U, I, C5 H5 N1, 0.42(C H), 0.08(N1)'
_chemical_formula_sum            'C42.42 H44.42 Co I N8.08 O4 U'
_chemical_formula_weight         1155.30
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2016-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   43.0624(8)
_cell_length_b                   43.0624(8)
_cell_length_c                   12.2847(2)
_cell_measurement_reflns_used    24771
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      31.6750
_cell_measurement_theta_min      3.3547
_cell_volume                     19728.4(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -77.00   39.25   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.7031  -57.0000 -180.0000 155

  2 omega  -45.00   68.25   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7355  -77.0000  -60.0000 151

  3 omega  -21.00   83.25   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7355  -99.0000 -150.0000 139

  4 omega   76.00  119.50   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7355  125.0000    0.0000 58

  5 omega  -39.00   -1.50   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7355  132.0000  146.5604 50

  6 omega -114.00    2.25   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.1417  -57.0000  150.0000 155

  7 omega -115.00    2.00   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.1417  -57.0000   60.0000 156

  8 omega   32.00   95.00   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.7031 -179.0000  120.0000 84

  9 omega -116.00    4.00   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.1417  -57.0000  -60.0000 160
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0068522000
_diffrn_orient_matrix_UB_12      0.0118558000
_diffrn_orient_matrix_UB_13      -0.0055483000
_diffrn_orient_matrix_UB_21      0.0177153000
_diffrn_orient_matrix_UB_22      0.0146717000
_diffrn_orient_matrix_UB_23      -0.0049484000
_diffrn_orient_matrix_UB_31      -0.0008620000
_diffrn_orient_matrix_UB_32      -0.0024132000
_diffrn_orient_matrix_UB_33      -0.0572798000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            71679
_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         28.275
_diffrn_reflns_theta_min         3.361
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.821
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'lustrous dark black'
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_description       needle
_exptl_crystal_F_000             10071
_exptl_crystal_size_max          0.921
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.094
_refine_diff_density_max         4.101
_refine_diff_density_min         -2.088
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         10873
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0378P)^2^+211.9863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9272
_reflns_number_total             10873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04558h2.cif
_cod_data_source_block           lc213
_cod_depositor_comments
'Adding full bibliography for 7041724--7041725.cif.'
_cod_original_cell_volume        19728.4(8)
_cod_database_code               7041725
_chemical_oxdiff_formula         'U Co O12 N12 C80 H80'
_shelx_estimated_absorpt_t_max   0.660
_shelx_estimated_absorpt_t_min   0.095
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N101, C101}
3. Uiso/Uaniso restraints and constraints
C42 \\sim N41 \\sim C41 \\sim C45 \\sim C44 \\sim C43 \\sim C41A \\sim N41A
\\sim C45A \\sim C42A \\sim C43A \\sim C44A: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N101) = Uanis(C101)
4. Others
 Sof(H8BC)=Sof(H8BD)=Sof(H11C)=Sof(H11D)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=
 Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C19B)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(H8AA)=Sof(H8AB)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=
 Sof(H11A)=Sof(H11B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(N41A)=Sof(C41A)=Sof(H41A)=Sof(C45A)=Sof(H45A)=Sof(C42A)=Sof(H42A)=
 Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(H44A)=1-FVAR(2)
 Sof(N41)=Sof(C41)=Sof(H41)=Sof(C45)=Sof(H45)=Sof(C42)=Sof(H42)=Sof(C44)=
 Sof(H44)=Sof(C43)=Sof(H43)=FVAR(2)
 Fixed Sof: C101(0.416667) H101(0.416667) N101(0.08333)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8AA,H8AB), C8(H8BC,H8BD), C9(H9A,H9B), C10(H10A,H10B), C11(H11C,H11D),
 C11(H11A,H11B), C9B(H9BA,H9BB), C10B(H10C,H10D), C21(H21A,H21B), C27(H27A,
 H27B), C33(H33A,H33B)
5.b Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C3(H3), C4(H4), C5(H5), C7(H7), C12(H12), C14(H14), C15(H15),
 C16(H16), C17(H17), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30),
  C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), C41(H41), C45(H45),
 C42(H42), C44(H44), C43(H43), C38(H38), C41A(H41A), C45A(H45A), C42A(H42A),
 C43A(H43A), C44A(H44A), C101(H101)
5.c Fitted hexagon refined as free rotating group:
 N41(C41,C45,C42,C44,C43), N41A(C41A,C45A,C42A,C43A,C44A)
5.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C19B(H19D,H19E,H19F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'