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_7039734
_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         'C68 H58 N10 O3 Pb U, 4(C5 H5 N)'
_chemical_formula_sum            'C88 H78 N14 O3 Pb U'
_chemical_formula_weight         1824.86
_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             2016-04-29
_audit_creation_method
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-17 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                97.6520(10)
_cell_angle_beta                 97.1410(10)
_cell_angle_gamma                110.0560(10)
_cell_formula_units_Z            2
_cell_length_a                   13.4766(2)
_cell_length_b                   14.4442(2)
_cell_length_c                   23.4695(3)
_cell_measurement_reflns_used    37782
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.9040
_cell_measurement_theta_min      3.3300
_cell_volume                     4181.79(11)
_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
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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 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -45.00   53.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518   38.0000  120.0000 98

  2 omega  -92.00    6.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518  -38.0000  -60.0000 98

  3 omega  -25.00   22.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518  -99.0000   90.0000 47

  4 omega  -50.00   51.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518   77.0000 -150.0000 101

  5 omega   -9.00   49.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   80.0000  -65.0000 58

  6 omega  -25.00   22.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518  -99.0000    0.0000 47

  7 omega  -49.00   11.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518  -80.0000  170.0000 60

  8 omega  -88.00    2.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518  -57.0000 -180.0000 90

  9 omega  -25.00   64.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -99.0000  120.0000 89

 10 omega   32.00   98.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518 -179.0000   30.0000 66

 11 omega    1.00   91.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   57.0000  120.0000 90

 12 omega  -25.00   64.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -99.0000    0.0000 89

 13 omega  -47.00   43.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -57.0000  -30.0000 90

 14 omega  -25.00   64.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -99.0000 -150.0000 89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0321813000
_diffrn_orient_matrix_UB_12      -0.0484791000
_diffrn_orient_matrix_UB_13      -0.0162281000
_diffrn_orient_matrix_UB_21      -0.0218355000
_diffrn_orient_matrix_UB_22      0.0219749000
_diffrn_orient_matrix_UB_23      -0.0211358000
_diffrn_orient_matrix_UB_31      0.0416551000
_diffrn_orient_matrix_UB_32      0.0006871000
_diffrn_orient_matrix_UB_33      -0.0158700000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_number            19171
_diffrn_reflns_point_group_measured_fraction_full 0.998
_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         2.867
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.000
_exptl_absorpt_correction_T_max  0.289
_exptl_absorpt_correction_T_min  0.094
_exptl_absorpt_correction_type   analytical
_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)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.3765
_exptl_crystal_size_mid          0.3244
_exptl_crystal_size_min          0.1829
_platon_squeeze_details
;
;
_refine_diff_density_max         1.918
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         19171
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+3.0009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15630
_reflns_number_total             19171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01948j2.cif
_cod_data_source_block           UO2PbLApyPY-O
_cod_depositor_comments
'Adding full bibliography for 7039733--7039741.cif.'
_cod_original_cell_volume        4181.79(10)
_cod_database_code               7039734
_chemical_oxdiff_formula         'C50 H60 N5 U O3 Pb'
_reflns_odcompleteness_completeness 99.86
_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 C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N11 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
N21 \\sim N12 \\sim C122 \\sim C123 \\sim C124 \\sim C125: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
N21 \\sim C131 \\sim C132 \\sim C133 \\sim C134 \\sim C135: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
N21 \\sim C151 \\sim N151 \\sim C153 \\sim C154 \\sim C155: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N11, C111, C112, C113, C114, C115
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N21, N12, C122, C123, C124, C125
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N21, C131, C132, C133, C134, C135
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N21, C151, N151, C153, C154, C155
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C4(H4A,H4B), C2(H2A,H2B), C33(H33A,H33B)
4.b Aromatic/amide H refined with riding coordinates:
 C154(H154), C17(H17), C47(H47), C39(H39), C57(H57), C54(H54), C8(H8),
 C115(H115), C43(H43), C52(H52), C36(H36), C41(H41), C10(H10), C14(H14),
 C25(H25), C27(H27), C56(H56), C46(H46), C18(H18), C112(H112), C153(H153),
 C12(H12), C7(H7), C23(H23), C64(H64), C28(H28), C37(H37), C132(H132), C68(H68),
  C133(H133), C123(H123), C111(H111), C60(H60), C59(H59), C121(H121),
 C113(H113), C65(H65), C21(H21), C51(H51), C50(H50), C63(H63), C22(H22),
 C125(H125), C152(H152), C122(H122), C131(H131), C67(H67), C66(H66), C42(H42),
 C124(H124), C13(H13), C61(H61), C62(H62), C134(H134), C151(H151), C155(H155),
 C114(H114), C135(H135)
4.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C34(H34A,H34B,H34C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'