2,6-Diiminopiperidin-1-ol: an overlooked motif relevant to uranyl and transition metal binding on poly(amidoxime) adsorbents.
Kennedy, Zachary C.; Cardenas, Allan Jay P.; Corbey, Jordan F.; Warner, Marvin G.; Chemical communications (Cambridge, England) 52 (2016) 8802–8805; doi:10.1039/c6cc02488b

data_7124627
_publ_section_title
;
 2,6-Diiminopiperidin-1-ol: an overlooked motif relevant to uranyl and
 transition metal binding on poly(amidoxime) adsorbents.
;
_journal_issue                   57
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8802
_journal_page_last               8805
_journal_paper_doi               10.1039/c6cc02488b
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C15 H36 N9 Ni3 O9, 3(Cl), 4(H2 O)'
_chemical_formula_sum            'C15 H44 Cl3 N9 Ni3 O13'
_chemical_formula_weight         841.07
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-18 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.774(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1605(12)
_cell_length_b                   13.4761(10)
_cell_length_c                   14.8097(11)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.342
_cell_measurement_theta_min      2.556
_cell_volume                     3180.5(4)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  Bruker-APEXII-CCD
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32907
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         1.98
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.081
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0827 before and 0.0403 after correction.
The Ratio of minimum to maximum transmission is 0.8595.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.371
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7953
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+5.2250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                7035
_reflns_number_total             7953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc02488b2.cif
_cod_data_source_block           fuls
_cod_database_code               7124627
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1AB-H1AD
 0.84 with sigma of 0.01
 O1AB-H1AC
 0.84 with sigma of 0.01
 O1AA-H1AA
 0.84 with sigma of 0.01
 O1AB-O33
 2.909 with sigma of 0.01
 H1AD-H30A
 2.289 with sigma of 0.01
 H1AD-H1AA
 0.543 with sigma of 0.01
 H1AD-H1AC
 1.34 with sigma of 0.02
3. Others
 Sof(O1AB)=Sof(H1AC)=Sof(H1AD)=1-FVAR(1)
 Sof(O1AA)=Sof(H1AA)=Sof(H1AB)=FVAR(1)
 Sof(H32C)=Sof(H32D)=Sof(H38C)=Sof(H38D)=Sof(C36A)=Sof(H36C)=Sof(H36D)=1-FVAR(2)
 Sof(H32A)=Sof(H32B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H38A)=Sof(H38B)=FVAR(2)
4.a Free rotating group:
 O19(H19A,H19B), O33(H33A,H33B), O0AA(H0AA,H0AB), O1AA(H1AA,H1AB), O1AB(H1AC,
 H1AD)
4.b Rotating group:
 O2(H2A,H2B), O4(H4A,H4B), O5(H5A,H5B), O7(H7A,H7B), O12(H12A,H12B), O14(H14A,
 H14B)
4.c Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C32(H32C,H32D), C34(H34A,H34B), C36(H36A,H36B),
 C38(H38A,H38B), C38(H38C,H38D), C36A(H36C,H36D)
;
_olex2_submission_special_instructions 'No special instructions were received'