Low-valent germanium and tin hydrides as catalysts for hydroboration, hydrodeoxygenation (HDO), and hydrodesulfurization (HDS) of heterocumulenes.
Mukhopadhyay, Sayantan; Sahoo, Rajata Kumar; Patro, A. Ganesh; Khuntia, Anwesh Prasad; Nembenna, Sharanappa; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18207–18216; doi:10.1039/d3dt04080a

data_7717213
_publ_section_title
;
 Low-valent germanium and tin hydrides as catalysts for hydroboration,
 hydrodeoxygenation (HDO), and hydrodesulfurization (HDS) of
 heterocumulenes.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18207
_journal_page_last               18216
_journal_paper_doi               10.1039/d3dt04080a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C14 H20 B N O3'
_chemical_formula_sum            'C14 H20 B N O3'
_chemical_formula_weight         261.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2022-04-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2023-10-10 deposited with the CCDC.	2024-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.259(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0059(7)
_cell_length_b                   7.2872(4)
_cell_length_c                   16.3747(9)
_cell_measurement_reflns_used    8664
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.2790
_cell_measurement_theta_min      3.7600
_cell_volume                     1473.80(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.9974
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -65.00  17.00   0.50   41.79    --    3.35 -10.00 -99.00  164
  2  \w     21.00  62.00   0.50   41.79    --   -4.14  10.00  74.00   82
  3  \w    -41.00   5.00   0.50   41.79    --    3.35 -37.00  90.00   92
  4  \w     -3.00  35.00   0.50   41.79    --    3.35 -99.00-180.00   76
  5  \w    -63.00   6.00   0.50   41.79    --    3.35 -37.00-180.00  138
  6  \w    -24.00   1.00   0.50   41.79    --   -4.14  77.00-180.00   50
  7  \w     -7.00  20.00   0.50   41.79    --   -4.14 -99.00-150.00   54
  8  \w    -15.00  16.00   0.50   41.79    --   -4.14 -99.00  60.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0247235000
_diffrn_orient_matrix_UB_12      -0.0837538000
_diffrn_orient_matrix_UB_13      0.0056317000
_diffrn_orient_matrix_UB_21      -0.0478828000
_diffrn_orient_matrix_UB_22      0.0482020000
_diffrn_orient_matrix_UB_23      -0.0012217000
_diffrn_orient_matrix_UB_31      -0.0199463000
_diffrn_orient_matrix_UB_32      -0.0116870000
_diffrn_orient_matrix_UB_33      -0.0452228000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15737
_diffrn_reflns_theta_full        25.3498
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.30
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.1768
_exptl_crystal_description       block
_exptl_crystal_F_000             560.2820
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.6154
_refine_diff_density_min         -0.4098
_refine_diff_density_rms         0.1098
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             6.1710
_refine_ls_goodness_of_fit_ref   1.0404
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0404
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1493P)^2^+0.3282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1838
_refine_ls_wR_factor_ref         0.1887
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -15
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -9
_reflns_number_gt                2429
_reflns_number_total             2695
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt04080a2.cif
_cod_data_source_block           SN_AGP_231
_cod_depositor_comments          'Adding full bibliography for 7717213.cif.'
_cod_original_cell_volume        1473.80(14)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7717213
_chemical_oxdiff_formula         'C56 H80 B4 N4 O12 '
_diffrn_oxdiff_digest_frames
;
013f85f9efaa60e77de79b5f8b209044b000025296e
;
_diffrn_oxdiff_digest_hkl
;
015d751fdba3664bfdbbb6e7d2a5f2071e1d44
;
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C0aa(H0aa), C3(H3), C4(H4), C1(H1)
2.b Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C16(H16a,H16b,H16c), C18(H18a,H18b,H18c), C17(H17a,H17b,
 H17c), C10(H10a,H10b,H10c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.722
_oxdiff_exptl_absorpt_empirical_full_min 0.636