1,10-phenanthroline-2,9-dicarboxamides as ligands for separation and sensing of hazardous metals
Alyapyshev, Mikhail; Ashina, Julia; Dar'in, Dmitry; Kenf, Ekaterina V.; Kirsanov, Dmitry; Tkachenko, Lyudmila I.; Legin, Andrey; Starova, Galina L.; Babain, Vasiliy; RSC Adv.  (2016) –; doi:10.1039/C6RA08946A

data_7225784
_publ_section_title
;
 1,10-phenanthroline-2,9-dicarboxamides as ligands for separation and
 sensing of hazardous metals
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA08946A
_journal_year                    2016
_chemical_formula_moiety         'C68 H68 Cd N8 O4, 3(N O3), C3'
_chemical_formula_sum            'C71 H68 Cd N11 O13'
_chemical_formula_weight         1395.76
_chemical_name_systematic
;
 ? 
;
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-01
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2015-09-29 deposited with the CCDC.
2016-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                69.773(3)
_cell_angle_beta                 81.128(3)
_cell_angle_gamma                70.968(3)
_cell_formula_units_Z            2
_cell_length_a                   14.2531(4)
_cell_length_b                   16.5873(5)
_cell_length_c                   17.4309(5)
_cell_measurement_reflns_used    20586
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2470
_cell_measurement_theta_min      3.5900
_cell_volume                     3651.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 0.9846
_diffrn_measured_fraction_theta_max 0.9846
_diffrn_measurement_details
;
  1 omega  -33.00    0.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9931  -57.0000 -150.0000 33

  2 omega  -14.00   14.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8681   77.0000   30.0000 28

  3 omega  -40.00  -12.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8681  -38.0000 -120.0000 28

  4 omega  -20.00   62.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8681  -99.0000   90.0000 82

  5 omega   23.00   54.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8681   38.0000   90.0000 31

  6 omega   36.00  108.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8681  178.0000  -90.0000 72

  7 omega  -56.00   46.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8681  -38.0000  -60.0000 102

  8 omega   62.00   95.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8681   38.0000  -60.0000 33

  9 omega  -11.00   39.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8681   77.0000 -120.0000 50
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0374718000
_diffrn_orient_matrix_UB_12      -0.0379629000
_diffrn_orient_matrix_UB_13      -0.0061726000
_diffrn_orient_matrix_UB_21      -0.0146949000
_diffrn_orient_matrix_UB_22      -0.0276872000
_diffrn_orient_matrix_UB_23      0.0379979000
_diffrn_orient_matrix_UB_31      -0.0340187000
_diffrn_orient_matrix_UB_32      -0.0081206000
_diffrn_orient_matrix_UB_33      -0.0200673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40195
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.03
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1446
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         2.643
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         16543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+2.2241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1224
_reflns_number_gt                14270
_reflns_number_total             16543
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra08946a2.cif
_cod_data_source_block           dvdcd1
_cod_original_cell_volume        3651.52(19)
_cod_database_code               7225784
_chemical_oxdiff_formula         'C34 O8 H38 N8'
_reflns_odcompleteness_completeness 98.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01