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_1549474
_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         'C21 H26 Cl2 K O6, C H2 Cl2, C49 H50 B2 N'
_chemical_formula_sum            'C71 H78 B2 Cl4 K N O6'
_chemical_formula_weight         1243.86
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-07-07
_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                 112.9484(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4096(14)
_cell_length_b                   23.693(2)
_cell_length_c                   19.0628(17)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    110
_cell_measurement_theta_max      25.541
_cell_measurement_theta_min      2.201
_cell_volume                     6409.0(10)
_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)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0670
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            140726
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.614
_diffrn_reflns_theta_min         2.074
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0797 before and 0.0572 after correction. The Ratio of minimum to maximum transmission is 0.9277. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.915
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         14800
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0785P)^2^+7.7626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10757
_reflns_number_total             14800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01877d2.cif
_cod_data_source_block           1CN
_cod_depositor_comments
'Adding full bibliography for 1549471--1549474.cif.'
_cod_database_code               1549474
_shelx_shelxl_version_number     2014/7
_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
B2 \\sim B1 \\sim N2 \\sim C72: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
B2 \\sim B1 \\sim N1 \\sim C71: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(N1) = Uanis(N2)
Uanis(C71) = Uanis(C72)
3. Others
 Sof(N2)=Sof(C72)=1-FVAR(1)
 Sof(N1)=Sof(C71)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C57(H57A,H57B), C58(H58A,H58B), C65(H65A,H65B), C67(H67A,
 H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B)
4.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C52(H52), C53(H53), C54(H54), C61(H61), C62(H62), C63(H63),
 C64(H64), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C15(H15),
 C17(H17), C24(H24), C26(H26), C33(H33), C35(H35), C42(H42), C44(H44)
4.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              92069
_olex2_submission_special_instructions 'No special instructions were received'