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_7039735
_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         'C52 H50 N10 Pb2, 2(C5 H5 N)'
_chemical_formula_sum            'C62 H60 N12 Pb2'
_chemical_formula_weight         1387.60
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-07
_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                90.548(2)
_cell_angle_beta                 90.690(2)
_cell_angle_gamma                99.117(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5029(3)
_cell_length_b                   13.3149(3)
_cell_length_c                   17.9962(6)
_cell_measurement_reflns_used    8668
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.0720
_cell_measurement_theta_min      3.3070
_cell_volume                     2721.10(13)
_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 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
  1 omega  -24.00   19.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -99.0000  -60.0000 43

  2 omega  -16.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -99.0000 -150.0000 40

  3 omega  -44.00   37.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0277  -57.0000 -180.0000 81

  4 omega    0.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0277   57.0000   60.0000 86

  5 omega    4.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0277   57.0000  150.0000 52

  6 omega  -54.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0277  -19.0000 -120.0000 110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0515230000
_diffrn_orient_matrix_UB_12      0.0329026000
_diffrn_orient_matrix_UB_13      0.0120627000
_diffrn_orient_matrix_UB_21      -0.0166884000
_diffrn_orient_matrix_UB_22      -0.0085507000
_diffrn_orient_matrix_UB_23      0.0375083000
_diffrn_orient_matrix_UB_31      0.0311097000
_diffrn_orient_matrix_UB_32      -0.0419001000
_diffrn_orient_matrix_UB_33      0.0012290000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23523
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.869
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.232
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.564
_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    1.694
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.4602
_exptl_crystal_size_mid          0.2091
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.703
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         11982
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9191
_reflns_number_total             11982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01948j2.cif
_cod_data_source_block           Pb2LMe
_cod_depositor_comments
'Adding full bibliography for 7039733--7039741.cif.'
_cod_database_code               7039735
_chemical_oxdiff_formula         'C70 H70 N2 O2 Pb U'
_reflns_odcompleteness_completeness 96.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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
2. Restrained distances
 C70-N69
 1.36 with sigma of 0.02
 N69-C74
 1.36 with sigma of 0.02
 N69-C70 = N69-C74
 1.33 with sigma of 0.02
 C72-C71 = C73-C72
 1.36 with sigma of 0.02
 C71-C70 = C74-C73
 1.35 with sigma of 0.02
 C71-C70 = C74-C73
 1.35 with sigma of 0.01
 N69-C74 = N69-C70
 1.33 with sigma of 0.01
 C72-C71 = C73-C72
 1.36 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C71 \\sim C70 \\sim N69 \\sim C74 \\sim C73 \\sim C72: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C72) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(N69)
\\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C72) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(N69)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C71, C70, N69, C74, C73, C72
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Aromatic/amide H refined with riding coordinates:
 C37(H37), C62(H62), C42(H42), C58(H58), C9(H9), C34(H34), C20(H20), C12(H12),
 C45(H45), C30(H30), C61(H61), C17(H17), C31(H31), C60(H60), C6(H6), C59(H59),
 C22(H22), C5(H5), C47(H47), C48(H48), C23(H23), C56(H56), C64(H64), C65(H65),
 C66(H66), C67(H67), C68(H68), C52(H52), C53(H53), C55(H55), C54(H54), C70(H70),
  C71(H71), C72(H72), C73(H73), C74(H74)
5.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C41(H41A,H41B,H41C),
 C14(H14A,H14B,H14C), C39(H39A,H39B,H39C), C15(H15A,H15B,H15C), C28(H28A,H28B,
 H28C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'