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_7225781
_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 N8 O4 Zn, C H2 Cl2, 2(N O3), H2 O'
_chemical_formula_sum            'C69 H72 Cl2 N10 O11 Zn'
_chemical_formula_weight         1353.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-08
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2015-06-02 deposited with the CCDC.
2016-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.656(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5779(9)
_cell_length_b                   19.4068(8)
_cell_length_c                   20.2775(10)
_cell_measurement_reflns_used    5367
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.3220
_cell_measurement_theta_min      3.3040
_cell_volume                     6696.5(6)
_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 0.9932
_diffrn_measured_fraction_theta_max 0.9932
_diffrn_measurement_details
;
  1 omega   12.00   40.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0061   38.0000  -30.0000 28

  2 omega -115.00  -90.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0061  178.0000  -60.0000 25

  3 omega   40.00  101.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811 -178.0000   90.0000 61

  4 omega    4.00  109.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811   77.0000   90.0000 105

  5 omega  -43.00    7.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811  -57.0000   30.0000 50
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0053625000
_diffrn_orient_matrix_UB_12      0.0242785000
_diffrn_orient_matrix_UB_13      0.0237621000
_diffrn_orient_matrix_UB_21      -0.0028518000
_diffrn_orient_matrix_UB_22      0.0268698000
_diffrn_orient_matrix_UB_23      -0.0246611000
_diffrn_orient_matrix_UB_31      -0.0412453000
_diffrn_orient_matrix_UB_32      -0.0049829000
_diffrn_orient_matrix_UB_33      -0.0168790000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.1888
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37530
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03405
_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            green-light
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         15293
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1786
_refine_ls_R_factor_gt           0.1057
_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^)+(0.1063P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2623
_reflns_number_gt                7581
_reflns_number_total             15293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra08946a2.cif
_cod_data_source_block           dvdzn
_cod_original_cell_volume        6696.5(5)
_cod_database_code               7225781
_chemical_oxdiff_formula         'zn1 c34 h34 n8 o8'
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     35.02