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_7225783
_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
'4(C68 H68 La N10 O10), 8(N O3), 4(C0.75 Cl1.5)'
_chemical_formula_sum            'C275 H272 Cl6 La4 N48 O64'
_chemical_formula_weight         6041.75
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-17
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2015-07-17 deposited with the CCDC.
2016-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 125.906(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   24.5353(9)
_cell_length_b                   19.3002(6)
_cell_length_c                   17.7952(6)
_cell_measurement_reflns_used    7585
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.2730
_cell_measurement_theta_min      3.3500
_cell_volume                     6825.4(4)
_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 0.9974
_diffrn_measured_fraction_theta_max 0.9974
_diffrn_measurement_details
;
  1 omega  -19.00   61.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8681  -99.0000 -180.0000 80

  2 omega   -9.00   93.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8681   77.0000  -30.0000 102

  3 omega   44.00   76.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8681   38.0000 -120.0000 32

  4 omega    7.00   34.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8681  -38.0000 -120.0000 27
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0049173000
_diffrn_orient_matrix_UB_12      -0.0322472000
_diffrn_orient_matrix_UB_13      0.0170094000
_diffrn_orient_matrix_UB_21      -0.0143084000
_diffrn_orient_matrix_UB_22      -0.0174682000
_diffrn_orient_matrix_UB_23      -0.0305197000
_diffrn_orient_matrix_UB_31      0.0374966000
_diffrn_orient_matrix_UB_32      -0.0023836000
_diffrn_orient_matrix_UB_33      -0.0073395000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19093
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78291
_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            colorless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             3100
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.555
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+13.2235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1309
_reflns_number_gt                6367
_reflns_number_total             7814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra08946a2.cif
_cod_data_source_block           dvdlareal
_cod_database_code               7225783
_chemical_oxdiff_formula         'c34 h38 n8 o8 la1'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01