Inner-sphere vs. outer-sphere reduction of uranyl supported by a redox-active, donor-expanded dipyrrin.
Pankhurst, James R.; Bell, Nicola L.; Zegke, Markus; Platts, Lucy N.; Lamfsus, Carlos Alvarez; Maron, Laurent; Natrajan, Louise S.; Sproules, Stephen; Arnold, Polly L.; Love, Jason B.; Chemical science 8 (2017) 108–116; doi:10.1039/c6sc02912d

data_1544406
_publ_section_title
;
 Inner-sphere vs. outer-sphere reduction of uranyl supported by a
 redox-active, donor-expanded dipyrrin.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              108
_journal_page_last               116
_journal_paper_doi               10.1039/c6sc02912d
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety    'C25 H24 Cl F5 N4 O2 U, C10 H10 Co, 0.5(C4 H8 O)'
_chemical_formula_sum            'C37 H38 Cl Co F5 N4 O2.5 U'
_chemical_formula_weight         1006.12
_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             2016-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-09-30 deposited with the CCDC.
2016-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.247(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.0945(2)
_cell_length_b                   28.2241(4)
_cell_length_c                   19.2594(3)
_cell_measurement_reflns_used    32843
_cell_measurement_temperature    170
_cell_measurement_theta_max      29.4340
_cell_measurement_theta_min      3.2910
_cell_volume                     8440.7(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)'
_diffrn_ambient_temperature      170.0
_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 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -88.00  10.00   0.50   25.00    --  -18.84 -77.00  90.00  196
  2  \w    -93.00 -34.00   0.50   25.00    --  -18.84-179.00  90.00  118
  3  \w    -25.00  22.00   0.50   25.00    --  -18.84 -99.00 -30.00   94
  4  \w    -89.00   3.00   0.50   25.00    --  -18.84 -38.00 -30.00  184
  5  \w     34.00  95.00   0.50   25.00    --   20.40 179.00 -30.00  122
  6  \w    -87.00   0.00   0.50   25.00    --  -18.84 -57.00-120.00  174
  7  \w    -48.00  39.00   0.50   25.00    --   20.40 -57.00 -30.00  174
  8  \w    -25.00  14.00   0.50   25.00    --   20.40 -99.00 150.00   78
  9  \w    -48.00  39.00   0.50   25.00    --   20.40 -57.00  30.00  174
;
_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      -0.0445080000
_diffrn_orient_matrix_UB_12      0.0002830000
_diffrn_orient_matrix_UB_13      -0.0180763000
_diffrn_orient_matrix_UB_21      0.0024326000
_diffrn_orient_matrix_UB_22      -0.0241043000
_diffrn_orient_matrix_UB_23      -0.0097038000
_diffrn_orient_matrix_UB_31      -0.0100268000
_diffrn_orient_matrix_UB_32      -0.0070975000
_diffrn_orient_matrix_UB_33      0.0321819000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            117037
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.926
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.346
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.757
_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    1.583
_exptl_crystal_description       plate
_exptl_crystal_F_000             3912
_exptl_crystal_size_max          0.506
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.646
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         19317
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+19.6817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16343
_reflns_number_total             19317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc02912d2.cif
_cod_data_source_block           p16174_sq
_cod_depositor_comments
;
 Adding full bibliography for 1544404--1544406.cif.

2019-02-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C74 H76 Cl2 Co2 F10 N8 O5 U2'
_cod_original_formula_weight         2012.24
_cod_original_formula_moiety
'2(C25 H24 Cl F5 N4 O2 U), 2(C10 H10 Co), C4 H8 O'
_cod_original_formula_units_Z            4
_cod_database_code               1544406
_chemical_oxdiff_formula         'C25 H24 N4 O2 Co U Cl'
_reflns_odcompleteness_completeness 99.81
_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
C103 \\sim C104 \\sim C105 \\sim O101 \\sim C102: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C104, C103, C102, O101, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C27(H27), C31(H31), C35(H35)
4.b Secondary CH2 refined with riding coordinates:
 C104(H10A,H10B), C103(H10C,H10D), C105(H10E,H10F), C102(H10G,H10H)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C21(H21), C55(H55), C58(H58), C7(H7), C18(H18), C71(H71), C57(H57),
 C19(H19), C69(H69), C8(H8), C68(H68), C84(H84), C82(H82), C85(H85), C83(H83),
 C30(H30), C81(H81), C26(H26), C28(H28), C33(H33), C29(H29), C34(H34), C32(H32),
  C80(H80), C77(H77), C78(H78), C79(H79), C76(H76)
4.d Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C51(H51A,H51B,H51C), C1(H1A,H1B,H1C), C53(H53A,H53B,
 H53C), C74(H74A,H74B,H74C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C73(H73A,H73B,
 H73C), C75(H75A,H75B,H75C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C24(H24A,
 H24B,H24C)
;
_shelx_fab_checksum              92618
_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 1.587
_oxdiff_exptl_absorpt_empirical_full_min 0.817