Synthesis, Characterization, and PGSE (1H and 19F) NMR Diffusion Studies on Cationic (η6- Arene)Mn(CO)3+ Complexes: Boron Counterion, Ion Pairing, and Solvent Dependences
Daniele Schott; Paul S. Pregosin; Béatrice Jacques; Murielle Chavarot; Françoise Rose-Munch; Eric Rose; Inorganic Chemistry 44 (2005) 5941–5948; doi:10.1021/ic0506409

data_4309365
_publ_section_title
;
Synthesis, Characterization, and PGSE (1H and 19F) NMR Diffusion Studies on
Cationic (\h6- Arene)Mn(CO)3+ Complexes: Boron Counterion, Ion Pairing,
and Solvent Dependences
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5941
_journal_page_last               5948
_journal_paper_doi               10.1021/ic0506409
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C36 H32 B Mn O6'
_chemical_formula_sum            'C36 H32 B Mn O6'
_chemical_formula_weight         626.40
_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
_audit_creation_date             05-06-27
_audit_creation_method           CRYSTALS_ver_12.24
_cell_angle_alpha                74.428(15)
_cell_angle_beta                 88.031(14)
_cell_angle_gamma                71.735(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4965(11)
_cell_length_b                   11.9045(16)
_cell_length_c                   14.029(2)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    295
_cell_measurement_theta_max      2
_cell_measurement_theta_min      1
_cell_volume                     1601.2(4)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.121
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17662
_diffrn_reflns_theta_full        28.198
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.046
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_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   refdelf
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_exptl_crystal_description       block
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_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0856
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4311
_refine_ls_number_restraints     0
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_refine_ls_shift/su_max          0.000330
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.477 0.326 0.227 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1317
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_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                4311
_reflns_number_total             9229
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.3073(6)
_oxford_structure_analysis_title '6011436 Compound X'
_cod_data_source_file            ic0506409si20050627_011506.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

2020-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C10.29 H9.14 B0.29 Mn0.29 O1.71'
_cod_original_formula_weight         178.97
_cod_original_formula_moiety         'C10.29 H9.14 B0.29 Mn0.29 O1.71'
_cod_original_formula_units_Z            7
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4309365