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_7714188
_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         'C22 H9 Co6 O17 P'
_chemical_formula_sum            'C22 H9 Co6 O17 P'
_chemical_formula_weight         929.84
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2023-07-18 deposited with the CCDC.	2023-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                81.547(5)
_cell_angle_beta                 83.899(5)
_cell_angle_gamma                68.045(6)
_cell_formula_units_Z            2
_cell_length_a                   8.6816(6)
_cell_length_b                   11.1058(6)
_cell_length_c                   17.5276(11)
_cell_measurement_reflns_used    1624
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      58.507
_cell_measurement_theta_min      4.322
_cell_volume                     1547.93(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Oxford Diffraction, Gemini R Ultra'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7513
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        59.000
_diffrn_reflns_theta_max         58.507
_diffrn_reflns_theta_min         4.322
_exptl_absorpt_coefficient_mu    25.768
_exptl_absorpt_correction_T_max  0.438
_exptl_absorpt_correction_T_min  0.096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_recrystallization_method
'The material was recrystallised from n-hexane by by cooling to +5 deg'
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         4280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0914P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3094
_reflns_number_total             4280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02472e2.cif
_cod_data_source_block           1
_cod_database_code               7714188
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              58352
_olex2_diffrn_ambient_temperature_device 'Oxford Instruments CryoJet'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre with inert oil'
_olex2_submission_special_instructions 'No special instructions were received'