Very weak electron‒electron exchange interactions in paramagnetic dinuclear tris(pyrazolyl)boratomolybdenum centres with extended bridging ligands: estimation of the exchange coupling constant J by simulation of second-order EPR spectra †
Shonfield, Peter K. A.; Behrendt, Andreas; Jeffery, John C.; Maher, John P.; McCleverty, Jon A.; Psillakis, Elefteria; Ward, Michael D.; Western, Colin; Journal of the Chemical Society, Dalton Transactions  (1999) 4341–; doi:10.1039/a908138k

data_7027823
_publ_section_title
;
 Very weak electron--electron exchange interactions in paramagnetic
 dinuclear tris(pyrazolyl)boratomolybdenum centres with extended bridging
 ligands: estimation of the exchange coupling constant J by simulation of
 second-order EPR spectra&#x200A;&#x2020;
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4341
_journal_paper_doi               10.1039/a908138k
_journal_year                    1999
_chemical_formula_sum            'C69 H94 B2 Cl2 Mo2 N16 O6'
_chemical_formula_weight         1528.00
_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
_cell_angle_alpha                107.15(3)
_cell_angle_beta                 110.24(3)
_cell_angle_gamma                104.79(3)
_cell_formula_units_Z            2
_cell_length_a                   15.366(3)
_cell_length_b                   16.789(3)
_cell_length_c                   18.212(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3863(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0817
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18101
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.558
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.138
_refine_ls_goodness_of_fit_obs   1.161
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         12313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.233
_refine_ls_restrained_S_obs      1.161
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_obs          0.0918
_refine_ls_shift/esd_max         0.180
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+35.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2499
_refine_ls_wR_factor_obs         0.1927
_reflns_number_observed          8728
_reflns_number_total             12793
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            908138Ksup1.cif
_cod_data_source_block           jj
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+35.9000P] 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^)+(0.0525P)^2^+35.9000P] 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        3863.0(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027823