Reactions of a diborylstannylene with CO<sub>2</sub> and N<sub>2</sub>O: diboration of carbon dioxide by a main group bis(boryl) complex.
Protchenko, Andrey V.; Fuentes, M Ángeles; Hicks, Jamie; McManus, Caitilín; Tirfoin, Rémi; Aldridge, Simon; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9059–9067; doi:10.1039/d1dt01216a

data_7707232
_publ_section_title
;
 Reactions of a diborylstannylene with CO<sub>2</sub> and N<sub>2</sub>O:
 diboration of carbon dioxide by a main group bis(boryl) complex.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9059
_journal_page_last               9067
_journal_paper_doi               10.1039/d1dt01216a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C57 H80 B2 Br Li N4 O4 Sn'
_chemical_formula_sum            'C57 H80 B2 Br Li N4 O4 Sn'
_chemical_formula_weight         1112.41
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-13 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.717(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7798(9)
_cell_length_b                   16.8149(5)
_cell_length_c                   19.3768(9)
_cell_measurement_reflns_used    9581
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.1680
_cell_measurement_theta_min      3.6420
_cell_volume                     5705.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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    -78.00 -36.00   1.00    4.22    --    0.00 178.00 120.00   42
  2  \w      2.00  49.00   1.00    4.22    --    0.00 -99.00   0.00   47
  3  \w      1.00  26.00   1.00    4.22    --    0.00 -99.00-180.00   25
  4  \w    -97.00 -47.00   1.00    4.22    --    0.00-178.00-150.00   50
  5  \w    -48.00  24.00   1.00   16.90    --  -60.50  30.00  60.00   72
  6  \w    -46.00  28.00   1.00   16.90    --  -60.50  45.00 -30.00   74
  7  \w   -150.00 -79.00   1.00   16.90    --  -60.50-125.00 -60.00   71
  8  \w   -131.00 -91.00   1.00   16.90    --  -60.50 -94.00 -30.00   40
  9  \w    -44.00   4.00   1.00   16.90    --  -60.50  30.00 -60.00   48
 10  \w     94.00 137.00   1.00   16.90    --   60.50 125.00 -90.00   43
 11  \w    112.00 139.00   1.00   16.90    --   60.50 113.00  91.00   27
 12  \w     39.00  75.00   1.00   20.00    --  121.00 -37.00 -90.00   36
 13  \w     31.00 102.00   1.00   20.00    --  121.00 -50.00-120.00   71
 14  \w     52.00  90.00   1.00   20.00    --  121.00 -25.00-150.00   38
 15  \w     30.00  63.00   1.00   20.00    --  121.00 -25.00  90.00   33
 16  \w     41.00  84.00   1.00   20.00    --  121.00 -50.00  90.00   43
 17  \w     90.00 124.00   1.00   20.00    --  121.00  50.00-180.00   34
 18  \w    113.00 171.00   1.00   20.00    --  121.00  63.00  30.00   58
 19  \w     77.00 105.00   1.00   20.00    --  121.00 -50.00 -90.00   28
 20  \w     30.00  84.00   1.00   20.00    --  121.00 -37.00  30.00   54
 21  \w     52.00  83.00   1.00   20.00    --  121.00 -25.00  30.00   31
 22  \w    136.00 164.00   1.00   20.00    --  121.00  50.00-180.00   28
 23  \w     31.00  82.00   1.00   20.00    --  121.00 -25.00 -60.00   51
 24  \w     26.00 177.00   1.00   20.00    --  121.00   0.00-180.00  151
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0602743000
_diffrn_orient_matrix_UB_12      -0.0382378000
_diffrn_orient_matrix_UB_13      -0.0762299000
_diffrn_orient_matrix_UB_21      -0.0623577000
_diffrn_orient_matrix_UB_22      0.0529624000
_diffrn_orient_matrix_UB_23      0.0026387000
_diffrn_orient_matrix_UB_31      0.0154089000
_diffrn_orient_matrix_UB_32      0.0641497000
_diffrn_orient_matrix_UB_33      -0.0475312000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25422
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.540
_diffrn_reflns_theta_min         3.644
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.738
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.501
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         11843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+3.8902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1441
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9830
_reflns_number_total             11843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01216a2.cif
_cod_data_source_block           33apcm19
_cod_depositor_comments
'Adding full bibliography for 7707232--7707239.cif.'
_cod_database_code               7707232
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H40 N4 B2 O4 Sn1 Li1 Br1'
_shelx_estimated_absorpt_t_max   0.649
_shelx_estimated_absorpt_t_min   0.537
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C50(H50), C12(H12), C24(H24), C9(H9), C35(H35), C47(H47), C38(H38), C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C103(H10A,H10B), C101(H10C,H10D), C102(H10E,H10F), C100(H10G,H10H)
2.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C2(H2), C28(H28), C1(H1), C19(H19), C17(H17), C18(H18), C44(H44),
 C7(H7), C43(H43), C45(H45), C33(H33), C31(H31), C32(H32), C5(H5), C6(H6)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C52(H52A,H52B,H52C), C14(H14A,H14B,H14C), C51(H51A,H51B,
 H51C), C36(H36A,H36B,H36C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C23(H23A,
 H23B,H23C), C10(H10I,H10J,H10K), C25(H25A,H25B,H25C), C37(H37A,H37B,H37C),
 C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C22(H22A,H22B,
 H22C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              62870
_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 1.999
_oxdiff_exptl_absorpt_empirical_full_min 0.677