Structural variety in nitrate complexes of the heavy lanthanides with 2,2':6',2″-terpyridine, and stereoselective replacement of nitrate
Ahrens, Birte; Cotton, Simon A.; Feeder, Neil; Noy, Oliver E.; Raithby, Paul R.; Teat, Simon J.; Journal of the Chemical Society, Dalton Transactions  (2002) 2027–; doi:10.1039/b200480c

data_7011482
_publ_section_title
;
 Structural variety in nitrate complexes of the heavy lanthanides with
 2,2':6',2&#x2033;-terpyridine, and stereoselective replacement of
 nitrate
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2027
_journal_paper_doi               10.1039/b200480c
_journal_year                    2002
_chemical_formula_sum            'C17 H17 N6 O10 Yb'
_chemical_formula_weight         638.41
_chemical_name_systematic
; 
Complex 3
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6800(10)
_cell_length_b                   21.8770(10)
_cell_length_c                   11.2990(10)
_cell_measurement_reflns_used    33287
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.998
_cell_volume                     2144.8(3)
_computing_cell_refinement       'Nonius HKL Scalepack'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius HKL Denzo & Scalepack'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7217
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.53
_diffrn_standards_number         'not applicable'
_exptl_absorpt_coefficient_mu    4.429
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.6913
_exptl_absorpt_correction_type   'semi empirical multiple scans'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.00182(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    'methyl and OH rigid, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         3735
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0015P)^2^+7.3432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0631
_reflns_number_gt                3280
_reflns_number_total             3735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200480c.txt
_cod_data_source_block           pr9928
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7011482