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_7124626
_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 H30 Cu3 N9 O6, 3(N O3), H2 O'
_chemical_formula_sum            'C15 H32 Cu3 N12 O16'
_chemical_formula_weight         827.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2016-02-09
_audit_creation_method
;
Olex2 1.2
(compiled Sep 16 2015 11:44:03 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-05-09 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.192(3)
_cell_angle_beta                 96.380(3)
_cell_angle_gamma                113.941(3)
_cell_formula_units_Z            4
_cell_length_a                   12.6421(9)
_cell_length_b                   14.2612(10)
_cell_length_c                   17.0125(11)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      1.56
_cell_volume                     2782.0(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9937
_diffrn_measured_fraction_theta_max 0.9937
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50230
_diffrn_reflns_theta_full        30.5000
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    2.371
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0625 before and 0.0382 after correction.
The Ratio of minimum to maximum transmission is 0.7825.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.9747
_exptl_crystal_description       block
_exptl_crystal_F_000             1688.9139
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.1713
_refine_diff_density_min         -0.9269
_refine_diff_density_rms         0.1084
_refine_ls_d_res_high            0.7478
_refine_ls_d_res_low             13.0157
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0620
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    83
_refine_ls_number_parameters     903
_refine_ls_number_reflns         13844
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.0617
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          3.5255
_refine_ls_shift/su_mean         0.0292
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+2.1466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                11639
_reflns_number_total             13844
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6cc02488b2.cif
_cod_data_source_block           fuls_a
_cod_database_code               7124626
_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
 O888-H88b
 0.95 with sigma of 0.02
 O010-H88b
 2 with sigma of 0.02
 O888-H88a
 1 with sigma of 0.02
 O00Q-H88a
 2.06 with sigma of 0.02
 O00M-H00k
 0.992 with sigma of 0.02
 O224-H00k
 1.75 with sigma of 0.02
 C02M-H02u
 0.99 with sigma of 0.02
 C02L-H02s
 0.99 with sigma of 0.02
3. Others
 Sof(H02i)=Sof(H02j)=Sof(H02q)=Sof(H02r)=Sof(C02M)=Sof(H02u)=Sof(H02v)=1-FVAR(1)
 Sof(H02g)=Sof(H02h)=Sof(H02o)=Sof(H02p)=Sof(C02L)=Sof(H02s)=Sof(H02t)=FVAR(1)
4.a Rotating group:
 O00D(H00e,H00f), O00E(H00a,H00b), O00G(H00g,H00h), O00H(H00i,H00j), O00I(H00c,
 H00d), O999(H99a,H99b)
4.b Rotating group with stretchable bonds:
 C02M(H00k,H00l)
4.c Secondary CH2 refined with riding coordinates:
 C01X(H01a,H01b), C021(H02w,H02x), C024(H02y,H), C026(H02z,Ha), C027(H02a,
 H02b), C028(H02,Hb), C029(H02c,H02d), C02A(H02e,H02f), C02B(H0aa,Hc),
 C02C(H1aa,Hd), C02D(H2aa,He), C02E(H3aa,Hf), C02F(H02g,H02h), C02F(H02i,H02j),
 C02G(H02k,H02l), C02H(H02m,H02n), C02I(H02o,H02p), C02I(H02q,H02r), C02J(H4aa,
 Hg), C02L(H02s,H02t), C02M(H02u,H02v)
;
_olex2_submission_special_instructions 'No special instructions were received'