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_7039733
_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 Ge N8 O4 U, C4 H8 O'
_chemical_formula_sum            'C70 H72 Ge N8 O5 U'
_chemical_formula_weight         1415.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-04-28
_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                 98.0274(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.44279(12)
_cell_length_b                   22.2890(2)
_cell_length_c                   24.0677(2)
_cell_measurement_reflns_used    35068
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.0840
_cell_measurement_theta_min      3.4100
_cell_volume                     6078.28(10)
_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    -25.00  22.00   1.00   27.50    --  -18.53 -99.00 -60.00   47
  2  \w    -37.00  50.00   1.00   27.50    --  -18.53  57.00-150.00   87
  3  \w      2.00  89.00   1.00   27.50    --   20.25  57.00  90.00   87
  4  \w    -48.00  39.00   1.00   27.50    --   20.25 -57.00 -90.00   87
  5  \w     -2.00  91.00   1.00   27.50    --   20.25  38.00  60.00   93
  6  \w    -25.00  61.00   1.00   27.50    --   20.25 -99.00 150.00   86
  7  \w      2.00  89.00   1.00   27.50    --   20.25  57.00-120.00   87
  8  \w     34.00  94.00   1.00   27.50    --   20.25 179.00-180.00   60
  9  \w    -69.00 -38.00   1.00   27.50    --  -18.53 117.00 146.56   31
 10  \w      2.00  89.00   1.00   27.50    --   20.25  57.00-180.00   87
 11  \w    -25.00  61.00   1.00   27.50    --   20.25 -99.00 -30.00   86
 12  \w    -25.00  61.00   1.00   27.50    --   20.25 -99.00  30.00   86
 13  \w      2.00  89.00   1.00   27.50    --   20.25  57.00 -60.00   87
 14  \w     34.00  94.00   1.00   27.50    --   20.25 179.00 120.00   60
;
_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      -0.0471954000
_diffrn_orient_matrix_UB_12      -0.0066594000
_diffrn_orient_matrix_UB_13      0.0152212000
_diffrn_orient_matrix_UB_21      0.0408237000
_diffrn_orient_matrix_UB_22      -0.0039527000
_diffrn_orient_matrix_UB_23      0.0247505000
_diffrn_orient_matrix_UB_31      -0.0049555000
_diffrn_orient_matrix_UB_32      0.0308652000
_diffrn_orient_matrix_UB_33      0.0064521000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            139112
_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         2.801
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.215
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.838
_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    1.547
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.105
_refine_diff_density_max         1.324
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         13933
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0260P)^2^+8.0902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11376
_reflns_number_total             13933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01948j2.cif
_cod_data_source_block           UO2GeLAthf
_cod_depositor_comments
'Adding full bibliography for 7039733--7039741.cif.'
_cod_original_cell_volume        6078.29(10)
_cod_database_code               7039733
_chemical_oxdiff_formula         'C66 H64 N8 O4 Ge U'
_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 C80 \\sim C82 \\sim C81 \\sim C83: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 O5, C80, C82, C81, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=1-FVAR(1)
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C70(H70A,H70B), C33(H33A,H33B), C63(H63A,H63B), C62(H62A,H62B), C80(H80A,
 H80B), C4(H4A,H4B), C73(H73A,H73B), C71(H71A,H71B), C82(H82A,H82B), C2A(H2AA,
 H2AB), C81(H81A,H81B), C31(H31A,H31B), C60(H60A,H60B), C72(H72A,H72B),
 C83(H83A,H83B), C61(H61A,H61B), C2B(H2BA,H2BB)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C46(H46), C25(H25), C43(H43), C39(H39), C23(H23), C42(H42),
 C22(H22), C52(H52), C27(H27), C28(H28), C56(H56), C20(H20), C14(H14), C54(H54),
  C10(H10), C13(H13), C36(H36), C12(H12), C49(H49), C51(H51), C41(H41),
 C50(H50), C7(H7), C8(H8), C21(H21), C57(H57), C37(H37)
5.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C5(H5A,H5B,H5C), C3A(H3AA,H3AB,
 H3AC), C3B(H3BA,H3BB,H3BC)
;
_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 1.194
_oxdiff_exptl_absorpt_empirical_full_min 0.880