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_7701326
_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         'C18 H42 Cu P2, C3 H12 B11'
_chemical_formula_sum            'C21 H54 B11 Cu P2'
_chemical_formula_weight         551.03
_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   geom
_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
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2019-04-17 deposited with the CCDC.    2019-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.697(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9970(7)
_cell_length_b                   15.5376(7)
_cell_length_c                   17.7707(8)
_cell_measurement_reflns_used    3366
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3864
_cell_measurement_theta_min      3.1942
_cell_volume                     3308.9(3)
_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      293(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -34.00   53.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683   38.0000  120.0000 87

  2 omega  -26.00   64.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683   77.0000  -30.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0468667000
_diffrn_orient_matrix_UB_12      0.0192472000
_diffrn_orient_matrix_UB_13      -0.0161638000
_diffrn_orient_matrix_UB_21      0.0355581000
_diffrn_orient_matrix_UB_22      -0.0184676000
_diffrn_orient_matrix_UB_23      0.0286306000
_diffrn_orient_matrix_UB_31      0.0066222000
_diffrn_orient_matrix_UB_32      -0.0370337000
_diffrn_orient_matrix_UB_33      -0.0227091000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13418
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         3.201
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88404
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_description       prism
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+0.7507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4378
_reflns_number_total             6266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03272j2.cif
_cod_data_source_block           171122_zk_cu_pipr3
_cod_database_code               7701326
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'c h n o B P CU'
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.635
_reflns_odcompleteness_completeness 99.53
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C17(H17), C21(H21), C24(H24), C27(H27)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C)
2.c Boron cage BH refined with riding coordinates:
 B1(H1A), B2(H2), B3(H3A), B4(H4), B5(H5), B6(H6), B7(H7), B8(H8), B9(H9),
 B10(H10)
2.d Boron cage BH refined with riding coordinates and stretchable bonds:
 C1(H1)
2.e :
 C3(H3)
;
_shelx_res_checksum              15777
_olex2_submission_special_instructions 'No special instructions were received'