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_7122262
_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_absolute_configuration unk
_chemical_formula_moiety         'C H2 Cl2, C28 H20 N2 O2'
_chemical_formula_sum            'C29 H22 Cl2 N2 O2'
_chemical_formula_weight         501.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_audit_update_record
;
2016-12-20 deposited with the CCDC.
2018-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1378(10)
_cell_length_b                   16.682(2)
_cell_length_c                   20.056(3)
_cell_measurement_reflns_used    3361
_cell_measurement_temperature    180.45
_cell_measurement_theta_max      23.052
_cell_measurement_theta_min      2.369
_cell_volume                     2388.1(6)
_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., 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.45
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9985
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17603
_diffrn_reflns_theta_full        28.6982
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0961 before and 0.0560 after correction. The Ratio of minimum to maximum transmission is 0.8052. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.3945
_exptl_crystal_description       prism
_exptl_crystal_F_000             1041.5971
_exptl_crystal_recrystallization_method 'Slow evaporation of a DCM solution'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.6454
_refine_diff_density_min         -0.6401
_refine_diff_density_rms         0.0920
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.10(7)
_refine_ls_d_res_high            0.7400
_refine_ls_d_res_low             10.0278
_refine_ls_goodness_of_fit_ref   1.0365
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    42
_refine_ls_number_parameters     318
_refine_ls_number_reflns         6177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0365
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.1921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.997
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              27
_reflns_limit_l_min              -26
_reflns_number_gt                4545
_reflns_number_total             6177
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8cc05242e2.cif
_cod_data_source_block           Emily073115_0m
_cod_depositor_comments
'Adding full bibliography for 7122262--7122263.cif.'
_cod_database_code               7122262
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C29(H29a,H29b)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C11(H11), C18(H18), C24(H24), C23(H23), C3(H3), C2(H2a),
 C8(H8), C7(H7), C13(H13), C14(H14), C15(H15), C16(H16), C26(H26), C27(H27),
 C22(H22), C21(H21), N1(H1)
;
_olex2_exptl_crystal_mounting_method
'Single crystal was mounted on a glass fibre in Paratone-N oil for data collection.'
_olex2_submission_special_instructions 'No special instructions were received'