Revisiting CO2Reduction with NaBH4under Aprotic Conditions: Synthesis and Characterization of Sodium Triformatoborohydride
Knopf, Ioana; Cummins, Christopher C.; Organometallics 34 (2015) 1601–1603; doi:10.1021/acs.organomet.5b00190

data_4085681
_publ_section_title
;
 Revisiting CO2Reduction with NaBH4under Aprotic Conditions: Synthesis and
 Characterization of Sodium Triformatoborohydride
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1601
_journal_page_last               1603
_journal_paper_doi               10.1021/acs.organomet.5b00190
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         .
_chemical_formula_sum            'C7 H14 B Na O8'
_chemical_formula_weight         259.98
_chemical_melting_point          .
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
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_cell_angle_beta                 95.4940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6216(2)
_cell_length_b                   17.5254(6)
_cell_length_c                   10.6602(4)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.79
_cell_measurement_theta_min      2.24
_cell_volume                     1231.39(7)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0212
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_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_min         2.244
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.153
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.402
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_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.190
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_refine_diff_density_max         0.391
_refine_diff_density_min         -0.199
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_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         3762
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+0.3844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                3086
_reflns_number_total             3762
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           re13079
_cod_depositor_comments          'Adding _journal_page_last.'
_cod_database_code               4085681
_shelx_estimated_absorpt_t_min   0.947
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_shelxl_version_number           2013-4
_shelx_res_checksum              68675
_shelx_hkl_checksum              36520