Coordination chemistry of a bulky redox-active cyanomanganese carbonyl ligand: N-bound tetrahedral complexes of 3d metals
Connelly, Neil G.; Hicks, Owen M.; Lewis, Gareth R.; Orpen, A. Guy; Wood, Andrew J.; Journal of the Chemical Society, Dalton Transactions  (2000) 1637–; doi:10.1039/b001782p

data_7009537
_publ_section_title
;
 Coordination chemistry of a bulky redox-active cyanomanganese carbonyl
 ligand: N-bound tetrahedral complexes of 3d metals
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1637
_journal_paper_doi               10.1039/b001782p
_journal_year                    2000
_chemical_formula_sum            'C60 H60 Cl2 Mn2 N O3 P4'
_chemical_formula_weight         1147.83
_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                110.087(9)
_cell_angle_beta                 106.829(8)
_cell_angle_gamma                99.213(8)
_cell_formula_units_Z            2
_cell_length_a                   13.3946(13)
_cell_length_b                   14.3660(8)
_cell_length_c                   16.995(2)
_cell_measurement_reflns_used    85
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      1.69
_cell_volume                     2814.6(6)
_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      73(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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17706
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'square plates'
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.026
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         12183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_restrained_S_obs      1.026
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_obs          0.0363
_refine_ls_shift/esd_max         0.040
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+2.8684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0978
_refine_ls_wR_factor_obs         0.0885
_reflns_number_observed          11037
_reflns_number_total             12194
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001782p.txt
_cod_data_source_block           2.thf
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+2.8684P] 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^)+(0.0382P)^2^+2.8684P] 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        2814.6(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009537