Synthesis, molecular structure and emission properties of benzoato-bridged lanthanide complexes with hydrotris(pyrazolyl)borate
Udai P. Singh; Shalu Tyagi; Chokhe Lal Sharma; Helmut Görner; Thomas Weyhermüller; J. Chem. Soc., Dalton Trans.  (2002) 4464–4470; doi:10.1039/b205053f

data_7011858
_publ_section_title
;
 Synthesis, molecular structure and emission properties of
 benzoato-bridged lanthanide complexes with hydrotris(pyrazolyl)borate
;
_journal_issue                   23
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4464
_journal_page_last               4470
_journal_paper_doi               10.1039/b205053f
_journal_year                    2002
_chemical_formula_structural     '[C46 H40 B2 Gd2 N12 O8], (C H2 Cl2)'
_chemical_formula_sum            'C47 H42 B2 Cl2 Gd2 N12 O8'
_chemical_formula_weight         1309.94
_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                72.56(1)
_cell_angle_beta                 83.37(1)
_cell_angle_gamma                89.58(1)
_cell_formula_units_Z            2
_cell_length_a                   12.5351(8)
_cell_length_b                   13.0435(8)
_cell_length_c                   16.3461(12)
_cell_measurement_reflns_used    7914
_cell_measurement_temperature    100(2)
_cell_volume                     2531.7(3)
_computing_cell_refinement       'Siemens SAINT 6'
_computing_data_collection       'Siemens SAINT 6'
_computing_data_reduction        'Siemens SAINT 6'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w, 0.3 deg./frame'
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28063
_diffrn_reflns_theta_max         33.18
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    2.767
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   'Gaussian, Face indexed'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.298
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.917
_refine_ls_goodness_of_fit_obs   1.002
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         16662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.917
_refine_ls_restrained_S_obs      1.002
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_obs          0.0292
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0584
_refine_ls_wR_factor_obs         0.0553
_reflns_number_observed          12664
_reflns_number_total             16666
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b205053f.txt
_cod_data_source_block           1
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0236P)^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^)+(0.0236P)^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_sg_symbol_H-M      P-1
_cod_database_code               7011858