Structural and thermodynamic study of the complexes of Nd(III) with N,N,N',N'-tetramethyl-3-oxa-glutaramide and the acid analogues.
Tian, Guoxin; Teat, Simon J.; Rao, Linfeng; Inorganic chemistry 53 (2014) 9477–9485; doi:10.1021/ic5004484

data_4341069
_publ_section_title
;
 Structural and thermodynamic study of the complexes of Nd(III) with
 N,N,N',N'-tetramethyl-3-oxa-glutaramide and the acid analogues.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9477
_journal_page_last               9485
_journal_paper_doi               10.1021/ic5004484
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C24 H48 N6 Nd O9, 3(Cl O4)'
_chemical_formula_sum            'C24 H48 Cl3 N6 Nd O21'
_chemical_formula_weight         1007.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.334(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.591(3)
_cell_length_b                   13.366(3)
_cell_length_c                   15.526(2)
_cell_measurement_reflns_used    5389
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.30
_cell_volume                     3999.6(12)
_computing_cell_refinement       'Bruker SAINT v7.07'
_computing_data_collection       'Bruker APEX2 v2.02'
_computing_data_reduction        'Bruker SAINT v7.07'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 36.23
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker PLatinum 200'
_diffrn_measurement_method       \w/2\q-scans
_diffrn_radiation_monochromator  'channel-cut Si-<111> crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77580
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_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14996
_diffrn_reflns_theta_full        29.01
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.986
_exptl_absorpt_correction_T_max  0.8573
_exptl_absorpt_correction_T_min  0.8261
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2006'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+11.6523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1195
_reflns_number_gt                3764
_reflns_number_total             4078
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5004484_si_001.cif
_cod_data_source_block           ndtmda
_cod_depositor_comments
'Adding full bibliography for 4341069--4341071.cif.'
_cod_original_cell_volume        3999.6(11)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4341069