Extraction and structural studies of an unexplored monoamide, N,N'-dioctyl, α-hydroxy acetamide with lanthanide(iii) and actinide(iii) ions.
Kannan, Shanmugaperumal; Vats, Bal Govind; Pius, Illipparambil C.; Noronha, Donald M.; Dhami, Prem S.; Naik, Prashant W.; Kumar, Mukesh; Dalton transactions (Cambridge, England : 2003) 43 (2014) 5252–5255; doi:10.1039/c3dt53529k

data_7029354
_publ_section_title
;
 Extraction and structural studies of an unexplored monoamide,
 N,N'-dioctyl, \a-hydroxy acetamide with lanthanide(iii) and actinide(iii)
 ions.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5252
_journal_page_last               5255
_journal_paper_doi               10.1039/c3dt53529k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C24 H52 N4 O10 Sm, 2(N O3)'
_chemical_formula_sum            'C24 H52 N6 O16 Sm'
_chemical_formula_weight         831.06
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-12-12
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.549(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9512(4)
_cell_length_b                   27.0203(9)
_cell_length_c                   13.0160(4)
_cell_measurement_reflns_used    8383
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.6230
_cell_measurement_theta_min      3.2570
_cell_volume                     3773.5(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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3200
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9888
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1304224000
_diffrn_orient_matrix_UB_12      -0.0136737000
_diffrn_orient_matrix_UB_13      -0.0186619000
_diffrn_orient_matrix_UB_21      0.0304483000
_diffrn_orient_matrix_UB_22      0.0553125000
_diffrn_orient_matrix_UB_23      -0.0085913000
_diffrn_orient_matrix_UB_31      0.0518541000
_diffrn_orient_matrix_UB_32      0.0018823000
_diffrn_orient_matrix_UB_33      0.1190342000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.1016
_diffrn_reflns_av_unetI/netI     0.0898
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22645
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.106
_diffrn_reflns_theta_min         3.271
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.306
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.137
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear yellowish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       needle
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.193
_refine_diff_density_min         -1.403
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7091
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0987P)^2^+16.3796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2243
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5015
_reflns_number_total             7091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53529k.txt
_cod_data_source_block           1
_cod_database_code               7029354
_chemical_oxdiff_formula         C24H52O16N6Sm1
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O7-H7
 0.85 with sigma of 0.01
 O5-H5
 0.85 with sigma of 0.01
 O2-H2
 0.85 with sigma of 0.01
 C18-H7
 1.888778 with sigma of 0.02
 Sm-H7
 3.043107 with sigma of 0.02
 C10-H5
 1.858612 with sigma of 0.02
 Sm-H5
 3.122561 with sigma of 0.02
 C1-H2
 1.909073 with sigma of 0.02
 Sm-H2
 3.043974 with sigma of 0.02
3.a Rotating group:
 O1(H1A,H1B)
3.b Ternary CH refined with riding coordinates:
 C22(H22), C6(H6), C3(H3), C11(H11), C14(H14), C19(H19)
3.c Secondary CH2 refined with riding coordinates:
 C1(H1C,H1D), C18(H18A,H18B)
3.d Aromatic/amide H refined with riding coordinates:
 C10(H10)
3.e Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C20(H20A,H20B,
 H20C), C16(H16A,H16B,H16C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C5(H5A,H5B,H5C),
 C15(H15A,H15B,H15C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C)
;
_shelxl_version_number           2013-4