An insight into the extraction of transition metal ions by picolinamides associated with intramolecular hydrogen bonding and rotational isomerization
Li, Yan; Jia, Yiming; Wang, Zhenwen; Li, Xianghui; Feng, Wen; Deng, Pengchi; Yuan, Lihua; RSC Advances 4 (2014) 29702–; doi:10.1039/C4RA02030H

data_7217080
_publ_section_title
;
 An insight into the extraction of transition metal ions by picolinamides
 associated with intramolecular hydrogen bonding and rotational
 isomerization
;
_journal_issue                   56
_journal_name_full               'RSC Advances'
_journal_page_first              29702
_journal_paper_doi               10.1039/C4RA02030H
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C25 H27 N3 O4'
_chemical_formula_sum            'C25 H27 N3 O4'
_chemical_formula_weight         433.50
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-11-01
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.09.07 svn.r1971, GUI svn.r3853)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.110(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0617(7)
_cell_length_b                   8.8547(6)
_cell_length_c                   17.7386(10)
_cell_measurement_reflns_used    2817
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1241
_cell_measurement_theta_min      2.9738
_cell_volume                     2347.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -76.00  -38.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8924  134.0000  -68.0000 38

  2 omega   -6.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8611 -113.0000  146.0000 60

  3 omega    8.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8611   38.0000 -120.0000 83

  4 omega   30.00   64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8611   38.0000  -60.0000 34

  5 omega   -6.00   19.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8611   38.0000  120.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0096702000
_diffrn_orient_matrix_UB_12      0.0770117000
_diffrn_orient_matrix_UB_13      0.0084086000
_diffrn_orient_matrix_UB_21      0.0041510000
_diffrn_orient_matrix_UB_22      -0.0165315000
_diffrn_orient_matrix_UB_23      0.0393965000
_diffrn_orient_matrix_UB_31      0.0462809000
_diffrn_orient_matrix_UB_32      -0.0146314000
_diffrn_orient_matrix_UB_33      -0.0002037000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9186
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0753
_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^)+(0.0741P)^2^+2.5589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1992
_refine_ls_wR_factor_ref         0.2198
_reflns_number_gt                2835
_reflns_number_total             4124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra02030h1.cif
_cod_data_source_block           111031_s5_ly
_cod_original_cell_volume        2347.6(2)
_cod_database_code               7217080
_chemical_oxdiff_formula         C20H20N2O5
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32