Neutral cyclic sp<sup>2</sup>-sp<sup>3</sup> and sp<sup>3</sup>-sp<sup>3</sup> diboranes from <i>N</i>,<i>N</i>'-dicyclohexylcarbodiimide insertion into 1,2-dichlorodiboranes(4).
Fırıncı, Erkan; Fırıncı, Rukiye; Sevinçek, Resul; Aygün, Muhittin; Şahin, Yüksel; Chemical communications (Cambridge, England) 56 (2020) 9807–9810; doi:10.1039/d0cc03454a

data_7126970
_publ_section_title
;
 Neutral cyclic sp<sup>2</sup>-sp<sup>3</sup> and
 sp<sup>3</sup>-sp<sup>3</sup> diboranes from
 <i>N</i>,<i>N</i>'-dicyclohexylcarbodiimide insertion into
 1,2-dichlorodiboranes(4).
;
_journal_issue                   68
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9807
_journal_page_last               9810
_journal_paper_doi               10.1039/d0cc03454a
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C17 H34 B2 Cl2 N4'
_chemical_formula_sum            'C17 H34 B2 Cl2 N4'
_chemical_formula_weight         387.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-07 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1674(7)
_cell_length_b                   10.6202(9)
_cell_length_c                   22.2091(16)
_cell_measurement_reflns_used    1685
_cell_measurement_temperature    294.41(10)
_cell_measurement_theta_max      24.8200
_cell_measurement_theta_min      4.0220
_cell_volume                     2162.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.41(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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     54.00  81.00   1.00   21.49    --   20.07 178.00-150.00   27
  2  \w    -67.00  42.00   1.00   21.49    --  -22.10 -19.00 -90.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0270484000
_diffrn_orient_matrix_UB_12      0.0502031000
_diffrn_orient_matrix_UB_13      -0.0179025000
_diffrn_orient_matrix_UB_21      -0.0367894000
_diffrn_orient_matrix_UB_22      0.0437842000
_diffrn_orient_matrix_UB_23      0.0186781000
_diffrn_orient_matrix_UB_31      0.0626118000
_diffrn_orient_matrix_UB_32      0.0042102000
_diffrn_orient_matrix_UB_33      0.0186580000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4857
_diffrn_reflns_point_group_measured_fraction_full 0.871
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.679
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         3.355
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.189
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.517
_exptl_crystal_size_mid          0.365
_exptl_crystal_size_min          0.307
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 796 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0303P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.532
_reflns_Friedel_fraction_full    0.709
_reflns_Friedel_fraction_max     0.709
_reflns_number_gt                2806
_reflns_number_total             3563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03454a2.cif
_cod_data_source_block           i
_cod_depositor_comments
'Adding full bibliography for 7126970--7126972.cif.'
_cod_database_code               7126970
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C17 H34 B2 Cl2 N4'
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.857
_reflns_odcompleteness_completeness 98.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C21(H21), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C6(H6A,H6B), C13(H13A,
 H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              56298
_shelx_hkl_checksum              45964
_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 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.865