Controlling uranyl oxo group interactions to group 14 elements using polypyrrolic Schiff-base macrocyclic ligands.
Bell, Nicola L.; Arnold, Polly L.; Love, Jason B.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15902–15909; doi:10.1039/c6dt01948j

data_7039737
_publ_section_title
;
 Controlling uranyl oxo group interactions to group 14 elements using
 polypyrrolic Schiff-base macrocyclic ligands.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15902
_journal_page_last               15909
_journal_paper_doi               10.1039/c6dt01948j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C46 H48 N8 O3 Pb U'
_chemical_formula_sum            'C46 H48 N8 O3 Pb U'
_chemical_formula_weight         1206.14
_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   geom
_audit_creation_date             2016-03-24
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
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_audit_update_record
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2016-06-17 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                106.269(2)
_cell_angle_beta                 97.424(2)
_cell_angle_gamma                101.336(2)
_cell_formula_units_Z            2
_cell_length_a                   12.9064(4)
_cell_length_b                   14.3173(3)
_cell_length_c                   17.8924(5)
_cell_measurement_reflns_used    21989
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.7530
_cell_measurement_theta_min      3.5270
_cell_volume                     3051.71(15)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details
;
  1 omega  -41.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277   38.0000    0.0000 93

  2 omega  -25.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -99.0000  150.0000 47

  3 omega  -48.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277   26.0000  -45.7048 101

  4 omega  -25.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -99.0000  -30.0000 47

  5 omega  -25.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -99.0000   60.0000 47

  6 omega  -89.00    4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -38.0000 -180.0000 93

  7 omega  -87.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -57.0000  150.0000 87

  8 omega    2.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465   57.0000  120.0000 87

  9 omega  -50.00   43.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -38.0000  -30.0000 93

 10 omega  -48.00   39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -57.0000  -60.0000 87

 11 omega  -41.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277   38.0000 -180.0000 93

 12 omega  -87.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -57.0000  -30.0000 87

 13 omega  -93.00  -32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  179.0000  -30.0000 61

 14 omega  -25.00   28.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -99.0000 -120.0000 53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0219981000
_diffrn_orient_matrix_UB_12      -0.0072042000
_diffrn_orient_matrix_UB_13      -0.0349302000
_diffrn_orient_matrix_UB_21      -0.0516558000
_diffrn_orient_matrix_UB_22      -0.0268729000
_diffrn_orient_matrix_UB_23      -0.0232159000
_diffrn_orient_matrix_UB_31      -0.0107071000
_diffrn_orient_matrix_UB_32      0.0453729000
_diffrn_orient_matrix_UB_33      -0.0037728000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29521
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.172
_diffrn_reflns_theta_min         2.913
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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_density_diffrn    1.313
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.3978
_exptl_crystal_size_mid          0.2668
_exptl_crystal_size_min          0.0297
_refine_diff_density_max         4.381
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1144
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_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^)+(0.0954P)^2^+26.8616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1814
_refine_ls_wR_factor_ref         0.2039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20366
_reflns_number_total             29521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01948j2.cif
_cod_data_source_block           UO2PbLMethf
_cod_depositor_comments
'Adding full bibliography for 7039733--7039741.cif.'
_cod_database_code               7039737
_chemical_oxdiff_formula         'C60 H70 N8 O4 U Pb'
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7028(9) 0.2972(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C43-C42
 1.39 with sigma of 0.02
 C44-C45
 1.39 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C42 \\sim O3 \\sim C45 \\sim C44 \\sim C43: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C12 \\sim C11 \\sim N4: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N4 \\sim C12 \\sim C11: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
5. Rigid body (RIGU) restrains
 C43, C42, O3, C45, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C12, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C42(H42A,H42B), C44(H44A,H44B), C43(H43A,H43B)
6.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C32(H32), C12(H12), C1(H1), C24(H24), C10(H10), C23(H23), C4(H4),
 C3(H3), C9(H9), C39(H39), C34(H34), C30(H30), C29(H29), C14(H14), C19(H19)
6.c Idealised Me refined as rotating group:
 C017(H01A,H01B,H01C), C7(H7A,H7B,H7C), C36(H36A,H36B,H36C), C27(H27A,H27B,
 H27C), C38(H38A,H38B,H38C), C18(H18A,H18B,H18C), C6(H6A,H6B,H6C), C16(H16A,
 H16B,H16C)
;
_shelx_res_checksum              66214
_shelx_fab_checksum              5723
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'