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_7126972
_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         'C30 H56 B2 Cl2 N6'
_chemical_formula_sum            'C30 H56 B2 Cl2 N6'
_chemical_formula_weight         593.32
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_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.	2020-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.6380(16)
_cell_length_b                   17.6380(16)
_cell_length_c                   24.541(3)
_cell_measurement_reflns_used    955
_cell_measurement_temperature    295.0
_cell_measurement_theta_max      22.1360
_cell_measurement_theta_min      3.6240
_cell_volume                     7634.7(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      295.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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    -51.00  62.25   0.75  200.61    --   20.07 -19.00 150.00  151
;
_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      0.0250454000
_diffrn_orient_matrix_UB_12      -0.0120607000
_diffrn_orient_matrix_UB_13      -0.0209189000
_diffrn_orient_matrix_UB_21      0.0200447000
_diffrn_orient_matrix_UB_22      0.0346212000
_diffrn_orient_matrix_UB_23      0.0019295000
_diffrn_orient_matrix_UB_31      0.0243970000
_diffrn_orient_matrix_UB_32      -0.0160562000
_diffrn_orient_matrix_UB_33      0.0198191000
_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  0.1050
_diffrn_reflns_av_unetI/netI     0.1479
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5667
_diffrn_reflns_point_group_measured_fraction_full 0.598
_diffrn_reflns_point_group_measured_fraction_max 0.598
_diffrn_reflns_theta_full        25.019
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         3.267
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.032
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.393
_exptl_crystal_size_mid          0.319
_exptl_crystal_size_min          0.283
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.16(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2016
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0313P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.199
_reflns_Friedel_fraction_full    0.204
_reflns_Friedel_fraction_max     0.204
_reflns_number_gt                1160
_reflns_number_total             2016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03454a3.cif
_cod_data_source_block           iii
_cod_depositor_comments
'Adding full bibliography for 7126970--7126972.cif.'
_cod_original_cell_volume        7634.6(16)
_cod_database_code               7126972
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C31 H56 B2 Cl4 N6'
_reflns_odcompleteness_completeness 97.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(H2B)=Sof(H4BC)=Sof(H4BD)=Sof(H5BC)=Sof(H5BD)=Sof(H7BC)=Sof(H7BD)=Sof(C3A)=
 Sof(H3AA)=Sof(H3AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(1)
 Sof(H2A)=Sof(H4AA)=Sof(H4AB)=Sof(H5AA)=Sof(H5AB)=Sof(H7AA)=Sof(H7AB)=Sof(C3B)=
 Sof(H3BA)=Sof(H3BB)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C2(H2A), C2(H2B), C10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4AA,H4AB), C4(H4BC,H4BD), C5(H5BC,H5BD), C5(H5AA,H5AB), C7(H7AA,H7AB),
 C7(H7BC,H7BD), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C3B(H3BA,H3BB), C6B(H6BA,H6BB), C3A(H3AA,H3AB), C6A(H6AA,H6AB)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              88128
_shelx_fab_checksum              63644
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 11.878
_oxdiff_exptl_absorpt_empirical_full_min 0.102