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_7701328
_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         'C13 H22 B11 Cu N2'
_chemical_formula_sum            'C13 H22 B11 Cu N2'
_chemical_formula_weight         388.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-21
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2019-04-17 deposited with the CCDC.    2019-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                71.393(7)
_cell_angle_beta                 79.489(7)
_cell_angle_gamma                70.380(8)
_cell_formula_units_Z            2
_cell_length_a                   8.2894(7)
_cell_length_b                   11.3934(10)
_cell_length_c                   11.7893(10)
_cell_measurement_reflns_used    2157
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      29.2953
_cell_measurement_theta_min      3.6363
_cell_volume                     990.43(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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      150.0
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -38.00   55.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -11.6246   77.0000 -120.0000 93

  2 omega   -5.00   88.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       11.9371   77.0000  150.0000 93

  3 omega  -15.00   81.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       11.9371   77.0000   30.0000 96
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0488519000
_diffrn_orient_matrix_UB_12      0.0238246000
_diffrn_orient_matrix_UB_13      0.0259344000
_diffrn_orient_matrix_UB_21      0.0032989000
_diffrn_orient_matrix_UB_22      0.0494050000
_diffrn_orient_matrix_UB_23      -0.0544585000
_diffrn_orient_matrix_UB_31      -0.0769009000
_diffrn_orient_matrix_UB_32      0.0415539000
_diffrn_orient_matrix_UB_33      0.0205092000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6342
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         3.644
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0408P)^2^+0.2265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3067
_reflns_number_total             3596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03272j2.cif
_cod_data_source_block           171018_zk_cu_py_sec
_cod_database_code               7701328
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'c h n o cu'
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.614
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13)
2.b Boron cage BH refined with riding coordinates:
 B2(H2), B3(H3A), B4(H4A), B5(H5A), B6(H6A), B7(H7A), B8(H8A), B9(H9A),
 B10(H10A), B11(H11A)
2.c Boron cage BH refined with riding coordinates and stretchable bonds:
 C1(H1)
;
_shelx_res_checksum              61328
_olex2_submission_special_instructions 'No special instructions were received'