Solvent and metal dependent (1)H NMR hyperfine shifts in paramagnetic pentaamminemetal cyanide-bridged mixed-valence complexes.
Laidlaw, William Michael; Thompson, Amber L.; Denning, Robert Gordon; Dalton transactions (Cambridge, England : 2003) 42 (2013) 4695–4703; doi:10.1039/c3dt32978j

data_7022756
_publ_section_title
;
 Solvent and metal dependent (1)H NMR hyperfine shifts in paramagnetic
 pentaamminemetal cyanide-bridged mixed-valence complexes.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4695
_journal_page_last               4703
_journal_paper_doi               10.1039/c3dt32978j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C6 H15 N6 O5 Re Ru, 3(C F3 O3 S), 3(H2 O)'
_chemical_formula_sum            'C9 H21 F9 N6 O17 Re Ru S3'
_chemical_formula_weight         1039.75
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-10-30
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 92.2195(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1564(2)
_cell_length_b                   14.5998(3)
_cell_length_c                   26.8390(5)
_cell_measurement_reflns_used    6937
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3193.64(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            30746
_diffrn_reflns_theta_full        25.324
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_min         5.117
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.582
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_yellow
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.57
_refine_diff_density_min         -1.12
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1145
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         4920
_refine_ls_number_restraints     163
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.002574
_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:
0.525 0.112 0.288
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0668
_refine_ls_wR_factor_gt          0.0395
_refine_ls_wR_factor_ref         0.0395
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                4920
_reflns_number_total             7213
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.10
_oxford_diffrn_Wilson_scale      102.81
_oxford_refine_ls_r_factor_ref   0.0401
_oxford_refine_ls_scale          0.10281(13)
_oxford_reflns_number_all        7212
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 5997
_cod_data_source_file            c3dt32978j.txt
_cod_data_source_block           3-water
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Monoclinic' changed to 'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C9 H21 F9 N6 O17 Re1 Ru1 S3'
_cod_database_code               7022756