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_7039741
_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         'C66 H64 N8 O4 Pb U, C4 H8 O'
_chemical_formula_sum            'C70 H72.5 N8 O5 Pb U'
_chemical_formula_weight         1551.08
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-29
_audit_creation_method
;
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
_cell_angle_beta                 97.5987(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.7520(2)
_cell_length_b                   22.2812(2)
_cell_length_c                   24.1927(3)
_cell_measurement_reflns_used    64694
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.2540
_cell_measurement_theta_min      3.1400
_cell_volume                     12156.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_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 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -88.00  10.00   1.00   30.00    --  -18.68 -77.00  60.00   98
  2  \w    -50.00  53.00   1.00   30.00    --  -18.68  23.00 -51.96  103
  3  \w    -25.00  22.00   1.00   30.00    --  -18.68 -99.00 -60.00   47
  4  \w    -25.00  22.00   1.00   30.00    --  -18.68 -99.00 -90.00   47
  5  \w    -37.00  50.00   1.00   30.00    --  -18.68  57.00 -90.00   87
  6  \w    -47.00  51.00   1.00   30.00    --  -18.68  77.00-180.00   98
  7  \w    -50.00  43.00   1.00   30.00    --   20.25 -38.00 -60.00   93
  8  \w     34.00  94.00   1.00   30.00    --   20.25 179.00 120.00   60
  9  \w    -89.00   4.00   1.00   30.00    --  -18.68 -38.00-150.00   93
 10  \w    -25.00  22.00   1.00   30.00    --  -18.68 -99.00 120.00   47
 11  \w    -87.00   0.00   1.00   30.00    --  -18.68 -57.00 -60.00   87
 12  \w    -93.00 -34.00   1.00   30.00    --  -18.68-179.00   0.00   59
 13  \w    -87.00   0.00   1.00   30.00    --  -18.68 -57.00 150.00   87
 14  \w    -16.00  66.00   1.00   30.00    --   20.25-109.00-170.00   82
 15  \w    -25.00  61.00   1.00   30.00    --   20.25 -99.00  30.00   86
 16  \w    -67.00 -36.00   1.00   30.00    --  -18.68 114.00  12.14   31
 17  \w    -76.00   0.00   1.00   30.00    --  -18.68 129.00-162.79   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0287241000
_diffrn_orient_matrix_UB_12      0.0011547000
_diffrn_orient_matrix_UB_13      -0.0154739000
_diffrn_orient_matrix_UB_21      0.0126487000
_diffrn_orient_matrix_UB_22      0.0076641000
_diffrn_orient_matrix_UB_23      -0.0243182000
_diffrn_orient_matrix_UB_31      0.0020727000
_diffrn_orient_matrix_UB_32      -0.0308801000
_diffrn_orient_matrix_UB_33      -0.0066151000
_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     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            332738
_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         27.485
_diffrn_reflns_theta_min         2.871
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.486
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
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_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       block
_exptl_crystal_F_000             6100
_exptl_crystal_size_max          0.555
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.690
_refine_diff_density_min         -1.869
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1539
_refine_ls_number_reflns         27853
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.003
_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          0.1180
_refine_ls_wR_factor_ref         0.1420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20316
_reflns_number_total             27853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01948j2.cif
_cod_data_source_block           UO2PbLAthf
_cod_depositor_comments
'Adding full bibliography for 7039733--7039741.cif.'
_cod_original_formula_sum        'C70 H72.50 N8 O5 Pb U'
_cod_database_code               7039741
_chemical_oxdiff_formula         'C66 H64 N8 O4 U Pb'
_reflns_odcompleteness_completeness 99.83
_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
O5 \\sim C504 \\sim C503 \\sim C502 \\sim C501: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
C554 \\sim C553 \\sim C552 \\sim C551 \\sim O55: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
C531 \\sim C532 \\sim C533 \\sim C534 \\sim O53: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
O3 \\sim C301 \\sim C302 \\sim C303 \\sim C304: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 C504, C503, C502, C501, O5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C554, C553, C552, C551, O55
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O53, C531, C532, C533, C534
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3, C301, C302, C303, C304
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C534(H53A,H53B), C541(H54A,H54B), C401(H40A,H40B), C304(H30A,H30B), C542(H54C,
 H54D), C402(H40C,H40D), C404(H40E,H40F), C301(H30C,H30D), C92(H92A,H92B),
 C543(H54E,H54F), C90(H90A,H90B), C544(H54G,H54H), C31(H31A,H31B), C531(H53C,
 H53D), C403(H40G,H40H), C4(H4A,H4B), C33(H33A,H33B), C61(H61A,H61B), C2(H2A,
 H2B), C63(H63A,H63B), C551(H55A,H55B), C501(H50A,H50B), C553(H55C,H55D),
 C533(H53E,H53F), C552(H55E,H55F), C532(H53G,H53H), C303(H30E,H30F), C302(H30G,
 H30H), C554(H55G,H55H), C503(H50C,H50D), C502(H50E,H50F), C504(H50G,H50H)
4.b Aromatic/amide H refined with riding coordinates:
 C84(H84), C54(H54), C46(H46), C76(H76), C17(H17), C113(H113), C105(H105),
 C25(H25), C86(H86), C23(H23), C81(H81), C39(H39), C7(H7), C52(H52), C12(H12),
 C49(H49), C82(H82), C56(H56), C27(H27), C22(H22), C79(H79), C87(H87), C95(H95),
  C69(H69), C111(H111), C98(H98), C72(H72), C28(H28), C109(H109), C108(H108),
 C57(H57), C20(H20), C80(H80), C37(H37), C8(H8), C96(H96), C115(H115), C73(H73),
  C101(H101), C21(H21), C10(H10), C71(H71), C43(H43), C50(H50), C41(H41),
 C102(H102), C116(H116), C100(H100), C14(H14), C36(H36), C67(H67), C42(H42),
 C110(H110), C51(H51), C13(H13), C66(H66)
4.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C91(H91A,H91B,H91C), C34(H34A,H34B,H34C), C93(H93A,H93B,
 H93C), C62(H62A,H62B,H62C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C64(H64A,H64B,
 H64C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.629
_oxdiff_exptl_absorpt_empirical_full_min 0.665