Novel N-bound thallium(I) complexes of redox-active cyanomanganese carbonyl ligands: cyanide as a μ3-κC∶κN∶κN triply bridging ligand
Connelly, Neil G.; Hicks, Owen M.; Lewis, Gareth R.; Moreno, M. Teresa; Orpen, A. Guy; Journal of the Chemical Society, Dalton Transactions  (1998) 1913–; doi:10.1039/a800765i

data_7028164
_publ_section_title
;
 Novel N-bound thallium(I) complexes of redox-active cyanomanganese
 carbonyl ligands: cyanide as a \m3-\kC&#x2236;\kN&#x2236;\kN triply
 bridging ligand
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1913
_journal_paper_doi               10.1039/a800765i
_journal_year                    1998
_chemical_formula_sum            'C68 H74 F12 Mn2 N2 O10 P8 Tl2'
_chemical_formula_weight         2073.68
_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                71.423(9)
_cell_angle_beta                 77.844(8)
_cell_angle_gamma                78.945(6)
_cell_formula_units_Z            1
_cell_length_a                   10.0840(8)
_cell_length_b                   13.297(2)
_cell_length_c                   15.921(2)
_cell_measurement_reflns_used    529
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.84
_cell_volume                     1960.2(4)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12579
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    4.659
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.472
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            cuboid
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_meas      ?
_exptl_crystal_description       colourless
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.368
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -9.99(999)
_refine_ls_extinction_coef       0.0027(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.124
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_obs          0.0284
_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^)+(0.0218P)^2^+4.4267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0684
_refine_ls_wR_factor_obs         0.0639
_reflns_number_observed          8131
_reflns_number_total             8662
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            i800765sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+4.4267P] 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^)+(0.0218P)^2^+4.4267P] 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        1960.3(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7028164