Effects of preorganization in the chelation of UO22+by hydroxamate ligands: cyclic PIPO−vs.linear NMA−
Sornosa-Ten, Alejandra; Jewula, Pawel; Fodor, Tamas; Brandès, Stéphane; Sladkov, Vladimir; Rousselin, Yoann; Stern, Christine; Chambron, Jean-Claude; Meyer, Michel; New Journal of Chemistry 42 (2018) 7765–; doi:10.1039/C8NJ00166A

data_7057014
_publ_section_title
;
 Effects of preorganization in the chelation of UO22+by hydroxamate
 ligands: cyclic PIPO&#x2212;vs.linear NMA&#x2212;
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7765
_journal_paper_doi               10.1039/C8NJ00166A
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C10 H18 N2 O7 U'
_chemical_formula_sum            'C10 H18 N2 O7 U'
_chemical_formula_weight         516.29
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-09
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-10 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.610(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.472(3)
_cell_length_b                   27.710(11)
_cell_length_c                   8.310(3)
_cell_measurement_reflns_used    8390
_cell_measurement_temperature    115(1)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.62
_cell_volume                     1394.9(10)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_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      115(1)
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            31311
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.673
_diffrn_reflns_theta_min         1.470
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.669
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1712 before and 0.0624 after correction.
The Ratio of minimum to maximum transmission is 0.3056.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.458
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_recrystallization_method
'The material was recrystallised from water by slow evaporation'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.013
_refine_diff_density_min         -2.351
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.309
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.309
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+7.9726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3156
_reflns_number_total             3243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj00166a2.cif
_cod_data_source_block           '[UO2(PIPO)2(H2O)]'
_cod_depositor_comments          'Adding full bibliography for 7057014.cif.'
_cod_original_cell_volume        1394.9(9)
_cod_database_code               7057014
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.242
_shelx_estimated_absorpt_t_min   0.089
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Everything fixed:
 H4A, H4B
2.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C5A(H5AA,H5AB), C4A(H4AA,H4AB), C3A(H3AA,H3AB), C3(H3A,H3B),
 C4(H4C,H4D), C5(H5A,H5B), C1(H1A,H1B)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_special_instructions 'No special instructions were received'