Lanthanide complexes of a new sterically hindered potentially hexadentate podand ligand based on a tris(pyrazolyl)borate core; crystal structures, solution structures and luminescence properties
Reeves, Zoe R.; Mann, Karen L. V.; Jeffery, John C.; McCleverty, Jon A.; Ward, Michael D.; Barigelletti, Francesco; Armaroli, Nicola; Journal of the Chemical Society, Dalton Transactions  (1999) 349–; doi:10.1039/a808724e

data_7027170
_publ_section_title
;
 Lanthanide complexes of a new sterically hindered potentially hexadentate
 podand ligand based on a tris(pyrazolyl)borate core; crystal structures,
 solution structures and luminescence properties
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              349
_journal_paper_doi               10.1039/a808724e
_journal_year                    1999
_chemical_formula_sum            'C27 H27 B Gd N11 O7'
_chemical_formula_weight         785.65
_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
_cell_angle_alpha                70.356(7)
_cell_angle_beta                 82.054(8)
_cell_angle_gamma                73.900(13)
_cell_formula_units_Z            4
_cell_length_a                   10.870(2)
_cell_length_b                   16.4827(13)
_cell_length_c                   18.996(2)
_cell_measurement_temperature    173(2)
_cell_volume                     3075.8(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method       '\w rotation with narrow frames (0.3 degrees)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31882
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    2.221
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.621
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.916
_refine_ls_goodness_of_fit_obs   0.971
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         13905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_restrained_S_obs      0.971
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_obs          0.0226
_refine_ls_shift/esd_max         0.143
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0579
_refine_ls_wR_factor_obs         0.0557
_reflns_number_observed          11633
_reflns_number_total             13905
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808724esup1.cif
_cod_data_source_block           choc
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3076.0(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027170