Probing the Structure, Conformation, and Stereochemical Exchange in a Family of Lanthanide Complexes Derived from Tetrapyridyl-Appended Cyclen
Louise S. Natrajan; Ntai M. Khoabane; Benjamin L. Dadds; Christopher A. Muryn; Robin G. Pritchard; Sarah L. Heath; Alan M. Kenwright; Ilya Kuprov; Stephen Faulkner; Inorganic Chemistry 49 (2010) 7700–7709; doi:10.1021/ic100447m

data_4316336
_publ_section_title
;
 Probing the Structure, Conformation, and Stereochemical Exchange in a
 Family of Lanthanide Complexes Derived from Tetrapyridyl-Appended Cyclen
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7700
_journal_page_last               7709
_journal_paper_doi               10.1021/ic100447m
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C35 H42 F9 Gd N8 O10 S3'
_chemical_formula_weight         1158.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 92.5000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.6601(2)
_cell_length_b                   16.1690(2)
_cell_length_c                   42.9290(6)
_cell_measurement_reflns_used    10669
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     8779.3(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics
;
Ortep-3 for Windows (Farrugia, 1997) and Bruker SHELXTL (Sheldrick, 1997)
;
_computing_publication_material
;
WinGX publication routines (Farrugia, 1999) and Bruker SHELXTL (Sheldrick, 1997)
;
_computing_structure_refinement
;
maxus (Mackay et al., 1999) and SHELXL-97 (Sheldrick, 1997)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'Enraf Nonius FR590'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            15167
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    1.699
_exptl_absorpt_correction_T_max  0.9200
_exptl_absorpt_correction_T_min  0.7067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4647
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.222
_refine_diff_density_min         -2.384
_refine_diff_density_rms         0.239
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.30(3)
_refine_ls_extinction_coef       0.0020(2)
_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   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1146
_refine_ls_number_reflns         12070
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1594
_refine_ls_R_factor_gt           0.1084
_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^)+(0.1579P)^2^+345.6840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2679
_refine_ls_wR_factor_ref         0.3170
_reflns_number_gt                8168
_reflns_number_total             12070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100447m_si_004.cif
_cod_data_source_block           ln720
_cod_depositor_comments
;

2020-11-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C280 H336 F72 Gd8 N64 O80 S24'
_cod_original_formula_weight         9270.72
_cod_original_formula_units_Z            1
_cod_database_code               4316336