Enhanced Carbon Dioxide Hydrogenation Facilitated by Catalytic Quantities of Bicarbonate and Other Inorganic Salts
Drake, Jessica L.; Manna, Cesar M.; Byers, Jeffery A.; Organometallics 32 (2013) 6891–; doi:10.1021/om401057p

data_4082057
_publ_section_title
;
 Enhanced Carbon Dioxide Hydrogenation Facilitated by Catalytic Quantities
 of Bicarbonate and Other Inorganic Salts
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6891
_journal_paper_doi               10.1021/om401057p
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C29 H29 O3 P Ru (H2 O)'
_chemical_formula_sum            'C29 H31 O4 P Ru'
_chemical_formula_weight         575.58
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.3520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0094(3)
_cell_length_b                   14.3971(4)
_cell_length_c                   21.0729(6)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.38
_cell_measurement_theta_min      3.72
_cell_volume                     2725.47(14)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker Kappa DUO CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0139
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4890
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         69.88
_diffrn_reflns_theta_min         3.72
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\uS'
_exptl_absorpt_coefficient_mu    5.463
_exptl_absorpt_correction_T_max  0.6111
_exptl_absorpt_correction_T_min  0.4079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G.M. (2008). SADABS v2008/1. Bruker AXS Inc. Madison, WI USA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
disordered ether molecule that can not be refined satisfactory. coordinates are
PART -1
O2S   3   -0.010834   -0.013225    0.007319    10.50000    0.07437    0.10409 =
         0.08571   -0.02770   -0.01436   -0.00684
C1S   1    0.081130    0.067412   -0.007939    10.50000    0.08420    0.07504 =
         0.05163   -0.03485   -0.01094    0.02580
AFIX  23
H1S1  2    0.151063    0.049614   -0.039882    10.50000   -1.20000
H1S2  2    0.139916    0.089026    0.030860    10.50000   -1.20000
AFIX   0
 
C2S   1   -0.022919    0.146057   -0.034627    10.50000    0.12751    0.08702 =
         0.05255   -0.02026    0.01276    0.01393
AFIX  33
H2S1  2    0.035405    0.202648   -0.039785    10.50000   -1.50000
H2S2  2   -0.099458    0.158048   -0.005001    10.50000   -1.50000
H2S3  2   -0.070563    0.127257   -0.075987    10.50000   -1.50000
AFIX   0
C3S   1    0.095965   -0.082757    0.035693    10.50000    0.08819    0.06937 =
         0.02475    0.01258    0.01459    0.03618
AFIX  23
H3S1  2    0.141040   -0.061420    0.077472    10.50000   -1.20000
H3S2  2    0.176188   -0.095189    0.007226    10.50000   -1.20000
AFIX   0
C4S   1   -0.001569   -0.170515    0.043179    10.50000    0.12751    0.08702 =
         0.05255   -0.02026    0.01276    0.01393
AFIX  33
H4S1  2    0.057581   -0.218481    0.066382    10.50000   -1.50000
H4S2  2   -0.036359   -0.194036    0.001007    10.50000   -1.50000
H4S3  2   -0.087443   -0.154376    0.066869    10.50000   -1.50000
PART 0
;
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       na
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4890
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+3.8258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0540
_reflns_number_gt                4857
_reflns_number_total             4890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401057p_si_002.cif
_cod_data_source_block           C29H31O4PRu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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 2(1)/c'
_cod_database_code               4082057