Neptunyl(VI) centred visible LMCT emission directly observable in the presence of uranyl(VI)
Sean D. Woodall; Adam N. Swinburne; Nidhu lal Banik; Andrew Kerridge; Poppy Di Pietro; Christian Adam; Peter Kaden; Louise S. Natrajan; Chem.Commun. 51 (2015) 5402–; doi:10.1039/C4cc08718F

data_7116777
_publ_section_title
;
 Neptunyl(VI) centred visible LMCT emission directly observable in the
 presence of uranyl(VI)
;
_journal_name_full               Chem.Commun.
_journal_page_first              5402
_journal_paper_doi               10.1039/C4cc08718F
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C66 H55 N2 O7 P5 U, C H2 Cl2'
_chemical_formula_sum            'C67 H57 Cl2 N2 O7 P5 U'
_chemical_formula_weight         1465.92
_chemical_name_common            '[U(TPIP)2Ph3PO)'
_chemical_name_systematic        2
_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     iterative
_audit_creation_date             2014-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.21 svn.r3092 for OlexSys, GUI svn.r4949)
;
_audit_update_record
;
2014-12-13 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.334(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7808(5)
_cell_length_b                   23.6970(7)
_cell_length_c                   26.1815(8)
_cell_measurement_reflns_used    9052
_cell_measurement_temperature    101.8(3)
_cell_measurement_theta_max      27.8420
_cell_measurement_theta_min      2.8714
_cell_volume                     6042.0(4)
_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
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction
'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, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101.8(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3367
_diffrn_detector_type            'Sapphire2, large Be window'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega  -70.00  -36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1807 -179.0000   90.0000 34

  2 omega  -17.00  101.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1807   37.0000 -120.0000 118

  3 omega  -35.00   36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1807  -77.0000   60.0000 71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0037946000
_diffrn_orient_matrix_UB_12      0.0282585000
_diffrn_orient_matrix_UB_13      0.0089800000
_diffrn_orient_matrix_UB_21      0.0338476000
_diffrn_orient_matrix_UB_22      -0.0093205000
_diffrn_orient_matrix_UB_23      0.0236198000
_diffrn_orient_matrix_UB_31      0.0643365000
_diffrn_orient_matrix_UB_32      0.0033125000
_diffrn_orient_matrix_UB_33      -0.0101082000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22263
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.871
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57149
_exptl_absorpt_correction_type   multi-scan
_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) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       needle
_exptl_crystal_F_000             2920
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2'
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.473
_refine_diff_density_min         -2.377
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         12024
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+18.4858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10453
_reflns_number_total             12024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08718f2.cif
_cod_data_source_block           olsn147
_cod_database_code               7116777
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C44.67 H38.67 Cl1.33 N1.33 O4.67 P3.33 U0.67'
_reflns_odcompleteness_completeness 97.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 Cl2, C67, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B)
3.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C62(H62), C20(H20), C54(H54), C21(H21), C39(H39), C36(H36),
 C22(H22), C38(H38), C44(H44), C35(H35), C2(H2), C14(H14), C15(H15), C4(H4),
 C27(H27), C16(H16), C17(H17), C26(H26), C48(H48), C18(H18), C6(H6), C40(H40),
 C41(H41), C30(H30), C66(H66), C23(H23), C3(H3), C11(H11), C64(H64), C33(H33),
 C9(H9), C5(H5), C50(H50), C28(H28), C53(H53), C34(H34), C29(H29), C12(H12),
 C10(H10), C24(H24), C60(H60), C46(H46), C45(H45), C56(H56), C32(H32), C65(H65),
  C51(H51), C47(H47), C8(H8), C52(H52), C63(H63), C59(H59), C58(H58), C57(H57)
;
_shelx_res_checksum              71700
_olex2_date_sample_data_collection 2012-04-20
_olex2_submission_special_instructions 'No special instructions were received'