An Example of Unusual Pyridine Donor Schiff Base Uranyl (UO22+) Complexes
Hardy, Emily Elizabeth; Wyss, Kevin M.; Eddy, Madeleine A.; Gorden, Anne E. V.; Chem. Commun.  (2017) –; doi:10.1039/C7CC02747H

data_7120066
_publ_section_title
;
 An Example of Unusual Pyridine Donor Schiff Base Uranyl (UO22+) Complexes
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02747H
_journal_year                    2017
_chemical_formula_moiety         'C37 H49 N3 O4 U, C2 H3 N'
_chemical_formula_sum            'C40 H52 N3 O4 U'
_chemical_formula_weight         876.87
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2839 for OlexSys, GUI svn.r4713)
;
_audit_update_record
;
2016-03-17 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.9974(3)
_cell_length_b                   23.5111(5)
_cell_length_c                   23.6244(5)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.36
_cell_measurement_theta_min      2.42
_cell_volume                     7774.7(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            93148
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.527
_diffrn_reflns_theta_min         1.693
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.217
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS was used for absorption correction. wR2(int) was 0.1453 before and 0.0458 after correction. The Ratio of minimum to maximum transmission is 0.5149. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       plate
_exptl_crystal_F_000             3496
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         11887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0263P)^2^+6.9842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8605
_reflns_number_total             11887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02747h2.cif
_cod_data_source_block           Emily021716_1_0m
_cod_database_code               7120066
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H16A(0.036) H16B(0.036) H15(0.032) H13(0.035) H7(0.035)
 H4A(0.063) H4B(0.063) H4C(0.063) H6A(0.063) H6B(0.063) H6C(0.063) H5A(0.05)
 H5B(0.05) H5C(0.05) H10A(0.146) H10B(0.146) H10C(0.146) H9A(0.14) H9B(0.14)
 H9C(0.14) H11A(0.116) H11B(0.116) H11C(0.116) H18(0.046) H19(0.052) H20(0.044)
 H22A(0.038) H22B(0.038) H23(0.033) H31(0.036) H29A(0.076) H29B(0.076)
 H29C(0.076) H28A(0.07) H28B(0.07) H28C(0.07) H30A(0.065) H30B(0.065)
 H30C(0.065) H25(0.034) H36A(0.081) H36B(0.081) H36C(0.081) H34A(0.1) H34B(0.1)
 H34C(0.1) H35A(0.092) H35B(0.092) H35C(0.092) H38A(0.117) H38B(0.117)
 H38C(0.117)
 Fixed X: H16A(0.8551) H16B(0.9042) H15(0.8066) H13(0.7279) H7(0.4425)
 H4A(0.3874) H4B(0.3177) H4C(0.4304) H6A(0.3151) H6B(0.2488) H6C(0.3153)
 H5A(0.4336) H5B(0.32) H5C(0.3796) H10A(0.5254) H10B(0.4575) H10C(0.5463)
 H9A(0.591) H9B(0.4847) H9C(0.5533) H11A(0.6825) H11B(0.7091) H11C(0.7286)
 H18(1.0479) H19(1.0987) H20(0.9894) H22A(0.7804) H22B(0.8244) H23(0.7181)
 H31(0.3754) H29A(0.3496) H29B(0.3968) H29C(0.4064) H28A(0.5831) H28B(0.5726)
 H28C(0.6406) H30A(0.5496) H30B(0.4881) H30C(0.4355) H25(0.6387) H36A(0.398)
 H36B(0.3188) H36C(0.4259) H34A(0.2792) H34B(0.2459) H34C(0.2088) H35A(0.264)
 H35B(0.2991) H35C(0.3714) H38A(0.582) H38B(0.6637) H38C(0.5589)
 Fixed Y: H16A(0.2794) H16B(0.2955) H15(0.3023) H13(0.3169) H7(0.3251)
 H4A(0.4163) H4B(0.3858) H4C(0.387) H6A(0.2895) H6B(0.3263) H6C(0.3574)
 H5A(0.2766) H5B(0.2809) H5C(0.2416) H10A(0.3662) H10B(0.3613) H10C(0.4041)
 H9A(0.2325) H9B(0.2574) H9C(0.2602) H11A(0.3305) H11B(0.3672) H11C(0.3001)
 H18(0.3476) H19(0.4338) H20(0.4947) H22A(0.5126) H22B(0.4969) H23(0.4702)
 H31(0.369) H29A(0.4072) H29B(0.421) H29C(0.4655) H28A(0.4646) H28B(0.4197)
 H28C(0.4058) H30A(0.3132) H30B(0.3288) H30C(0.3153) H25(0.4345) H36A(0.2818)
 H36B(0.2995) H36C(0.3225) H34A(0.3153) H34B(0.3805) H34C(0.3385) H35A(0.4015)
 H35B(0.446) H35C(0.4249) H38A(0.4386) H38B(0.4774) H38C(0.5028)
 Fixed Z: H16A(0.2688) H16B(0.3281) H15(0.395) H13(0.4817) H7(0.4885)
 H4A(0.3736) H4B(0.3292) H4C(0.318) H6A(0.4449) H6B(0.4036) H6C(0.4491)
 H5A(0.3125) H5B(0.3185) H5C(0.3611) H10A(0.6264) H10B(0.5722) H10C(0.5715)
 H9A(0.5639) H9B(0.5674) H9C(0.6216) H11A(0.6262) H11B(0.5714) H11C(0.5721)
 H18(0.2872) H19(0.2476) H20(0.2057) H22A(0.2185) H22B(0.1578) H23(0.1033)
 H31(0.0408) H29A(-0.0417) H29B(-0.1019) H29C(-0.0509) H28A(-0.0629) H28B(-
 0.1135) H28C(-0.0608) H30A(-0.0441) H30B(-0.099) H30C(-0.0404) H25(0.0264)
 H36A(0.1632) H36B(0.2087) H36C(0.2149) H34A(0.0918) H34B(0.0914) H34C(0.14)
 H35A(0.214) H35B(0.1672) H35C(0.2153) H38A(0.4301) H38B(0.4025) H38C(0.4122)
;
_shelx_res_checksum              16788
_shelx_hkl_checksum              9537
_olex2_submission_special_instructions 'No special instructions were received'