A K-Arylacetylide Complex for Catalytic Terminal Alkyne Functionalization using KOtBu as a Precatalyst
Mandal, Swadhin K.; Ahmed, Jasimuddin; Swain, Asim Kumar; Das, Arpan; Govindarajan, R.; Bhunia, Mrinal; Chemical Communications  (2019) –; doi:10.1039/C9CC07833A

data_7124365
_publ_section_title
;
 A K-Arylacetylide Complex for Catalytic Terminal Alkyne Functionalization
 using KOtBu as a Precatalyst
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07833A
_journal_year                    2019
_chemical_formula_moiety         'C21 H31 K O6'
_chemical_formula_sum            'C21 H30 K O6'
_chemical_formula_weight         417.55
_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             2019-07-12
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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
;
2019-07-13 deposited with the CCDC.    2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.977(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1050(2)
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_cell_length_c                   14.1234(4)
_cell_measurement_reflns_used    4858
_cell_measurement_temperature    100.00
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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;
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omega____ theta____ kappa____ phi______ frames
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  2 omega   57.00  121.00   1.0000   13.0000
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  3 omega    1.00   81.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega  -12.00  102.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000 -180.0000 114

  5 omega   57.00  121.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega   30.00  144.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega  100.00  153.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega  100.00  153.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega  100.00  153.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  111.0000 -120.0000 53

 10 omega  100.00  153.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
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 11 omega   -4.00  109.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  -94.0000    0.0000 113

 12 omega   57.00  150.00   1.0000   42.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  178.0000   30.0000 93

 13 omega   69.00  178.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   54.0000  120.0000 109

 14 omega  101.00  178.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000 -180.0000 77

 15 omega   31.00  147.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -54.0000    0.0000 116

 16 omega   86.00  178.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  138.0000   90.0000 92

 17 omega   21.00  109.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000    0.0000 88

 18 omega  112.00  176.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   30.0000 64

 19 omega   96.00  151.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   43.0000  -90.0000 55

 20 omega   88.00  177.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 89

 21 omega  101.00  144.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   90.0000 43

 22 omega   31.00   68.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000  -30.0000 37

 23 omega  123.00  154.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000  120.0000 31

 24 omega   55.00   81.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   32.0000 -120.0000 26

 25 omega  119.00  145.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   32.0000 -120.0000 26

 26 omega  101.00  168.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   60.0000 67

 27 omega   87.00  121.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   54.0000   30.0000 34

 28 omega   26.00   52.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -21.0000   60.0000 26

 29 omega  140.00  177.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -21.0000   60.0000 37

 30 omega  104.00  146.00   1.0000   62.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -32.0000  -60.0000 42
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_31      0.0697160000
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_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.996
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_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
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_diffrn_reflns_number            11784
_diffrn_reflns_point_group_measured_fraction_full 0.996
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_diffrn_reflns_theta_full        66.241
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_diffrn_reflns_theta_min         3.883
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.382
_exptl_absorpt_correction_T_max  1.00000
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
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_exptl_crystal_description       block
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_refine_ls_R_factor_all          0.0394
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_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^)+(0.0449P)^2^+0.5130P] where P=(Fo^2^+2Fc^2^)/3'
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_refine_ls_wR_factor_gt          0.0815
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_reflns_number_gt                3323
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_cod_database_code               7124365
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_chemical_oxdiff_formula         'C H O K'
_shelx_estimated_absorpt_t_max   0.797
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_reflns_odcompleteness_completeness 98.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,
 H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              5816
_olex2_date_sample_data_collection 2019-05-28
_olex2_submission_special_instructions 'No special instructions were received'