Bioorganometallic Chemistry. 13. Regioselective Reduction of NAD+ Models, 1-Benzylnicotinamde Triflate and β-Nicotinamide Ribose-5'-methyl Phosphate, with in Situ Generated [Cp*Rh(Bpy)H]+: Structure-Activity Relationships, Kinetics, and Mechanistic Aspects in the Formation of the 1,4-NADH Derivatives
H. Christine Lo; Carmen Leiva; Olivier Buriez; John B. Kerr; Marilyn M. Olmstead; Richard H. Fish; Inorganic Chemistry 40 (2001) 6705–6716; doi:10.1021/ic010562z

data_4320704
_publ_section_title
;
 Bioorganometallic Chemistry. 13. Regioselective Reduction of NAD+ Models,
 1-Benzylnicotinamde Triflate and \b-Nicotinamide Ribose-5'-methyl
 Phosphate, with in Situ Generated [Cp*Rh(Bpy)H]+: Structure-Activity
 Relationships, Kinetics, and Mechanistic Aspects in the Formation of the
 1,4-NADH Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6705
_journal_page_last               6716
_journal_paper_doi               10.1021/ic010562z
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C22.3 H27 F6 N2 O7.7 Rh S2'
_chemical_formula_weight         728.29
_chemical_name_common
' [Cp*Rh(0.7H~2~O/0.3CH~3~OH)bipy](OTf)~2~.0.7H~2~O'
_chemical_name_systematic
;
?
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.44(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.411(3)
_cell_length_b                   15.811(3)
_cell_length_c                   14.258(3)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.1
_cell_measurement_theta_min      5.0
_cell_volume                     2774.3(11)
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens P3'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL 5 (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXTL 5 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL 5 (Sheldrick, 1994)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Siemens R3m/v'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8986
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        '< 0.1'
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   XABS2
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1470
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_hydrogen_treatment    'riding except H on H2O'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_obs          0.0535
_refine_ls_shift/esd_max         -0.190
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+2.9237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1144
_refine_ls_wR_factor_obs         0.1010
_reflns_number_observed          4701
_reflns_number_total             6371
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010562z.cif
_cod_data_source_block           mn761
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+2.9237P] 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^)+(0.0282P)^2^+2.9237P] 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        2774.3(10)
_cod_database_code               4320704