The Methanol-Methanolate CH3OH...OCH3-Bridging Ligand: Tuning of Exchange Coupling by Hydrogen Bonds in Dimethoxo-Bridged Dichromium(III) Complexes
Tapan Kanti Paine; Thomas Weyhermüller; Karl Wieghardt; Phalguni Chaudhuri; Inorganic Chemistry 41 (2002) 6538–6540; doi:10.1021/ic0204068

data_4319004
_publ_section_title
;
 The Methanol-Methanolate CH3OH...OCH3-Bridging Ligand: Tuning of Exchange
 Coupling by Hydrogen Bonds in Dimethoxo-Bridged Dichromium(III) Complexes
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6538
_journal_page_last               6540
_journal_paper_doi               10.1021/ic0204068
_journal_volume                  41
_journal_year                    2002
_chemical_formula_structural     '[NBu4]+, [C60 H93 Cr2 O8 Se2]-, 0.5 MeOH'
_chemical_formula_sum            'C76.5 H131 Cr2 N O8.5 Se2'
_chemical_formula_weight         1462.74
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 108.88(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.2757(8)
_cell_length_b                   29.351(3)
_cell_length_c                   13.910(10)
_cell_measurement_reflns_used    27423
_cell_measurement_temperature    100(2)
_cell_volume                     3970(3)
_computing_cell_refinement       'DENZO, Nonius Collect Software'
_computing_data_collection       'DENZO, Nonius Collect Software'
_computing_data_reduction        'DENZO, Nonius Collect Software'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius Kappa-CCD, rotating anode'
_diffrn_measurement_method       '372 images at 1 deg. in \w and 120 sec.'
_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  0.0866
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27423
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.241
_exptl_absorpt_correction_T_max  0.9408
_exptl_absorpt_correction_T_min  0.8103
_exptl_absorpt_correction_type   'Gaussian, face indexed'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       'transparent patelet'
_exptl_crystal_F_000             1562
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7825
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.396
_refine_ls_restrained_S_obs      1.130
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_obs          0.0594
_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^)+(0.0474P)^2^+8.9554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1915
_refine_ls_wR_factor_obs         0.1285
_reflns_number_observed          5596
_reflns_number_total             7907
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0204068_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+8.9554P] 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^)+(0.0474P)^2^+8.9554P] 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        3969.6(29)
_cod_original_formula_sum        'C76.50 H131 Cr2 N O8.50 Se2'
_cod_database_code               4319004