Complexes containing redox-active fluorenone-based ligands linked to redox-active tris(pyrazolyl)boratomolybdenum fragments: assignment of ligand-centred and metal-centred redox processes by EPR and UV/VIS/NIR spectroelectrochemistry †
Behrendt, Andreas; Couchman, Samantha M.; Jeffery, John C.; McCleverty, Jon A.; Ward, Michael D.; Journal of the Chemical Society, Dalton Transactions  (1999) 4349–; doi:10.1039/a907303e

data_7027795
_publ_section_title
;
 Complexes containing redox-active fluorenone-based ligands linked to
 redox-active tris(pyrazolyl)boratomolybdenum fragments: assignment of
 ligand-centred and metal-centred redox processes by EPR and UV/VIS/NIR
 spectroelectrochemistry&#x200A;&#x2020;
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4349
_journal_paper_doi               10.1039/a907303e
_journal_year                    1999
_chemical_formula_sum            'C62.5 H73 B2 Cl13 Mo2 N16 O3'
_chemical_formula_weight         1770.72
_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                105.48(2)
_cell_angle_beta                 93.23(2)
_cell_angle_gamma                100.63(2)
_cell_formula_units_Z            2
_cell_length_a                   9.401(2)
_cell_length_b                   17.730(4)
_cell_length_c                   25.841(7)
_cell_measurement_temperature    173(2)
_cell_volume                     4054.3(18)
_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  0.1575
_diffrn_reflns_av_sigmaI/netI    0.2333
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            27335
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_F_000             1798
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.002
_refine_ls_goodness_of_fit_obs   1.251
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         10454
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.259
_refine_ls_R_factor_all          0.2395
_refine_ls_R_factor_obs          0.1048
_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^)+(0.1533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3201
_refine_ls_wR_factor_obs         0.2433
_reflns_number_observed          4340
_reflns_number_total             10527
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            907303Esup1.cif
_cod_data_source_block           andys
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1533P)^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^)+(0.1533P)^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        4054.2(17)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C62.50 H73 B2 Cl13 Mo2 N16 O3'
_cod_database_code               7027795