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_7714185
_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         'C19 H3 Co6 O17 P'
_chemical_formula_sum            'C19 H3 Co6 O17 P'
_chemical_formula_weight         887.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 108.715(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1777(2)
_cell_length_b                   14.2641(2)
_cell_length_c                   16.3093(2)
_cell_measurement_reflns_used    4587
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      34.984
_cell_measurement_theta_min      4.451
_cell_volume                     2683.20(7)
_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    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Oxford Diffraction, Gemini R Ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22840
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.984
_diffrn_reflns_theta_min         2.324
_exptl_absorpt_coefficient_mu    3.763
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.198
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_recrystallization_method
'The material was recrystallised from n-hexane by by cooling to +5 degrees'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         10854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0239P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7790
_reflns_number_total             10854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02472e2.cif
_cod_data_source_block           em34
_cod_database_code               7714185
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.602
_shelx_estimated_absorpt_t_min   0.453
_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:
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              479
_olex2_diffrn_ambient_temperature_device 'Oxford Instruments CryoJet'
_olex2_submission_special_instructions 'No special instructions were received'