Stabilisation of the [Mn(CO)2]+ fragment by thioether macrocyclic ligands; synthesis, spectroscopic and structural characterisation
Patel, Bhavesh; Reid, Gillian; Journal of the Chemical Society, Dalton Transactions  (2000) 1303–; doi:10.1039/b000446o

data_7009372
_publ_section_title
;
 Stabilisation of the [Mn(CO)2]+ fragment by thioether macrocyclic
 ligands; synthesis, spectroscopic and structural characterisation
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1303
_journal_paper_doi               10.1039/b000446o
_journal_year                    2000
_chemical_formula_moiety         '[Mn(CO)2([12]aneS4)]CF3SO3.1/2CHCl3'
_chemical_formula_sum            'C11.5 H16.5 Cl1.5 F3 Mn O5 S5'
_chemical_formula_weight         560.16
_chemical_name_systematic
; 
 cis-dicarbonyl  manganese(I) 1,4,7,10-tetrathiacyclododecane . 1/2CHCl2 solvate 
;
_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-97
_cell_angle_alpha                90.983(17)
_cell_angle_beta                 90.332(14)
_cell_angle_gamma                86.531(13)
_cell_formula_units_Z            4
_cell_length_a                   14.0952(16)
_cell_length_b                   15.267(3)
_cell_length_c                   9.6411(15)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      17.9
_cell_measurement_theta_min      13.9
_cell_volume                     2070.6(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        Texsan
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  AFC7S
_diffrn_measurement_method       omege/2theta
_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  0.0683
_diffrn_reflns_av_sigmaI/netI    0.1242
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7633
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        -1.65
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.383
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.428
_refine_diff_density_min         -1.896
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         7306
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1631
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+9.5568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.2092
_reflns_number_gt                3708
_reflns_number_total             7306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b000446o.txt
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

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^)+(0.0936P)^2^+9.5568P] 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^)+(0.0936P)^2^+9.5568P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C11.50 H16.50 Cl1.50 F3 Mn O5 S5'
_cod_database_code               7009372