Solid-state structural elucidation and electrochemical analysis of uranyl naphthylsalophen.
Niklas, Julie E.; Hardy, Emily E.; Gorden, Anne E. V.; Chemical communications (Cambridge, England) 54 (2018) 11693–11696; doi:10.1039/c8cc05242e

data_7122263
_publ_section_title
;
 Solid-state structural elucidation and electrochemical analysis of uranyl
 naphthylsalophen.
;
_journal_issue                   83
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11693
_journal_page_last               11696
_journal_paper_doi               10.1039/c8cc05242e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '2(C28 H20 N2 O5 U), 4(C H2 Cl2)'
_chemical_formula_sum            'C60 H48 Cl8 N4 O10 U2'
_chemical_formula_weight         1744.75
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-03-03 deposited with the CCDC.
2018-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.655(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4659(12)
_cell_length_b                   19.3294(14)
_cell_length_c                   22.2346(16)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    180
_cell_measurement_theta_max      25.628
_cell_measurement_theta_min      2.183
_cell_volume                     6368.1(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9970
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            74217
_diffrn_reflns_theta_full        25.7632
_diffrn_reflns_theta_max         25.76
_diffrn_reflns_theta_min         1.42
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.476
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.3403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1471 before and 0.0559 after correction. The Ratio of minimum to maximum transmission is 0.4566. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.8197
_exptl_crystal_description       block
_exptl_crystal_F_000             3269.1361
_exptl_crystal_recrystallization_method 'Slow diffusion of Hex into DCM'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.3260
_refine_diff_density_min         -1.9575
_refine_diff_density_rms         0.2631
_refine_ls_d_res_high            0.8176
_refine_ls_d_res_low             14.3146
_refine_ls_goodness_of_fit_ref   1.0941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    90
_refine_ls_number_parameters     759
_refine_ls_number_reflns         12168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0941
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+77.0629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -18
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -12
_reflns_number_gt                9916
_reflns_number_total             12168
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8cc05242e2.cif
_cod_data_source_block           UO2L
_cod_depositor_comments
'Adding full bibliography for 7122262--7122263.cif.'
_cod_database_code               7122263
_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 O(H,H) groups
2.a Rotating group:
 O4(H4a,H4b), O6(H6a,H6b)
2.b Secondary CH2 refined with riding coordinates:
 C0aa(H0aa,H0ab), C1aa(H1aa,H1ab), C2aa(H2aa,H2ab), C3aa(H3aa,H3ab)
2.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C28(H28), C21(H21), C20(H20), C19(H19), C18(H18), C9(H9), C10(H10),
 C23(H23), C24(H24), C25(H25), C26(H26), C13(H13), C14(H14), C15(H15), C16(H16),
  C47(H47), C48(H48), C58(H58), C57(H57), C56(H56), C55(H55), C36(H36),
 C35(H35), C51(H51), C52(H52), C53(H53), C54(H54), C40(H40), C39(H39), C38(H38),
  C37(H37), C3(H3), C6(H6), C41(H41), C44(H44)
;
_olex2_exptl_crystal_mounting_method
'a suitable crystal as selected and mounted on a glass fiber usnig paratone-n oil'
_olex2_submission_special_instructions 'No special instructions were received'