Unusual cleavage of phosphaalkynes triple bond in the coordination sphere of transition metals
Moussa, Mehdi; Rummel, Eva-Maria; Eckhardt, Maria; Riesinger, Christoph; Scheer, Manfred; Dalton Transactions  (2023) –; doi:10.1039/D3DT02472E

data_7714187
_publ_section_title
;
 Unusual cleavage of phosphaalkynes triple bond in the coordination sphere
 of transition metals
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02472E
_journal_year                    2023
_chemical_formula_moiety         'C21 H7 Co6 O17 P'
_chemical_formula_sum            'C21 H7 Co6 O17 P'
_chemical_formula_weight         915.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-03-01
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.01.27 svn.rdd5efbe3 for OlexSys, GUI svn.r6708)
;
_audit_update_record
;
2023-07-16 deposited with the CCDC.	2023-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                88.761(4)
_cell_angle_beta                 79.668(4)
_cell_angle_gamma                68.320(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6531(4)
_cell_length_b                   11.1862(5)
_cell_length_c                   17.1189(8)
_cell_measurement_reflns_used    4222
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      72.6450
_cell_measurement_theta_min      4.2490
_cell_volume                     1513.04(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      123(1)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
  1 omega -118.00  -13.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9564  -77.0000 -180.0000 105

  2 omega  -19.00   75.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9564  -77.0000   30.0000 94

  3 omega  -38.00   67.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9564  -77.0000  -90.0000 105

  4 omega   66.00  120.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -77.0000  -45.0000 54

  5 omega   27.00   53.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -79.0000   57.0000 26

  6 omega   64.00  126.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -79.0000   57.0000 62

  7 omega   77.00  114.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -80.0000 -112.0000 37

  8 omega  104.00  131.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -15.0000  120.0000 27

  9 omega   31.00   74.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -45.0000   90.0000 43

 10 omega   32.00   69.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -45.0000 -120.0000 37

 11 omega   79.00  133.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017   45.0000   30.0000 54

 12 omega   31.00   58.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -45.0000  -60.0000 27

 13 omega   46.00   77.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -45.0000   30.0000 31

 14 omega   19.00  140.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017    0.0000 -180.0000 121

 15 omega   26.00   54.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -80.0000 -112.0000 28

 16 omega   22.00   99.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -15.0000  120.0000 77

 17 omega   28.00   60.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -77.0000  -45.0000 32

 18 omega   26.00  109.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.4017  -80.0000 -170.0000 83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9638
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         72.701
_diffrn_reflns_theta_min         4.258
_exptl_absorpt_coefficient_mu    26.350
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.126
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_description       plate
_exptl_crystal_F_000             892
_exptl_crystal_preparation       'Crystallized from concentrated hexanes'
_exptl_crystal_recrystallization_method
'The material was recrystallised from hexane by cooling to -30 degrees'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0688P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4440
_reflns_number_total             5743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02472e2.cif
_cod_data_source_block           ap_abs
_cod_original_cell_volume        1513.04(12)
_cod_database_code               7714187
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              5100
_olex2_submission_special_instructions 'No special instructions were received'