Structural studies of some mono- and bi-nuclear heteroleptic trispyrazolyborate complexes containing eight-co-oordinated europium and gadolinium†
Lawrence, Royston G.; Hamor, Thomas A.; Jones, Christopher J.; Paxton, Keith; Rowley, Natalie M.; Journal of the Chemical Society, Dalton Transactions  (2001) 2121–; doi:10.1039/b100896j

data_7702546
_publ_section_title
;
 Structural studies of some mono- and bi-nuclear heteroleptic
 trispyrazolyborate complexes containing eight-co-oordinated europium and
 gadolinium&#x2020;
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2121
_journal_paper_doi               10.1039/b100896j
_journal_year                    2001
_chemical_formula_sum            'C50 H50 B4 Eu2 N24 O4'
_chemical_formula_weight         1398.30
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.08(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.164(4)
_cell_length_b                   19.502(5)
_cell_length_c                   22.227(5)
_cell_measurement_reflns_used    30764
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.41
_cell_volume                     5955(3)
_computing_cell_refinement       'R-Axis II software'
_computing_data_collection       'R-Axis II software'
_computing_data_reduction        TeXsan
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  SHELXL-93
_computing_structure_solution    TeXsan
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku R-Axis II area detector'
_diffrn_measurement_method       'image-plate scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30764
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    2.152
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.923
_refine_diff_density_rms         '0.090 COMPOUND 4'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.969
_refine_ls_goodness_of_fit_obs   0.968
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         9976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_restrained_S_obs      0.968
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_obs          0.0483
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0735
_refine_ls_wR_factor_obs         0.0616
_reflns_number_observed          7225
_reflns_number_total             9976
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b100896j.txt
_cod_data_source_block           roy525rn
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[s^2^(Fo^2^)+( 0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to 'w=1/[s^2^(Fo^2^)+(
0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        5955.2(26)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7702546