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_7011860
_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 H36 B2 Cl4 Gd2 N12 O8], 4 CH2Cl2'
_chemical_formula_sum            'C50 H44 B2 Cl12 Gd2 N12 O8'
_chemical_formula_weight         1702.49
_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                74.750(10)
_cell_angle_beta                 76.040(10)
_cell_angle_gamma                83.290(10)
_cell_formula_units_Z            1
_cell_length_a                   9.3945(5)
_cell_length_b                   12.6965(8)
_cell_length_c                   14.2564(9)
_cell_measurement_reflns_used    12159
_cell_measurement_temperature    100(2)
_cell_volume                     1589.54(19)
_computing_cell_refinement       'Nonius Collect'
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'Nonius Collect'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w, 422 frames a 1 deg./170 sec.'
_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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17689
_diffrn_reflns_theta_max         33.18
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    2.633
_exptl_absorpt_correction_T_max  0.6785
_exptl_absorpt_correction_T_min  0.4038
_exptl_absorpt_correction_type   'Gaussian, Face Indexed'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.928
_refine_diff_density_min         -2.239
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.064
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         12035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_obs          0.0404
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+3.5196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1104
_refine_ls_wR_factor_obs         0.1067
_reflns_number_observed          11339
_reflns_number_total             12046
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b205053f.txt
_cod_data_source_block           3
_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^)+(0.0524P)^2^+3.5196P] 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^)+(0.0524P)^2^+3.5196P] 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        1589.5(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011860