Large-bite diboranes for the μ(1,2) complexation of hydrazine and cyanide.
Chen, Chang-Hong; Gabbaï, François P; Chemical science 9 (2018) 6210–6218; doi:10.1039/c8sc01877d

data_1549473
_publ_section_title
;
 Large-bite diboranes for the \m(1,2) complexation of hydrazine and
 cyanide.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              6210
_journal_page_last               6218
_journal_paper_doi               10.1039/c8sc01877d
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C77 H79 B2 K N O6, 2(C H2 Cl2)'
_chemical_formula_sum            'C79 H83 B2 Cl4 K N O6'
_chemical_formula_weight         1344.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-03-02 deposited with the CCDC.
2018-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.4764(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.407(3)
_cell_length_b                   13.6932(18)
_cell_length_c                   23.988(3)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    110
_cell_measurement_theta_max      23.912
_cell_measurement_theta_min      2.422
_cell_volume                     7025.0(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
%$getVar(solution_reference_short)%
;
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            70236
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.507
_diffrn_reflns_theta_min         1.942
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0849 before and 0.0757 after correction. The Ratio of minimum to maximum transmission is 0.9309. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             2836
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 5743 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         14546
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0583P)^2^+6.3374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                12954
_reflns_number_total             14546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01877d2.cif
_cod_data_source_block           2CN
_cod_depositor_comments
'Adding full bibliography for 1549471--1549474.cif.'
_cod_original_cell_volume        7025.2(16)
_cod_database_code               1549473
_shelx_shelxl_version_number     2014/7
_publ_section_exptl
;
Any special experimental details
;
_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. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(N2) = Uanis(C81) = Uanis(C82)
3. Others
 Sof(N2)=Sof(C82)=1-FVAR(1)
 Sof(N1)=Sof(C81)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C20(H20), C50(H50), C52(H52)
4.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C63(H63A,H63B), C64(H64A,H64B), C66(H66A,H66B), C73(H73A,
 H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
 C78(H78A,H78B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15),
 C16(H16), C17(H17), C23(H23), C25(H25), C32(H32), C34(H34), C41(H41), C43(H43),
  C58(H58), C59(H59), C60(H60), C61(H61), C68(H68), C69(H69), C70(H70), C71(H71)
4.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              51780
_olex2_submission_special_instructions 'No special instructions were received'