The 12-ethynylmonocarba-closo-dodecaborate anion as a versatile ligand for Cu(I) alkyne and heterobimetallic Cu(I)/M(II) (M = Pd, Pt) alkynide complexes
Jiang, Tao; Zhang, Kang; Shen, Yunjun; Hamdaoui, Mustapha; Dontha, Rakesh; Liu, Jiyong; Spingler, Bernhard; Duttwyler, Simon; Dalton Transactions  (2019) –; doi:10.1039/C9DT03272J

data_7701330
_publ_section_title
;
 The 12-ethynylmonocarba-closo-dodecaborate anion as a versatile ligand
 for Cu(I) alkyne and heterobimetallic Cu(I)/M(II) (M = Pd, Pt) alkynide
 complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03272J
_journal_year                    2019
_chemical_formula_moiety         'C15 H26 B11 Cu N2'
_chemical_formula_sum            'C15 H26 B11 Cu N2'
_chemical_formula_weight         416.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-17 deposited with the CCDC.    2019-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.206(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8275(7)
_cell_length_b                   10.7515(5)
_cell_length_c                   17.3597(9)
_cell_measurement_reflns_used    10530
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.03
_cell_volume                     2274.3(2)
_computing_cell_refinement       'PROCESS-AUTO  (Rigaku,2006)'
_computing_data_collection       'PROCESS-AUTO  (Rigaku,2006)'
_computing_data_reduction        'CrystalStructure (Rigaku,2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID/ZJUG'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19207
_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         25.997
_diffrn_reflns_theta_min         3.033
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.7189
_exptl_absorpt_correction_T_min  0.6341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Higashi, T. (1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1324
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+3.6863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2700
_reflns_number_total             4462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03272j2.cif
_cod_data_source_block           zk-cu1
_cod_database_code               7701330
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.729
_shelx_estimated_absorpt_t_min   0.644
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C15(H15A,H15B,H15C)
2.c Boron cage BH refined with riding coordinates:
 B7(H7A), B8(H8A), B9(H9), B10(H10A), B6(H6), B2(H2), B3(H3A), B4(H4A),
 B5(H5A), B1(H1A)
2.d Boron cage BH refined with riding coordinates and stretchable bonds:
 C1(H1)
;
_shelx_res_checksum              7027
_olex2_submission_special_instructions 'No special instructions were received'