Solid State and Solution Dynamics of Pyridine Based Tetraaza-Macrocyclic Lanthanide Chelates Possessing Phosphonate Ligating Functionality (Ln-PCTMB): Effect on Relaxometry and Optical Properties
Garry E. Kiefer; Mark Woods; Inorganic Chemistry 48 (2009) 11767–11778; doi:10.1021/ic901779k

data_4303865
_publ_section_title
;
Solid State and Solution Dynamics of Pyridine Based Tetraaza-Macrocyclic
Lanthanide Chelates Possessing Phosphonate Ligating Functionality
(Ln-PCTMB): Effect on Relaxometry and Optical Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11767
_journal_page_last               11778
_journal_paper_doi               10.1021/ic901779k
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C52 H114.5 N8 O27.25 P6 Tb2'
_chemical_formula_weight         1791.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.701(5)
_cell_angle_beta                 71.826(5)
_cell_angle_gamma                75.390(5)
_cell_formula_units_Z            2
_cell_length_a                   14.341(6)
_cell_length_b                   16.552(7)
_cell_length_c                   18.666(8)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    383(2)
_cell_measurement_theta_max      26.75
_cell_measurement_theta_min      2.18
_cell_volume                     3740(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      383(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52330
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    2.084
_exptl_absorpt_correction_T_max  0.8187
_exptl_absorpt_correction_T_min  0.3678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'colorless '
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'needle    '
_exptl_crystal_F_000             1841
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1070
_refine_ls_number_reflns         13015
_refine_ls_number_restraints     1576
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0450P)^2^+10.8415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                9117
_reflns_number_total             13015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901779k_si_002_1.cif
_cod_data_source_block           mc03
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C52 H114.50 N8 O27.25 P6 Tb2'
_cod_database_code               4303865