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_7701331
_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         'C26 H74 B22 Cu2 N2 P2 Pd, 2(C3 H6 O)'
_chemical_formula_sum            'C32 H86 B22 Cu2 N2 O2 P2 Pd'
_chemical_formula_weight         1064.26
_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
;
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                 97.622(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.7282(9)
_cell_length_b                   10.9616(6)
_cell_length_c                   17.0109(14)
_cell_measurement_reflns_used    2028
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3402
_cell_measurement_theta_min      3.0150
_cell_volume                     2906.9(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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
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      293.15
_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  -10.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7808   38.0000   90.0000 93

  2 omega  -48.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7808  -77.0000  120.0000 92
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0423909000
_diffrn_orient_matrix_UB_12      -0.0221179000
_diffrn_orient_matrix_UB_13      -0.0002075000
_diffrn_orient_matrix_UB_21      -0.0061211000
_diffrn_orient_matrix_UB_22      0.0014282000
_diffrn_orient_matrix_UB_23      -0.0420609000
_diffrn_orient_matrix_UB_31      0.0153083000
_diffrn_orient_matrix_UB_32      -0.0608113000
_diffrn_orient_matrix_UB_33      -0.0008438000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11737
_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         25.350
_diffrn_reflns_theta_min         3.188
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36602
_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    1.216
_exptl_crystal_description       needle
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5307
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0524P)^2^+0.7337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3566
_reflns_number_total             5307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03272j2.cif
_cod_data_source_block           180607_zk_pd
_cod_database_code               7701331
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'c h n o B PR CU'
_shelx_estimated_absorpt_t_max   0.851
_shelx_estimated_absorpt_t_min   0.664
_reflns_odcompleteness_completeness 99.49
_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, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-H1A
 0.96 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 N1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B), C8(H8A,H8B), C6(H6A,H6B), C12(H12A,H12B)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
3.d Boron cage BH refined with riding coordinates:
 B8(H8), B9(H9), B4(H4), B3(H3), B7(H7), B10(H10), B2(H2), B11(H11), B6(H6),
 B5(H5)
3.e Boron cage BH refined with riding coordinates and stretchable bonds:
 C1(H1A)
;
_shelx_res_checksum              4333
_olex2_submission_special_instructions 'No special instructions were received'