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_7701329
_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 H20 B11 Cu F6 N2'
_chemical_formula_sum            'C15 H20 B11 Cu F6 N2'
_chemical_formula_weight         524.78
_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
_audit_creation_method
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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                66.212(7)
_cell_angle_beta                 75.011(7)
_cell_angle_gamma                89.796(7)
_cell_formula_units_Z            2
_cell_length_a                   10.0994(8)
_cell_length_b                   11.2360(9)
_cell_length_c                   11.7320(9)
_cell_measurement_reflns_used    2356
_cell_measurement_temperature    168.3
_cell_measurement_theta_max      29.3554
_cell_measurement_theta_min      3.2184
_cell_volume                     1169.09(18)
_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      168.3
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -36.00   64.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683   38.0000 -180.0000 100

  2 omega  -10.00   90.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       11.7808   77.0000   60.0000 100

  3 omega  -22.00   84.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       11.7808   77.0000  -60.0000 106
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0214866000
_diffrn_orient_matrix_UB_12      0.0473117000
_diffrn_orient_matrix_UB_13      -0.0653190000
_diffrn_orient_matrix_UB_21      -0.0385633000
_diffrn_orient_matrix_UB_22      0.0455335000
_diffrn_orient_matrix_UB_23      0.0182520000
_diffrn_orient_matrix_UB_31      0.0583684000
_diffrn_orient_matrix_UB_32      0.0225919000
_diffrn_orient_matrix_UB_33      0.0118415000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0797
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8139
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         3.225
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70633
_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    1.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4264
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0525P)^2^+0.3961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3389
_reflns_number_total             4264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03272j2.cif
_cod_data_source_block           171129_zk_cu_cf3py
_cod_original_cell_volume        1169.09(17)
_cod_database_code               7701329
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N B CU'
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.648
_reflns_odcompleteness_completeness 99.67
_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. Restrained distances
 C3-H3
 0.95 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14)
3.b Boron cage BH refined with riding coordinates:
 B2(H2), B3(H3A), B4(H4A), B5(H5A), B6(H6), B7(H7A), B8(H8A), B9(H9),
 B10(H10A), B11(H11A)
3.c Boron cage BH refined with riding coordinates and stretchable bonds:
 C1(H1)
;
_shelx_res_checksum              94169
_olex2_submission_special_instructions 'No special instructions were received'